NGHieNCCrU-TRAOOOl TiNH CHAT CO HpC C O A HOP KIM X6P Ti-Nb-Zr CHt TAO B A N G PHUONG PHAP PHAN RA - THIEU KiT TRONG CHAN KHONG MECHANICAL PROPERTIES OF POROUS TiNbZr FABRICATED BY USI
Trang 1NGHieNCCrU-TRAOOOl
TiNH CHAT CO HpC C O A HOP KIM X6P Ti-Nb-Zr CHt TAO B A N G
PHUONG PHAP PHAN RA - THIEU KiT TRONG CHAN KHONG
MECHANICAL PROPERTIES OF POROUS TiNbZr FABRICATED BY USING A COMBINED PROCESS OF DECOMPOSITE - SINTERING METHOD
INVACUM
NguySn D|ng Thiiy, Tirin Vin DQng, Nguyin VJn Toin
Vi?n Khoa hoc va Ky thu?t Vat li?u, Trudng Dai hpc Bach Khoa Ha Npi
T 6 M TAT
Trong bdi bdo ndy, trinh bdy kil qud nghien cthi ve hign lupng ca hpc cua hpp kim Ti3.5Nb3.5Zr, iing dgng ldm vdl lieu cay ghep y sinh Cdc mdu Ihi ca tinh co du&ng kinh lOmmvd chiiu cao 10 mm, dtegc chi tgo bdng phttang phdp thieu kit tiai btt&c trong chdn khdng cao (10') Dteang cong ting suat - bien dgng dupe xay dung tit edc thi nghiem nen dpc tnic tren mdy thie keo nen vgn ndng MTS Ket qud thi nghigm cho thdy, cde mdu thi nghiem cd vd khdng cd chai phg gia lgo xop ed linh ettdt nhu sau: Dttang cong ieng sudt - bien dgng dlegc chia thdnh 3 viing ro rg: Vimg ddn ttdi tuyen tinh, viing ddn hdi - nh&t vd viing tdng ty trpng Dpi v&i cdc mdu cd chdt phg gia lgo xdp, ling xHcahpc tteang tit nhu cdc tne&ng hgp harp kim chi tgo bdng phucmg phdp luygn kim bpt klide, vgt ligu thugc dgng ddn, dttang cong ting sudt - bien difng chi ton tgi viing bien dgng ddn hdi Cdc ehi tieu ca - ly tinh deu ddm bdo yeu cdu doi v&i vgt lieu cay ghep y sinh,
Tir khda: Hgp kim titan, Ong xie ca hpc, vgt ligu edy ghep y sinh, thieu kit hai bu&c,
ABSTRACT
Present research work reporis a study on new mechanical phenomenon of the porousTl3.5Nb3.5Zr materials that addressed for implant materials in dentai The mechanical testing samples were prepared by two steps sintering method with dimension of 10 mm and height <f 10mm The compressive tests were carried on MTS instrument to determine the strain-stress curves Then mechanical behavior of the materials was analyzed from those curves For samples after sintering wilhoul space holder and binder addition, there were three deformation regions on Ihe curves that were linear elasticity, plateau and densification The mechanical behavior of materials were modelled, the main parameters in the model were identified from the strain - stress curve For sample after sintering with space holder and binder, materials were brittle The mechanical properties of those samples also were determined Microslruclures of materials before mechanical testing were observed by SEM, and the surface also analysed by XRD
Keywords: Porous titanium alloys, mechanical behavior, dental materials, two step sintering
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TAP CHI CO KHl V I £ T NAM, Sd 8 nam 2016
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1 MO DAU
Trong nhiing nam gan day, hpp kim titan
x6p da thu hiit dupe sp quan tam ciia nhidu nha
khoa hpc tren the gidi, da cd mpt s6 cdng trinh
nghien ciru phat tridn cdng nghf che tao he hpp
kim nay Cac hpp ldm titan xdp chu ydu dupc
nghien cuu ting dung Iam vgt lifu ciy ghep bao
gdm: Ti, TiNi va Ti4AI6V Tuy nhien, chua cd
nhieu cdng bd ve iing xii ca hpc cua hpp kim
x6p nay Do dd, hidu r5 ca tinh sd md rpng ITnh
vpc ling dung cua hf hpp kim xdp
Cung vdi sp phat trien kinh ti - xa hpi
va kp thuat d nudc ta trong nhihig nam gin day,
nhu cau ve vat lifu ciy ghdp trong y hpc nhim
mpe dich iam d^p, didu tri chin thuang sau tai
^ l ^ h o ^ thay th^ bf phgn thoai hda ciia con
ngudi Ky thugt ciy ^ d p trong y hpc d Vift
Nam tuang ddi phat trien, tuy nhidn; vft lifu
cay ghdp van phai nhfp ngogi toan bf vdi gia
thanh cao va tiidi gian chd dpi dai Day cflng
la ly do cin thidt phai phat tridn cdng nghf chl
tgo hpp kim xdp nhim phuc vp thi trudng trong
nudc
Vi tri cay ghdp chan rang va cau tnic
cua mpt chan rang dupc trinh bay trdn hinh I va
2 Vai trd cua vat lifu ciy ghdp la ldp trung gian
giiJa Ipi tp nhien va dinh vit ldm logi (titan ho$c
thdp khdng gi) Theo thdi gian cac md xuong se
phat trien vao cac lo xdp, iam cho vgt lifu cay
ghdp bam ch$t vko lpi, tgo dd chic chin dh bit
dinh vit va rfing gia len tren Vdi vai trd nay, vat
lifu ciy ghep cin dam bao tuong thich sinh hpc
bao gdm: Tuong thich hda sinh, tuang thich ca
hpc va vft 1^ Hf vft lifu Ti3.5Nb3.5Zr, dupc
thidt kh de thay thd cac hf vft lifu xdp tren co
sd titan trudc day cd chiia ckc nguyen td khdng
cd lpi cho Slic khde nhu: Ni, Al va V, nhung vin
phai dam bao cac tinh chit ca ly nhu: Modim
dan hdi thip, dp bdn cao va dp xdp hpp Iy
Hmh 1 Vi tri cay ghep chdn rdng nhdn tgo
tren hdm fl]
Hinh 2 Cdu tnic chdn rdng hpp kim titan xdp [1]
Trdn thd gidi, hpp kim titan xdp [2,3], da dupc phat trien tir nh&ng nam 1960, ngay nay,
hf vgt lifu nay da trd thanh san phim thuang mgi Tuy nhien, hf vft lifu nay vin chua dupc san xuat tgi nudc ta Rao can ldn nhat ma chting
ta chua vupt qua dupc dd la kha nang ve cdng nghf va thidt bi thieu kdt, vl titan la nguyen to rat nhay cam vdi oxy va de bi oxy hda trong qua trinh thieu kdt Vai nam gan day, hai cdng nghf thieu ket: Tdng hpp nhift dp cao tp lan truydn (Self-propagating high temperature synthesis SHS) va thieu ket hai budc: Phan ra - thidu ket da dupc iing dpng thanh cdng cho hf hpp kim TiNi [4,5] Trong dd, thieu kdt hai budc
cd tridn vpng unng dpng dupc cho he vft lifu Ti3.5Nb3.5Zr Theo phuang phap nay, hf vgt lifu ban dlu dupc sii dpng la TiH^, Nb va Zr, TiHj sd phan ra tao ra mdi trudng hoan nguyen
HJ d khoang nhift dp 400"C, them vao do qua trinh thieu ket thpc hifn trong chan khdng cao,
do dd qua trinh oxy hda cd thd s6 dupc hgn chd ^
ISSN 0866 - 7056 TAP CHf CO KHf VI|T NAM, Sd 8 nfim 2016
Trang 3NGHI6N CLfU-TRAODOI
ho&c Ichu hoan toiin
Trong bai bao nay, sc trinh bay cac Icet
qua nghien cuu tinh chSt co hgc cua cac miu
Ti3.5Nb3.5Zr, chd tao bang phuong phap
thieu Itit hai budc Ket qua nghien ciiu cd y
nghia quan trong trong viec Idiang dinh cdng
nghe chS tao vii md rdng img dung h^ vat lieu
Ti3.5Nb3.5Zry sinh
2 THV'C NGHIfM
Vat li^u ban diu la cac bdt kim loai: TiH,
(do sach > 99 %, kich thudc hat 300 nm), Nb (do
s?ch > 99 %, kich thudc hjt 20 (uii), Zr (dp sach
> 99 %, kich thudc h^it 400 nm), cua hStag Whole
Win (Beijing) Metarials Sci Tech Co., Ltd
Tdng khdi lupng hdn hpp bpt kim loai
mdi lan phdi li|u la 20 g, vdi timg thanh phan
TiRj, Nb, va Zr lin lupt la: 18,2 g, 1,27 g va
1,26 g dd dat dupc ty 1? Ti -3.5% Nh -3,5% Zr,
ttong dd 18,2 g TiHj tuong irng vdi I7,47g Ti
sau phan irng phan ri:
AWt^SOVC
lOidi lupng: 18,2 g 17,47g
Hon hpp bpt kim loai dupc nghidn trpn
Uen may upn tang trdng vdi cac thdng sd ky
thu?t: Kich thudc tang trdng LxD = 142x136
mmxmm, toe dp quay tang trdng 60 vg/ph, kich
thudc bi d = 10 mm, ty lp bi/bpt = 10/1; thdi
gian nghiin trpn: 2 h
De thay ddi dp xdp, hdn hpp bpt kim
lo»i ban diu dupc bd sung thdm chit phy gia
t?o xdp NH^HCO, vdi thanh phin 10, 20, 30,
40 50% ve khdi lupng Cac quy trinh tidp theo
diu giong nhau cho tit ca cdc mau cd va khdng
cd chit phy gia t?io xdp
Cdng d o ^ ep diroc th\rc hipn tren may
ep thuy luc 100 T Myc dich cdng do?n dp la tao hinh khdi va tao mdi lien ket ca hpc giila cac hat bpt kim loai Qua trinh ep t^o hinh dupc tiin hanh trong khudn kin vdi ap lyc 150 + 250 Mpa Khudn ep cd chidu cao 60 mm, dudng kinh trong 10 mm, vat li?u ichuon dp - thep C45 Cdng doan phan ra - thieu ket dupc tiio hanh nhu sau: Phan ra TiH, d iihi?t dp 400 -^ 500°C, trong khoang thdi gian giiJ nhi^t Ih va
thieu kit d nhi$t dp 1.050 + 1.250«C hPng 2 -^
4h, tao dieu ki$n cho qua trinh khuich tin va
hpp kim hoa \ky ra Trong qua trinh phfin r5
-thidu kgt, khi H, thai ra cd vai trd la chat hoiin nguyen
Qud trinh phan ta - thieu ket hon hpp b$t ' kim lo^i dupc thyc hien trong Id thieu ket chan khdng cao vdi mdi trudng chan khdng djt IO' torr Myc dich qud trinh phan ra - thieu kit lil lam dinh kit va hpp kim hda cdc bpt kim loai d6 dat dupc cdc tinh chat yeu ciu Nhi^t d$ phan
ra -thieu ket dupc xdc dinh tren ca sd khao sat nhiet dp phan rS TiH, tdi uu [4] va tucmg img vdi gidn dd pha Ti->Jb
Cdc mau vfit lipu ban dau va sau phan
rd - thieu kit dupc ddnh gid vd xdc djnh nhu sau: Thanh phdn pha bang nhieu xa Ronghen; ICich thudc hat, td chirc ti vi va cdc hipn tupng l>c mat miu bdng hien vi dipn tu qu^t; Quan h^ irng auit - biin dang, modun ddn hoi vd gidi h ^ bin dupc thyc hipn tren mdy thu k6o -ndn v ^ ndng (MTS); Cdc thdng sd md hinh biin d?ng dupc xdc dmh tir cdc sd lieu thyc nghidm nay;
Ty trpng mau bdng phuong phdp Atximet tren can tiiu ly dipn tir; Dp xdp cua mau dupc xdc dinh thdng qua ty trpng
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Trang 4NGHieNCD'U-TRAO Ddi
3 Ktr QUA VA THAO LUAN
3.f Pha va to chuc te vi cua miu sau thieu kit
Hinh 3 Gidn dd nhieu xg Ranghen ciia hgp kim
Ti3.5Nb3.SZr scm thieu kit hai bu&c trong cAdn khdr^
trudng hpp nay, hpp kim chiia mdt phan pha
^Ti, Ti, Nb va Zr
Hinh 4 la anh td chirc td vi cua bd mgt mau sau thieu kdt, mdt lln niia khing dinh, mpt phin pha p-Ti da hinh thanh, thd hifn tai cac vimg cd cac dudng thing song song xuat hifn Tren anh td chirc te vi nay Id xdp cd the dupc xae dinh vdi kich ca khoang vai chuc ^un Anh td chiic td vi ciing cho thiy, khdng tdn tai duang bien gidi giiia cac hat, qua trinh khuech tan khi thieu ket da dien ra hoan toan Kdt qua kidm tra thanh phin pha va td chiic te vi khing dinh, cac mau che tgo bfing phuang phap hai budc trong chan khdng cao dat ydu cau dd nghidn ciiu iing sii ca hpc
TSng ty trong
Hinh4.AnhSEMhgpkimTiH,3.5Nb3.5Zrsau
thieu ket hai bu&c trong chdn khdng
Gian dd nhteu xg ciia tit ca cfic mau sau
khi thieu ket cho thay, khdng tdn tgi cac pha
TiHj va cac oxit ciia Ti, Nb hofic Zr, dieu dd
cd nghTa la phan iing (I) da xay m hoan toan;
nhu vgy, trong trudng h ^ dp chan khdng cao
den 10'^ dli de bao vf hpp kim tgi nhift dp thieu
kdt Tren gian dd nhieu xg Ranghen, chi tdn tai
cac dinh ciia cac hpp kim Ti, Nb va Zr, trong dd
pha p-Ti da xult hifn (tgi 28 = 39"), pha p-Ti
tdn tgi trong hpp kim titan xdp, se tgo cho hpp
kim cd dp xdp cao, modun dan hdi thap, dp bdn
cao phil h(JT5 vdi irng dung trong y hpc Trong
Hinh 5 Du&ng cong quan hp img sudt - bien dpng cita mdu Ti3.5Nb3.5Zr sau thieu kit khdng cd chdi php gia
Quan hf giira img suit - bidn dgng cua hpp kim Ti3.5Nb3.5Zr chd tgo bing phuang phap hai budc, khdng su dung chit php gia tgo xdp, dupc trinh bay tren hinh 5 Qua trinh bidn dang tdn tgi ba viing: Vung bidn dgng dan hdi tuyen tinh, dan hdi - nhdt, vimg tang ty trpng
Dp Idn cua moi vung php thupc vao ty trpng cua =
ISSN 0866 - 7056
TAP CHf CO KHf V I £ T NAM, Sd 8 nam 2016
Trang 5vat lipu Tinh chit ca hpc khi ty trpng thay ddi
do biin d?ng dupc md td bing cac cdng thitc do
Gibson vd Ashby phdt triin [6,7], nhu sau:
Tai vimg dan hdi tuyen tinh:
£, I f t J
Tai viing dan hdi nhdt:
(2)
(3)
E* va ES - Modun dan hdi cua vft lifu d
mpt dp xdp nhit dinh va khi khdng cd dp
xop (vgt lifu dac)
p*/p^ - Ty trpng tuong ddi ciia vat lieu;
o* , - Gidi hgn ben cua vgt lifu xdp;
a,y - Gidi hgn bdn vgt lifu d trgng thai d$c;
C, va C, - cac hing sd xae dinh tir thpc
nghifm (trong hau het cac trudng hpp C, =
1 and Cj = 0.3 [8])
Trong bai bao nay, sir dpng mpt md hlnh
mdi dupc cdng bd de md ta iing xii ca hpc ciia
vgt lifu Ti3.5Nb3.5Zr, md hinh dupc phat tridn
bdi Goga Vladimir nam 2010 [9] Md hinh bao
gdm 3 hf dupc noi song song (hinh 6)
Hinh 6 Md hinh tuang lu doi v&i vgt ligu xdp [9]
He thii nhit, bao gdm Id xo (dp cirng
k) va piston (dp nhdt c), ddy chinh Id md hinh
Maxwell, hp so k cua Id xo tucmg img vdi
modun dan hdi cua vdt lipu xdp tai viing ddn
hdi tuyen tinh, hp sd nhdt tucmg duang ung suit ddn hdi - nhdt
Hai hd cdn lai gdm, hai Id xo cd dO ciing lin lupt Id: k, va k^ E)d ciing k Id dO nghifng ciia img sudt trong vimg ddn hdi nhdt, dp ciing
kD Id ham mu cua thdng so bien dang, dupc viit nhu sau [10]:
i „ ( e ) = r ( l - e ' ) ' (4)
Sau cdc ph^p bien ddi todn hpc vd dp dung tdc dp biin d?ng e = 1, md hinh todn hpc dupc dua ra nhu sau:
all) ^ ( - i ^ i ^-|A:, + 7(l-f')"]r(5)
k, c, kp Y - Cdc thdng so cua md hinh k,
va kp dupc xdc dinh tir dp ddc trong viing
l v d 2 ;
c - liTng suit trong vdng dan h^i-nhdt;
Y vd n dupc xdc djnh bdng phuong phdp binh
phuong cue tiiu, tir cdc s6 li$u ti£n dudng
cong dng suit - bien dang, gid tri cila cac thdng so md hinh dupc thi hipn d t)dng 1 LTng xir ca hpc cua h^ vat li$u xop sau thieu kit khdng sir dyng chat phy gia, dupc xip vdo loai bien dang ddn hdi - nhdt
Ddi vdi cdc mau cd sur dyng chat phy gia tao xdp NH^HCO,, tren dudng cong img suat -biin dang (hinh 7), khdng tdn t?i viing din hoi - nhdt vd vimg tdng ty trpng, vdt lipu ddn, bj phd huy trudc khi vdch kim loai biin d^g die
Bdng I Cde Ihdng sd md hinh:
9.3 MPa
9515 MPa
1485
T
IMPa 2.5
c,
M P t
315
D
6
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Trang 6NGHIEN CO-U-TRAO D O I
1
I
-09x^:18.6%
04 xdp: 45%
Bi^ndang
Hinh 7 Quan hg ieng sudt -biin dang eda hgp kim
xop Ti3.5Nb3.5Zr ed ehdi phg gia tgo xdp khi Ihieu kit
Day Id d^uig dudng cong tdt phd biin
cua kim loji xdp chi t^o bdng phuang phdp
6p-thi6u kit Svt khdc nhau ve umg xir co hpc
ciia mau khdng vd cd sit dung chat phy gia t?o
xdp cd thi gidi thich nhu sau: Trudc khi thi6u
kit, cdc chit phy gia dupc tr$n deu cimg vcH bp
kim lo^i, chdt kit dinh d d ^ g ldng, phii todn
bO bi mdt cdc hat b0t kim lojii, do dd chiing t?o
ta mdng ngdn cdch giiia cdc hji b§t, lam cho
tiip xiic giiia cdc hiit bpt kdm, (iin din han chi
qud trinh khuich tdn IChi cd tdi trpng tdc d^ng,
cdc lien kit bj phd vd trudc khi biin djmg deo
Tiong khi dd, cdc lien kit d cdc mau Ichdng su
dyng chit phy gia gin nhu khdng bj phd hiiy
trong khi thur co tinh (mau khdng bi vd sau khi
thd)
Bdng2 Vgtliguxdp ri3.5Nb3.5Zr v&i ham lugng
chat phg gia khde nhau trong qud trinh thieu kit
Chit phv
gl«C/.)
ichdng CO
30
40
SO l i p
(%)
9.4
18,6
45,4
Modun diin h6i E,
MPa
9515
11564
4711
MPa '
1791
1344
303
Ca tinh cua cac miu cd df xdp khac nhau
(bang 2), cac chi s^ ca tinh nay dupc xae dinh
tii quan hf iing suit -biln dgng (hlnh 6 va 7)
M$c dil cac mau cd sir dpng chat php gia khdng
tuan theo rod hhih trinh bay d trdn nhung cac
tinh chat ddu thda mfin cac ydu clu doi vft lifu
ciy ghdp y sinh
4 KETLUv^N
Md hinhj>hii hpp doi vdi cac mau che tao khdng cd chat php gia Cac hf sd trong md hinh da dupc xae djnh tii dudng cong quan hf ling suat - bien dang
Hpp kim titan Ti3.5Nb3.5Zr vdi cac df xdp khac nhau tCr (10-50%) da dupc chd tgo thanh cdng bfing phuang pimp thieu kit hai budc Pha hinh tfaanh, cau true va cac tfnfa cfaat ca hpc dap img ydu cau cua vat lidu cay ghep y sinfa Cac miu khi thieu ket cd chat php gia cd ling xu ca hpc thupc dgng vft lifu ddn, dudng
cong quan hf lin^ suit - biln dgng chi thn tgi
vimg dan hdi tuyen tinh, khdng tdn tgi vimg dan hdi nhdt va viing tfing ty trpng
^ Thdi gian thieu ket can dupc kdo dai ban ddi vdi tat ca cac mau de dgt dupc tinh ddo cho vat lieu xop •
Ngay nhgn bai: 05/7/2016 Ngay phan bifn: 12/8/2016 Tai Ufu tham Ichao:
[I].TrabecuIar Metal Materials, Metal Implant dental Materials Brochure
[2] Zena J Wally, Wlliam van Gninsven, Frederik Claeyssens, Russell Goodall and Gwendolen C Reilly, Porous Titanium for t)ental Implant Applications Metals, 5, 2015, 1902-1920 [3], A.E Aguilar Maya, D.R Grana, A Hazarabedian, GA Kokubu, M.I Luppo, G Vigna, 2r-Ti-Nb porous alloys for biomedical applic^rai Mater Sci Eng C, 32,2012, pp321-329 [4] Nguyin DJng Thiiy, TVAn VSn DQng, NguyJn V5n To4n,
Hoa Xuan Hoa; Nghien cuu cong nghf chi lgo Vgi lifu xop
TiNb3Zr3 Ij^g phmmg phdp phdn ra thiiu ket, T?p chl Khoa
hpc C6ng ngh$ Kim lo^i, Tfi/2016
[5] Nguyin D ^ g ThuJ, T r k Van DQng, HA K ^ Thanh,
NguySn Thj NhSn Nguy&i T\ka Vifc Tinh chat cohgcva cJu true hgp kim NiTixop che lgo t)dng phuang phdp phdn rH-thihi ket, T4/20I6, T^p chf Co khi Yi^ Nam
[6] Ashby, M.F Metall •Rans A, vol 14A (1983), p 1755- 69 [7], Gibsmi, LJ and M.F Ashby Proc R Soc London vol
A382,p.43.2, 1982
[8], Gibson LJ and M.F Ashby, Cellular Solids: Structure and [9] Goga Vladirair.Testing and Application of New Phenomenological Material Model
for Foam Materials, PottAI pre odbom^ publikovanie, 2010, i ^ I -11
ISSN 0866 - 7056
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