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We approve the thesis of Robert David Carneim.Date of Signature
____________________________________ ___________________Gary L. MessingProfessor of Ceramic Science and EngineeringThesis AdvisorChair of Committee
____________________________________ ___________________James H. AdairAssociate Professor of Materials Science and Engineering
____________________________________ ___________________Ian R. HarrisonProfessor of Polymer Science
____________________________________ ___________________John R. HellmannAssociate Professor of Ceramic Science and Engineering
____________________________________ ___________________Virendra M. PuriProfessor of Agricultural Engineering
____________________________________ ___________________Richard E. TresslerProfessor of Materials Science and EngineeringHead of the Department of Materials Science and Engineering
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Abstract
A model granulated ceramic powder system was studied with systematically varied
binder content and binder plasticity (binder glass transition temperature, Tg). A submicron
α-alumina was used as the inorganic component and poly(vinyl alcohol)–4 wt% glycerol
was the base binder system. Four compositions were spray dried containing ~2, 3, 4 and
5 wt% binder (dry weight basis alumina). The resulting powders were classified and the 75–
150 µm granule size range powders prepared for testing. These powders were conditioned
at five different relative humidities to adjust binder Tg to five different values between –
32°C and +35°C.
All twenty compositions were tested in uniaxial compaction in a 6.34 mm diameter
cylindrical steel die to stresses from ~6 MPa to ~175 MPa. Green strengths of the samples
produced were measured using the diametral compression test. Compaction curves were
constructed and springback on ejection was measured. A selection of similar samples was
prepared and dimensional changes after compaction were measured as a function of time. It
was found that the compositions with low Tg during compaction resulted in the highest
achievable densities and green strengths. However, green strength increased and achievable
green density decreased with increasing binder content. Dimensional changes on ejection
were found to be dominated by the instantaneous springback in the axial direction (~5–8%).
Radial springback was generally less than 1% and the total dimensional change due to time-
dependent relaxation was generally less than 0.5%.
It was observed that compaction behavior was affected by sample size. A technique
was developed which determines this effect. By measuring two compaction curves of a
powder of different sample size, it was possible to calculate the force opposing compaction
due to friction at the die wall. This allowed the calculation of the intrinsic compaction curve
of the material, i.e., its compaction behavior in a frictionless die. With these two parameters
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known it became possible to predict compaction curves of the powder for different sample
sizes. Compaction curves calculated in this manner predicted experimentally determined
compaction curves with correlation coefficients greater than 0.99.
To aid in the characterization of individual granules and their interaction during com-
paction, an analysis was developed that calculates granule strength and intergranular bond
strength during compaction and the free granule strength. In a series of pellets pressed to a
wide range of pressures, granule deformation and adhesion varied greatly between samples.
The strengths of these samples were measured by diametral compression and the fracture
surfaces were analyzed to determine the relative amounts of intergranular and intragranular
fracture. A quadratic curve was found to describe the relationship between the overall green
strength of the sample and the area fraction of intergranular fracture. By applying knowl-
edge of the physical process at the 0, 50 and 100% intergranular fracture points along this
curve, this curve was deconvoluted to the unique pair of linear functions that track the
intergranular bond strength and the intragranular strength throughout the compaction cycle.
The 100% intergranular fracture point corresponds to little or no consolidation of the pow-
der; therefore, the value of the determined intragranular strength line is a measure of the
free granule strength. The free granule strength measured by this technique results in values
much lower than the often-reported granule yield point measurement due to the difference
in loading of the granules.
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Table Contents
Page
List of Tables ................................................................................ viiList of Figures .............................................................................. viiiAcknowledgments ........................................................................ xiiChapter 1: Introduction ................................................................... 1
Powder Production ............................................................................................... 16Powder Preparation ............................................................................................... 17Powder and Binder Characterization .................................................................... 17
Results and Discussion ............................................................................17Summary..................................................................................................21
Chapter 3: Loading and Unloading Response .............................. 22Introduction .............................................................................................22
Experimental Procedure ..........................................................................25Compaction and Density ...................................................................................... 25Viscoelastic Relaxation......................................................................................... 25
Results and Discussion ............................................................................26Compaction and Density ...................................................................................... 26Instantaneous Springback ..................................................................................... 39Time-Dependent Relaxation ................................................................................. 45
Summary and Conclusion........................................................................48
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Table Contents (cont.)
Page
Chapter 4: A Model for Compaction Curve Prediction ................ 50Introduction .............................................................................................50
Background ........................................................................................................... 50Overview of Principle ........................................................................................... 51
Results and Discussion ............................................................................62Evaluation of k·µ................................................................................................... 62Compaction Curve Prediction .............................................................................. 63
Summary and Conclusion........................................................................64Chapter 5: Green Strength and Granule Strength Modeling ........ 67
Summary and Conclusion........................................................................77Chapter 6: Conclusion .................................................................. 79
Summary and Conclusions ......................................................................79Recommendations for Future Work.........................................................81
Referenced Works ..................................................................................100General References ................................................................................104
Vita Robert D. Carneim .............................................................. 111
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List of Tables
Page
Table 2.1 ........................................................................................................................... 21Total Binder Contents, Glass Transition Temperatures (Tg) and Granule Densi-ties of the Spray Dried Powders
Table 3.2 ........................................................................................................................... 42Stage IV Compaction Onset
Table 5.1 ........................................................................................................................... 77Granule Yield Points and Granule Strengths of Tg = 6°C (43 %RH) Samples
viii
List of Figures
Page
Figure 1.1 ............................................................................................................................ 2Schematic representation of uniaxial compaction. Region I: granule rearrange-ment, II: granule elastic deformation, III: extensive plastic deformation and/orfracture of granules, IV: particle rearrangement within compact, V: instantaneousspringback and time-dependent relaxation on ejection, VI: ultimate green partdensity.
Figure 2.1 .......................................................................................................................... 18Micrograph of 75–150 µm diameter spray dried powder containing ~4 wt%binder; other compositions used have similar appearance.
Figure 2.2 .......................................................................................................................... 18Equilibrium moisture content (EMC) of the binder as measured bythermogravimetric analysis (TGA).
Figure 2.3 .......................................................................................................................... 19Density of the binder in the relative humidity range used. Error bars indicate95% confidence intervals based on 3 measurements.
Figure 2.4 .......................................................................................................................... 20Glass transition temperature (Tg) as measured by differential scanning calorim-etry (DSC, 20°C·min–1). The inflection of the step transition is reported.
Figure 3.1a, b .................................................................................................................... 27Measured compaction curve and ejected densities of Tg = 35°C, 2 (a) and3 (b) wt% NBC system in a 6.34 mm diameter die.
Figure 3.1c, d .................................................................................................................... 28Measured compaction curve and ejected densities of Tg = 35°C, 4 (c) and5 (d) wt% NBC system in a 6.34 mm diameter die.
Figure 3.2a, b .................................................................................................................... 29Measured compaction curve and ejected densities of Tg = 18°C, 2 (a) and3 (b) wt% NBC system in a 6.34 mm diameter die.
Figure 3.2c, d .................................................................................................................... 30Measured compaction curve and ejected densities of Tg = 18°C, 4 (c) and5 (d) wt% NBC system in a 6.34 mm diameter die.
ix
Figure 3.3a, b .................................................................................................................... 31Measured compaction curve and ejected densities of Tg = 6°C, 2 (a) and 3 (b) wt%NBC system in a 6.34 mm diameter die.
Figure 3.3c, d .................................................................................................................... 32Measured compaction curve and ejected densities of Tg = 6°C, 4 (c) and 5 (d) wt%NBC system in a 6.34 mm diameter die.
Figure 3.4a, b .................................................................................................................... 33Measured compaction curve and ejected densities of Tg = –25°C, 2 (a) and3 (b) wt% NBC system in a 6.34 mm diameter die.
Figure 3.4c, d .................................................................................................................... 34Measured compaction curve and ejected densities of Tg = –25°C, 4 (c) and5 (d) wt% NBC system in a 6.34 mm diameter die.
Figure 3.5a, b .................................................................................................................... 35Measured compaction curve and ejected densities of Tg = –32°C, 2 (a) and3 (b) wt% NBC system in a 6.34 mm diameter die.
Figure 3.5c, d .................................................................................................................... 36Measured compaction curve and ejected densities of Tg = –32°C, 4 (c) and5 (d) wt% NBC system in a 6.34 mm diameter die.
Figure 3.6a, b .................................................................................................................... 37Measured compaction curve and ejected densities of Tg = 35 (a) and 6 (b)°C,3 wt% NBC system in a 12.6 mm diameter die.
Figure 3.6c ........................................................................................................................ 38Measured compaction curve and ejected densities of Tg = –32°C, 3 wt% NBCsystem in a 12.6 mm diameter die.
Figure 3.7 .......................................................................................................................... 39Achievable pellet density: 6.34 mm diameter samples pressed to ~175 MPa.
Figure 3.8 .......................................................................................................................... 39Stress required to achieve 52.9% relative alumina density in a 6.34 mm diam-eter die as a function of binder content and binder Tg. (Tg = 35°C, 5% NBC datapoint was extrapolated from available compaction curve data up to ~175 MPa.)
Figure 3.9a ........................................................................................................................ 41Degree of polymer saturation as a function of compact density, binder Tg duringcompaction and compaction stress.
x
Figure 3.9b ........................................................................................................................ 41Total solids content in granules and compacts as a function of compact density,binder Tg during compaction and compaction stress.
Figure 3.10a ...................................................................................................................... 43Instantaneous volumetric springback on ejection vs. binder Tg and compactionstress for samples pressed in a 6.34 mm diameter die to an aspect ratio of ~0.5.
Figure 3.10b ...................................................................................................................... 43Instantaneous volumetric springback on ejection vs. binder Tg and compactionstress for samples pressed in a 12.6 mm diameter die to an aspect ratio of ~0.4.
Figure 3.11a ...................................................................................................................... 44Example illustrating the anisotropy of instantaneous springback on ejection vs.compaction stress for 3 % NBC, Tg = 6°C samples pressed in a 6.34 mm diam-eter die to an aspect ratio of ~0.5.
Figure 3.11b ...................................................................................................................... 44Example illustrating the anisotropy of instantaneous springback on ejection vs.compaction stress for 3 % NBC, Tg = 6°C samples pressed in a 12.6 mm diam-eter die to an aspect ratio of ~0.5.
Figure 3.12 ........................................................................................................................ 45Example raw data and curve fit of the time-dependent strain recovery after ejec-tion. Example is of Tg = 6°C, 3% NBC system, 6.34 mm diameter pelletcompacted at ~175 MPa, relaxation in the axial direction.
Figure 3.13a ...................................................................................................................... 46The total, fractional, recoverable time-dependent strain as a function of binderTg for various samples as indicated in the legend. (The “A” parameter in thefunction: h = 1-A·exp(-t⁄τ)).
Figure 3.13b ...................................................................................................................... 46The characteristic relaxation time as a function of binder Tg for various samplesas indicated in the legend. (The “τ” parameter in the function: h = 1-A·exp(-t⁄τ)).
Figure 4.1 .......................................................................................................................... 59Measured compaction curves for Tg = –25°C, 5 wt% NBC samples. The aspectratio reported is the final aspect ratio of the pressed pellet. Note that this and allother compaction curve figures in this chapter plot the compaction stress as afunction of sample density.
Figure 4.4 .......................................................................................................................... 61The two original, measured, compaction curves and the calculated intrinsic com-paction curve for the Tg = –25°C, 5 wt% NBC system.
Figure 4.5 .......................................................................................................................... 63The black curves illustrate the predictive ability of this analysis for the Tg = -25°C,5 wt% NBC system. The solid line is the calculated compaction curve; the dashedline is the experimentally measured compaction curve for the same conditions.
Figure 4.6 .......................................................................................................................... 64The normalized compaction curve (single curve in magenta) and predicted (un-broken curves) and corresponding measured (dashed curves) compaction curvesfor the Tg = 6°C, 3 wt% NBC system.
Figure 5.1 .......................................................................................................................... 71High magnification micrograph of a pellet fracture surface clearly showing thedifference between intergranular fracture and intragranular fracture.
Figure 5.2 .......................................................................................................................... 72a) Representative pellet fracture surface micrograph showing the two differentfracture modes. b) Analysis of the fracture surface showing intergranular frac-ture (white) and intragranular fracture (black).
Figure 5.3 .......................................................................................................................... 73Pellet green strengths at 43% RH (Tg = 6°C): a) compacted to ~175 MPa andb) compacted to 52.9 % relative alumina density.
Figure 5.4 .......................................................................................................................... 74Intergranular fracture vs. pellet green strength (R2 ≥ 0.95).
Figure 5.5a ........................................................................................................................ 75Green strength deconvolution for the 2 wt% NBC, Tg = 6°C samples.
Figure 5.5b ........................................................................................................................ 75Green strength deconvolution for the 3 wt% NBC, Tg = 6°C samples.
Figure 5.5c ........................................................................................................................ 76Green strength deconvolution for the 4 wt% NBC, Tg = 6°C samples.
Figure 5.5d ........................................................................................................................ 76Green strength deconvolution for the 5 wt% NBC, Tg = 6°C samples.
xii
Acknowledgments
I can not possibly express in words how I feel about all the people who have affected
my life and, consequently, helped me reach this point. I would, however, like to single out a
few and simply thank them. My amazing wife, Tammy, who, for me, has transformed exist-
ence into Life. My parents, Sergei and Erika, for twenty-nine years (and counting) of love,
support and encouragement. My advisor, Gary Messing, for having given me this opportu-
nity and helping me develop the skills required to earn this degree and succeed after leaving
Dear Old State. And the universe for going to all the bother of existing.
Of course, there are many others whose presence and friendship helped me retain some
semblance of a sane, balanced life. To name a few: Leah Witzig, Paul & Erin, Eric & Chris,
Big Ed, Mike, 10100101101111110011111001011110010 & Maureen, Matt,
C. Scott & Jana, Ender & Bahar, Scott, Mitch, R.P. & Jen, Lisa, and everyone else in our
research group, past and present.
I would also like to thank The Particulate Materials Center (an NSF I/UCRC) for fund-
ing this research and my industrial mentor, Walt Shaffer of Spang. I am grateful to Spang
for the use of their spray drying facilities to prepare the powders used in this work. Finally,
thanks go out to the faculty, staff and students that I had the pleasure of working with at
Penn State; I was fortunate in that it seemed they all conspired to make my time here,
overall, a positive experience.
xiii
“Even if there is only one possible unified theory, it is just a set of rules and equations.
What is it that breathes fire into the equations and makes a universe for them to describe?
The usual approach of science of constructing a mathematical model cannot answer the
questions of why there should be a universe for the model to describe. Why does the
universe go to all the bother of existing? Is the unified theory so compelling that it brings
about its own existence? Or does it need a creator, and, if so, does he have any other
effect on the universe? And who created him?”
—Stephen W. Hawking, (A Brief History of Time, 1988)
1
Chapter 1:
Introduction
Background
Die compaction of ceramic powders is a widely used forming process which is auto-
mated to rapidly produce parts of low to moderate geometric complexity. Dry pressing
involves the uniaxial compaction of spray dried granules consisting of ceramic particles
bound by an organic binder. A schematic compaction curve for this process is shown in
figure 1.1. During compaction, part density increases due to granule rearrangement and
deformation, and particle rearrangement. Upon releasing the compaction pressure the part
expands, relieving internal stresses. The expansion occurs as both an elastic (instantaneous)
springback, due to the energy stored in the structure, and a viscoelastic (time-dependent)
relaxation, due to the viscoelastic character of the organic binder.
For the application of dry pressing, submicron powders are often intentionally granu-
lated to improve flow properties. This is necessary since submicron particles tend to
spontaneously form large, irregular, low-density aggregates as a result of the dominance of
surface forces (e.g., van der Waals) over inertial forces (i.e., particle weight). The presence
of such aggregates results in poor powder flow and inhomogeneous and inconsistent die
filling. Organic binders are added to impart strength to the granules and green part, and to
enhance compaction. A popular and effective granulation method, which also facilitates the
addition of a binder phase, is spray drying. In this process, the powder is dispersed in a
liquid medium with a chemical dispersant and a binder. This slurry is atomized in the spray
drier and exposed to a flow of heated air. The liquid evaporates and is carried away leaving
relatively dense, spherical granules on the order of tens to hundreds of micrometers in di-
ameter. As a result of the increase in scale of the “particles” comprising the powder, inertial
2
forces dominate the interaction between the now-granules and the powder flows easily and
consistently.
A raw submicron ceramic powder, if placed in uniaxial compression, is difficult to
efficiently compact. Aside from the problems associated with poor flow and die-filling (which
are largely alleviated by the scale increasing effect of granulation), difficulties arise from
friction between the rigid and potentially rough and irregular particles.1 During compac-
tion, particles can lock together forming rigid spans which dramatically impede
consolidation.1–3 The incorporation of an organic binder phase between particles minimizes
this problem. The binder is, effectively, an interparticle lubricant.1,4 With an appropriate
binder selection, the force required to rearrange particles by shear deformation of the
interparticular binder is much less than the force required to overcome the friction between
particles in direct contact.
Given the preceding discussion, it becomes apparent that the compaction behavior of a
binder-containing granulated powder will be dominated by the type and amount of binder
I II
III
IV V VI
Time
Com
pact
Rel
ativ
e D
ensi
ty
Applied U
niaxialC
ompressive Stress
0
Figure 1.1: Schematic representation of uniaxial compaction. Region I: granule rearrangement,
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Vita
Robert D. Carneim
Education
Experience
Publications
Presentations
Bachelor of Science, Ceramic Engineering – January 1995New York State College of Ceramics at Alfred University, Alfred, NY
Doctor of Philosophy, Material Science (Ceramics) – December 2000The Pennsylvania State University, University Park, PA
March 1999–July 2000Computer Lab Administrator – Particulate Materials Center, Materials ResearchLaboratory, The Pennsylvania State University, University Park, PA
August 1995–September 2000Graduate Research Assistant – Particulate Materials Center, Materials ResearchLaboratory, The Pennsylvania State University, University Park, PA
January 1995–August 1995Research Assistant – Associated Western Universities Fellowship at Pacific NorthwestNational Laboratory, Battelle Memorial Institute, Richland, WA
1990–1994Computer Lab Assistant – New York State College of Ceramics at Alfred University,Alfred, NY
R.D. Carneim, G.L. Messing, “Response of Granular Powders to Uniaxial Loading andUnloading,” in press, Powder Technology (2000).
R.D. Carneim, G.L. Messing, “Characterization of Agglomerate Mechanical Properties,”pp. 377–79 in 1999 Fine Powder Processing International Conference Proceedings(Proceedings of Fine Powder Processing ’99, University Park, PA, September 20th–22nd,1999), Edited by V.M. Puri, J.H. Adair, C.L. Knobloch, C.C. Huang, The PennsylvaniaState University, University Park, PA, 2000.
R.D. Carneim, G.L. Messing, “Compaction Curve Normallization With Respect toSample Size,” Presented at the 102nd Annual Meeting of the American Ceramic Society,St. Louis, MO, May 2st, 2000.
R.D. Carneim, G.L. Messing, “Granule Characterization During Uniaxial Compaction,”Presented at the 102nd Annual Meeting of the American Ceramic Society, St. Louis, MO,May 1st, 2000.
R.D. Carneim, G.L. Messing, “Processing Effects on the Sintered Properties of AluminaPellets,” Poster Presentation at Sintering ’99, University Park, PA, November 1st–3rd, 1999.
R.D. Carneim, G.L. Messing, “Characterization of Agglomerate Properties,” Presented atFine Powder Processing ’99, University Park, PA, September 21st, 1999.
R.D. Carneim, G.L. Messing, “Dimensional Stability of Dry–Pressed, Organic Binder–Containing Ceramic Powders,” Presented at the 101st Annual Meeting of the AmericanCeramic Society, Indianapolis, IN, April 26th, 1999.
R.D. Carneim, G.L. Messing, V.M. Puri, “Organic Additive Effects on the Compaction ofGranulated Ceramic Powders,” Presented at the 100th Annual Meeting of The AmericanCeramic Society, Cincinnati, OH, May 6th, 1998.