- 1. K.S. Harishanand, H. Nagabhushana, B.M. Nagabhushana,
Parimesh Panda, A H Adarsha, M.M. Benal, N Raghavendra, K R Vishnu
Mahesh / International Journal of Engineering Research and
Applications (IJERA) ISSN: 2248-9622 www.ijera.comVol. 3, Issue 1,
January -February 2013, pp.1569-1576 Corrosion, Mechanical and Wear
Properties of nano-ZnO doped AluminiumK.S. Harishanand1, H.
Nagabhushana2, B.M. Nagabhushana3, ParimeshPanda 1, A H Adarsha1,
M.M. Benal4, N Raghavendra1, K R Vishnu Mahesh5 1 (Department of
Mechanical Engineering, R.V. College of Engineering,
Bengaluru-560059, India)2(Department of Physics, Tumkur University,
Tumkur-572103, India)3(Department of Chemistry, M.S. Ramaiah
Institute of Technology, Bengaluru-560054, India) 4 (Department of
Mechanical Engineering, Govt. Engineering College,
Kushalnagar-571234, India) 5 (Department of Chemistry, ACS College
of Engineering, Bengaluru-560074, India)ABSTRACT Zinc Oxide (ZnO)
Nano powder was metal components to the effects of
media-drivenproduced by Solution Combustion Synthesis corrosion
[1-3].(SCS) at 350 10 C temperature using sugarsolution as fuel.
The final product was Superior properties of metal oxides such
ascharacterized by means of XRD, SEM and EDX. refractoriness, high
hardness, high compressiveThe powder blends of ZnO/Al were prepared
bystrength, wear resistance etc. make them suitable forlow energy
ball milling and the composite blocksbeing used as reinforcement
material in metalof ZnO/Al were fabricated by powder
metallurgymatrix. Incorporating ultra-fine particles of
metal-technique. The microhardness, wear resistance oxides
significantly improves mechanical propertiesand corrosion
resistance of ZnO/Al blocks wereof the metal matrix by reducing the
inter-particlestudied.The resultsshow that thespacing and providing
their inherent properties tomicrohardness, wear resistance and
corrosionthe metal matrix since they get embedded
uniformlyresistance can be improved significantly with into it.
However, fine particles show higheraddition of ZnO nano powder up
to 1 wt%; at tendency towards agglomeration. Therefore,the same
time, the optimal microhardness andoptimum particle size, amount of
reinforcement andmicrostructure were obtained when the
massprocessing parameters (compaction pressure,fraction of ZnO nano
powder is 1wt% where assintering temperature, sintering time)
should besample with 5 wt% of ZnO nano powder show determined for
each technique and matrix. Nano-best wear resistance. Corrosion
tests reveal that particles represent appropriate wettability with
metalthere was a slight mass loss due to corrosion.at the time of
sintering and good stability as well[4-8].Keywords ZnO,
Microhardness, Wearresistance, Corrosion resistance and
Microstructure. ZnO metal oxide plays a very importantrole in many
areas of chemistry, physics, and1. INTRODUCTION material science.
In technological applications, ZnOAluminium and its alloys are
widely usedis used in the fabrication of microelectronic
circuits,in services such as transportation, armory andsensors,
piezoelectric devices, fuel cells, coatingsmarine industries due to
their high strength to for the passivation of surfaces against
corrosion.weight ratio. They relatively resist corrosion when The
nanometric field is governed by numerousexposed to various
aggressive environments. These surface phenomena (photosynthesis,
catalysis,environments may include water vapour, acid and
precipitation, reactivity, deformation, reflectivity,base
solutions. Most of these environments degradeluminosity). This is
so because in nanomaterials thethe quality of Aluminium and its
alloys and affects number of atoms which are localized on freethe
mechanical properties of the system thereby surfaces as well as on
internal interfaces may bereducing their life-span. This makes them
unstableequal or higher than the number of atoms localizedin
certain environment that enhances their chemical inside the grains.
On this account, the properties arecombination with other elements
in the environmentstrongly influenced by the interfaces presentto
form stable compounds. On the return to their(surfaces, grain
boundaries) [9-13].natural stable form of ground state known as
ores anaccompanying reduction in the free energy of the Among the
functional mineral compoundssystem occurs. These structural defects
could be asuch as Perovskite (CaTiO3), Rutile (TiO2), CaF2 ,major
determinant in the degree of resistance ofSpinel (MgAl2O4),
Wurtzite (ZnS) and Zincite(ZnO), the last one being unique because
of its dual1569 | P a g e
2. K.S. Harishanand, H. Nagabhushana, B.M. Nagabhushana,
Parimesh Panda, A H Adarsha, M.M. Benal, N Raghavendra, K R Vishnu
Mahesh / International Journal of Engineering Research and
Applications (IJERA) ISSN: 2248-9622 www.ijera.comVol. 3, Issue 1,
January -February 2013, pp.1569-1576semiconducting and
piezoelectric properties. Due to attention in various applications,
hence in thisthe combination of interesting piezoelectric,
electric, work, the nano-ZnO/Al powder blends were used tooptical
and thermal properties, ZnO-doped prepare ZnO/Al blocks by cold
pressing followed bynanomaterials are of highinterestforsintering
and the performance of the fabricatedmultifunctional applications
in gas sensors,blocks were studied for hardness, wear
resistanceultrasonic oscillators or transparent electrodes in and
corrosion resistance.solar cells [14-18].2.
EXPERIMENTALNanostructured ZnO is a material that may 2.1.
Synthesis of ZnO powderpresent various structures, whose
configurations areThe ZnO powder was prepared bymuch richer than
for any known nanomaterial dissolving Zinc Nitrate (Zn(NO3)2.6H2O)
and sugarincludingcarbonnanotubes.The n-type solution in a minimum
quantity of double distilledconductivity of ZnO is relatively easy
to be obtained water in a Pyrex dish. The dish containing theby
using Zn in excess or by doping ZnO with Al, solution was
introduced into a pre-heated muffleGa, In. The most promising
dopants for obtaining p- furnace maintained at 350 10C. The
solutiontype conductivity are the elements from the Vth initially
boils and undergoes dehydration followedgroup. Different routes to
obtain doped ZnO thatby decomposition with the evolution of
largehave been studied yet are : the incorporation ofamount of
gases. At the point of spontaneoustransition metal ions into a
semiconductor photocombustion, the solution begins burning
andcatalyst by ion implantation or by co-precipitation;releases lot
of heat. All the solution vaporizesintroduction of oxygen vacancies
by treating a photoinstantly and becomes a burning solid. The
entirecatalyst with hydrogen plasma or X-ray irradiation;
combustion process for producing ZnO powdercoupling semiconductors
(ZnO or TiO2) with oxides takes only 5 min. The formation of ZnO
nanoor sulfides that enable visible light absorption (WO3,powder by
combustion synthesis can be representedFe2O3, CdS) by
co-precipitation or impregnation;by following reaction:doping of
N-atoms into the substitution sites in theZn(NO3)2 + C2H6N4O2 ZnO +
3N2 + 2CO + 3H2Ocrystal structure of a photo catalyst. In the
science.. (1)and technology of ZnO, several key issues that haveto
be achieved includes controlling the morphology2.2. Preparation of
ZnO/Al powder blends andand chemical composition of the ZnO
powders,ZnO/Al blockscontrolling the purity and particle size
during theZnO nano powder produced by Solutionsynthesis process of
ZnO powders, controlling the Combustion Synthesis(SCS) was added to
99.5%amount of the dopants. ZnO powders with different pure
commercially available Aluminium powdermorphology (prismatic,
ellipsoidal, bi-pyramidal, with wt% of ZnO nano powder varying from
0 todumbbell-like, nanowire, nanorod) have been 5% with an
increment of 0.25, 0.5, 1, 2.5 and 5obtained till date [18-23].
wt%. They were mixed for 30 minutes by handmixing and loaded in
metal die for compaction. The Different physical or chemical
synthetic powder metallurgy technique was used to
fabricateapproaches have been developed to produce nano- the ZnO
doped Al blocks. Powder blends were coldsized ZnOparticlesincluding
thermal pressed at 200 MPa to approximately 90 %decomposition,
thermolysis, chemical vaporcompression and then sintered at 500 C
for 1 hour.deposition, solgel, spray pyrolysis, precipitation The
sintered ZnO/Al blocks were polished with finevapor phase
oxidation, thermal vapor transport, emery papers with grit size
ranging from 200 tocondensation and hydrothermal. Generally, these
2000 followed by diamond paste polishing to obtainpreparation
methods involve complex procedures, mirror finish surface on the
specimen blocks.sophisticated equipment and rigorous
experimentalconditions. Most of these techniques require high 2.3.
XRD, Surface Morphology, EDX andtemperatures and long processing
time. Indeed,Microstructures of ZnO and ZnO/Al blocksthere is great
demand for economically viableX-ray Diffractometer (XRD:
Shimandzusynthesis techniques.SolutionCombustion 700 S, Japan),
Scanning Electron MicroscopySynthesis (SCS) is emerging as a
promising(SEM: JEOL, Japan, JSM 840A) were employed totechnique for
the preparation of nanopowder. This analyze the powder and
morphology of the ZnOprocess is simple, fast, economic and does
notpowder and polished surfaces of ZnO/Al blocks.require high
temperature furnaces and complicated The grain size and
microstructure were studied bylab set-ups. It can be used for the
preparation of allusing optical microscope.kinds of oxides
[23-28].2.4. Micro-hardness test From the open literature [1-28],
the ZnO Micro hardness was tested using Vickersbased Aluminium
composites attracted much Micro-hardness tester with diamond
indenter in the 1570 | P a g e 3. K.S. Harishanand, H.
Nagabhushana, B.M. Nagabhushana, Parimesh Panda, A H Adarsha, M.M.
Benal, N Raghavendra, K R Vishnu Mahesh / International Journal of
Engineering Research and Applications (IJERA) ISSN: 2248-9622
www.ijera.comVol. 3, Issue 1, January -February 2013,
pp.1569-1576form of right pyramid and a square base. An
opticalmicroscope with up to 400X magnification alongwith a
Micrometer attachment in the eye piece wasused to observe and
measure the length of thediagonal of indentation. Microscope
attachmenthelps in determining the distribution of ZnO nanopowder
dopant in the Al matrix doped with varyingpercentages ranging from
0 to 5%.2.5. Wear resistance test Pin on disc apparatus was used to
measurethe wear resistance of the samples. ZnO/Al samplesof size
101020 mm3 were fabricated and mountedon Pin on disk apparatus and
made to rub against therotating stainless steel disk. Area exposed
to wearwas 1010 mm2. Relative velocity of wear testFigure.1 XRD
Pattern of ZnO nano powdersample with respect to the rotating disk
was 2.6 ms-1and sliding distance was 1.57 km. Mass loss due to 3.2.
Morphological study using SEM andwear was calculated for each
sample afterElemental composition using EDXcompletion of wear test.
From the SEM analysis as shown in the Fig.2a, Fig.2b, Fig.2c,
Fig.2d, Fig.2e, Fig.2f, it is2.6. Corrosion resistance test
observed that the circular shaped primary particles Two separate
tests were performed toare agglomerated with varying sizes with
aluminumevaluate the corrosion resistance of the ZnO/Alpowder.
Here, the particle size was greatlyblocks.dependent on the
calcination temperature. As2.6.1. The specimens were soaked in the
spray tank calcination temperature increases the size alsowith 3.5%
NaCl solution for 50 hr and then wereincreases, due to congregation
effect, which isrinsed, dried and weighed. The corrosion
resistancereflected in surface area and XRD measurements.was
evaluated by mass loss per area, m/S (m is From the EDX Spectrum,
it is clearlythe mass loss and S is the surface area).observed that
no or relatively a small peak at 0.5 wt2.6.2. The specimens were
soaked in the spray tank % ZnO doped aluminum composites sample
andwith 0.5 mol MgSO4 solution for 10 hr and then remarkably high
peaks of ZnO presence at 5 wt %were rinsed, dried and weighed.ZnO
doped Aluminium composites sample is a clear indication shown in
Fig.3a and Fig.3b.The3. RESULTS AND DISCUSSIONS spectrum reveals
only the presence of Aluminium3. 1 X-Ray Diffractometer (XRD)
Studiesand ZnO elements and the absence of other elementsThe
crystallinity and purity of the prepared as the spectrum exhibits
the peaks for aluminum andproduct has been confirmed by powder
X-ray ZnO only. Therefore, it can be stated that thediffraction.
Fig.1 shows PXRD of ZnO physical and mechanical parameters can
benanoparticles which shows a well defined peaks attributed to the
presence of above said twolocated at Bragg angles (2) = 30, 33, 35
elements in the composition.corresponding to planes having Miller
Indices (100),(002), (101) respectively. The characteristic
peaksare higher in intensity which indicates that theproducts are
of good crystalline nature. No peakscorresponding to impurities are
detected, showingthat the final product is purely ZnO. It is
observedthat intensity of the peaks increases with thermaltreatment
due to agglomeration, which means thatthe crystallinity has been
improved. The full widthat half maxima of major peaks decreases
andconfirms the grain size growth [29]. Figure.2a SEM Micrograph of
Bare Aluminium 1571 | P a g e 4. K.S. Harishanand, H. Nagabhushana,
B.M. Nagabhushana, Parimesh Panda, A H Adarsha,M.M. Benal, N
Raghavendra, K R Vishnu Mahesh / International Journal of
EngineeringResearch and Applications (IJERA) ISSN: 2248-9622
www.ijera.com Vol. 3, Issue 1, January -February 2013,
pp.1569-1576Figure.2b SEM Micrograph of 0.25% ZnO dopedFigure.2f
SEM Micrograph of 5% ZnO doped AlAlFigure.2c SEM Micrograph of
0.5%ZnO doped Al Figure.3a EDX of 0.25% doped ZnO/Al
compositeFigure.2d SEM Micrograph of 1% ZnO doped Al Figure.3b EDX
of 5% doped ZnO/Al composite 3.3. Micro-hardness or Vickers
hardness testHardness of a material is defined as the resistance to
deformation, particularly permanent deformation, indentation or
scratching. Vickers hardness value increased by 3.3, 9.09, 21.05,
18.91 and 9.09 % with the addition of 0.25, 0.5, 1, 2.5 and 5 wt%
ZnO nano powder respectively in AluminiumFigure.2e SEM Micrograph
of 5% ZnO doped Almatrix.Micro hardness of nano-ZnO doped Aluminium
blocks increased with increase in 1572 | P a g e 5. K.S.
Harishanand, H. Nagabhushana, B.M. Nagabhushana, Parimesh Panda, A
H Adarsha, M.M. Benal, N Raghavendra, K R Vishnu Mahesh /
International Journal of Engineering Research and Applications
(IJERA) ISSN: 2248-9622 www.ijera.comVol. 3, Issue 1, January
-February 2013, pp.1569-1576percentage of ZnO up to 1 wt% and
further nosignificant increase is observed. The microhardnessgraph
shown in Figure4 clearly indicates a slowgrowth in hardness at
lower wt% of nano-ZnO. Aremarkable and substantial increment in
hardness isobserved at 1 wt% nano-ZnO concentration due touniform
distribution of nano-ZnO in the substrate.With further addition of
nano-ZnO, adecline in the hardness is observed which could
beattributed to an uneven distribution of the nano-ZnOparticles and
their tendency to agglomerate atFigure.5a Microstructure of 0.5%
doped ZnO/Alconcentrations higher than 1 wt% of nano-ZnO.
compositeThis means superior interfacial bond strength andrelated
high value of hardness can be achieved at1 wt% of nano-ZnO as the
optimal value.Figure.5b Microstructure of 1% doped
ZnO/AlcompositeFigure.4 Variation of Wear Resistance withaddition
of nano-ZnO3.4. Micro structure and Morphology analysis ofsintered
ZnO/Al blocksThe micro structure at different dopingconcentrations
is shown in Fig.5a, Fig.5b, Fig.5c,Fig.5d. ZnO particles can be
seen well embedded inthe grains of Aluminium matrix shown as a
result ofwhich the structure becomes closer and grainscompact. ZnO
nano particles are uniformly Figure.5c Microstructure of 2.5% doped
ZnO/Aldistributed in Al matrix in case of lower wt% ofcompositeZnO
powder up to 1 wt% and agglomeration of ZnOcannot be seen in major
part of the Al matrix asshown. This reveals that the sample has
uniformstructure and steady performance at dopingpercentages less
than 1%. At higher dopingpercentages (2.5% and 5%), agglomeration
of ZnOis more common in the aluminium matrix and theZnO particles
are not evenly distributed as shown.This uneven distribution and
agglomeration of ZnOin the Al matrix leads to density variations
from oneregion of the matrix to another. The presence ofnano
particles in the grain boundaries was the causeFigure.5d
Microstructure of 5% doped ZnO/Alfor suppression of non-coulombic
loss of the grains compositeand hence self-corrosion.3.5. Wear
resistance test The evaluation of wear resistance of theZnO doped
Aluminium samples are carried out onthe basis of mass loss method
and the results are 1573 | P a g e 6. K.S. Harishanand, H.
Nagabhushana, B.M. Nagabhushana, Parimesh Panda, A H Adarsha,M.M.
Benal, N Raghavendra, K R Vishnu Mahesh / International Journal of
EngineeringResearch and Applications (IJERA) ISSN: 2248-9622
www.ijera.com Vol. 3, Issue 1, January -February 2013, pp.1569-1576
placed in Table1 and the corresponding graph ischemical baths; one
containing NaCl and other with displayed in Fig.6. An incremental
order was MgSO4 standard solutions. The samples were tested
observed in reduction of wear loss from lower to for 50 hours in
NaCl solution and 10 hours in higher wt % of nano-ZnO. However a
relative steepMgSO4 solution. In both the conditions the drop from
6.0589 % wear loss at pure aluminum to corrosive properties of the
nano-ZnO doped 1.590 % wear loss at 1 wt% dopant is the maximum
Aluminium have been shown in Table2, Table3 and percentage
reduction in wear loss. A further corresponding graphs are
displayed in Fig.7, Fig.8. increase in nano-ZnO wt % has shown only
a In NaCl solution, the pure Aluminium is having marginal reduction
in wear value 1.590 % wear loss 1.0380 % of corrosion and by doping
only 0.25 % at 1 wt % to 1.300 % wear loss at 5 wt % nano-ZnO, the
corrosion has scale down to 0.3488 %. At 0.5 wt which doesnt
indicate much reduction in the wear% dopant corrosion drops to
0.2211% and 5% value. This increase in wear resistance can be
dopant the corrosion drops to 0.00127%. A sharp attributed to
addition of ultra-fine ceramic drop in corrosion value is observed
by adding only a reinforcement which possess high hardness,
wearsmall wt % of nano-ZnO to Aluminium substrate. resistance and
at the same time a strong interfacial bonding with the host matrix.
This may be due to formation of an oxide Table 1. Weight loss in
samples after wear layer due to quick reaction. Further drop
incorrosion is almost proportion scale that can be as itWt% of0%
0.25 % 0.5 %1%5% is seen 0.2211 % corrosion value at 0.5% dopant
toZnO doped 0.00127 % of corrosion at 5% dopant can beAl Blocks
tabulated as the corrosion resistance increases 10Initial 4.9365
5.8713 4.4251 4.88525.3963 times by increasing the dopant 10
times.Weight(gm) In MgSO4, the corrosion resistanceFinal 4.6374
5.6608 4.2872 4.80715.3261 property of the nano-ZnO doped
AluminiumWeightincreased at and above 0.5 wt% nano-ZnO
dopant.(gm)Further the corrosion resistance property of theWeight
Loss 0.2991 0.2105 0.1379 0.07810.0702 sample indicated the same
trend as in the case of(gm)NaCl solution. It can be inferred from
the result thata minimum of 0.5 wt% of nano-ZnO dopant isWear6.0589
3.5852 3.1163 1.59871.3008 sufficient for the corrosion resistance
when theResistanceenvironment contains MgSO4.in % weightlossTable
2. After corrosion of 50 hours with 3.5%NaCl solutionWt% of
CorrosionZnO Initial Final Weight Resistancedoped weightweightloss
(% weightAl(gm)(gm)(gm) loss)blocks0 23.7861 23.5392 0.2469
1.03800.2524.9387 24.8517 0.0870 0.34880.5 23.6523 23.6000 0.0523
0.22111.0 23.9736 23.9725 0.0011 0.00452.5 24.4241 24.4012 0.0229
0.0937 Figure.6 Variation of Wear Resistance with addition of
nano-ZnO5 23.5856 23.5853 0.0003 0.0012 3.6. Corrosion resistance
test The corrosion test on the nano-ZnO doped Aluminium specimens
were conducted in two 1574 | P a g e 7. K.S. Harishanand, H.
Nagabhushana, B.M. Nagabhushana, Parimesh Panda, A H Adarsha, M.M.
Benal, N Raghavendra, K R Vishnu Mahesh / International Journal of
Engineering Research and Applications (IJERA) ISSN: 2248-9622
www.ijera.comVol. 3, Issue 1, January -February 2013,
pp.1569-1576nano powder was found to be 1wt% with regard touniform
distribution of the reinforcement andhighest micro hardness value
for 1 wt % ZnO nanopowder. Increasing trend in wear resistance
ofsamples with increase in wt% of ZnO nano powdershows that ceramic
particles as nano-reinforcementcan impart superior wear resistance
to the hostaluminium matrix. Metal oxide nano particles arevery
efficient in imparting their inherent propertiesto the host matrix
like high hardness and strengthsince they have high surface area to
volume ratio. Figure.7 Variation of Corrosion Resistance with
addition of nano-ZnO after corrosion of 40 hours REFERENCES with
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