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2. i 6
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2. 3 tf? 2±<D$im................................................. 10
2 . 4 Czfc^TJimm..................................................................................................................... 11
2 . 5 • ###&%..........,............................................................................................. 12
Chapter 2 Outline of the reseach and development results ............................................................ 18
2 . 1 Measurements of thermophysical properties of semiconductors......................... 18
2 . 2 Computer simulations............................................................................................................... 22
2 . 3 Experimental validation of the global simulation code......................................... 23
2 . 4 Model Experiment of Cz Furnace................................................................................. 24
2.5 Outcomes............................................................................................................................ 25
ss 3 s ..........................................................................31
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3 . 3 312
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APPENDIX- 1 iKa## - (t ......................................................334
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(Iflli:#) 1999 ¥ 3 n11) K.Nagata, E.Yamasue, H.Fukuyama, M.Hayashi and M.Susa
“Thermal Conductivity Measurement of Liquid Silicon under Microgravity
0cs i [ufflE-t^'>3 >) ^ os in, 1999 ¥ u ^, #
# (h 7° nt % , 12, [4], 857 (1999)
12) LU ¥ SO, # $, # lij t# ±: ri4 ^EtcS0@#:43 cfc
m 125 im, 1999 ¥
11 ^, 535
13) E.Yamasue, M.Susa, M.Hayashi, H.Fukuyama and K.Nagata: “Contribution from Phonon and
Electron to Thermal Conductivities of Solid and Liquid Silicon 15th European Conference
on Thermophysical Properties, Wuzburg, Germany, Sep. (1999)
14) H.Watanabe, M.Susa, H.Fukuyama and K.Nagata: “Emissivities of Liquid and Solid Silicon at
Melting Point 15th European Conference on Thermophysical Properties, Wuzburg, Germany,
Sep.(1999)
15) : “^u n >*©**»*&” . 0*^sfi£S¥^, sg 4i mm
1999 ¥ 5 ft 20 0
( 2 ) '> S n. 1/ - 3 >
1) ill 1*1 , G.Mika, # ¥, Three-dimensional Numerical Simulation of Melt Flow and Its Thermal
Characteristics in Cz Crucible (Further Report), SB36[HlB¥'Ei^:S/^/7^>?r^A l (1999) p75
2) K.Suzuki, T.Yamauchi, G.Mika and J.Szmyd, Unsteady Three-dimensional Melt Flow
Computation of Czochralski Single Crystal Growth of Super-Conducting Material, PCC99
AMIF European Science Foundation Workshop Phase Change with Convection : Modeling and
Validation. (1999)
3) #, 3 ? B *#
*¥= 1999 = , 1999 ^ 7 fl 29 B
4) S.H.Hahn, 0tt
4-5*2.: -mm&migfficomuizm-fz&mmtff”, 32
%*#%###, B204, 1999.
-13-
5) "Uniaxial strain observed in solid/liquid interface during crystal growth from melted Si : A
molecular dynamics study" by Ken Nishihira, Shinji Munetoh, and Teruaki Motooka 8th Int.
Conf. on Defects-Recognition, Imaging and Physics in Semiconductors, Narita, Japan,
September 15-18, 1999
6) "Molecular dynamics simulations of solid phase epitaxy of Si: Growth mechanism and defect
formation" by T.Motooka and K.Nisihira, S.Munetoh, K.Moriguchi, and A.Shintani Materials
Reasearch Society meeting, Boston, USA, November 29-December 5, 1999
7) ammm, wmmm s >”
2. s. 2
(i)
1) H.Fujii, M.Yamamoto, S.Hara and K.Nogi, “Effect of Gas Evolution at Solid-Liquid Interface
on Contact between Liquid Si and Si02”, J. Mater. Sci., 34 (1999) 3165-3168.
2) K.Mukai, Z.Yuan, K.Nogi and T.Hibiya, “Influence of Oxygen Partial Pressure in Atmosphere
on Temperature Coefficient of Surface Tension of Molten Silicon”, Proc. Twentieth Jpn Symp.
Thermophysical Properties, Tokyo, October (1999) 264-267.
3) K.Nogi, T.Matsumoto and H.Fujii, “Surface Tension Measurements of Molten Silicon in
Microgravity Environment”, 20th Jpn Symp. Thermophysical Properties, (1999) October 20-
22, Tokyo, 268-271.
4) K.Mukai, Z.Yuan, T.Hibiya and K.Nogi, “Effect of Oxygen partial Pressure on Temperature
Coefficient of Surface Tension of Molten Silicon”, Proc. Int. Astronautical Federation, IAF-
99-J1.06, p.1-6, 4-8, Oct. 1999.
5) K.Nogi, T.Nakano, T.Matsumoto and H.Fujii, “Effect of Droplet Distortion on Surface
Tension in Electromagnetic Levitation Method”, ISIJ int. Vol.40 (2000) in press.
6) K.Mukai, Z.Yuan, K.Nogi and T.Hibiya, “Effect of Oxygen Partial Pressure on the Surface
Tension of Molten Silicon and its Temperature Coefficient”, ISIJ int. Vol.40 (2000) in press.
7) Y.Asakuma, S.H.Hahn, Y.Sakai, T.Tsukada, M.Hozawa, T.Matsumoto, H.Fujii and K.Nogi,
—14 —
“Equilibrium Shape of a Molten Silicon Drop in an Electromagnetic Levitator in Microgravity
Environment”, Metall. Trans. A (2000) in press.
8) H.Fujii, T.Matsumoto, N.Hata, T.Nakano, M.Kohno and K.Nogi, “Surface Tension of Molten
Silicon Measured by Electromagnetic Levitation Method under Microgravity”, Metall. Trans.
A (2000) in press
9) H.Fujii, T.Matsumoto, M.Kohno, N.Hata and K.Nogi, “Analysis of Surface Oscillation of
Levitated Droplet in Microgravity”, submitted to Space Forum
10) H.Fujii, T.Matsumoto and K.Nogi, “Analysis of Surface Oscillation of Droplet under
Microgravity for the Determination of its Surface Tension”, submitted to Acta Metall.
11) K.Nogi, A.Shiraki, T.Nakano, T.Matsumoto and H.Fujii, “Surface Tension of Liquid Silicon”,
submitted to Proc. Spacebound 2000.
12) Yuzuru Sato, Takefumi Nishizuka, Ttomohiro Tachikawa, Masayoshi Hoshi, Tsutomu
Yamamura and Yoshio Waseda : Viscosity and Density of Molten Germanium, High Temp.
High Press., 32 (2000),
13) E.Yamasue, M.Susa, H.Fukuyama and K.Nagata “Non-stationary hot wire method with silica
coated probe for measuring thermal conductivities of molten metals” Metallurgical and
Materials Transactions A Vol.30A [8] (1999), p.1971-1979
14) H.Watanabe, M.Susa, H.Fukuyama and K.Nagata “Emissivities of Liquid and Solid Silicon at
the Melting Point” High Temp.-High Press., Vol.31 (1999), p.587-593
15) H.Fukuyama, E.Yamasue, M.Hayashi, M.Susa and K.Nagata : “ Challenge to Thermal
Conductivity Measurement of Liquid Silicon under Microgravity” , B 5/ > ^ V
^ AS 20 [Hi, C, 1999 ¥ 10 , Sg^lro^tS, A216, 280-283
16) H.Watanabe, M.Susa, H.Fukuyama and K.Nagata: “Measurement of Spectral Emissivity for
Metals and Semiconductors Using Cold Crucible” , 20 Ini,
1999 ¥ 10/3, A226, 308-311
17) D.Mitev, M.Saito and Y.Waseda, “Theoretical Estimation of Diffusion Coefficients of
Impurities in Silicon Melt”, High Temp. Mater. Proc., 19 (2000), f=P fiM 41.
-15-
(2) y 5 a 1/ — is s y
1) Z.Guo, S.Maruyama, A.Komiya, “Rapid yet accurate measurement of mass diffusion
coefficients by phase shifting interferometer”, Journal of Physics. D, Applied Physics, Vol.32,
pp.995-999, 1999.
2) Z.Guo, S.H.Hahn, S.Maruyama and T.Tsukada, “Global Heat Transfer Analysis in Czochralski
Silicon Furnace with Radiation on Curved Specular Surfaces”, Heat and Mass Transfer,
Vol.35, pp.185-190, 1999
3) muaii : “ttwfeufttusoinmitomr’, % 36
BWLmJCM, Vol.n, pp. 467-468, 1999.
4) SJA#-, S.H.Hahn, #0#^, R ill S S , #,
— 615, : “SiCz4p30^#&8lt###T”, B Vol.26, p.18, 1999.
5) S.H.Hahn, T.Tsukada, M.Hozawa, S.Maruyama and N.Imaishi, “Analysis of Radiation Heat
Transfer in CZ Crystal Growth Process”, 1999 JSME Annual Meeting, Vol.3, No.99-1,
pp.000-000, 1999.
6) K.Kakimoto, T.Umehara and H.Ozoe, ’’Molecular dynamics analysis on diffusion of point
defects” J.Crystal Growth, in print.
7) K.Kakimoto, T.Umehara and H.Ozoe, ’’Molecular dynamics analysis of point defects in silicon
near solid-liquid interface”, J.Vacuum Science, in print.
8) K.Kakimoto, Shin Kikuchi and H.Ozoe, ’’Molecular dynamics simulation of oxygen in silicon
melt”, J.Crystal Growth, 198/199 (1999) 114.
9) Y.Asakuma, S.H.Hahn, Y.Sakai, T.Tsukada, M.Hozawa, T.Matsumoto, H.Fujii, K.Nogi and
N.Imaishi : “Equilibrium Shape of a Molten Silicon Drop in an Electromagnetic Levitator in
Microgravity Environment”, Metall. Trans. B, in press.
10) M.Ishimaru and T.Motooka:"Molecular dynamics simulations of crystal growth from melted
silicon: defect formation processes" Mat. Res. Symp. Proc. Vol.538, 247-250 (1999).
11) Ken Nishihira, Shinji Munetoh, and Teruaki Motooka:"Uniaxial Strain Observed in
Solid/Liquid Interface during Crystal Growth from Melted Si: A Molecular Dynamics
Study" J.Crystal Growth, in press (2000)
12) T.Motooka, K.Nisihira, S.Munetoh, K.Moriguchi, and A.Shintani : "Molecular dynamics
—16 —
simulations of solid phase epitaxy of Si: Growth mechanisms" Phys. Rev. B, in press (2000)
13) T.Motooka, K.Nisihira, S.Munetoh, K.Moriguchi, and A.Shintani : "Molecular dynamics
simulations of solid phase epitaxy of Si: Growth mechanism and defect formation" Mat. Res.
Symp. Proc. , in press (2000)
-17-
Chapter 2 Outline of the Research and Development of Results
2 . 1 Measurement of Thermophysical Properties of Semiconductors
Kiyoshi Nogi
Joining and Welding Research Institute
Osaka University
The surface tension and density of liquid silicon were measured using the elctromagnetic
method in a high quality microgravity condition which is produced at JAMIC. The main results
are summarised as follows:
(1) The surface tension of liquid silicon was measured with a spherical droplet, the shape of
which was controlled by changing the current ratio between the quadru-pole coil and the
di-pole coil. The values were obtained in a wide temperature range of 1460K (below melting
point) to 1880K, and the temperature dependency are expressed by the following equation:
T =733-0.062 (T-1687)
T : surface tension (mN/m), T : temperature (K)
(2) The measured surface tension values of liquid silicon in purified Ar-H2 atmosphere (Po2 is at
least less than 1.1 x 10'14) and in Ar atmosphere are not significantly different. Therefore, it
is considered that the surface tension value during the actual production process of silicon
crystals can be expressed by the above equation.
(3) When the distortion of a droplet is small (approximately less than 1%), the surface tension
of the liquid can be calculated using Cummings' equation. However, as the distortion is
larger, the error in the surface tension value is also larger. This result indicates that when
the equation is applied to the results obtained in a terrestrial condition, the calculated value
includes a large error.
(4) Only 1% distortion can shift peaks in the frequency spectrum. Accordingly, in order to
obtain an precise surface tension value, it is essential to confirm that five modes exist (at
the same place) even when one peak is obtained.
-18
(5) The density of liquid silicon was precisely measured by obtaining the volume of the droplet
both from the top and side views. The temperature dependency can be expressed by the
following equation:
P =2.39 -2.47 X 10"4 (T-1687)
P : density (Mg/m3), T: temperature (K).
The experiments were carried out to obtain the precise and reliable viscosity and density of
molten semiconductors for improving the industrial crystal growth and studying the
thermophysics of the semiconductors. Viscosity has been measured by using the oscillating
viscometer which was suitable for high temperature melt with low viscosity. Density was
measured by using the pycnometric method which was suitable for oxidizable high temperature
molten metals. For the viscosity measurement of molten silicon, various refractories which have
different wettability with molten silicon were used for the crucible materials to study the effect
on the measurement. Alumina crucible was used for molten germanium. GaSb and InSb were
sealed perfectly in the quartz crucible to avoid the evaporation of Sb. All the results on the
viscosity showed good Arrhenian behavior and no abnormality was found near the melting
temperatures. Most results for molten silicon showed almost same viscosity independently of the
crucible materials. The feature of molten semiconductors on the viscosity are low viscosity, low
activation energy compared with other molten metals. Furthermore, the semiconductors studied
show not so different viscosities. It is very interesting on the viewpoint of the structure of molten
semiconductors. Densities of molten silicon and germanium were measured by using the
pycnometer made of boron nitride showed good linear relationship against the temperature and
the absolute values were intermediate values compared with literature values.
The thermal conductivity and normal spectral emissivity of solid and liquid silicon are
required to develop mathematical models of the heat flow in manufacturing processes for silicon
single crystals. This work aimed at obtaining accurate values for these thermophysical
properties.
The non-stationary hot wire method was used to measure thermal conductivities of solid and
liquid silicon, where hot-wire probes were insulated electrically from silicon samples using silica
films. The thermal conductivity of solid silicon decreased with increasing temperature. In solid
silicon, heat is principally transported by phonon conduction at temperatures below 1000 K, and
above 1000 K electronic conduction also contributes to heat transfer. The thermal conductivities
-19-
(X) in the respective temperature ranges can be expressed as a function of temperature (T) as
follows:
rt < T < 1000 K Xsolidilow tcmp = (1.40x10 2 + 1.90x10 + 2.92X10'5)1 Wm 'K'1
1000 K < T < 1673K Xsolidhigh tcmp = Xsoljd low temp + Xe Wm K
where Xe = 8.28 - 2.35x10 2T + 2.01x10 2 - 4.30x10 3 Wm 'K1
The thermal conductivity of liquid silicon measured under microgravity is 6 to 8 Wm^K"1 at
1698-1737K.
On the other hand, the normal spectral emissivity of silicon was derived as the ratio of the
normal radiation intensity from silicon sample to that from a blackbody at the same temperature
as the sample. The sample and the blackbody were heated up using the cold crucible. Normal
spectral emissivities of liquid and solid silicon were determined at the melting point in the
wavelength ranges of 650-850 nm and 1000-2500 nm. For example, values of emissivities
measured at 650 nm and 1500 nm are as follows:
650 nm: 0.231 for the liquid, 0.377 for the solid,
1500 nm: 0.137 for the liquid, 0.480 for the solid,
The emissivity in solid is larger than that in liquid at the wavelength investigated. The emissivity
in liquid decreases slightly with increasing wavelength, which indicates that molten silicon is
metallic. On the contrary, the emissivity in solid increases with increasing wavelength, which
indicates solid silicon is still semiconductor even at high temperature such as the melting point.
The solubilities of oxygen, nitrogen and carbon in liquid silicon equilibrated with silica,
silicon nitride and silicon carbide, respectively, were measured. The melting and analytical
methods were developed and accurate data on the solubilities were obtained. The standard Gibbs
free energy changes for dissolution of oxygen, nitrogen and carbon in liquid silicon were
determined. The effect of alloying elements on oxygen and carbon solubilities was clarified.
The relationship between SiO partial pressure in gas phase and oxygen contents in liquid
silicon was discussed thermodynamically, which is an important factor for removing of the
dissolved oxygen from liquid silicon. The maximum SiO partial pressure was calculated to be
around 0.01 atm at 1685 K. The SiO partial pressure was graphically shown as a function of the
dissolved oxygen contents.
Oxygen solubility in solid silicon at the melting point of silicon (Cs) was measured by a
chemical equilibrium method. The value of oxygen equilibrium distribution coefficient
(segregation coefficient, Cs / CL) was evaluated to be from 0.7 to 0.9 by using Cs and oxygen
-20-
solubility in liquid silicon at the melting point (CL) which has been reported by the authors.
The self-diffusion coefficient in pure silicon melt and diffusion coefficients of O, Al, B and
P impurities in silicon melt have been calculated on the basis of the Enskog theory implemented
with a pair-correlation function at contact between dissimilar atoms. The activation energies for
diffusion were also estimated by taking in account the temperature dependence of packing
fraction of silicon melt. Although only limited experimental data are available for comparison,
the present theoretical approach appears to work well and to be useful for predicting diffusion
coefficients of impurities in silicon melts.
-21-
2 . 2 Computer Simulations
Nobuyuki Imaishi
Institute of Advanced Material Study
Kyushu University
Numerical simulation codes have been developed during these 5 years. The most important
simulation codes are such as the gas phase transport phenomena code (flow, heat transfer and
mass transfer in the gas phase), melt phase transport phenomena code, heat transfer in the solid
phases together with radiative heat transfer between partially specular diffuse gray surfaces, 2
and 3 dimensional melt flow analysis codes based on a k-e turbulent model, 3 dimensional
unsteady melt phase transport phenomena codes and a main program which enables the global
simulation by combining the whole set of program codes to determine the pseudo steady state of a
Cz furnace under a given geometry and heat input. As of the end of January 2000, this global
analysis code has been developed and confirmed its validity for a small scale Cz furnace.
However, the code is subjected to some difficulties for application to a large scale Cz furnaces,
since the 3-D unsteady simulation of melt flow in a large crucible requires very long CPU time on
the conventional computers. More powerful Computer and/or a further development of a reliable
turbulent model, which is applicable to such a weak turbulent flow accompanied by rotating flow.
In addition to these macro-scale simulations, micro-scale simulations, such as the Molecular
Dynamics (MD) simulation and the Monte Carlo (MC) simulation, have been conducted in order
to investigate fundamental aspect of crystal growth from atomistic viewpoints. The results of
these micro-scale simulations must be explained and connected with the realistic crystal growth
phenomena via some, yet unknown, scaling laws. MD simulations investigated on 1) behavior of
silicon crystal under highly compressive or tensile forces, 2) diffusion of point defects in crystal
and 3) diffusion of oxygen atom in silicon melt.
-22-
2 . 3 Experimental validation of the global simulation code
Nobuyuki Imaishi
Institute of Advanced Material Study
Kyushu University
It is necessary to place some experimental works to confirm the validity of the developed
global simulation code. This research project could not expect the cooperation from industry.
Then we decided to conduct some cold model experiments by using silicone oil and low
temperature liquid alloys. But these experiments provide only information on flow velocity and
temperature distribution in the model fluids. These do not represent the complex phenomena in
silicon Cz furnaces. Then, we asked Prof. Hoshikawa of Shinshu University and the Fundamental
Research Laboratories of NEC Corporation to conduct some crystal growth experiments and
provide the results for the sake of validity check. Prof. Hoshikawa has provided us temperature
distribution in his Cz furnace (crucible diameter: 168mm) with and without a funnel shaped gas
guide. His experiments confirmed the simulation’s results that the gas guide would reduce power
consumption and also provide easier control of temperature gradient in the growing crystal. Prof.
Hoshikawa is going to install a power supply meter to his furnace and will provide us more
detailed data.
The Cz furnace at NEC was operated and a 35mm diameter crystal was grown from a crucible
(diameter: 75mm). An X ray radiographic observation of the melt-crystal interface was conducted
and the results were provided. The melt-crystal interface shape was well simulated by the global
simulation code. Further, a simulated oxygen concentration is compared with an experimental
result that was reported by the NEC researchers using the same furnace, although the
experimental condition was slightly different from the present experiment. The simulated oxygen
concentration falls very close to their experimental result. The present simulation requires no
adjustable parameters on oxygen mass transfer. These results suggest the validity of the global
analysis code developed by this research project.
-23-
2 . 4 Model Experiment of Cz Furnace
Kimihisa Itoh
Department of Science & technology,
Waseda University
The precise experimental data are important to develop and verify a computer simulation
program of the unsteady convection flow of melt. The following experiments were conducted to
establish the database of the melt flow in a cold model using water, silicone oil and Wood's metal
as model materials.
(1) Temperature profile measurement in the melt: The temperatures in Wood's metal which is a
low Pr melt as silicon were continuously measured using telemeter system. The obtained results
were arranged in a visible form and stored as a database.
(2) Velocity profile measurement in the model crucible: The larger single crystal was employed
and the experimental furnace was modified to rotate at very low rate. This modification made the
model experiments more close to the actual operating conditions of Cz furnace. Time change of
melt flow was measured by LDV and the flow profile was measured by PIV. The obtained results
were arranged and stored as a database.
— 24 —
2 . 5 Outcomes
2 . 5 . 1 Symposiums
( 1 ) Measurements of Physical Properties
1) mm m, uhxdsm:*?, es
SJ S^ 30 (NCCG-30) * /t ;i/ ^7 fiKS ^ 5/ ^7 A , 1999 ¥
7 /! 22 0
2) m#^#, ew m, si
m 89 1999 ¥ 11 ^ 26 0
3) B^EsE, m, LU# f] : HD*6$ ; SB 124 00*Am
(1999), 110. (1999 ¥ 3 £ 29 0), Mm.
4) &B I : '> U 3 ; 0 **§B(S 30 HI £S B S ffl ft £
S) , 26 (1999), 14. (1999 ¥ 7 ^ 22 0), # 0 .
5) Yuzuru Sato, Takefumi Nishizuka, Tomohiro Tachikawa, Masayoshi Hoshi, Tsutomu
Yamamuraand Yoshio Waseda : Viscosity and Density of Molten Germanium ; 15th Europian
Conference on Thermophysical Properties Abstract, (1999), 165. (1999 ¥ 9 ^ 8 0), H -T
V * Wurzburg.
6) &m m, m a#, m# am
; m 31 (1999) , 1.
(1998 ¥ 11 ft 11 0), Mii?.
7) &m m, am * : ^s* insb <d*ss ■, m 125 00^^!^
(1999), 540. (1998 ¥ 11 £ 21 0), A2R.
8) , S£ES, # #, is Lilith, TkfflfnS : f&{£'> U n ><D BASSOS
gi^j , ^ 1999 ¥ 3 ^
9) tmsx, m&m®, miumz, 3d m
j , (m^%#±#) 1999 ¥
3 n
10) WfflSX, 3I£E®, : ryij3>-^fJK-7A0
-25-
(iMli^f) 1999 ¥ 3 B
11) H.Fukuyama, E.Yamasue, M.Hayashi, M.Susa and K.Nagata : “ Challenge to Thermal
Conductivity Measurement of Liquid Silicon under Microgravity”, B¥l^$£J ft X > ^ V
AS 20 HI, 1999 ¥ 10 ^ A216, 280-283
12) H.Watanabe, M.Susa, H.Fukuyama and K.Nagata : “Measurement of Spectral Emissivity for
Metals and Semiconductors Using Cold Crucible”, B ^ ft S/ > # v ^ A S 20 HI, $
1999 ¥ 10 ^ A226, 308-311
13) K.Nagata, E.Yamasue, H.Fukuyama, M.Hayashi and M.Susa “ Thermal Conductivity
Measurement of Liquid Silicon under Microgravity” B (S 1 HI @1 IE
-k y '> 3 >) S 138 HI, 1999 ¥ 11 £ , yntx, 12, [4], 857(1999)
14) OJ^SI, M&m®, # $, tg Lilith, : ri4 #70^00#:^ j; a'##: I:
s 125hi, 1999¥ 11 n, 535
15) E.Yamasue, M.Susa, M.Hayashi, H.Fukuyama and K.Nagata : “Contribution from Phonon and
Electron to Thermal Conductivities of Solid and Liquid Silicon” 15th European Conference on
Thermophysical Properties, Wilzburg, Germany, Sep. (1999)
16) H.Watanabe, M.Susa, H.Fukuyama and K.Nagata : “Emissivities of Liquid and Solid Silicon
at Melting Point” 15th European Conference on Thermophysical Properties, Wuzburg,
Germany, Sep. (1999)
i?) : “vun i 41 mi
1999 ¥ 5 20 B
( 2 ) Computer Simulations
1) ill 1*1, G.Mika, In Tfc, Three-dimensional Numerical Simulation of Melt Flow and Its Thermal
Characteristics in Cz Crucible (Further Report), S 36 HlB^fc;#&S/>3^;/^A \ (1999)
P75
2) K.Suzuki, T.Yamauchi, G.Mika and J.Szmyd, Unsteady Three-dimensional Melt Flow
Computation of Czochralski Single Crystal Growth of Super-Conducting Material, PCC99
-26-
AMIF European Science Foundation Workshop Phase Change with Convection : Modeling and
Validation.(1999)
3) ** «t, ff : “^3 » B*«
1999 # 1999 # 7 fl 29 H
4) «###. TfflStil, S.H.Hahn, «B|S£*, SiR^E, $**¥, *#£*, »» ».
: “»ESili$#©S«iCier-5.»<*)R#r", 32
%*!*#$ WS, B204, 1999.
5) "Uniaxial strain observed in solid/liquid interface during crystal growth from melted Si : A
molecular dynamics study" by Ken Nishihira, Shinji Munetoh, and Teruaki Motooka 8th Int.
Conf. on Defects-Recognition, Imaging and Physics in Semiconductors, Narita, Japan,
September 15-18, 1999
6) "Molecular dynamics simulations of solid phase epitaxy of Si: Growth mechanism and defect
formation" by T.Motooka and K.Nisihira, S.Munetoh, K.Moriguchi, and A.Shintani Materials
Reasearch Society meeting, Boston, USA, November 29-December 5, 1999
?> ammm, mmmm )iuzs a
>” 1999 B
2 . 5 . 2 Submitted Papers
( 1 ) Measurements of Physical Properties
1) H.Fujii, M.Yamamoto, S.Hara and K.Nogi, “Effect of Gas Evolution at Solid-Liquid Interface
on Contact between Liquid Si and Si02”, J. Mater. Sci., 34 (1999) 3165-3168.
2) K.Mukai, Z.Yuan, K.Nogi and T.Hibiya, “Influence of Oxygen Partial Pressure in Atmosphere
on Temperature Coefficient of Surface Tension of Molten Silicon”, Proc. Twentieth Jpn Symp.
Thermophysical Properties, Tokyo, October (1999) 264-267.
3) K.Nogi, T.Matsumoto and H.Fujii, “Surface Tension Measurements of Molten Silicon in
Microgravity Environment”, 20th Jpn Symp. Thermophysical Properties, (1999)October 20-22,
Tokyo, 268-271.
4) K.Mukai, Z.Yuan, T.Hibiya and K.Nogi, “Effect of Oxygen partial Pressure on Temperature
-27-
Coefficient of Surface Tension of Molten Silicon”, Proc. Int. Astronautical Federation, IAF-
99-J1.06, p.1-6, 4-8, Oct. 1999.
5) K.Nogi, T.Nakano, T.Matsumoto and H.Fujii, “Effect of Droplet Distortion on Surface
Tension in Electromagnetic Levitation Method”, ISIJ int. Vol.40 (2000) in press.
6) K.Mukai, Z.Yuan, K.Nogi and T.Hibiya, “Effect of Oxygen Partial Pressure on the Surface
Tension of Molten Silicon and its Temperature Coefficient”, ISIJ int. Vol.40 (2000) in press.
7) Y.Asakuma, S.H.Hahn, Y.Sakai, T.Tsukada, M.Hozawa, T.Matsumoto, H.Fujii and K.Nogi,
“Equilibrium Shape of a Molten Silicon Drop in an Electromagnetic Levitator in Microgravity
Environment”, Metall. Trans. A (2000) in press.
8) H.Fujii, T.Matsumoto, N.Hata, T.Nakano, M.Kohno and K.Nogi, “Surface Tension of Molten
Silicon Measured by Electromagnetic Levitation Method under Microgravity”, Metall. Trans.
A (2000) in press
9) H.Fujii, T.Matsumoto, M.Kohno, N.Hata and K.Nogi, “Analysis of Surface Oscillation of
Levitated Droplet in Microgravity”, submitted to Space Forum
10) H.Fujii, T.Matsumoto and K.Nogi, “Analysis of Surface Oscillation of Droplet under
Microgravity for the Determination of its Surface Tension”, submitted to Acta Metall.
11) K.Nogi, A.Shiraki, T.Nakano, T.Matsumoto and H.Fujii, “Surface Tension of Liquid Silicon”,
submitted to Proc. Spacebound 2000.
12) Yuzuru Sato, Takefumi Nishizuka, Ttomohiro Tachikawa, Masayoshi Hoshi, Tsutomu
Yamamura and Yoshio Waseda : Viscosity and Density of Molten Germanium, High Temp.
High Press., 32 (2000),
13) E.Yamasue, M.Susa, H.Fukuyama and K.Nagata “Non-stationary hot wire method with silica
coated probe for measuring thermal conductivities of molten metals Metallurgical and
Materials Transactions A Vol.30A [8] (1999), p.1971-1979
14) H.Watanabe, M.Susa, H.Fukuyama and K.Nagata “Emissivities of Liquid and Solid Silicon at
the Melting Point” High Temp.-High Press., Vol.31 (1999), p.587-593
15) D.Mitev, M.Saito and Y.Waseda, “Theoretical Estimation of Diffusion Coefficients of
Impurities in Silicon Melt”, High Temp. Mater. Proc., 19 (2000), EP MW 41.
-28-
( 2 ) Computer Simulations
1) Z.Guo, S.Maruyama, A.Komiya, “Rapid yet accurate measurement of mass diffusion
coefficients by phase shifting interferometer”, Journal of Physics. D, Applied Physics, Vol.32,
pp.995-999, 1999.
2) Z.Guo, S.H.Hahn, S.Maruyama and T.Tsukada, “Global Heat Transfer Analysis in Czochralski
Silicon Furnace with Radiation on Curved Specular Surfaces”, Heat and Mass Transfer, Vol.35,
pp.185-190, 1999.
3) ff 36
M&mlCM, Vol.H, pp. 467-468, 1999.
4) S.H.Hahn, HOlSS, ## #,
— 615, MiWMM : “SiCz B Vol.26, p.18, 1999.
5) S.H.Hahn, T.Tsukada, M.Hozawa, S.Maruyama and N.Imaishi, “Analysis of Radiation Heat
Transfer in CZ Crystal Growth Process”, 1999 JSME Annual Meeting, Vol.3, No.99-1,
pp.000-000, 1999.
6) K.Kakimoto, T.Umehara and H.Ozoe, ’’Molecular dynamics analysis on diffusion of point
defects” J.Crystal Growth, in print.
7) K.Kakimoto, T.Umehara and H.Ozoe, ’’Molecular dynamics analysis of point defects in silicon
near solid-liquid interface”, J.Vacuum Science, in print.
8) K.Kakimoto, Shin Kikuchi and H.Ozoe, "Molecular dynamics simulation of oxygen in silicon
melt”, J.Crystal Growth, 198/199 (1999) 114.
9) Y.Asakuma, S.H.Hahn, Y.Sakai, T.Tsukada, M.Hozawa, T.Matsumoto, H.Fujii, K.Nogi and
N.Imaishi : “Equilibrium Shape of a Molten Silicon Drop in an Electromagnetic Levitator in
Microgravity Environment”, Metall. Trans. B, in press.
10) M.Ishimaru and T.Motooka : "Molecular dynamics simulations of crystal growth from melted
silicon: defect formation processes" Mat. Res. Symp. Proc. Vol.538, 247-250 (1999).
11) Ken Nishihira, Shinji Munetoh, and Teruaki Motooka: "Uniaxial Strain Observed in
Solid/Liquid Interface during Crystal Growth from Melted Si: A Molecular Dynamics Study"
J.Crystal Growth, in press (2000)
-29-
12) T.Motooka, K.Nisihira, S.Munetoh, K.Moriguchi, and A.Shintani : "Molecular dynamics
simulations of solid phase epitaxy of Si : Growth mechanisms" Phys. Rev. B, in press (2000)
13) T.Motooka, K.Nisihira, S.Munetoh, K.Moriguchi, and A.Shintani : "Molecular dynamics
simulations of solid phase epitaxy of Si: Growth mechanism and defect formation" Mat. Res.
Symp. Proc. , in press (2000)
-30-
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P =2.39 ~ 2.47X 10'4 (T-1687) (T : B8, K)
Precise measurements for surface tension, density
Kiyoshi Nogi, Hidetoshi Fujii and Taihei Matsumoto
Joining and Welding Research Institute,
Osaka University
Abstract:
The surface tension and density of liquid silicon were measured using the elctromagnetic
method in a high quality microgravity condition which is produced at JAMIC. The main results
are summarised as follows:
(1) The surface tension of liquid silicon was measured with a spherical droplet, the shape of
which was controlled by changing the current ratio between the quadru-pole coil and the di
pole coil. The values were obtained in a wide temperature range of 1460K (below melting
point) to 1880K, and the temperature dependency are expressed by the following equation:
T =733-0.062 (T-1687)
T : surface tension (mN/m), T : temperature (K)
(2) The measured surface tension values of liquid silicon in purified Ar-H2 atmosphere (Po2 is at
least less than 1.1 x 10'14) and in Ar atmosphere are not significantly different. Therefore, it
is considered that the surface tension value during the actual production process of silicon
crystals can be expressed by the above equation.
(3) No effect of the addition of 20ppm antimony to silicon was observed.
-32-
(4) When the distortion of a droplet is small (approximately less than 1%), the surface tension
of the liquid can be calculated using Cummings’ equation. However, as the distortion is
larger, the error in the surface tension value is also larger. This result indicates that when the
equation is applied to the results obtained in a terrestrial condition, the calculated value
includes a large error.
(5) Only 1 % distortion can shift peaks in the frequency spectrum. Accordingly, in order to
obtain an precise surface tension value, it is essential to confirm that five modes exisit (at
the same place) even when one peak is obtained.
(6) The density of liquid silicon was precisely measured by obtaining the volume of the droplet
both from the top and side views. The temperature dependency can be expressed by the
following equation:
P =2.39 -2.47X10-4 (T-1687)
P : density (Mg/m3), T: temperature (K).
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— 44 —
(6)
1) H.Fujii, M.Yamamoto, S.Hara and K.Nogi, “Effect of Gas Evolution at Solid-Liquid Interface
on Contact between Liquid Si and Si02”, J.Mater. Sci., 34 (1999) 3165-3168.
2) K.Mukai, Z.Yuan, K.Nogi and T.Hibiya, “Influence of Oxygen Partial Pressure in Atmosphere
on Temperature Coefficient of Surface Tension of Molten Silicon”, Proc. Twentieth Jpn Symp.
Thermophysical Properties, Tokyo, October (1999) 264-267.
3) K.Nogi, T.Matsumoto and H.Fujii, “Surface Tension Measurements of Molten Silicon in
Microgravity Environment”, 20th Jpn Symp. Thermophysical Properties, (1999) October 20-22,
Tokyo, 268-271.
4) K.Mukai, Z.Yuan, T.Hibiya and K.Nogi, “Effect of Oxygen partial Pressure on Temperature
Coefficient of Surface Tension of Molten Silicon”, Proc. Int. Astronautical Federation, IAF-
99-J1.06, p.1-6, 4-8, Oct. 1999.
5) K.Nogi, T.Nakano, T.Matsumoto and H.Fujii, “Effect of Droplet Distortion on Surface Tension
in Electromagnetic Levitation Method”, ISIJ int. Vol.40 (2000) in press.
6) K.Mukai, Z.Yuan, K.Nogi and T.Hibiya, “Effect of Oxygen Partial Pressure on the Surface
Tension of Molten Silicon and its Temperature Coefficient”, ISIJ int. Vol.40 (2000) in press.
7) Y.Asakuma, S.H.Hahn, Y.Sakai, T.Tsukada, M.Hozawa, T.Matsumoto, H.Fujii and K.Nogi,
“Equilibrium Shape of a Molten Silicon Drop in an Electromagnetic Levitator in Microgravity
Environment”, Metall. Trans. A (2000) in press.
8) H.Fujii, T.Matsumoto, N.Hata, T.Nakano, M.Kohno and K.Nogi, “Surface Tension of Molten
Silicon Measured by Electromagnetic Levitation Method under Microgravity”, Metall. Trans.
A (2000) in press.
9) H.Fujii, T.Matsumoto, M.Kohno, N.Hata and K.Nogi, “Analysis of Surface Oscillation of
Levitated Droplet in Microgravity”, submitted to Space Forum
10) H.Fujii, T.Matsumoto and K.Nogi, “Analysis of Surface Oscillation of Droplet under
Microgravity for the Determination of its Surface Tension”, submitted to Acta Metall.
11) K.Nogi, A.Shiraki, T.Nakano, T.Matsumoto and H.Fujii, “Surface Tension of Liquid Silicon”,
submitted to Proc. Spacebound 2000.
-45
12) B# tit, UnxyftBMA, $$
81 St, ^ 30 BlSSB8ft¥ = a A = E (NCCG-30) • fig ft'>>#>*■? A, 1999 ¥
7 E 22 B
13) m##@, e*±v, m, si <Dawmti&£tf®
$©8J$, SHE • BtSSBft SB 89 0ff5Sil#, 1999 ¥ 11 fl 26 B
( 7 ) *#X«
1) B.J.Keen, Surface Inteface, Annal., 10 (1987), 367.
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13) K.Eckler, I.Egry and D.M.Herlach, Mater. Sci. Eng., A133, (1991) 718.
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23 (1996), 374.
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18) M.Przyborowski, T.Hibiya, M.Eguchi and I.Egry, J.Crystal Growth, 151 (1995) 60.
— 46 —
gas inlet
gas outlet
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57-
Measurement of Viscosity of Molten Silicon, Germanium, GaSb and InSb,
and Density of Molten Silicon and Germanium
* Yuzuru Sato and **Yoshio Waseda
* Graduate School of Engineering, Tohoku University
** Institute for Advanced Materials Processing, Tohoku University
Abstract:
The experiments were carried out to obtain the precise and reliable viscosity and density of
molten semiconductors for improving the industrial crystal growth and studying the thermophys
ics of the semiconductors. Viscosity has been measured by using the oscillating viscometer which
was suitable for high temperature melt with low viscosity. Density was measured by using the
pycnometric method which was suitable for oxidizable high temperature molten metals. For the
viscosity measurement of molten silicon, various refractories which have different wettability
with molten silicon were used for the crucible materials to study the effect on the measurement.
Alumina crucible was used for molten germanium. GaSb and InSb were sealed perfectly in the
quartz crucible to avoid the evaporation of Sb. All the results on the viscosity showed good Ar-
rhenian behavior and no abnormality was found near the melting temperatures. Most results for
molten silicon showed almost same viscosity independently of the crucible materials. The feature
of molten semiconductors on the viscosity are low viscosity, low activation energy compared
with other molten metals. Furthermore, the semiconductors studied show not so different vis
cosities. It is very interesting on the viewpoint of the structure of molten semiconductors. Densi
ties of molten silicon and germanium were measured by using the pycnometer made of boron
nitride showed good linear relationship against the temperature and the absolute values were
intermediate values compared with literature values.
-58-
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til tC S £F ft Arrhenius S! © iBStic W14 £ ^ ft . Glazov # C. 41 5 1C 3 It % 4^ Arrhenius $
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(6) *3t«W
1) Yuzuru Sato, Hongmin Zhu, Yuichi Kameda, Takeshi Nagasawa and Tsutomu Yamamura :
Viscosity Measurement of Molten Fe base Si Alloy ;
S 17 @&t#ltt->>7it>'>.ftS#S5ii!5t* (1996), 119-122 (1996 11 fl 29 B ) , O < tt.
2) ft* e, lu# *, * as, j$s s* is, mm*-, m = >u 3 >m
«©fflStiSEie ; S 120 @H*6S¥S#IS«tE, (1997), 331. (19973 fl 27 B),
3) Yuzuru Sato, Shinpei Moriguchi and Tsutomu Yamamura : Viscosity of Molten Iron *,
# 18 0%##>>Ai>')ftMiK#3t# (1997), 149. (1997 ¥ 10 fl 24 B), $6
4) ftS m. Hi# ft : SStS# ©®tt ; S#X^E%0r» 6 @E%M
ms, (1997 ¥ 11 Ji 13 H), Ml6
5) feS E, 111# ft : *##:m#:0#*IC3HT ; (1998),
14. (1998 ¥ 7 fl 25 B), ftE.
6) Yuzuru Sato, Yuichi Kameda, Toru Nagasawa, Takeshi Sakamoto, Shinpei Moriguchi and
-69-
Tsutomu Yamamura : Viscosity of Molten Silicon and its Temperature Dependence ; Proceed
ings of the 5th Asian Thermophysical Properties Conference (ATPC’98) (1998), 511. (1998 ¥
9 ft 2 0), 1 Seoul.
7) m, ti: mm-v'DKomm.; % 123 @8*##
(1998), 181. (1998 ^9^ 28 0), Yk Ol.
8) Yuzuru Sato, Takeshi Sakamoto, Shinpei Moriguchi, Tsutomu Yamamura and Yoshio
Waseda : Viscosity Measurement of Molten Silicon and its Behavior near the Melting Point ;
(1998), 119. (1998 ¥ 10 £ 22 0 ), IB3.
9) m, m, m m#, ti:; m 30 (1998), 57. (1998 ¥ 11 n 12 B),
;kE.
10) *jhm, m 124 mi8$A
(1999), 110. (1999 ¥ 3 ft 29 8 ), 3EM.
u) &jm m : v u n ; b^sssu&s^ss ob 30
, 26 (1999), 14. (1999 ¥ 1 ft 22 0), #0.
12) Yuzuru Sato, Takefumi Nishizuka, Tomohiro Tachikawa, Masayoshi Hoshi, Tsutomu Yama-
muraand Yoshio Waseda : Viscosity and Density of Molten Germanium ; 15th Europian Con
ference on Thermophysical Properties Abstract, (1999), 165. (1999 ¥ 9 ft 8 0), Y ¥ V m
Wurzburg.
13) &# m, b#pm®, m re, m# ts, subs* :
^31 imgmmfk#####;#### (1999), 1.
(1998 ¥ 11 fl 11 0), fill#.
14) HSHis, &m m, m# * = mm insb ©tss ; s 125 @0*#*
(1999), 540. (1998 ¥ 11 J? 21 0), AiR.
15) Yuzuru Sato, Takefumi Nishizuka, Ttomohiro Tachikawa, Masayoshi Hoshi, Tsutomu Yama
mura and Yoshio Waseda : Viscosity and Density of Molten Germanium, High Temp. High
Press., 32 (2000),
-70-
( 7) ####
1) V.M.Glazov, S.N.Chizhevskaya and N.N.Glagoleva : Liquid Semiconductors (1969), Plenum
Press, NY.
2) K.Kakimoto, M.Egichi, H.Watanabe and T.Hibiya : J.Cryst.Growth, 94 (1989), 412-420.
3) H.Sasaki, E.Tokizaki, X.M.Huang, K.Terashima and S.Kimura : Jpn.J.Appl.Phys., 34 (1995),
3432-3436.
(1997), 59-88.
5) H.Sasaki, E.Tokizaki, K.Terashima and S.Kimura : Jpn.J.Appl.Phys., 33 (1994), 3803-3807, 34
(1995), 6078-6081.
6) L.-D.Lucas : Mem.Sci.Rev.Metal., 61, 1 (1964), 1-24.
7) W.K.Rhim, S.K.Chung, A.J.Rulison and R.E.Spjut : Int.J.Thermophys., 18 (1997), 459-469.
8) Yu.N.Taran-Zhovnir, N.M.Kochegura, S.P.Kazachkov, V.R.Pilipchuk, E.A.Markovskii, V.Z.
Kutsova and K.V.Uzlov : Sov.Phys.Dokl., 34 (1989), 282-284.
9) N.P.Mokrovski and A.R.Regel : J.Phys.Tech., 22 (1952), 1281.[Ref.l3 K)
10) % m 14
5:S, (1993), 319-322.
11) L.Martin-Garin, M.Gomez, P.Bedon and P.Desre : J.Less-Common Metal.. 41 (1975), 65-76.
12) W.Klemm et.al : Monatsch.Chem., 83 (1952), 629. [Ref.ll 0 31 ]
13) & mm, m, a:
14) R.Roscoe : Proc. Phys.Soc., 72 (1958), 576.
15) ebjes, s, afinite, *s m,
51(1987), 328-337.
16) Y.Sato, T.Yamamura, H-M.Zhu, M.Endo, T.Yamazaki, H.Kato, T.Ejima and G.J.Janz :
Proc.Third Intern.Sympo.Carbonate Fuel Cell Tech., (1993), 416-428.
(1998), 50-69.
18) K.Yanaba, M.Akasaka, M.Takeuchi, M.Watanabe, T.Narushima and Y.Iguchi : Mater. Trans.
JIM, 38 (1997), 990.
-71-
Data processing
Wire(Pt-13%Rh)TimeCounter
Phototransistor
Inertia diskLaser light
Colimator lens Oscillationinitiator
Convex lens —i Tungsten rod
CrucibleHe-Ne laser
m 3.1.2-1
‘ e1 *""1 1 , , , ' ' 1
§8
1 i8...... «... ....a......
■
■ ■ ■ ■ ■ ■ , . , . . ,) —i—i—i—i—i—i .-I —i—i—i ,—>—i—, i—i—0.0 2.0 4.0 6.0 8.0 10.0
ratio, h/r
m 3.1.2-2awt 4-a. a 26m
(molten Sn, Temp.=573K, radius=8mm)
3.1.2-1 tHEIEibEBSIHc
Substance TempVK Obtained /mPa s
Literature /mPa s
Deviation(%)
289.5 1.095 1.101 -0.5
Water 293.6 1.010 0.933 +1.7296.6 0.927 0.925 +0.2
Mercury 288.4 1.578 1.583 -0.3
305.0 1.497 1.489 +0.5
-72-
11: Head Com 2: Gas Inlet 3: Torsion Wire 4: Water Circulation Pipe 5: Reflection Mirror 6: Window 7: Inertia Disk 8: Oscillation Initiator 9: Water Jacket
10: WRod 11: Mo plate 12: Crucible13: Three divided Furnace 14: Zr sponge 15: Thermocouple
9
m 3.i.2-3
60
55
E 5001 45
3
5 40
8 35
5G 30
251600 1650 1700 1750 1800 1850 1900
7VK
m 3.i.2-4
•
1 —
<
•;• :• i
IT • !• :
i crucibl| _Lher
i * :* :
•;• i• :• :
i _ _ _ _ _ _ _ _ _ _ i_ _ _ _ _ _ _ _ _
5 4 3
CoolingWater
1: Alumina outer tube 2: Water jacket 3: Gas inlet4: Alumina tube for pushing 5: Thermocouple 6: Tungsten rod 7: Molybdenum plate 8: Pycnometer 9: Zirconium sponge
10: MoSi2 Furnace 11: Alumina support tube 12: Graphite rod
___ CoolingWater
H3.1.2-5
push4
4pull down
0 3.1.2-6
-73-
-0.18
Boron Nitride-0.22
-0.24
-0.26
-0.28
-0.32
1000/Tm 3.1.2-7
v u n
-0.18
-0.20Alumina
-0.22
^ -0.24
pr -0.26
-0.28
-0.30
-0.320.53 0.54 0.55 0.56 0.57 0.58 0.59 0.60 0.61
1000/Tm 3.1.2-8
-0.18
-0.20
-0.22
-0.24
-0.28
-0.30
-0.320.53 0.54 0.55 0.56 0.57 0.58 0.59 0.60 0.61
1000/T
m 3.1.2-9 u u >
-0.18
-0.20■*— Silicon Nitride
-0.22
cd -0.24
-0.26
-0.28
-0.30
-0.320.53 0.54 0.55 0.56 0.57 0.58 0.59 0.60 0.61
1000/Tb 3.1.2-10 sfctisoatcj;-5
-74-
Graphite - Run 1
Graphite - Run 2-0.18
-0.20
-0.22
-0.24
-0.26
-0.28
-0.30
-0.320.53 0.54 0.55 0.56 0.57 0.58 0.59 0.60 0.61
-0.18 -
Silicon Carbide-0.20 —
Cd -0.22
P: -0.24
-0.26
-0.28
-0.300.53 0.54 0.55 0.56 0.57 0.58 0.59 0.60 0.61
looo/r0 3.1.2-11 jcaisa*
> u 3
1000/Tm 3.1.2-12
'>u 3
-0.18
-0.20
8mol% YSZ-0.22
td -0.24
-0.26
-0.28
-0.30
-0.320.52 0.53 0.54 0.55 0.56 0.57 0.58 0.59 0.60
1000/T
0 3.1.2-13 -T y h U
-75-
g
8IO
03btio
0.030
0.025
0.020
0.015
0.010
0.005
0.0000
• • •
* e
10 3015 20 25Time / min
3.1.2-16(r 1656k)
35 40
-0.20
-0.22 -
-0.24 -
c2
O
-0.26
Average : log r| =-0.758 + 874/Ti----- 1----- 1----- 1----- 1----- 1----- r -i----- 1----- r i r
-0.32
Average (Limited Temp.)Boron NitrideSilicon NitrideAluminaQuartz8mol% YSZ
-0.28 -
—0.30 —........-*4
0.52 0.53 0.54 0.55 0.56 0.57 0.58 0.59 0.60 0.61
1000/T
m 3.1.2-17 u 3
-77-
log (
r) /
mPa
s )
-0.10
— Present work
x Glazov
-0.15
-0.20 -
-0.25 -
“0.30
-0.35
1000/T
m 3.1.2-18
—78 —
log (
r| /
mPa
s )
log (
Tl /
mPa
s )
■o— Present work x Glazov
-0.10
-0.20
-0.300.65 0.70 0.75 0.80 0.85 0.90 0.95 1.00
1000/T
m 3.1.2-19 feM GaSb t XUU
0.40 - ■o— Present work x Glazov
-0.10
—0.20
-0.30
1000/T
m 3.1.2-20 ## InSb <D ¥6 ^ CD £ IS <h ;£ gR fit
-79-
log (
r| /
mPa
s)
0.50
0.40
0.30
0.20 -
0.10 -
0.00
-0.10
-0.20 -
-0.30
-0.400.50 0.60 0.70 0.80 0.90 1.00 1.10 1.20 1.30 1.40
1000/T
m 3.1.2-21 Six Gex GaSb £ InSb 0 & 14 ¥ Ml ^ ^ £Glazov 0 # o' # £: 0 .fcfct£
-80-
Den
sity
/g cm
3
2.70
2.65 ™~
2.60 -
2.55 -
2.50 -
2.45 -
2.40
Present work *— Mukai *— Mukai
Glazov *— Lucas
Taran-Inc.Temp. Tar an-Dec. Temp. Sasaki-Quartz Sasaki-SiC
1650 1700 1750 1800 1850 1900 1950 2000 2050 2100
Temperature / K
m 3.1.2-22 ^|y'j3 >©?g&0«|j£J|g£:i3<k
-81-
Den
sity
/ g c
m
5.65
5.60
5.55
5.50 -
5.45 -
5.40 -
5.35 —
5.301100 1200 1300 1400 1500 1600 1700 1800
Temperature / K
m 3.1.2-23 —
3. l. 3 '>U 3
#%###% M
##%##% g#
#%###% HI ill IS 2:
#####% # #
( l ) s@
u 3 >(Dmfcmmtmmttyti&Mm<Dm&t&^£t£z>0
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c a & 99 6, & k: L, en^n<D^S^tc45tj-^^eSS(X)ejBS(r)om^:
CioTilfCo
S^~1000K Xso.id.low temp = (1.40xl0 8r 2 + 1.90x10 T + 2.92X10-5)1 Wm 'K1
1000K~1673K Xsolid high temp = Xsolid>low temp + Xe Wm *K 1
fzfzls, X, = 8.28 - 2.35x10 2T + 2.01x10^7 2 - 4.30x10 »T 2 Wm^K1
£fz, i^y'j3>0|ii|}t 0/JxS*T^45 V^T 1698~1737K O^SSeBTSJS
Lfzffig:, 6-8Wm-1K-1T^ofco
-Jj, 3-;i/H • 2 )l—i'Zf)l\Z&-DTlNl&LrcUnfrt>
£ £ l/to £<D%&lzJ:9 , M&lz&zmftRZfimfci/ U 3 >td3 V>T,
<DES^, 650~850nm 1000~2100nm £45 T 54 ?£;&$: Srfi1 o fco C CT
«> LT&g 650, 1500nm £4^3^#:£0ftCD547£ifcM$£^T£^To
650nm, ##: :0.231. @ ft:: 0.377
— 83 —
150011111, ##:0.173, @ ft: 0.480
#ft L BfttelE
0 * m&lZ&l* TfcHftv'U n Ztifiti
fr-o ft e
Thermal Conductivity and Normal Spectral Emmisivity of Molten and Crystal Silicon
Kazuhiro Nagata, Masahiro Susa*, Hiroyuki Fukuyama and Miyuki Hayashi
Department of Chemistry and Materials Science
*Department of Metallurgy and Ceramics Science
Tokyo Institute of Technology
Abstract:
The thermal conductivity and normal spectral emissivity of solid and liquid silicon are
required to develop mathematical models of the heat flow in manufacturing processes for silicon
single crystals. This work aimed at obtaining accurate values for these thermophysical properties.
The non-stationary hot wire method was used to measure thermal conductivities of solid and
liquid silicon, where hot-wire probes were insulated electrically from silicon samples using silica
films. The thermal conductivity of solid silicon decreased with increasing temperature. In solid
silicon, heat is principally transported by phonon conduction at temperatures below 1000 K, and
above 1000 K electronic conduction also contributes to heat transfer. The thermal conductivities
(X) in the respective temperature ranges can be expressed as a function of temperature (T) as
follows:
rt < T < 1000 K Xsoli<Uow temp = (1.40xl0'8r 2 + 1.90x10 5T + 2.92x10 ") ' Wm ’K1
1000 K < T < 1673K Xsolid high temp = Xsolid low temp + Xe Wm 1K 1
where Xe = 8.28 - 2.35xl0 2T + 2.01x10 "T 2 - 4.30xl0"9r 3 Wm 'K1
The thermal conductivity of liquid silicon measured under microgravity is 6 to 8 Wm^K1 at
1698-1737K.
— 84 —
On the other hand, the normal spectral emissivity of silicon was derived as the ratio of the
normal radiation intensity from silicon sample to that from a blackbody at the same temperature
as the sample. The sample and the blackbody were heated up using the cold crucible. Normal
spectral emissivities of liquid and solid silicon were determined at the melting point in the
wavelength ranges of 650-850 nm and 1000-2500 nm. For example, values of emissivities
measured at 650 nm and 1500 nm are as follows:
650 nm: 0.231 for the liquid, 0.377 for the solid,
1500 nm: 0.137 for the liquid, 0.480 for the solid,
The emissivity in solid is larger than that in liquid at the wavelength investigated. The
emissivity in liquid decreases slightly with increasing wavelength, which indicates that molten
silicon is metallic. On the contrary, the emissivity in solid increases with increasing wavelength,
which indicates solid silicon is still semiconductor even at high temperature such as the melting
point.
(2)
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(6)
a.
1) M.Susa, H.Watanabe, H.Fukuyama and K.Nagata : “Emissivity measurement on liquid metals
using cold crucible technique” , Proceedings of The 5th Asian Thermophysical Properties
Conference, (1998), p.479
2) H.Watanabe, M.Susa, H.Fukuyama and K.Nagata: “Measurement and Theoretical modeling for
emissivities of liquid noble metals in the infrared region” Proceedings of The 5th Asian
Thermophysical Properties Conference, (1998), p.483
3) Lii^so, m&m®, Isanti, *ea*n;£ : rFz n >¥rB<DB
SSJ, B p.184, 1998 ¥ 9 /!
4) maitm, wmm*K, m&m®, : ri*,&t:;mta#ft#ztmft
m&mvvsmmz&rtzftytj&ttmi, P.i83, 1998 ¥
9 %
5) m&m®, # #, fmiiiit±, ^cbb^p^ : rEftyij □ ><Dmfc^&<Dmm
m mM 1999*3 ft
6) Eiaitii, nmmiK, m&m®, mmit^, 3d m
Bft&M M S* (^Mll^) 1999 ¥ 3 £
7) ̂ j21#jI, ttfflSX, tsiiilt;*., : r~>un> • >r ;i/ ~ r7 a <D 5>
M 3C* OK
5KXM±¥) 1999 ¥ 3 £
8) H.Fukuyama, E.Yamasue, M.Hayashi, M.Susa and K.Nagata : “ Challenge to Thermal
—104 —
Conductivity Measurement of Liquid Silicon under, Microgravity” 0 ^ v > ^ v ^7
A B 20 IhJ, 1999 ¥ 10 A216, 280-283
9) H.Watanabe, M.Susa, H.Fukuyama and K.Nagata : “Measurement of Spectral Emissivity for
Metals and Semiconductors Using Cold, Crucible” 0 >" > V ^ A ^ 20 IhJ, 3fEM ,
1999 ¥ 10 £ , SSElm^S, A226, 308-311
10) K.Nagata, E.Yamasue, H.Fukuyama, M.Hayashi and M.Susa : “ Thermal Conductivity
Measurement of Liquid Silicon under Microgravity”, 0 (SB 1 ©HI
IE "tl y '> 3 >) S 138 HI, 1999 ¥ 11 ^ 12, [4], 857 (1999)
11) # #, : ri4 # O @ ## # I: &
m 125@, 1999 ¥ n^, 535
12) E.Yamasue, M.Susa, M.Hayashi, H.Fukuyama and K.Nagata : “Contribution from Phonon and
Electron to Thermal Conductivities of Solid and,Liquid Silicon” 15th European Conference
on Thermophysical Properties,Wurzburg, Germany, Sep. (1999)
13) H.Watanabe, M.Susa, H.Fukuyama and K.Nagata: “Emissivities of Liquid and Solid Silicon at
Melting Point ” 15th European, Conference on Thermophysical Properties, Wurzburg,
Germany, Sep. (1999)
b . Ws3C
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2) H.Watanabe, M.Susa, H.Fukuyama and K.Nagata : “Emissivities of Liquid and Solid Silicon at
the Melting Point” , High Temp. - High Press., Vol.31 (1999), p.587-593
(7)
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-105-
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375
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No.3, (1968), pp.765-782
—106 —
(3)-22 Private communication with T.Okutani
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(3)-24 N.B.Hannay, Semiconductors (Reinhold Publishing Corporation, New York, 1959), p.332
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No.3, (1968), pp.765-782
(4) -l F.G.Allen, J. Appl. Phys., 28, 1510 (1957).
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107 —
3.1.3-1 Experimental conditions for thermal conductivity measurement od liquid silicon
## mam) JUJf (jUm) ISSlA) S«(K) 11*
A-1 JUG 180 1.998 1698 6.10A-2 JUG 180 1.998 1699 4.31A-3 JUG 350 1.998 1737 7.60A-4 JUG 350 2.003 1719 6.75 •B-1 JUG 350 1.998 1724C-1 1G 350 1.498 1695C-2 1G 350 1.498 1695C-3 1G 350 1.249 1695C-4 1G 350 1.249 1695C-5 1G 350 2.253 1695 ?Q-;/|'©E**ttA<ES.;h,fcA'bfcD-1 1G 350 2.000 1735D-2 1G 350 2.000 1735 «*IC***t**tiLfcD-3 1G 350 1.743 1735D-4 1G 350 1.743 1735D-5 1G 350 2.498 1735E-1 1G 180 2.000 1716E-2 1G 180 2.500 1716 ^a-yKDE»tt*<»c>h.»6'ofcE-3 1G 180 2.500 ' 1716 ^□•yh(DE6ii14A<EP)tL»A'-ofcE-4 1G 180 1.498 1716 ^□-yKDEEttA<E5>n<?6'-ofc
3.1.3-2 Physical property data used for the calculation of the electronic component in thermal conductivity of silicon at temperatures between 1000 and 1673K
r/K 6(3)-= Eg /eV3)"24 cr/Q'W1^"251000 0.43 0.85 21031200 0.43 0.78 64611400 0.43 0.71 144021600 0.43 0.55 262721673 0.43 0.52 31416
-109-
3.1.3-3 Results of emissivity for Si at melting point.
LiquidWavelengt Run 1 Run 2 Run 3 Average values
500 0.203 0.187 0.197 0.196550 0.194 0.191 0.196 0.194600 0.225 0.214 0.217 0.219650 0.231 0.230 0.231 0.231700 0.236 0.234 0.229 0.233750 0.231 0.234 0.226 0.230800 0.227 0.229 0.222 0.226
1000 0.190 0.197 0.194 0.1941100 0.191 0.192 0.189 0.1911200 0.186 0.187 0.184 0.1861300 0.182 0.180 0.182 0.1811400 0.177 0.176 0.1771500 0.172 0.176 0.1741600 0.180 0.180 0.1801700 0.164 0.164 0.1641800 0.166 0.170 0.1681900 0.160 0.164 0.1622000 0.161 0.164 0.1632100 0.155 0.159 0.1572200 0.157 0.163 0.1602300 0.148 0.152 0.1502400 0.154 0.156 0.1552500 0.161 0.167 0.164
Solid500 0.274 0.286 0.264 0.275550 0.278 0.305 0.289 0.291600 0.343 0.359 0348 0350650 0.369 0.400 0362 0377700 0.389 0.439 0385 0.404750 0.415 0.462 0.432 0.436800 0.406 0.456 0.422 0.428
1000 0.404 0.453 0.460 0.4391100 0.443 0.428 0.449 0.4401200 0.457 0.459 0.470 0.4621300 0.465 0.460 0.475 0.4671400 0.474 0.463 0.4681500 0.484 0.477 0.4801600 0.485 0.515 0.5001700 0.488 0.496 0.4921800 0.514 0.515 0.5141900 0.491 0.518 0.5042000 0.512 0.519 0.5162100 0.526 0.514 0.5202200 0.523 0.532 0.5272300 0.505 0.526 0.5162400 0.539 0.531 0.5352500 0.551 0.570 0.560
-no-
THER
MA
L CO
ND
UCT
IVIT
Y, W
all cm
'
IH 3.1.3-1 Thermal conductivity for solid silicon as a function of temperature.
-Ill-
(f (B In
f + C
))/(ln
t +A
) X10
0 /%
Time/s
0 3.1.3-2 Relation between the deviation from Eq.(3)-2 and time.
0 3.1.3-3 Instrumental setup of the nonstationary hot wire method in this study.
-112-
Oxide layer(~100nm)
0.15mm* Pt-15%Rh wire
0.15mm* Ft wire
Chart Recorder
@ 3.1.3-4 Schematic diagram of the experimental apparatus for measurements of solid silicon.
-113-
Oneway valve
Emfaft
Thermocouple
0.15mm<|) Mo
Silica insulator
0 3.1.3-6 Schematic diagram of experimental probe and crucible.-115-
Ther
mal
Con
duct
ivity
X /W
• m
"1 • 293K
Current,//A
HI 3.1.3-10 Relation between the thermal conductivity for mercury and the current supplied to the wire.
-119-
/t/W
-m
60F
40b
20b
Temperature /°C500 1000
Sn
H O&OvOv&r OO
500
M.P.«S0SK 1
1000Temperature ZK
1500
• This study □ Pashaev o Konno et al O Yurchak et al a Brown —Nikolskii et alv Filippov
— Wiedemann-Franz law
0 3.1.3-11 Thermal conductivity for tin as a function of temperature.
-120-
A/W
m
^ 30-
20-
10-
M.P, = 600.5K
500
Temperature /°C
500 1000
Pb
.» »»»»■# m......
1000Temperature /K
• This study o Berman et al.o Fillipov O Yurchak et al.a Dutchak et al. @ Nakamura et al.v Powell et al. 0 Duggin
— Wiedemann-Franz law
0 3.1.3-12 Thermal conductivity for lead as a function of temperature.
150'0Temperature /°C
500 1000
a ioo£
50
0 J---------L
500
r------- 1------- 1------- 1------- 1------- j------- 1——i------- 1------- 1------- 1------- 1--------r------ 1—
9 A Boboneetal.v Beers et al.
o ° Glassbrenner et al.: fc> D Fulkerson et al.r ® Kimura et al.
rift ® Yamamoto et al.• This study
TXcpqp gD
J t 1 L J t:i i i............... t.1000
Temperature ZK1500
0 3.1.3-13 Thermal conductivity of solid silicon compared with reported values.
-122-
A,.<H IA V
0.9 T T
U G1737K
mm 350Iim
y=a + b In xa=6.125717e-01b=7.230423e-022.622845e-03|r|=9.967875e-01
Tl sec
HI 3.1.3-14 Effect of gravity on A V vs In t profile.
-123-
Temperature/^
W - F Law
Temperature/K
0 3.1.3-16 Temperature dependence of thermal conductivity of liquid silicon.
-125-
Focusing lensSpectroscope
Short cut filterChart recorderWindow Prism
Diaphragm
• V Detector MonochromatorSample
Cold crucibleCamera
WindowBN plate
Induction coilsGraphite plate
yGraphite crucible
Zr sponge
Alumina crucible
Alumina tube
Air-tight chamberPositioning rod
0 3.1.3-17 Instrumental setup to record the normal spectral radiation from sample.
-126-
Nor
mal
Spec
tral
Em
issiv
ity
Wavelength/nm
Jellison and LowndesLiquid
+Solid
Aoyamaetal.Liquid♦
Solid
Allen B Linde et al. B
Lange et al. B Krishnan et al. +
Li and Fauchet * Takasukaet al.
Shvarev 0 Present study " # ' -o-Lamport B □
0 3.1.3-18 Comparison of the reported values of the normal spectral emissivity of liquid and solid Si at and near the melting temperature.
-127-
Tota
l Hem
isph
eric
al Em
issi
vity
Measured Values • 78 Qcm Sia 0.012 Qcm Si
Calculated Values j o From Sato :D From Vandenabeele-^
and Maex :
200 .300 400 500 600 700 800 .900Temperature (°C)
@ 3.1.3-19 The total hemispherical emissivity of the lightly(78 Q cm) and heavily (0.012Qcm) doped silicon specimens as a function of temperature. The solid curves are fits to the data point. (Reprinted from the Journal of Applied Physics,74,6353(1993).)
3. i. 4 u3
auc*# >?-
#□ ##
Equilibrium of Liquid Silicon and Segregation Coefficient of Oxygen in Silicon.
Yasutaka Iguchi
New Industrial Creation Hatchery Center,
Tohoku University
3. 1. 4. 1 Si yUk h/Si02$fctt Si3N4, SiC lifl © iS JR ¥ W
(1) S8
tky^sigisasaiitctc± o«Ett©i6
Stc$©-> V 3
h41'x©B#C#'5ffiiFB6x*;|y*-$rt;:£:BtBUA:. S 6>fc, -> V 3
Equilibrium between Liquid Silicon and Si02, Si3N4 or SiC,
Abstract:
The solubilities of oxygen, nitrogen and carbon in liquid silicon equilibrated with silica,
silicon nitride and silicon carbide, respectively, were measured. The melting and analytical
methods were developed and accurate data on the solubilities were obtained. The standard Gibbs
free energy changes for dissolution of oxygen, nitrogen and carbon in liquid silicon were
-129-
determined. The effect of alloying elements on oxygen and carbon solubilities was clarified.
( 2 ) ti c ft 1C
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3.1.4.1-1 3.1.4.1-2 ic ^ ttb Tito
(4)
(a) Si x;i/ h/Si02rB1(D^S¥E 9)
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iog(ca) a i/T <Dm\zw.%km%$:fafeL, tmm^ u 3
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log(Co/mass%) =-4620/T+0.332(±0.06) (T:1693~1823K) (1)
g4I" 43 tt £ St^39 mass ppm (3.4xl018atoms/cm3) <k St IF c? tl >£: „ y'J 3>i
Si(l) + 2Q. (lmass%, in liquid silicon) = Si02(s) (2)
(2)^(d5f^se k2te(3)5t'r^*r
K2 = a$i02/(aSi * aQ2) (3)
C CT, ai(ii<Z)ffii$^to t ppm gg
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-131-
aD Henry SVJ tC X £ 43 S > mass% TS^ L V U=i>41(D^#BS<7)?$
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= l/(f0* [mass% O])2 (4)
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AG2° = -RTln(K2)
= -1.77xl05+12.7T(J) (5)
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Si(l) + Oz(g) = Si02(s) (6)
40,' = -9.527xl05+203.8T (J) (7)
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l/202 = Q. (lmass% , in liquid silicon) (8)
AG8° =-3.88x10s + 95.6T (J) (9)
Si / ;i/ h/Si02 fm ©##?#(: MB 10 E 3.1.4.1-2 tC fi£ * % ^ £ 4l T
U5'>U3>#fr0#$gillSSt»TSf 9)< 15)’26)o '> U 3 >E*Jc43tt^ES^S
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LTwa.
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Hirata and Hoshikawa19) CD |g ^ fil te 1685K—1800K CDj£ W&SE^C
+ 5ppm O®0T — Ifc LT^5,
(b) Si *)l h©|*a«*«^R«T^JP7C*oaa 12)
ES^SSC&ETSIjDtuS (Sb, B, p, As) cD##^##JT6 a*C#mE#%^
mi^n^^tzo -mtLx, e 3.1.4.1-3 c~> u * <b¥Et*5 v u u ymw-ommmmSCXfff B McD%W£^t" „ lifn®I«l:*UTt>, B #m^±#T6C#wE
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C0(Si-X)«^CDi; o CfBj$T'££ C 12)o
log(CG(Si-X) / mass% ) = log(C0 / mass% ) - eDx[Cx / mass% ] (10)
EL, Cott«'>U3>0i**iflt4 eGx ttffiSfPJflttf&ft'C* 0 , »»'>U3>o#
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e 3.1.4.1-4 c#af#m###:(D&^###
tcsmc<£des
£ fctfE t>fr£Uz>tzo
eQSb = -0.02
e0B = -0.03
eQp = 1.60 - 3.02x103/T
e0As = 2.08 - 3.85x103/T
(U)
(12)
(13)
(14)
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-gcLT^ 0 , iy'Jn >SfcfctttfllBT?£fc„
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m 3.i.4.i-6 \z&mmm (cN) mamm# ±#c#
5 SSSS<9itiJll^E§§l£:hfc = log(CN) ± 1/T ®MK:fi«W«£®j£ L, S/hS^&T
mw?z>£ '> U 3 >tt#©as*s*£©fflgft#a£ LT(15)5£j&«fc£ns.
log (CN/mass%) =2.410 - 9759/T (±0.24) (T:1723^ 1873K) (15)
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bt^to
— ^ (1685K) $T^#LTf#e>n5SS
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Yatsurugi 6 18)(D cr® 60ppm D 1 ^ % 2k #) # i=r "TT
lrp\ZWZE-rZ>5fcmffi Si3N4 ^ ^ 41 T active nitrogen i%
®&n zntzbo) tmm £ n* „
3Si(l) + 4K (lmass% , in liquid silicon) = Si3N4( /3 ,s) (16)
ESdS^r±|WIStc#xtitf, (i6)^<DS2FS6x^;i/^-^<b, ag16° > te(i7)5£T
AG,; =-7.473x10s + 184.6T (J) (17)
Hendry28* <£> SS ® £ £ *1)3 -Si3N4 <D *P £ § * X ^ - te(19)^T^ $ ±1 £ 0
—134 —
3Si(l) + 2N2(g) = Si3N4( & ,s)
AG18° = -9.252x10s + 450T (J)
(18)
(19)
%m< z. o
1/2N2 = K.(lmass%, in liquid silicon) (20)
AG20° = -4.45xl04 + 66.4T (J) (21)
(d) si >;i/ H/sicn)
m 3.1.4.1-8 iCKilS (Cc) (DU&fcWfe&Tik'to log(Cc) t. 1/T ©Pal \ZUUWl%%:fo.
(j3M) <h¥Wr^>^H$'>U n XDj^S^SS
^S^#ttH(22)^T^$ n^> =
log (Cc/mass%) = 3.63 - 9660/T (±0.02) (T:1693~ 1823K) (22)
M & \z& 79ppm (9.1xl018atoms/cm3) tstW'ZtlfZo E 3.1.4.1-9 \Z%£
*#e$nTV^^E'>U3l id* i3). 29)-32)o
tmmoyomik^&j&wUZ'k o, e(T©iA*iUiTt«.
Si(l) + C(lmass% , in liquid silicon) = SiC( & , s) (23)
AG23° = -1.85x10s + 69.5T (J) (24)
C(s) = C(lmass%, in liquid silicon) (25)
AG25 ° = -7.20xl04 - 11.4TlogT + 6.20T (J) (26)
(e) si *)i b<dfemmmg.fcR&'tmmjtmvmwi3)
U n > (p, B, Ca, Ah Th V, Cr, Fe, Co, Nh
Cu, Mn) (D&W&W&TB8 ZfrlZLfCo E 3.1.4.1-10 \Z B }JD7C *jft&t ft <D H
-135-
. P. B, Ca, A1 rosin Ti, V, Cr, Fe- Co, Ni. Cu,
Mn ©Ss in (4 C fc. H4>©iS«©«#± 0 K*S(W*
aiwtme#ammmm» (ecx) s*mut5ct«*T?«5. i5.u.i.ucEfi^ifi
( ecx) a©w#e*T.
s t- s ■$> „
£ cx = 230 (Mx/28.09) ecx + (28.09 - Mx)/28.09 (27)
fit. Mx ttjc* X ©B?#T&-5. iSSl Fe-C-X * C *3tA T Bf#§ t fflS ##
IctoreicliB^tiZiSSiHtAtseshTHS ”>■ 34>. si-c-x Sic45HTfcttfaliK^#*§©«
sole#5 £cx©±#ASHBSnfc,
(5) it®
-> U 3 >H#:4I©«#69e7nS^itoiWT»5)ES. a*45 =k tXKSICH U
(a) ->u*. a-fb-T-T1 **j:¥«r•£.->■;3>a*4i©®s, a*43j=o=6 A4I: L E.SIC45tt5SIB*tt. KS : 39ppm (3.4xl0,satoms-cm-3),
8 * : 4ppm (4xlOl7aloms'em"3). 6< * : 79ppm (9.1xl018atoms• cm"3)7? 3) o fc =
(b) m*. a*. ^*®<s*©ta*t6#tt45 =t:y:'>u», aib^'f*, *©a#t&x*)b*-<k 0 K*. a*. «*©->U n 5®*pasx^.
(C) -> v n >#»©$** ±o:%*s#«tcRSt"$iiDSS©ieesrS9e,»'ic vfc. m 4 m
(«amm«») aa?#^a©m$.5>aa$rfl,Via'Ufc„
(d) 3/ V 3 >##:©%A 1:45)4 5#*. a*. ^*##*45 Z 0 #6ase*
-> U 3 >©at.^e45t4 5>E*. a*. SSSSFSJ: 0 - cne>©5cS©B*6¥ffi#K«&
£#g L4c.
-136-
( 6)
( a) 85C5B8
1) K.Yanaba, M.Akasaka, M.Takeuchi, M.Watanabe, T.Narushima and Y.Iguch, “Gabon Solubility
in Liquid Silicon Equilibrated with Silicon Carbide,” Mater.Trans.JIM, 38 (1997), 990.
2) K.Yanaba, Y.Matsumura, T.Narushima and Y.Iguch, “Effect of Alloying Elements on Gabon
Solubility in Liquid Silicon Equilibrated with Silicon Carbide,” Mater.Trans.JIM, 39 (1998),
819.
(b)
1) mmmm, 0n
&m", Sll9@l»8l*S, 1996 ¥ 9 £ 24-26 0
2) #□£*,
1996 1996 ¥ 10 ^
21 — 23 0
3) mmm*}, mm m, fc&smz., n
7cS(DS^”, 0 ^ 121 1997 ¥ 9 24—26 0
1997 ¥ 11 ^ 13 0
(7)
1) Oxygen, Carbon, Hydrogen and Nitrogen in Crystalline Silicon, Ed. By J.C.Mikkelsen, Jr.,
S.J.Pearton, J.W.Corbett and S.J.Pennycook, Materials Research Society, PA, (1986).
2) F.Shimura, Semiconductor Silicon Crystal Technology, Academic Press, (1989), p.307.
3) T.Abe, K.Kikuchi, S.Shirai and S.Muraoka, Semiconductor Silicon 1981, Ed. By H.R.Huff,
R.K.Kriegler and Y.Takeishi, Electrochem.Soc., Pennington, (1981), p.54.
4) F.Shimura and R.S.Hockett, Appl.Phys.Lett., 48 (1986), 224.
5) H.J.Stein, P.P.Peercy and C.R.Hills, J.Mat.Res., 4 (1989), 616.
6) Y.Shimanuki, H.Furuya and I.Suzuki, J.Electrochem.Soc., 136 (1984), 2058.
-137-
7) S.Kishino, Y.Matsushita and M.Kanamori, Appl.Phys.Lett., 35 (1979), 213.
8) F.Shimura, J.Appl.Phys., 59 (1986), 3251.
9) T.Narushima, K.Matsuzawa, Y.Mukai and Y.Iguchi, Mater.Trans.JIM, 35 (1994), 522.
10) T.Narushima, N.Ueda, M.Takeuchi, F.Ishii and Y.Iguchi, Mater.Trans.JIM, 35 (1994), 821.
11) K.Yanaba, M.Akasaka, M.Takeuchi, M.Watanabe, T.Narushima and Y.Iguchi, Mater.Trans.
JIM, 38 (1997), 990.
12) T.Narushima, K.Matsuzawa, M.Mamiya and Y.Iguchi, Mater.Trans.JIM, 35 (1994), 763
13) K.Yanaba, Y.Matsumura, T.Narushima and Y.Iguchi, Mater.Trans.JIM, 39 (1998), 819.
14) O.Kubaschewski and C.B.Alcock, Metallurgical Thermochemistry 5th ed., Pergamon Press,
New York, (1979).
15) T.Carlberg, T.B.King and A.F.Witt, J.Electrochem.Soc., 129 (1982), 189.
16) W.Kaiser and P.H.Keck, J.Appl.Phys., 28 (1957), 882.
17) W.Kaiser and J.Breslin, J.Appl.Phys., 29 (1958), 1292.
18) Y.Yatsurugi, N.Akiyama, Y.Endo and T.Nozaki, J.Electrochem.Soc., 120 (1973), 975.
19) H.Hirata and K.Hoshikawa, J.Crystal Growth, 106 (1990), 657.
20) X.Huang, K.Terashima, H.Sasaki, E.Tokizaki and S.Kimura, Jpn.J.Appl.Phys., 32 (1993),
3671.
21) L.Ottem, private communication.
22) S.Otsuka and Z.Kozuka, Trans.JIM, 22 (1981), 558.
23) A.E.Organ and N.Riley, J.Crystal Growth, 82 (1987), 465.
24) A.Seidl and G.Muller, J.Electrochem.Soc., 144 (1997), 3243.
25) S.W.Tu and D.Yanke, Z.Metallld., 85 (1994), 701.
26) H.Nafe, J.Electrochem.Soc., 146 (1999), 1130.
27) W.Kaiser and C.D.Thurmond, J.Appl.Phys., 30 (1959), 427.
28) A.Hendry, p.183 in Nitrogen Ceramics, ed. by F.L.Riley, Noordhoff International Publishing,
Netherlands, (1977).
29) S.Suhara, N.Yuge, M.Fukai and F.Aratani, CAMP-ISIJ, 2 (1989), 1341.
30) L.L.Oden and R.A.McCune, Metall.Trans.A, 18A (1987), 2005.
31) R.N.Hall, J.Appl.Phys., 29 (1958), 914.
32) R.I.Scace and G.A.Slack, J.Chem.Phys., 30 (1959), 1551.
-138-
3. 1. 4. 2 SiO
( 1 ) S©
'> U n >^;i/ 5 ©JKIft *»#!£« jib Tfigfc&ffl* SiO ftl±£'> V 31 y %)]/ v
(a) >u n >e
A (1685K) 13 ^3 If 6 # ± SiO O.Olatm T & -5 C fco 1685-1800K
13331** sio ft&tmftmmm&oMm&fe&it-rz t&izm&itLrzo
Relationship between SiO Partial Pressure in Gas Phase and Oxygen in Silicon Melt.
Abstract:
The relationship between SiO partial pressure in gas phase and oxygen contents in liquid
silicon was discussed thermodynamically, which is an important factor for removing of the
dissolved oxygen from liquid silicon. The maximum SiO partial pressure was calculated to be
around 0.01 atm at 1685 K. The SiO partial pressure was graphically shown as a function of the
dissolved oxygen contents.
(2) #081:
v u 31 y* )v h s #xi sio ©fit fctfe nJiSflTHJ. a^T, CZ 7,n-irX->5al/-->3 SiO #K
^SffE*SS®$eB9¥«IS«6^£>BT'*5. tit. CZ&\Z
-140
(3)
(a) SiO
SiO $ £ b T® fcSig&®*Fg te, Kubaschewski
and Alcock1^ JANAF2)4d =k ZS Knacke et al .3)Of—^ # ck D # 6 tl -5 « ■?■ tl ^tl (D x “ ^
^<k 0 $ n%> Si(i)-Si02(s)-Si0(g)¥^it ((i)it) (DS^FS — (Ag/ )
Si(l) + Si02(s) = 2SiO(g) (1)
A GUiefA ° = 658980 + 53.9736TlogT - 489.946T (J)^ (2)
A Gj.^f.2 ° = 618618 - 290.61T (J)2) (3)
A Gx.ref.3 ° = 622254 - 289.94T (J)3> (4)
(2)''w,(4)j£ (D & it % U T E3 3.1.4.2-1 tC Trt't* o Kubaschewski and Alcock £ JANAF
(DAG/ ££&£>&%, Knacke et al.(D#####(D 2 ^XDbCDtit
^ # T Wx x — Kubaschewski and
Alcock (DS@E> ^(2)^:& SiO(g)^ — ##(D(^
Cm W-5 C a a Ltz c
(b) '> u n >>;i/ SiO
'> u 3 >*)V sio #jE©lfi#tt43cfctff&£®
SiO(g)> Si(g)> Si02(g)T$>5o volatility
diagram ^ ^ T & & » volatility diagram Z> 33 X 7" 2/ is -Y )]/ \Z%t fo't' <5 fl! ;k
4)o Si(l)£fc«
Si02(s)/^#S L. e> <D^£S^&(5)& <£t£(6)^Tl&Wt‘'5
—141 —
Si(l) + 02(g) = Si02(s) (5)
AG/ = -952697 + 203.76T (J)^
= RTln(Po2) (6)
'> U 3 > E & (1685K) £43 HTte. (6)^:^ 6st#$4l6?###^E^ 1.28x10'^atm
T&6. lot, 1.28xl019atm <D m M ft E ^ T £ 43 V> T tt ^ t L T Si(l)^£)£T.
6#X$£ Si(g)43£tf SiO(g). 1.28xl0-19atm &±T& Si02(s)^^^EEffiT
SiO(g)> Si02(g)^#ET6^4X#T$)6o 3 1685K
£ $) It 6 volatility diagram £E 3.1.4.2-2 C^to T~ ^ £ LT&E£
Kubaschewski and Alcock <D SBfS 1}£ <A £: <, £ ® £ Y) . 1685K £43tt6 SiO (DMXftR
\%fcJ O.Olatm T & D . -ZrtUZ Si(l)43£££ SiG2(s)v^5£ # T 6 IE £ # 6 4l6<> T> £ D > (1)43
zitwztiz sio ft& ((7)^mm)
PSiG = exp (-AG^./ /(2RT)) (7)
10-27^10-4atm 3;T(7)K(Am##E#£43(AT. SiO
$6 C <h^4D^6o
(c) sio ftj£t'>v z
volatility diagram tt. SiO ^E-SrBISi^EOlSEIIfc^: L'T@7KL/c!fc>(DT$>6o (D CZ
& £ J; 6 '> U 3 SiO ^E^rSE^mS^Ed: V
miE<o cz yotxc^^Tii.
Z'VIZfc h W3##T#$&^4l6. -
<£>£:£>'> U 3 >*;i/ hS@£43rt6 Sio
4l6 6#A6(D^#^T^6. ##6(D Si02(s)£ ¥«T 6 feM zs U 3
5)j;o. (8)^o#mgH(9)^:Tm$4i6.
—142 —
Si(l) + 2Q (mass%, in liquid silicon) = Si02(s) (8)
(9)AG8° = -177000 + 12.7T (J)
(l), (2)^&£EX(8)> (9)5t<£ 0 SiO(g)£ m M <D ¥■&£(10)£ £ ^ <D & ti x^;i/
Si(l) + Q (mass % , in liquid silicon) = SiO(g) (10)
AG10 ° = 240990 + 26.9868TlogT - 238.623T (J) (11)
(10), (11)^4: 0 SiO # EE £ [mass %£]<£> HI £ LTggt^. H *tt£(12)
1685K, 1750K, 1800K \Z 43 % 1*1 B# \Z
Psio = [mass%Q]exp(-AG10° / (RT)) (12)
= 2.789x[mass % Q.] at 1685 K
= 5.008x[mass% Q] at 1750 K
= 7.625x[mass % QJ at 1800 K
(12)atf*ffi3ft® SiO -Jtfi
sio t,
^>o e 3.1.4.2-3 £(i2)^6<z)tt-sss^£^t*o a*,
Si02(s)£¥«f DISKS' U 3
Si02(s)<h Si(l)^##f SiO ((7)S fc J: 0 WrW- £
fia SiO #E)
(4) ̂ a A
Sio frE^SSv U 3 Sio t;i
*t* @ A % 4V1/ 4r — <h L T kt Kubasche wski and Alcock
sio ftj££®&mmmm(Dm&&mn'?z> £&\z, fneoi
—143 —
1685K~ 1800K 1C & 1A T 0 W IZ St £ JIMS L „
(5)
1) O.Kubaschewski and C.B.AIcock, Metallurgical Thermochemistry 5th ed., Pergamon Press,
NY, (1979).
2) JANAF Thermochemical Tables, 3rd ed., ed. by M.W.Chase,Jr et al., ACS and AIP for NBS,
NY, (1985).
3) Thermodynamic Properties of Inorganic Substances, ed. by O.Knacke et al., Springer-Verlag,
Germany, (1991).
4) A.H.Heuer and V.L.K.Lou, “Volatility Diagram for Silica, Silicon Nitride and Silicon Carbide
and Their Application to High-Temperature Decomposition and Oxidation”, J.Am.Ceram.Soc.,
73 (1990), 2785.
5) T.Narushima, K.Matsuzawa, Y.Mukai and Y.Iguchi, “Oxygen Solubility in Liquid Silicon”,
Mater.Trans.JIM, 35(1994), 522.
—144 —
3. i. 4. 3 '> u 3
(1)5©
Si02 (Cs) #&
##v =z(cL>
'> U n '> U n >%#:.$/ V 3 >*§#18 0##
o@i¥I^Eit k=cs/cL) £ 0.7-0.9 <hStti Lfc„
Equilibrium Distribution Coefficient of Oxygen between Solid and Liquid Silicon.
Abstract:
Oxygen solubility in solid silicon at the melting point of silicon (Cs) was measured by a
chemical equilibrium method. The value of oxygen equilibrium distribution coefficient
(segregation coefficient, Cs / CL) was evaluated to be from 0.7 to 0.9 by using Cs and oxygen
solubility in liquid silicon at the melting point (CL) which has been reported by the authors.
(2) #C&I:
f0K##* (c,„ ,oMa) k-c,. ,lquld T#
-fc c c-r k c,„ tt -> v 3 > * in- f ©E**«
T&-5. 3> W 9 , v 9 3 >#ieSct>®**#aE->3 a. v-'y a > 0 » It B, -> U 3 > ;*
«£#, ->'J 3
<o&0#e#&o,*3.1.4.3-i c*iue>T*-r
-£03iS658;Bi86J$S£
flBLTHs. a#;*-$>ro
T. a9J»HS^*fr0ES^»UH. fit, *E%T'Hlt¥V«&li$eiS*ny5:0)g
V1t. if, Si02 a:¥Ef-S>B#:^U3>0KS®®$^
—145 —
8J56L, •> V 3 >6$S|-
* tt S K * ID B S ¥ ffi & E « » Sr S titi f 5.
( 3 ) SiSS
Si02 U 3 >08 SSSSese^teSScf. ttfttttt FZ y'J3>*8
S*e.fflyitiLy5:$t)i->U3> (lOmm X 15 mm x 1.5mm) SrfflVifc. CZ v U 3 > T- tt &
< fz ->u3¥*»«
©M*£BWtt, itfiitssii tti Ufc. C®KS6KSfliSittF. 1673K l=*®TR#
L, *S®¥E$r + ti-afi8Sti--5 (H 3.1.4.3-1 #E).
Si(s) + 2Q.(in solid silicon) = Si02(s) (1)
ttfiSSCfa. »*#7. tOKJ&lcJ: OffiBtt Si02 ftliiif < S^Sti5.®T,
WSB®*Kfl:-> U 3 >S®ES#$tt(i)Slc =fc DftSSiU. -> U 3>4-©K*»lfTtt
S#->U3>©**»**ffc#Sl/ft#^ "6R#. *EIC®f$$nfcK'fb6IKS:E«l»
ibfca, J: 0 it* Vfc.
(4)
(a) ¥#em®#w
*STtt¥#eera®ft$^SBT*-6. ¥###i=*&s. mm:j:D¥#ir»io#s
efT^Dfc. ffl-*Ltt-*5cTff»n, sesiic±ogtseufcBtF*sx8ES#« 5PPm, ?
30PPm. H*->U 3 >4>®KSi6E«$IC 3.5xlO-9cm2/s,0>-l2>$«-S®B
I:#rn Fick ®#c&mj&±B®#:#®T?#<**6#»&
l:J:58c#«-SSffiv>fc. -etoittBSH 3.1.4.3-2 c$f. Pick ®S — ftlto =kat«#i£
lc«k 0 S-*UfcK**flEtt6< -StLTHS C 4:* j:tFAerSa6*«t"ti« 500 BEGS
-146-
( b )
E 3.1.4.3-3 S: 1673K tC* tt •$> fitS#[ffl t K ##$0 H# £ ^f „ *0J;O 1673K
C*5tt5ESSl@*li 26~36mass ppm (2.3~ 3.1xlOl8/cm3) b Itl t> -5 C b¥*T" £ i>.
1673K 7»>6 1685K C 43 tt S B # S'U 3 C©«&
S' U 3 >Bt 'J 3 /®8ISi# (Cs) -> U
3 >8t,&C43tt5SSi'> U 3 >©g£$i§JW6 (CL) CBLttt 39mass ppm (3.4xl018/cm3)
iOItfli S lc«t 0 l&sntus ”©T, -> 'J 3 >8l!,'±U;:43tt3K*©0*¥*#K
(k0 =cs/cL) a. o.7~o.9itftti.. *e%©s«e«-
J: 0 Wtti Ufc Cs43cL£tefll LT k & HW- l-Tc Z b I:
&&. ctxttftSEWiisajss&ifiifflUfcT&fttfiattofciwmsat?****.
entikii, *e, 1 htt***< 0.8 a«i ^ 3 Kakimoto and Ozoe7>¥ Huang et al.8)©^ A — Ht U T V1 5 »
(5) iti6
(t4f¥*SI:i!) 1673K (2* BfcS' 'J 3 > © & * ig* S £ M it L£ i £ 5 26 ~
36mass ppm (2.3~3.1xl018/cm3) b !-> tlfco £©x— ^7
»» v u 3 d tc j: o u 3 ><t»#*©¥*s»E«*£
o.7~o.9 <hfl,at)3fc„ c©ma. -mu
f- o
(6) ##%*
(a) n«fi*
1) ^»NS±, #P*#:“y'J3>fOS*»*K', $ 41 EE3ES,
1999 ¥ 5 fl 20 B
—147 —
(7) rnmicm
1) F.A.Trumbore, Bell.Syst.Tech.J., 39 (1960), 205.
2) Y.Yatsurugi, N.Akiyama, Y.Endo and T.Nozaki, J.Electrochem.Soc., 120 (1973), 975.
3) A.Murgai, H.C.Gatos and W.A.Westdrop, J.Electrochem.Soc., 120 (1979), 2240.
4) W.Lin and W.Hill, J.Appl.Phys., 54 (1983), 1082.
5) W.Lin and M.Stavola, J.Electrochem.Soc., 132 (1985), 1412.
6) — , S56JIIS, B 20 (1993), 37.
7) K.Kakimoto and H.Ozoe, J.Electrochem.Soc., 145 (1998), 1692
8) X.Huang, T.Nakazawa, K.Terashima and K.Hoshikawa, Jpn.J.Appl.Phys., 37 (1998), L1504.
9) T.Narushima, K.Matsuzawa, Y.Mukai and Y.Iguchi, Mater.Trans.JIM, 35 (1994), 522.
10) S.T.Lee and D.Nichols, Appl.Phys.Lett., 47 (1985), 1001.
11) R.A.Logan and A.J.Peters, J.Appl.Phys., 30 (1959), 1627.
12) M.J.Binns, C.A.Londos, S.A.McQuaid, R.C.Newman, N.G.Semaltianos and J.H.Tucker, JMS,
Materials in Electronics 7 (1996), 347.
-148-
3.i.4.i-i
Elements Temperature / K Atmosphere Holding time / ks Crucible Solid phase equilibrated
with liquid silicon
Oxygen 1693-1823 o2 7.2 Si02 0 -cristobaliteNitrogen 1723-1873 N2: H2 = 4 : 1 20 Si3N4
(sintered)
(3 -Si3N4
Carbon 1723-1873 CO : Ar = 1 :19 15 SiC(sintered)
g-SiC
3.1.4.1-2
Elements Oxygen Nitrogen CarbonAnalytical method Inert gas fusion-IR absorption
(TC436E, LECO)
Sn 4- Fe as metal bath
3500W for furnace power
Kjeldahl method
Dissolution in the mixture
of hydrofluoric acid and
chromic acidNessler’s reagent as color
indicator
Measurement of absorption
Combustion-IR absorption
(IR212, LECO)
Combustion-coulometric
titration
(VK-1C, Kokusai Electric)
Fe 4- Cu as metal bath
Calibration Fe standard sample
Si 4- Si02Ammonium chloride solution Fe standard sample
Si 4- SiC
OXY
GEN
CO
NTE
NT,
Cnl m
ass% M.P. of Si
0 3.1.4.l-i -> V * iTitSy V 3 >8t#*©E*Sg
59(/)(/)ci 10"2 E
HII-zoO
m 10"3O
£O
Temperature, 7/ K 1800;1700
M.P. of Si
o Kaiser et al.A Yatsurugi et al.O Caiiberg et al.
■ — ■ ■ * Hirata and Hoshikawaffl Huang et al.
----- — - Ottem---- - - - - Otsuka and Kozuka
Organ and Riley— — - Seidl and Muller
Present works Tu and Janke
— — - Nafe
40 ppm
20 ppm
5.4 5.6 5.8T"1 /10" K"1
0 3.1.4.1-2 '>'J
-150-
fr-r
rv£ H
„.oi
. / t.l
INTERACTION PARAMETER, 6q
o o o oco Kd Ll o
D» 0
• > □ o
▻ # □ o
OXYGEN CONTENT, Co / mass%
w oo
ri
9%4-4
m8%#
m5
30)(Z)%
r2.2
0 3.1.4.1-6 ->'J 3
NITROGEN CONTENT,/ mass%
cn ^ m
(D O
OO CP' o o o
0 ° oo o 03 CO
o OO
T'1 /10 K
0 3.1.4.1-5
OXYGEN CONTENT, CQ / mass%
• > □ o
00 CO 00 GO
> "0 oo co
CA
RB
ON
CO
NTE
NT,
Cr /
mas
s%
NIT
RO
GEN
CO
NTE
NT,
C., / m
ass%
: Kaiser and Thurmond : Yatsurugi et al.: Present work
M.P. of Si
m 3.1.4.1-7
M.P. of Si
m 3.1.4.1-8 V U 3
-153-
: Sahara et al.
: Yatsurugi et al.
: Oden and McCune
-: Hall
-: Scace and Slack
-: Ottem
M.P. of Si: Present work
r1/io4K1
I3.U1-9 v'j n
<o
-2.0 1--------------------------------------- 1--------------------------------------- 1--------------------------------------- 1----------------------------------------0 2 4 6 8
ELEMENT CONTENT, Cx / mass%H 3.1.4.1-10 ->'J 3
—154 —
20
U)
DC111I—ill
<DC<CLZOI—
%DCLU
10
0
-10
-20
-300
——----------- 1
Mn^ *•?
su
e Ni•>
B* >
we
Al i *Ca
______ _______
1
_______
*p_______i_______
10 15 20ATOMIC NUMBER
25 30
3.1.4.1-n
—155 —
: Kubaschewski and Alcock
- : JANAF
-: Knacke et al.
MR of Si
v 1700 1800 1900 20Temperature, T / K
m 3.1.4.2-1 (1)^0^*P6
$iO' (s) stablb
SiO(g)
-J -8
-35 —30 —25 “20 —15 —10Log(Po2 / atm)
m 3.1.4.2-2 Si-02 % , 1685K \Z & £ Volatility diagram
-156-
/ atm
Co / 1018 cm"3
0 1 2 3 4 5 6
1800 K
Oxygen solubility in silicon meltiequilibrated with silica
1685 K
Co / mass ppm
m 3.i.4.2-3 sio
-157-
3.1.4.3-1 Previous studies on equilibrium
distribution coefficient of oxygen in silicon.Reference No. Investigators k
1) Trumbore 0.52) Yatsurugi et al. 1.253) Mrugai et al. >14) Lin and Hill 0.255) Lin and Stavola 0.36) 0.2-0.47) Kakimoto and Ozoe 0.35-0.88) Huang et al. 0.5—0.8
Heating element
O2 gas
Alumina / reaction tube
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SITION
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0 3.1.4.3-2 500
OXYGEN CONTENT, Cy ppm
—^ ^ ro ro co coocnooi ocnocn
3. i. 5 yu3
Mil
# # B
Theoretical Estimation of Diffusion Coefficients of Impurities in Silicon Melt.
Yoshio Waseda
Institute for Advanced Materials Processing,
Tohoku University
Abstract:
The self-diffusion coefficient in pure silicon melt and diffusion coefficients of O, Al,
B and P impurities in silicon melt have been calculated on the basis of the Enskog theory
implemented with a pair-correlation function at contact between dissimilar atoms. The
activation energies for diffusion were also estimated by taking in account the temperature
dependence of packing fraction of silicon melt. Although only limited experimental data
are available for comparison, the present theoretical approach appears to work well and to
be useful for predicting diffusion coefficients of impurities in silicon melts.
(i) # C 8 c
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£ Z)s fi (2.0xl0'8~2.6xl0‘8m2/s) 8) Z & ^ B L & V> C Z ri* $8 S "C # £:»
tljS^T, SL&S±# Ds Z £d \$s ^tl^n (TJM)1/2VmU3 (Va : M&£ jo )Vfc
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*C, y'J n vitjg'f’lw-fclts 4 SHO'F&E® (o, B, PisitfAi) ©$£B®I6:©#:
ai$R3fc„ iM6i®-*WftiiiiftBS«Efflic5iT#i$nTv>afflt. *w
%Ttt, *ffid©S*l:3i,)T*iM t*SS^ tifcBSTSIMx —L &HI#s*it
# C cro=0.122nm > <7B = 0.137nm. <7p=0.190nm> aA, = 0.253nm) 111 £ tA . $ fc. #
iEH?!i C„(0) = 1.1, C1(A1) = C1(P) = 1.2. C„(B) = 0.9 iLfc. E 3.1.5-1
t£E«* Da(l©a*JEfl:SSS»:««* ©s cesi*£if. Sfc. * 3.1.5-1 12, m
,6 it Jt 12 25(2-5 onP«*±OJ»ttftx^;u^-S* i»fc*S*t?*4. J8tA5 g^osi
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%^#I2 Al : 0.2~7.0xl0'8m2/s, B : 1.8-3.3x10 8m2/s. P : 2.3-5 .lxlO'8m2/s12,T <6 <0 .
n m m * * if © s h ^ # it t s t s « t 12+# - » -r -s is * t m * s « « ®r u r t- »s.
(4) asrfsa
1) D.Mitev, M.Saito and Y.Waseda, “Theoretical Estimation of Diffusion Coefficients
of Impurities in Silicon Melt”, High Temp. Mater. Proc., 19 (2000), EP R(j f.
(5)
1) S.Chapman and T.G.Cowling, The Mathematical Theory of Non-Uniform Gases,
Cambridge University Press , London, (1970).
2) P.Protopapas and N.A.D.Parlee, High Temp. Sci., 8 (1976), 141.
3) B.J.Alder, W.E.Alley and J.H.Dymond, J.Chem. Phys., 61 (1974), 1415.
4) N.F.Carnahan and K.E.Starling, Phys. Rev., Al (1970), 1672.
5) T.L.Lebowitz, Phys. Rev., A133 (1964), 895.
6) X.Huang, K.Terashima, K.Izunome, and S.Kimura, Jpn. J. Appl. Phys., 33 (1994),
136.
-163-
7) P.D.Mitev, M.Saito and Y.Waseda, High Temp. Mater. Proc., 19 (2000), in press.
8) I.Stich, Phys. Rev., A44 (1991), 1401.
9) T.Iida and R.I.L.Guthrie, The Physical Properties of Liquid Metals, Clarendon
Press, Oxford, 1988.
10) Y.Waseda, The Structure of Non-Crystalline Materials, McGraw-Hill, New York,
1980.
11) Y.Waseda, K.T.Jacob, Y.Iguchi, T.Narushima, J. Crystal Growth, 139 (1994), 357.
12) K.H.Hellwege and O.Madelung (eds.), Numerical Data and Functional Relationship
in Science and Technology, Landolt-Bornstein Vol.17, Springer-Verlag, Berlin,
1984.
—164 —
T /K1840 1800 1760 1720 1680
— - cs
1 IT / 10 V
W 3.1.5-1 Temperature dependence of diffusion coefficients of several impurities insilicon melts, together with results for self-diffusion coefficient in pure silicon melt.
-165-
Diff
usio
n co
effic
ient
s / 10
" m s
20
HI 3.1.5-2 Comparison for self-diffusivities of liquid metals at their melting points as a function of (Tm/M)l/2Vml/3. The diamond denotes the present result for silicon melt. Points linked by a vertical line represent the range of different experimental values for a single metal.
—166 —
Act
ivat
ion E
nerg
y / eV Normal metals
Semi-metals
T / 10 K
- M 3.1.5-3 Comparison for activation energies of self-diffusivity in liquid metals at their melting points. A diamond denotes the present result for silicon melt.
-167-
3.1.5-1 Self-diffusion coefficient in pure silicon melt and impurity diffusion coefficients of O, Al, B and P in silicon melt at the melting point. Pre-exponential factors and activation energies for diffusion are also given.
Si melt - self-diffusionDs (-10V/S) at T„ D0 (*10'8m2/s) G(eV)
1.9 11.9 0.27O in Si melt
B„„(-10V/s)atTm D0 (‘10"8m2/s) G(eV)L 4.4 21.0 0.23
PP 4.1 21.5 0.24CS 4.2 21.4 0.24
Al in Si meltL 1.9 9.4 0.23
PP 1.7 9.6 0.25CS 1.7 9.5 0.25
B in Si meltL 3.7 17.9 0.23
PP 3.4 18.2 0.24CS 3.5 18.1 0.24
P in Si meltL 2.5 12.5 0.23
PP 2.3 12.8 0.25CS 2.4 12.7 0.24
—168 —
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-169-
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O $, 6.
Computer Simulations
Nobuyuki Imaishi
Inst. Advanced Material Study
Kyushu University
Abstract:
In order to realize a large-scale numerical simulation code, the members of the research
project have developed a large set of numerical codes. The global analysis code is composed of
four element simulation codes each of which treats the transport phenomena in the gas phase, the
melt phase, conductive heat transport in various solid parts and radiative heat transfer between
partially specular diffuse gray surfaces. These four element codes share the global analysis of a
Cz furnace through interactions by exchanging the values and/or fluxes at phase boundaries. At
the end of the research project, we have developed a global simulation code and confirmed its
validity for a small scale Cz furnace. This global analysis code remains some problems.
Extraordinary long CPU time requirement for the 3-D unsteady simulations of melt phase
transport phenomena makes the iterative calculation almost impossible on a conventional
computer. The alternative candidate must be the introduction of a turbulence model for melt flow.
We have developed numerical code that can adopt a turbulent model. However, we could not pick
up a reliable turbulent model applicable to such a weak turbulence accompanied by rotating flow.
Beside these macro-scale simulations, Molecular Dynamics (MD) simulation and Monte
Carlo (MC) simulation have investigated fundamental aspect of crystal growth from atomistic
viewpoints. Some members searched a scaling law to connect the results of these micro-scale
-170-
simulations and the realistic crystal growth phenomena. The MD simulations have been applied
for studying diffusion coefficients of point defect in silicon crystal and diffusion coefficient of
oxygen atoms in silicon melt.
-171
3. 2. 2
4-5 m±
( 1 ) BB
^ 3 2 7 llX^r— (Cz) ftlCj3tt-5^fXffll*lfSibS®lRyt SiO fflftf l*SlS«ft5 t
iSiai:±43-K0||%, t w 0 SiLfettJlT-ffiSt c^rxfflrtos*
©SttSffSfT ofc, IPi»!0l*tt»it}»£ST»li *>©£<R£t.
SSlctiSSS&eS#*. Ar «X0Mtt£Sft#6i#*Lfc.
e©K*6@ATA*t:-&L,. JFFSIcSSiSSrESt"-E. C i:T.
###»»**< A 0 , SiO <DMm&&mT£ 5 £ ££SL£. L, fflUftC/Rh*
miC*e%-&A,*A&Rtgf t A, x;l- h®S«lA 5'->^ES©S«J#tt$E'(bS1jr-5
c ££*!* Lfc. C©7,D^7Atti®6#6r©itIt*E*a$tiTH3>„
Numerical Analysis of Transport Phenomena in Gas Phase in a Cz furnace.
Nobuyuki Imaishi
Inst. Advanced Material Study, Kyushu University
Abstract:
A finite element code was developed for analysis of flow, convective heat transfer and mass
transfer of SiO in the gas phase in a Cz furnace. The code was run in stand-alone mode, by
assigning the boundary temperature and velocity values independently. The results suggest that a
gas guide duct significantly increase the mass transfer coefficient at the melt surface, i.e. the
increase of evaporation rate of SiO from the melt surface and reduction of oxygen concentration
in the melt. But at the same time, the increased gas flow velocity would cause an increase of drug
force to the melt surface and may change flow pattern and oxygen transport characteristics in the
-172-
melt.
The over-all effect of the gas-guide duct will be clarified by the global analysis.
This program has been successfully combined into the global analysis code.
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-173-
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(6 #i (D ^) pgCPUg-VTg= V- (*, VP,) 3-2-2-(3)
pgug V to, = V (p,Z), V to,) 3-2-2-(4)
p,=p,M,/Rr, 3-2-2-(5)
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— 174 —
W. C @ *§ $ 13 Brown S> t U tb X &$? 1C-gt U T S . 21 © © * ;H- SB _hT © SiO
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(6) ##5tK
1) Bornside, D.E., and Brown, R.A.; J.Electrochem. Soc., vol. 142, 2790 (1995)
-175-
A®= 0.02
(b)
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AVq= QJkm/s Ay= 1.5E-4 g/s
500cm/s
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-177-
tou>
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a
V0=0.286m
/s <D
i£i$ V
0=0.57m/s
<D
Evaporation coefficient [cm/s]
Stress on the melt surface [N/m2]
Stress on the rpelt surface
Evaporation coefficient [cm/s]
3.2.3 EiSfiSSKStfi
(DEB
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Numerical Simulation of Melt Convection and Heat Transfer in Czochralski Single Crystal
Growth Processes
Kenjiro SUZUKI
Department of Mechanical Engineering
Graduate School of Engineering
Kyoto University
-179-
Abstract:
Two-dimensional and three-dimensional unsteady numerical computations have been made
for the melt convection and related heat transfer in Czochralski single crystal growth processes.
Characteristics of flow and thermal fields have been analyzed for two cases of different Prandtl
number; namely Silicon Oil of Pr=4,580, which is popularly used for melt flow simulation
experiments, and Si of Pr=0.0133. Two- and three-dimensional computations with Launder-
Sharma turbulence model have also been conducted for the larger crucible size and mass transfer
of Oxygen in the melt has been discussed. In the case of Silicon Oil, the flow pattern in the melt
obtained from the three-dimensional computation was found to remain axi-symmetric, and good
agreement was confirmed to exist between present computations and experiment. In the case of Si,
the melt convection could not hold axi-symmetry and no agreement was observed between two-
dimensional computation and three-dimensional computation. It was found that the crucible
rotation could affect the melt flow to keep the axi-symmetric flow structure in laminar case,
contrary to the turbulent case where the crucible rotation may result in the asymmetric flow field.
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( 6)
1) U.Bueckle, M.Osumi, K.Suzuki and T.Yamamoto, Flow and Temperature Field in a Model
Czochralski Low-Prandtl Number Melt, The 2"1 International Symposium on Heat and Mass
Transfer.(1997)
2) J.S.Szmyd, T.Yamamoto, K.Suzuki and U.Bueckle, An Analysis of the Melt Convection for
Superconductor YBa2Cu307.x Single Crystal Growth by a Modified Czochralski Method, The
10th International Symposium on Transport Phenomena. (1997)
3) lilF*U, M.Jaszczur, 41 §15, $u A, Three-dimensional Simulation of Melt Flow and its Thermal
Characteristics in Cz Crucible, B 4-tilto^TSH!M5j£§1S$S 73 (1998)
4) J.S.Szmyd, G.Mika, M.Jaszczur and K.Suzuki, Osillatory Convection in InSb Single Crystal
Growth, Fifth International Conference on Advanced Computational Methods in Heat Transfer
(1998).
-191-
5) ill F*9 , G.Mika, $p /fc, Three-dimensional Numerical Simulation of Melt Flow and Its Thermal
Characteristics in Cz Crucible (Further Report), HI 36 HI E Wk is ^ ^ V ^ A 1 (1999)
P?5
6) K.Suzuki, T.Yamauchi, G.Mika and J.Szmyd, Unsteady Three-dimensional Melt Flow
Computation of Czochralski Single Crystal Growth of Super-Conducting Material, PCC99
AMIF European Science Foundation Workshop Phase Change with Convection : Modeling and
Validation. (1999)
( 7 )
1) H.Ozoe, K.Toh, T.Inoue, J.Crystal Growth, 110 (1991), p472.
2) S.Nakamura, M.Eguchi, T.Azami, T.Hibiya, J.Crystal Growth, 207 (1999), p55.
3) H.Tomonari, M.Iwamoto, K.Kakimoto, H.Ozoe, K.Suzuki, T.Fukuda, Chemical Engineering
Journal 71 (1998), pl91.
4) Hyung-Tae Chung, Seung-Cheol Lee, Jong-Kyu Yoon, J.Crystal Growth, 163 (1996), p249.
5) A.Lipchin, R.A.Brown, J.Crystal Growth, 205 (1999), p71.
6) T.A.Kinney ,R.A.Brown, J.Crystal Growth, 132 (1993), p551.
7) B.E.Launder, B.I.Shama, Letters in Heat and Mass Transfer 1 (1974), pl31.
8) G.H.Hoffmann, Phys. Fluids 18 (1975), p309.
9) A.A.Mohamad, R.Viskanta, Funadmentals of Mixed Convection ASME 213 (1992), p43.
10) S.Hassid, M.Porch, J.Fluid Engng 100 (1978), pl07.
-192-
Silicon oil, Monitoring point(r*,z*)=(0.0,0.7)
l/tp[l/s]
ATa [K]O ^ K) U) ^ Ui a
p
o o o o o o0 0 0*000 O O O O O H-Lt\ <1 00 \o o
□ > X □ > XMill CO CO
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3.0 x 10 7[m2/s\ a2.25 x 10-5[m2/s]
p 1.41 x 10-"[1/K] Pr 1.33 x 10~2
P 2530.0 [kg/m3] A 54.0[W7(m/O]
e 0.318 Tcold 1683.0[/<]
Rc 0.1965[m] Rs 0.078[m]
H 0.1765[m] T0 1645.0[JV]
3.2.3-2 ^ HI fro Izi/ U n
(r=Rc, or z=0) smmm# (t = Thot)
(r< Rs, z=H) #S$f4= (T = Tcold)
(r> Rs, z=H) (" A^- = cre(T4 — Tq))
t l < (E = o)
j.z.j-j y 'j j y
Case ljs [rad/s] bjc [rad/s] AT[K] grid points Free surface condition
CaseAl 0.0 0.0 2.0 55 x 55 x 56 adiabatic
CaseA2 0.0 0.0 5.0 55 x 55 x 56 adiabatic
CaseBl 0.0 0.0 2.0 55 x 55 x 56 radiative
CaseB2 1.0 0.0 2.0 55 x 55 x 56 radiative
CaseB3 2.0 0.0 2.0 55 x 55 x 56 radiative
CaseB4 0.0 -0.1 2.0 55 x 55 x 56 radiative
CaseBS 1.0 -0.1 2.0 55 x 55 x 56 radiative
CaseBO 2.0 -0.1 2.0 55 x 55 x 56 radiative
CaseB7 0.0 -0.5 2.0 55 x 55 x 56 radiative
CaseBS 1.0 -0.5 2.0 55 x 55 x 56 radiative
CaseBO 2.0 -0.5 2.0 55 x 55 x 56 radiative
CaseCl 0.0 0.0 5.0 55 x 55 x 56 radiative
CaseC2 1.0 0.0 5.0 55 x 55 x 56 radiative
CaseC3 2.0 0.0 5.0 55 x 55 x 56 radiative
CaseC4 0.0 -0.1 5.0 55 x 55 x 56 radiative
CaseC5 1.0 -0.1 5.0 55 x 55 x 56 radiative
CaseCO 2.0 -0.1 5.0 55 x 55 x 56 radiative
CaseC7 0.0 -0.5 5.0 55 x 55 x 56 radiative
CaseCS 1.0 -0.5 5.0 55 x 55 x 56 radiative
CaseCO 2.0 -0.5 5.0 55 x 55 x 56 radiative
-204-
3.2.3-4 SL
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(C = 6.6 x 105exp(2.0 x 10~4Thot)[niol/m3])
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(ns = -D|^(ns = V0k0C[mol/m2s))
xV^IW (r> Rg, z=H) S A ###{4^ (C = 0[mol/m3])
3.2.3-5 3 L Xh-D
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Numerical simulation of heat and mass transfer in CZ melt
Hiroshi Kawamura
Faculty of Science & Technology,
Science University of Tokyo
Abstract:
Numerical analyses with two dimensional boundary fitted and three dimensional cylindrical
coordinates have been performed to analyze the heat and mass transfer during the silicon crystal
growth by the Czochralski method.
The developed numerical methods were compared with two experiments and found to give
-207-
good agreements.
As a result of calculation, the crucible rotation was found to cause an internal recirculating
flow with the same rotational direction as the one caused by the buoyancy. An azimuthal
instability was captured through the simulation. The mode number was found to decrease as the
crystal Reynolds number increased. With the increase of the crucible rotation speed, the
azimuthal modal structure was observed more clearly.
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-217-
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-222-
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Numerical analyses of conductive heat transfer in the solid and radiative heat transfer between
the solid surfaces
Shigenao Maruyama* and Takao Tsukada"
* Institute of Fluid Science, Tohoku University
** Institute for Chemical Reaction Science,
Tohoku University
-223-
Abstract:
To understand accurately the transport phenomena during the silicon crystal growth by the
Czochralski (CZ) method, the computer simulation code for a global analysis of heat transfer in
the CZ furnace was developed, in which the radiative heat transfer between the surfaces that
possess both specular and/or diffuse reflectance components was taken into account, and the
effect of the radiative characteristic of crystal and melt surfaces on the silicon CZ crystal growth
process was theoretically investigated. As a result, it was found that the puling rate of the crystal
with a purely specular surfaces becomes faster than that with a diffuse surface to maintain the
crystal diameter constant for a given heater power. Also, the effect of the radiative characteristic
of the melt surface on the crystal growth strongly depends on the surface shape. In addition, in
order to improve the computational accuracy and to speed up the calculation, the simulation code
for the radiative heat transfer was modified.
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we*r, 0*itt»6»x# (bH), $62#- 595
#, pp.1091-1097, 1996.
2) S.Maruyama and T.Aihara: “Radiation Heat Transfer of Arbitrary 3-D Absorbing, Emitting and
Scattering Media and Specular and Diffuse Surfaces”, ASME Journal of Heat Transfer, Vol.119,
No.l, pp.129-136, 1997.
3) S.Maruyama and M.Higano : “Radiative Heat Transfer of Torus Plasma, in Large Helical
Device by Generalized Numerical Method REM2”, Journal of Energy Conversion and
Management, Vol.38, No.10-13, pp.1187-1195, 1997.
4) Z.Guo, S.Maruyama and T.Tsukada : “Radiative Heat Transfer in Curved Specular Surfaces in
Czochralski Crystal Growth Furnace”, Numerical Heat Transfer, Part A, Vol.32, pp.595-611,
1997.
5) S.Maruyama : “Radiative Heat Transfer in Anistoropic Scattering Media with Specular Boundary
Subjected to Collimated Irradiation”, International Journal of Heat and Mass Transfer, Vol.41,
pp.2847-2856, 1998.
6) Z.Guo, S.Maruyama and S.Togawa : “Radiative Heat Transfer in Silicon Floating Zone Furnace
with Specular Reflection on Concave Surfaces”, JSME International Journal, Vol.41, No.4,
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pp.888-894, 1998.
7) M.Higano, S.Maruyama and T.Takagi, “Numerical Analysis of Radiative Heat Flux on Large
Helical Device”, Fusion Engineering and Design, Vol.39, No.40, pp.341-346, 1998.
8) Z.Guo, S.Maruyama and S.Togawa : “Combined Heat Transfer in Floating Zone Growth of
Large Silicon Crystals With Radiation on Diffuse and Specular Surfaces”, Journal of Crystal
Growth, Vol.194, pp.321-330, 1998.
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of Heat Transfer in Si CZ Furnance With Specular and Diffuse Surfaces”, Journal of Crystal
Growth, Vol.191, pp.413-420, 1998.
10) Z.Guo, S.Maruyama, A.Komiya, “Rapid yet accurate measurement of mass diffusion coefficients
by phase shifting interferometer”, Journal of Physics. D, Applied Physics, Vol.32, pp.995-999,
1999.
11) Z.Guo, S.H.Hahn, S.Maruyama and T.Tsukada, “Global Heat Transfer Analysis in Czochralski
Silicon Furnace with Radiation on Curved Specular Surfaces”, Heat and Mass Transfer, Vol.35,
pp.185-190, 1999.
b. tgoanEiiix
12) noise, : -a> x• »
S 32 Vol. 2, PP.591-
592, 1995.
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15S\ PP.211-213, 1996.
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PP.467-470, 1996.
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s 34 0B*eiss->>#>!')A»sss:i, m 1 #, PP.i33-134, 1997.
16) M.Hihano, S.Maruyama and T.Takagi : “Numerical Analysis of Radiative Heat Flux on Large
Helical Device”, Abstract of the Fourth International Symposium on Fusion Nuclear
Technology, p.69, 1997.
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17) RlJUSS : REM2 #6# ( — 'A
”, m34m i#, pp.m-m,
1997.
18) S.H.Hahn, T.Tsukada, M.Hozawa, S.Maruyama, N.Imaishi and S.Kitagawa : “Global Analysis
of Heat Transfer in Si CZ Furnace with Specular and Diffuse Surfaces”, {b#ZC#^^ 62
m2^#, p.27, 1997.
19) S.H.Hahn, ROlSfi, : “SiCz
B Vol.24, p.13, 1997.
20) S.H.Hahn, W ^2R%E, RlilME : “CZ&C
t^Sly^^ya/”, rx-Z't-n >Ha.-
5^^ <h SCFS ’97, pp.33-39, 1997.
21) rojss, % : “LBL
^”, m 35 Avoi.i, PP.ii5-ii6, 1998.
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Floating Zone Growth of Large Silicon Crystals”, I" X —
A ——f-xT a # ##%#:## J SCFS'98, pp.95-102, 1998.
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Floating Zone Furnace with Diffuse and Specular Surfaces”, B
~%M, No.98-7, pp.44-50, 1998.
24) Z.Guo, S.Maruyama and S.Togawa : “Radiative Heat Transfer in Needle-eye Floating Zone
Crystal Growth Furnace”, Proc. 75th JSME Spring Annual Meeting, Vol.5, No.98-1, pp.98-
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25) Z.Guo and S.Maruyama : “Numerical Prediction of Radiation Transfer in a Boiler with Non-
isothermal, Non-gray Gases and Anisotropic Particles”, 35th National Heat Transfer
Symposium of Japan, Vol.2, pp.481-482, 1998.
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Furnace With Radiation on Curved Specular Surfaces”, The 75th JSME Spring Annual
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28) mii
Vol.II, pp.467-468, 1999.
29) 4"5g±, S.H.Hahn, ROjSS, #,
— S, ttJH j|S : “SiCz B Vol.26, p.18, 1999.
30) S.H.Hahn, T.Tsukada, M.Hozawa, S.Maruyama and N.Imaishi, “Analysis of Radiation Heat
Transfer in CZ Crystal Growth Process”, 1999 JSME Annual Meeting, Vol.3, No.99-1,
pp.000-000, 1999.
c. mm, mm, ##
31) miima : m36# 141 40-52, 1997.
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32) S.Maruyama and T.Aihara : "Radiation Heat Transfer of Arbitrary 3-D Participating Media
and Surfaces Using Radiation Element Method by Ray Emission Model (REM2)", Proc.
ASME/JSME Thermal Engineering Conference, Vol.3, pp.235-242, 1995.
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Device by Generalized Numerical Method REM2”, Proc. International Symposium on
Advanced Energy Conversion System and Related Technology, pp.387-394, 1995.
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and Surfaces with Non-Participating Media by a Generalized Numerical Method REM2”,
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Collimated Irradiation”, Radiative Transfer- II, Proc. International Symposium on Radiative
Transfer, Ed. M.P. Menguc, Begel House, Inc., pp.157-172, 1998.
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Anisotropically Scattering Media And Surfaces”, Heat Transfer 1998, Proc. of 11th
International Heat Transfer Conference, Vol.7, pp.457-462, 1998.
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Transfer in Si CZ Furnace with Specular and Diffuse Surfaces”, Proc. The 14th KACG Tech.
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-234-
3.2.5-1 #### j3 ^ * — 9
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Property/parameter Value
Emissivity 0.55 (Crystal, Chamber wall)0.318 (Melt)0.50 (Quartz crucible) 0.90 (Graphite crucible, Heater, Pedestal, Radiation shield, Supporter)0.20 (Puller)0.70 (Insulator)
Thermal conductivity (W/mK) 22.0 (Crystal)64.0 (Melt)2.89 (Quartz crucible)60.0 (Graphite crucible, Heater, Pedestal, Radiation shield, Supporter,)58.94 (Puller)1.31 x 103/T (Insulator)
Melting temperature of silicon (K) 1683Density of solid silicon (kg/m3) 2.3 x 103Specific heat of solid silicon (J/kgK) 1.0 x 103Heat of fusion (J/kg) 1.8x10*Electric conductivity (1/Qm) 1.2 x 105 (Graphite)Crucible inner diameter (m) 0.0720/0.3872Crystal diameter (m) 0.0350/0.1524Chamber wall temperature (K) 300
Chamber
GraphiteCrucible
QuartzCrucible
Crystal
Heater
InsulatorPedestal
Chamber
Puller
RadiationShield
Crystal / Melt
Heater
Pedestal
E 3.2.5-2 '> U 3 > CZ @
— 235 —
□ Case 1A Case 2O Case 3
Crystal length [-]
0 3.2.5-3 CZ($&## 3.5cm
0 3.2.5-53.5cm
AT = 50K
1683K
2183K
Case 3Case 2Case 1
□ Case 1A Case 2O Case 3
0 =17.657[-]Q =18.533[-] O =17.998[-]
O □O D
Crystal length [-]
0 3.2.5-4 CZ
15.24cm (Dm a)
0 3.2.5-6 PeWLt<Dm&15.24cm (Dm&)
3.2.5-2( SSSiS : 1.0 [-]
: 12.415 [-] )
Curved Flat
Case 1 0.0643 0.0614
Case 2 0.0709 0.0693
Case 3 0.0669 0.0515
-236-
0 3.2.5-7 CZiPrtS(teflS 15.24cm,
3.2.5-3 PeWit AztCKJf-f «W**J£iKffc©;S5#
Q/Qo Case 1 Case 2 Case 3a 1.000 Pe =8.363 XI0"2
Az=3.345X10'2Pe=1.666 X101 Az=5.479 X10'2
Pe =7.909X102 Az=3.077X10’2
b 0.856 Pe=1.364 XI O’1 Az=2-225X10"2
Pe=1.901 X10"' Az=3.714X10‘2
Pe =1.144X10' Az=1237X10"2
c 0.829 Pe=2.618X10"' Az =5.528 XI0"2
Pe =3.189 XI O'1 Az=7.368 X10'2
Pe =2.400X10"' Az=4.511 X10'2
a: without a shield, b, c: with a shield.
a b c
0 3.2.5-8 CZ 3.5cm <Z>Mn)
a. Case 1 b. Case 2 c.Case3
Pe 0.0304 0.0351 0.0422
-237-
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Molecular dynamics simulation of vacancy and self-interstitial in silicon under constant pressure
and temperature
Koichi KAKIMOTO
Institute of Advanced Material Study,
Kyushu University
Abstract:
Molecular dynamics simulation was carried out to estimate diffusion constants and
mechanism of point defects such as a single vacancy and a self-interstitial atom under hydrostatic
pressure. Stillinger-Weber potential was used as a model potential, which is widely accepted for
modeling of silicon crystals and melts. We obtained the following results on a self-interstitial
atom from the calculation. 1) Diffusion constants of self-interstitial are almost independent of
pressure within a range from ?50 to +50 k bar. 2) A self-interstitial atom diffuses with a
-238-
formation of dumbbell structure, which is aligned in [110] direction. For single vacancy, the
followings were clarified. 1) Diffusion constants of vacancy are also independent of pressure
within a range from ?40 to +40 k bar. 2) A vacancy diffuses with a switching mechanism to
nearest neighbor atoms in lattice site.
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(6)
1) K.Kakimoto, T.Umehara and H.Ozoe, ’’Molecular dynamics analysis on diffusion of point
defects” J. Crystal Growth, in print.
2) K.Kakimoto, T.Umehara and H.Ozoe, ’’Molecular dynamics analysis of point defects in silicon
near solid-liquid interface”, J. Vacuum Science, in print.
-243-
(7)
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5) H.Bracht, N.A.Stolwijk and H.Mehrer: Semicond. Silicon, ECS, Pennington N. J., p.593
(1994).
6) T.Y.Tan and U.Goesele, Appl. Phys. A37 (1985), 1.
7) H.J.Gossmann, C.R.Rafferty and H.S.Luftmann, Appl. Phys. Lett., 63 (1993), 639.
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Scientific, p.169. (1985)
10) R.Habu, A.Tomiura and H.Harada, Semicond. Silicon, ECS, Pennington N. J., p.635 (1994).
11) B.Leroy, J. Appl. Phys., 50 (1979), 7996.
12) C.Boit, J. Crystal Growth, 53 (1981), 563.
13) T.Abe, K.Kikuchi, S.Shirai and S.Muraoka, Semiconductor Silicon 1981, ed. H.R.Huff,
R.K.Kriegler and Y.Takeishi (Electrochem. Soc., Pennnington, 1981) p.54
14) H.Zimmermann and H.Ryssel, Appl. Phys. A55 (1992), 121.
15) K.Taniguti, D.A.Antoniadis and Y.Matsushita, Apll. Phys. Lett., 42 (1983), 961.
16) M.Yoshida and K.Saito, Jpn. J. Appl. Phys., 6 (1967), 573.
17) K.Tempellhoff, Appl. Phys. Lett., 42 (1988), 961.
18) C.W.Gear, “Numerical initial value problems in ordinary differential equations”, Englewood
Cliffs, Prentice Hall, 1971.
19) F.H.Stillinger and T.A.Weber, Phys. Rev., B31 (1985), 5262.
-244-
Diff
usio
n coef
ficie
nt
Interstitial
Vacancy43 (1/2,1/2,1/2)
0 3.2.6-1 Initial positions of a vacancy and an interstitial atom in silicon crystal. The initial positions of the defects are indicated by reduced units.
Vacancy
InterstitialPerfect lattice
Time [sec]
0 3.2.6-2 Mean-square displacements of silicon atoms as a function of time for cases of vacancy, interstitial and perfect crystal.
-245 —
--------PJ.Ungar '94 ---------R.Habu '94..........RA.Brown '94 —X— B.Leroy '79
A H.Bracht '94 —A— C.Boit '90—T.Y.Tan '85 □ TAbe '86—h— HJ.Gossmann '93 —■— H.Zimmermann '92 —♦— G.B.Bronner '87 —V— K.Taniguti '83
A K.Wada '81
0 3.2.6-5 Arrhenius plot of diffusion constants of an interstitial atom.
-------- R.Habu 94 ...........R.A.Browa '94--A--K.Wada '87 —•—T.Y.Tam '85
H.Zimmeraiana '89 —■—H.Ziaimeruiaun '92—ffl—M.Yoshida '67 -------- PJ.Ungar '94—B— K.Tempelhoff '82
T [K]1250 1000
E elect P attern
11X10
1/T [K~l]
0 3.2.6-6 Arrhenius plot of diffusion constants of a vacancy.
-247-
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Molecular dynamic simulation of an oxygen atom in silicon crystal
Koichi KAKIMOTO
Institute of Advanced Material Study,
Kyushu University
Abstract:
Molecular dynamic simulation of an oxygen atom in silicon crystal and the melt was carried
out to obtain diffusion constants of oxygen in the melt. The simulation using mixed potential in
the melt in which an oxygen atom and 216 silicon atoms were taken into account has been carried
out. Vibration frequencies of oxygen and vacancy-oxygen (V-O) pair in the crystal have been
calculated. Calculated frequency of oxygen and V-O pair were 1000 and 800 cm-1, respectively,
while experimental results which were obtained from Fourier transform spectra of infrared
absorption (FTIR) are 1100 and 830 cm-1, respectively. Oxygen diffusion constant was obtained
-248-
in elevated temperature of 1700 K. Calculated diffusion constant of oxygen in the melt was
2x10-4 cm2/sec.
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(6) tf&ffiiHX
1) K.Kakimoto, Shin Kikuchi and H.Ozoe, ’’Molecular dynamics simulation of oxygen in silicon
melt”, J. Crystal Growth, 198/199 (1999) 114.
(7) ##%m
1) Z.Jiang and R.A.Brown, Chemical Engineering Science, 49 2991 (1994).
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Numerical simulation of drop behavior in an electromagnetic levitator
Takao Tsukada
Institute for Chemical Reaction Science,
Tohoku University
Abstract:
A mathematical model, which can predict the equilibrium shape of a molten silicon drop and
additionally the nonlinear drop oscillations, has been developed for the improvement and
determination of the optimal processing conditions in an electromagnetic levitation device
developed in Japan to accurately measure the thermophysical properties such as surface tension
and density of silicon melt. As a result, the effects of the electric current and frequency in the RF
— 256 —
coil on the equilibrium shape and the average temperature of the drop were clarified numerically,
and it was demonstrated that the present model is useful for determination of the operating
condition to make the shape of the molten drop spherical. Also, the mathematical model for the
drop oscillations revealed that the frequency decreases as the ratio of the electric current ratio
(heating coil/levitation coil) increases.
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(7)
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8) A.Gagnoud and J.F.Brancher, IEEE Trans. Mag., 1985, vol.21, pp.2424-2427
9) O.A.Basaran, J.Fluid Mech., 1992, vol.241, pp.169-198
— 266 —
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Properties or parameters Unit ValueEmissivity - 03
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—274 —
Crystal and Interface Analysis (molecular dynamics simulation)
T. Motooka
Dept, of Materials Science and Engineering,
Kyushu University
Abstract:
We have investigated growth mechanisms and defect formation processes during
crystallization from melted Si and solid phase epitaxy (SPE) by using large-scale molecular
dynamics simulations combined with the Tersoff potential. Structural changes and energy levels
in impurity (B, P, AJ-doped Si have been also analyzed by using first-principle molecular orbital
calculations based on a cluster model. The main results are as follows: (i) Liquid Si is, in a short
time-scale, composed of the j3 -S„ and simple hexagonal structures which may give rise to an
anomaly in the density near the melting point; (ii) The solid/liquid Si interface is a rough surface
composed of {111} facets in the [001] pulling, while it is essentially a flat (111) surface in the
[111] pulling; (iii) The melt growth in the [001] direction occurs by attaching Si atoms in melt at
the kink sites associated with the {111} facets formed at the solid/liquid Si interface, while in the
[111] direction double-layered two-dimensional nucleation is first created and then followed by
double-step layer-by-layer growth; (iv) In the case of SPE, layer-by-layer crystallization along
the (111) plane can be seen at higher temperatures, while at lower temperatures layer-by-layer
crystallization occurs along the (001) plane; (v) Defect formation can be initiated by 5-membered
rings created at the interfaces which give rise to interstitials and {111} stacking faults in the melt
and SPE growth, respectively; (vi) The Si band structure and impurity levels can be well
reproduced by cluster model calculations including 38 Si atoms; (vii) The uniaxial strain induced
near the solid/liquid interface becomes smaller than equilibrium thermal expansion and it
gradually changes to compressive as the temperature gradient increases.
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(6)
a.
1) "Uniaxial strain observed in solid/liquid interface during crystal growth from melted Si: A
molecular dynamics study" by Ken Nishihira, Shinji Munetoh, and Teruaki Motooka 8-th Int.
Conf. on Defects-Recognition, Imaging and Physics in Semiconductors, Narita, Japan,
September 15-18, 1999
2) "Molecular dynamics simulations of solid phase epitaxy of Si: Growth mechanism and defect
formation" by T.Motooka and K.Nisihira, S.Munetoh, K.Moriguchi, and A.Shintani Materials
Reasearch Society meeting, Boston, USA, November 29-December 5, 1999
— 281 —
b . !ro 5C jx
1) M.Ishimaru and T.Motooka:"Molecular dynamics simulations of crystal growth from melted
silicon: defect formation processes" Mat. Res. Symp. Proc. Vol. 538, 247-250 (1999).
2) Ken Nishihira, Shinji Munetoh, and Teruaki Motooka:"Uniaxial Strain Observed in
Solid/Liquid Interface during Crystal Growth from Melted Si: A Molecular Dynamics Study" J.
Crystal Growth, in press (2000)
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simulations of solid phase epitaxy of Si: Growth mechanisms" Phys. Rev. B, in press (2000)
4) T.Motooka, K.Nisihira, S.Munetoh, K.Moriguchi, and A.Shintani: "Molecular dynamics
simulations of solid phase epitaxy of Si: Growth mechanism and defect formation" Mat. Res.
Symp. Proc. , in press (2000)
( 7) ####
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-282-
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Global Simulation Code
Nobuyuki Imaishi Takao Tsukada Shigenao Maruyama Hiroshi Kawamura Kenjiro Suzuki
Inst. Advanced Material Study, KyushuUniv. Res. Inst. Chem. Reaction Sci., Tohoku Univ. Res. Inst. Fluid Science, Tohoku Univ.Fac. of Sci&Tech, Science Univ. of Tokyo Graduate School of Engineering, Kyoto Univ.
Abstract:
A large scale numerical code was developed for a global analysis of silicon Cz furnace to
understand transport phenomena in details. The code is composed of four major element codes
each of which analyzes transport phenomena in the gas, melt and solid phases and the radiative
heat transfer between partly specular diffuse gray surfaces. Each code has been developed by the
-299-
research project members, separately. A main program was developed to manage the exchanges of
velocity, temperature and concentration values as well as the momentum, heat and mass fluxes on
the phase boundaries in order to proceed the iterative convergence process for a pseudo steady
state. After the 5 year long project, a global simulation code has been developed. The code is able
to calculate successfully the transport phenomena and melt-crystal interface shape in a small Cz
furnace.
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1) D.E.Bornside and R.A.Brown, J.Electrochem. Soc., vol. 142,2790(1995)
2) T.Carlberg, J.Electrochem. Soc., vol.133, 1940(1986)
3) M.Watanabe, K.W.Yi, T.Hibiya and K.Kakimoto, Progress in Crystal Growth and
Characterization of Materials (1999) 215-238
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WM&a**Aaar* A&a
Experimental validation of the global simulation code
Nobuyuki Imaishi
Institute of Advanced Material Study
Kyushu University
Abstract:
The validity of the developed global simulation code must be verified by comparing the
numerical results with the corresponding experimental results. Two sets of experiments have been
conducted at Shinshu Universit and NEC Corporation, respectively. The results of Shinshu
University confirmed the simulation result that a funnel shaped gas guide installed in the furnace,
between the crucible and the crystal, would provide a reduction of heater power and provide
easier temperature control. Further experiments will be provided by Shinshu University after
their installation of a power meter. A X-ray radiographic observation of the crystal-melt interface
was conducted at the Fundamental Research Laboratory of NEC Corporation. The crystal-melt
interface shape was reasonablly reproduced by the global analysis code. The global simulation
code predicted the oxygen concentration in the grown crystal. The predicted result fell very close
to the NEC’s experimental result that was reported elsewhere and the growth conditions were
slightly different from the present ones. These experimental results suggest the validity of the
developed global simulation code.
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Crystal periphery Crucible periphery
radius (cm)
radius (cm)
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Model Experiment of Cz Furnace
Kimihisa Itoh
Department of Science & technology,
Waseda University
Abstract:
The precise experimental data are important to develop and verify a computer simulation
program of the unsteady convection flow of molten silicon in Cz furnace. The following
experiments were conducted to establish the database of the melt flow in a cold model using
-321-
; * *=#**#*
water, silicone oil and Wood's metal as model materials.
(1) Temperature profile measurement in the Cz melt: The temperatures in Wood's metal which is a
low Pr melt as silicon were continuously measured using telemeter system. The obtained results
were arranged in a visible form and stored as a database.
(2) Velocity profile measurement in the Cz melt: The larger single crystal was employed and the
experimental furnace was modified to rotate at very low rate. This modification made the model
experiments more close to the actual operating conditions of Cz furnace. Time change of melt
flow was measured by LDV and the flow profile was measured by PIV. The obtained results were
arranged and stored as a database.
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-331-
APPENDIX-1 • SWJSt/r (t >x* 11/ n 80
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-334-
Analysis of Crystalline and Interface (Monte Carlo Method)
Toshiharu Irisawa
Computer Center, Gakushuin University
Abstract:
Monte Carlo simulation of the melt growth was performed to study the interface process. At
first, we investigated in detail the process of the solid's holding the melt. This process affects the
introducing the point defect in a crystal. We find that the point defect density in the case of the
slow growth rate is less than that in the equilibrium states, in spite of the usual knowledge that
the defect density is the increase function of the growth rate. Next, we examined the taking-in
process of the impurities for the melt growth. In the condition that the interaction of the impurity
atoms can be ignored, the impurity atoms concentration in the melt and the growth rate become
steady state. However, in the condition that the concentration of the impurity atoms becomes
super saturate in melt, the impurities nucleate the front of the interface in melt, and it is included
in the solid. Then, we fined that the concentration of the impurity atoms in the melt and the
growth rate cannot become the steady state. In the case of the diamond lattice, we found that
(111) surface is flat in the atomic level but the (100) surface is a rough surface, and the (110)
surface is surrounded by the (111) surface when the effective bond energy (|)eff =3kT. The
equilibrium and effective distribution coefficient can be evaluated by simulation. When the
growth rate is small, it was found that the impurity concentration, which is contained in the solid,
can be used the equilibrium concentration. Also, in the case where it is easy for impurities to be
taken in, and the growth rate is small, it was found that the diffusion of impurities becomes the
rate determining process but when the growth rate is large, the heat diffusion becomes the rate
determining process.
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