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NGHieNCCrU-TRAOOOl TiNH CHAT CO HpC COA HOP KIM X6P Ti-Nb-Zr CHt TAO BANG 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 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 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 viing ro rg: Vim ddn ttdi tuyen tinh, viing ddn hdi - nh&t vd viing tdng ty trpng Dpi v&i cdc mdu cd chdt phg gia l xdp, ling xHcahpc tteang tit nhu cdc tne&ng hgp harp kim chi tgo bdng phucmg phdp luygn kim bp klide, vgt ligu thugc dgng ddn, dttang cong ting sudt - bien difng chi ton tgi viing bien dgng ddn hd 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 < 10mm The compressive tests were carried on MTS instrument to determine the strain-stress curve 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 mechanica testing were observed by SEM, and the surface also analysed by XRD Keywords: Porous titanium alloys, mechanical behavior, dental materials, two step sinterin ISSN 0866-7056 TAP CHI CO KHl V I £ T NAM, Sd nam www.cokhivietnaiii.vn 2016 NGHieNCCrU-TRAOOOl 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 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 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 nhihig nam gin day, nhu cau ve vat lifu ciy ghdp y hpc nhim mpe dich iam d^p, didu tri chin thuang sau tai ^ l ^ h o ^ thay th^ bf phgn thoai hda ciia ngudi Ky thugt ciy ^ d p y hpc d Vift Nam tuang ddi phat trien, nhidn; vft lifu cay ghdp van phai nhfp ngogi toan bf vdi gia cao va tiidi gian chd dpi dai Day cflng la ly cin thidt phai phat tridn cdng nghf chl tgo hpp kim xdp nhim phuc vp thi trudng nudc Vi tri cay ghdp chan rang va cau tnic cua mpt chan rang dupc trinh bay trdn hinh I va Vai trd cua vat lifu ciy ghdp la ldp trung gian giiJa Ipi 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 Vi tri cay ghep chdn rdng nhdn tgo tren hdm fl] Hinh 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, nay, hf vgt lifu da trd san phim thuang mgi Tuy nhien, hf vft lifu 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 qua trinh thieu kdt Vai nam gan day, hai cdng nghf thieu ket: Tdng hpp nhift dp cao lan truydn (Self-propagating high temperature synthesis SHS) va thieu ket hai budc: Phan - thidu ket da dupc iing dpng 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 tao mdi trudng hoan nguyen HJ d khoang nhift dp 400"C, them vao qua trinh thieu ket thpc hifn chan khdng cao, dd qua trinh oxy hda cd thd s6 dupc hgn chd ^ ISSN 0866 - 7056 TAP CHf CO KHf VI|T NAM, Sd nfim 2016 www.cokhivietnam.vn NGHI6N CLfU-TRAODOI diu giong cho tit ca cdc mau cd va khdng cd chit phy gia t?io xdp 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 viec Idiang dinh cdng nghe chS tao vii md rdng img dung h^ vat lieu Ti3.5Nb3.5Zry sinh 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 khudn kin vdi ap lyc 150 + 250 Mpa Khudn ep cd chidu cao 60 mm, dudng kinh 10 mm, vat li?u ichuon dp - thep C45 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 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 TiH,-.Ti + H, lOidi lupng: 18,2 g (1) Cdng doan phan - thieu ket dupc tiio hanh nhu sau: Phan TiH, d iihi?t dp 400 -^ 500°C, khoang thdi gian giiJ nhi^t Ih va thieu kit d nhi$t dp 1.050 + 1.250«C hPng -^ 4h, tao dieu ki$n cho qua trinh khuich tin va hpp kim hoa \ky Trong qua trinh phfin r5 thidu kgt, H, thai cd vai trd la chat hoiin nguyen Qud trinh phan ta - thieu ket hon hpp b$t ' kim lo^i dupc thyc hien Id thieu ket chan khdng cao vdi mdi trudng chan khdng djt IO' torr Myc dich qud trinh phan - thieu kit lil lam dinh kit va hpp kim hda cdc bpt kim loai d6 dat dupc cdc tinh chat yeu ciu Nhi^t d$ phan -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 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: 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 phin 10, 20, 30, 40 50% ve khdi lupng Cac quy trinh tidp theo 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 ISSN 086« 7056 TAP CHf CO KHI V I £ T SAM, S6 nam 2016 NGHieNCD'U-TRAO Ddi Ktr QUA VA THAO LUAN trudng hpp nay, hpp kim chiia mdt phan pha ^Ti, Ti, Nb va Zr 3.f Pha va to chuc te vi cua miu sau thieu kit Hinh 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 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 thieu ket da dien hoan toan Hinh Gidn dd nhieu xg Ranghen ciia hgp kim Ti3.5Nb3.SZr scm thieu kit hai bu&c cAdn khdr^ Kdt qua kidm tra phin pha va td chiic te vi khing dinh, cac mau che tgo bfing phuang phap hai budc chan khdng cao dat ydu cau dd nghidn ciiu iing sii ca hpc TSng ty Hinh4.AnhSEMhgpkimTiH,3.5Nb3.5Zrsau thieu ket hai bu&c chdn khdng Gian dd nhteu xg ciia tit ca cfic mau sau 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, 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, dd pha p-Ti da xult hifn (tgi 28 = 39"), pha p-Ti tdn tgi 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 y hpc Trong Hinh 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 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 nam www.coklilvietnam.vn 2016 NGHieNCCrU-TRAODOl vat lipu Tinh chit ca hpc ty trpng thay ddi biin d?ng dupc md td bing cac cdng thitc Gibson vd Ashby phdt triin [6,7], nhu sau: Tai vimg dan hdi tuyen tinh: (2) £, IftJ Tai viing dan hdi - nhdt: 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 vimg ddn hdi nhdt, dp ciing kD Id ham mu cua thdng so bien dang, dupc viit nhu sau [10]: E* va ES - Modun dan hdi cua vft lifu d mpt dp xdp nhit dinh va 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$c; C, va C, - cac hing sd xae dinh tir thpc nghifm (trong hau het cac trudng hpp C, = and Cj = 0.3 [8]) (4) i„(e) = r ( l - e ' ) ' (3) Sau cdc ph^p bien ddi todn hpc vd dp dung tdc dp biin d?ng e = 1, md hinh todn hpc dupc dua nhu sau: ^ ( - i ^ i all) ^-|A:, + 7(l-f')"]r(5) k, c, kp Y - Cdc thdng so cua md hinh k, va kp dupc xdc dinh tir dp ddc viing lvd2; c - liTng suit vdng dan h^i-nhdt; Y vd n dupc xdc djnh bdng phuong phdp binh phuong cue tiiu, tir cdc s6 li$u ti£n dudng cong dng suit - bien dang, gid tri cila cac thdng so md hinh dupc thi hipn d t)dng 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 hf dupc noi song song (hinh 6) LTng xir ca hpc cua h^ vat li$u xop sau thieu kit khdng sir dyng chat phy gia, dupc xip vdo loai bien dang ddn hdi - nhdt Ddi vdi cdc mau cd sur dyng chat phy gia tao xdp NH^HCO,, tren dudng cong img suat -biin dang (hinh 7), khdng tdn t?i viing din hoi - nhdt vd vimg tdng ty trpng, vdt lipu ddn, bj phd huy trudc vdch kim loai biin d^g die Hinh Md hinh tuang lu doi v&i vgt ligu xdp [9] He thii nhit, bao gdm Id xo (dp cirng k) va piston (dp nhdt c), ddy chinh Id md hinh Maxwell, hp so k cua Id xo tucmg img vdi modun dan hdi cua vdt lipu xdp tai viing ddn Bdng I Cde Ihdng sd md hinh: 9.3 ISSN08««-705< TAP CHI CO KHl V I £ T NAM, Sd ndm www.cokhivietnam.vn 2016 MPa MPa T IMPa c, MPt D 9515 1485 2.5 315 NGHIEN CO-U-TRAO D O I 09x^:18.6% Md hinhj>hii hpp doi vdi cac mau che tao khdng cd chat php gia Cac hf sd md hinh da dupc xae djnh tii dudng cong quan hf ling suat - bien dang 04 xdp: 45% I - KETLUv^N Hpp kim titan Ti3.5Nb3.5Zr vdi cac df xdp khac tCr (10-50%) da dupc chd tgo cdng bfing phuang pimp thieu kit hai budc Pha Hinh Quan hg ieng sudt -biin dang eda hgp kim hinh tfaanh, cau true va cac tfnfa cfaat ca hpc dap xop Ti3.5Nb3.5Zr ed ehdi phg gia tgo xdp Ihieuimg kit ydu cau cua vat lidu cay ghep y sinfa Bi^ndang Day Id d^uig dudng cong tdt phd biin cua kim loji xdp chi t^o bdng phuang phdp 6p-thi6u kit Svt khdc ve umg xir co hpc ciia mau khdng vd cd sit dung chat phy gia t?o xdp cd thi gidi thich nhu sau: Trudc thi6u kit, cdc chit phy gia dupc tr$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, 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 biin djmg deo Tiong dd, cdc lien kit d cdc mau Ichdng su dyng chit phy gia gin nhu khdng bj phd hiiy thur co tinh (mau khdng bi vd sau thd) Bdng2 Vgtliguxdp ri3.5Nb3.5Zr v&i ham lugng chat phg gia khde qud trinh thieu kit Chit phv gl«C/.) SO l i p ichdng CO 30 40 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 (bang 2), cac chi s^ ca tinh dupc xae dinh tii quan hf iing suit -biln dgng (hlnh va 7) M$c dil cac mau cd sir dpng chat php gia khdng tuan theo rod hhih trinh bay d trdn nhung cac tinh chat ddu thda mfin cac ydu clu doi vft lifu ciy ghdp y sinh Cac miu thieu ket cd chat php gia cd ling xu ca hpc thupc dgng vft lifu ddn, dudng cong quan hf lin^ suit - biln dgng chi thn tgi vimg dan hdi tuyen tinh, khdng tdn tgi vimg dan hdi nhdt va viing tfing ty trpng ^ Thdi gian thieu ket can dupc kdo dai ban ddi vdi tat ca cac mau de dgt dupc tinh ddo cho vat lieu xop • Ngay nhgn bai: 05/7/2016 Ngay phan bifn: 12/8/2016 Tai Ufu tham Ichao: [I].TrabecuIar Metal Materials, Metal Implant dental Materials Brochure [2] Zena J Wally, Wlliam van Gninsven, Frederik Claeyssens, Russell Goodall and Gwendolen C Reilly, Porous Titanium for t)ental Implant Applications Metals, 5, 2015, 1902-1920 [3], A.E Aguilar Maya, D.R Grana, A Hazarabedian, GA Kokubu, M.I Luppo, G Vigna, 2r-Ti-Nb porous alloys for biomedical applic^rai Mater Sci Eng C, 32,2012, pp321-329 [4] Nguyin DJng Thiiy, TVAn VSn DQng, NguyJn V5n To4n, Hoa Xuan Hoa; Nghien cuu cong nghf chi lgo Vgi lifu xop TiNb3Zr3 Ij^g phmmg phdp phdn thiiu ket, T?p chl Khoa hpc C6ng ngh$ 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 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 Properties Pe^amon 3.Press, Oxford, United Kingdom, 1988 [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 T ^ CHl CO KHl VI|T NAM, Sd nfim 2016 www.cokliivietnam.vn ... bpt kim loai mdi lan phdi li|u la 20 g, vdi timg 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. .. Hinh4.AnhSEMhgpkimTiH,3. 5Nb3 .5Zrsau thieu ket hai bu&c chdn khdng Gian dd nhteu xg ciia tit ca cfic mau sau thieu ket cho thay, khdng tdn tgi cac pha TiHj va cac oxit ciia Ti, Nb hofic Zr, dieu dd... 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, dd pha p -Ti da xult hifn (tgi 28 = 39"), pha p -Ti tdn tgi hpp kim titan xdp,
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