Doped Alumina

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Effect of Zirconia Dopant Concentration on Abrasive

Properties of Sintered Alumina


Muhammad Afsar Raza

, Mamoona Zaheer Bilal Abbas a!vi, Abdul "a#ee, "usnain Ali tari!
School of Chemical and Materials Engineering (SCME),
National University of Sciences and Technology (NUST) H-1
MuhammadAfsar512@gmail.com
mamoonazaheer@gmail.com
Abstract$Zr%& doped Al&%' ceramics have been studied
e(tensivel# mainl# for their hi)h abrasive resistance and bio
compatibilit#* +n our stud# ,- Al&%' .as studied for abrasive
resistance properties .ith var#in) concentrations of Zr%&
dopant* /he dopin) .as carried out usin) a simple ball millin)
operation .ith &0, 10 and 20 .ei)ht percent dopant* /he
pellets formed easil# .ith Pol# 3in#l Alcohol Binder and
pressure of 45 ton for 45 minutes* /he pallets .ith &5mm dia
.ere then sintered in at 4255 C for four hours* Althou)h the
dopin) of Zr%& into Al&%' predicted an increase in hardness of
the doped samples as compared to the pure alumina sintered
.ith e(act conditions, the unachievable sinterin) temperature
.ithin the premises of SCME limited the )rain )ro.th of all
the samples and therefore the hardness properties*
+* +/R%D6C/+%
Alumina po.der has versatile applications and several
properties can be obtained b# var#in) parameters
includin) sinterin) temperature, dopant concentration,
pressure*
Dopin) Zirconia into Alumina has been e(tensivel# used
to alter microstructure of en)ineerin) alumina ceramics for
several applications748* /he applications mostl# re!uire
hi)h abrasiveness of the material* 9e doped Zirconia in
different concentrations to stud# the effect on abrasive
properties* Main applications include dental implants due
to bein) bio-compatible and hi)h .ear resistance7&8* and
cuttin) tools due to hi)h abrasive and .ear resistance7'8*
++* E:PER+ME/A; AA;<S+S
Alumina po.der =,> manufactured b# +me( Chemicals Co*
;td* .as emplo#ed and initiall# characterized usin) :-Ra#
Diffraction* Alumina po.der .as doped usin) different
concentrations of zirconia and formed into pellets and sintered
to form the ceramic* /he ceramic?s microstructure .as seen
under an optical microscope as .ell as a scannin) electrode
microscope, to compare the microstructures .ith the abrasive
resistance of the ceramic samples formed*
!" #o$der characteri%ation
:RD anal#sis of Al&%'@ Zr%& po.der .as done to reveal
its cr#stal structure and )eometr#* S/%E po.der
diffraction s#stem .as used for this purpose* /he
diffraction of alumina pattern .as matchin) to that of
corundum .hich is also called , alumina* +t has a
rhombohedra bravais lattice* /he obtained pattern is A& 0
matchin) to that of in data base728 7B8* 9hile zirconia has
monoclinic structure at room temperature Cin temperature
ran)e 44D5 oC to &'D5 oC tetra)onal and above &'D5
o
C it
is cubic718* /his morpholo)# chan)e induces the
tou)henin) effect on Alumina and it is Eno.n as Z/A
=zirconia tou)hened alumina>* Also :RD pattern helps to
identif# the constituents present and their cr#stal structure*
*
Fi)ure 4* :RD pattern of alumina po.der used in the e(periment
%nce the po.der composition .as determined, Particle size
distribution of the alumina po.der and zirconia po.der bein)
used .as found out usin) a particle size anal#ser* /he mean
particle sizes .ere '*4D15Gm and H*'4&AGm of zirconia and
alumina respectivel# before millin)*
&" Sam'le #re'aration
/he initial step .as dopin) the samples b# var#in) dopant
amount usin) ball mill* Ball mill .as operated at HB rpm for
45 minutes, 45 zirconia c#linders .ere used as millin) media*
Different .ei)ht percenta)e .as used to stud# the effect on
hardness of dopant concentration* +n order to achieve hi)h
densification and improved sinterin) Pol# 3in#l Alcohol
=P3A> 7D8 used as a binder* Pressure needed for this s#stem for
the compaction .as 42*D ton7H8* 9e used unia(ial press and a
pressure of 45 ton due to limitation of the e!uipment* +n order
to facilitate the removal of the )reen compacts from die, it .as
oiled before pressin) samples then it .as cleaned and re-oiled
a)ain for each sample*
C" Sintering
%nce the pallets .ere formed, the# .ere sintered in a
muffle furnace* /he temperature re!uired for sinterin)
zirconia doped alumina .as 4D55
o
C 7&8 but .ith the available
furnace and limitations due to load sheddin) in PaEistan, the
hi)hest achievable temperature .as 4255
o
C* /he furnace
tripped seven times in total, .ith the temperature drop of
455
o
C appro(imatel# each time* /he soaEin) time .as ' hours
and the samples .ere then furnace cooled for 41 hours*

+++* RES6;/S
/he prepared samples .ere subIect to the follo.in) testin)
methods to checE the effect of our preparation parameters on
the properties of the sample*
!" Scanning Electron Microsco'y (SEM)
SEM ima)es of sintered pellet =Zr%& 45 0> .ere taEen
from JE%; Anal#tic SEM at ma)nifications of 455(, 4555(,
B555( and 45,555(* /hese ima)es sho. ver# little )rain
)ro.th and lots of porosit#* As )rain )ro.th is dependent
upon the mass transport form one particle to the other i*e*
diffusion* For diffusion to occur a particular amount of ener)#
=activation ener)#> is needed to be )iven to atom*

Due to limitation of sources the sinterin) .as done at 4B55
o
C*
9hile the sinterin) temperature needed to for alumina is
around 4D55
o
C* So at 4255
o
C atoms .ouldn?t )et enou)h
mobilit# to diffuse amon) the particles* /hat?s .h# there is
ver# little or no )rain )ro.th*
"irlin)er and ;an)e proposed that addition of second phase
zirconia particles in alumina can si)nificantl# increase the
sinterin) rate b# pinnin) the )rain boundaries and hence can
reduce the sinterin) temperatures* Because sinterin) rate in
inversel# related to the absolute temperature*

"ere b K dpLdt is the instantaneous rate of densification, d
is the )rain size is a function onl# of the densit#, M is the
activation ener)#, # is surface ener)#, 3 is the molar volume,
R is the )as constant, / is the absolute temperature, C is a
constant, and A is a material parameter that is insensitive to
*
But the activation ener)# needed for diffusion is increased
upon the addition of zirconia to alumina* Nupta7A8 has
su))ested that chan)e in activation ener)# for boundar#
diffusion is due to the bondin) at the boundaries* /hus this
increase in activation ener)# is accompanied b# the lo.erin)
of the interfacial ener)# of interfacial particles* /hus
activation ener)# for aluminaLzirconia is D55EJLmol* /his
value is 4*B times the activation ener)# for alumina i*e*
225EJLmol7458*
Fi)ure &* SEM +ma)es at different ma)nifications
&" Hardness
Due the unachievable sinterin) temperature, the zirconia
dopant concentration rendered no si)nificant effect on the
sample?s hardness* /he samples remained hi)hl# susceptible
to abrasion* Althou)h if the )rain )ro.th .as achieved, a
hardness increase .as e(pected*
+3* C%C;6S+%
/he e(periment .as carried out to stud# the effect of
zirconia dopant concentration on abrasive resistance of
alumina for applications that re!uire hi)h abrasive resistant
ceramics* A sinterin) temperature of 4D55
o
C is at least
re!uired for )rain )ro.th of the ceramic and to minimize the
porosit#, ho.ever, the temperature not bein) achieved, the
results .ere not satisfactor# to the title of the research*
ACO%9;EDNME/
/he )roup .ishes to acEno.led)e Dr* "aris Ansari, SCME
6S/ for providin) us .ith our first learnin) e(perience of
the Eind* 9e further acEno.led)e Dr* Fahim "ashmi, +nstitute
of Space /echnolo)# =+S/> for arran)in) the ball millin)
facilit# and P3A binder for our proIect* 9e .ould also liEe to
thanE Dr* Amir "abib, SCME 6S/, for helpin) us in the
SEM ima)in) of our sample* And finall#, all the lab en)ineers
that helped us .ith all our lab .orE*
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