Luận án nghiên cứu tổng hợp màng hydroxyapatit bằng phương pháp điện hóa trên nền thép không gỉ 316l có và không có màng titan nitrua

B GIO DC V O TO VIN HN LM KHOA HC V CễNG NGH VIT NAM HC VIN KHOA HC V CễNG NGH ***** PHM TH NM NGHIấN CU TNG HP MNG HYDROXYAPATIT BNG PHNG PHP IN HểA TRấN NN THẫP KHễNG G 316L Cể V KHễNG Cể MNG TITAN NITRUA Chuyờn ngnh: Húa lý thuyt v Húa lý Mó s: 62440119 LUN N TIN S HểA HC H Ni 2016 I B GIO DC V O TO VIN HN LM KHOA HC V CễNG NGH VIT NAM HC VIN KHOA HC V CễNG NGH ***** PHM TH NM NGHIấN CU TNG HP MNG HYDROXYAPATIT BNG PHNG PHP IN HểA TRấN NN THẫP KHễNG G 316L Cể V KHễNG Cể MNG TITAN NITRUA Chuyờn ngnh: Húa lý thuyt v Húa lý Mó s: 62440119 LUN N TIN S HểA HC NGI HNG DN KHOA HC PGS.TS inh Th Mai Thanh PGS.TS Trn i Lõm H Ni 2016 II LI CM N Tụi xin by t lũng bit n sõu sc ti PGS.TS inh Th Mai Thanh v PGS.TS Trn i Lõm ó ch o, hng dn tn tỡnh, sõu sỏt v giỳp tụi sut quỏ trỡnh thc hin cng nh hon thnh bn lun ỏn ny Tụi xin chõn thnh cm n cỏc ng nghip ti Phũng n mũn v bo v kim loi Vin K thut nhit i, Vin Hn lõm KH&CN VN ó luụn ng viờn v giỳp tụi quỏ trỡnh thc hin lun ỏn Tụi xin trõn trng cm n Ban Lónh o v B phn o to Vin K thut nhit i ó giỳp tụi sut thi gian hc tp, nghiờn cu v hon thnh lun ỏn Tụi xin trõn trng cm n Vin Khoa hc vt liu, Vin V sinh dch t Trung ng, Vin Cụng ngh ng dng, Hc Vin K thut Quõn s, i hc Bỏch khoa H Ni, i hc Pierre v Marie Currie (Phỏp) v Vin CIRIMAT (Phỏp) ó giỳp quỏ trỡnh thc hin lun ỏn Cui cựng, tụi xin chõn thnh cm n ti ton th gia ỡnh v bn bố ó luụn ng viờn, chia s v giỳp tụi sut thi gian thc hin lun ỏn H Ni, thỏng nm 2016 Tỏc gi lun ỏn Phm Th Nm i LI CAM OAN Tụi xin cam oan rng tt c cỏc s liu, kt qu trỡnh by lun ỏn ny l trung thc v cha cú cụng b bt k cụng trỡnh no khỏc Tỏc gi lun ỏn Phm Th Nm ii MC LC Trang DANH MC CC Kí HIU V CH VIT TT vii DANH MC CC BNG ix DANH MC CC HèNH V, TH xi M U CHNG 1: TNG QUAN 1.1 Tng quan chung v titan nitrua(TiN) 1.1.1 Tớnh cht ca TiN 1.1.1.1 Tớnh cht vt lý 1.1.1.2 Tớnh cht húa hc 1.1.2 Mt s phng phỏp tng hp mng TiN 1.1.3 ng dng ca TiN 1.2 Tng quan chung v hydroxyapatit (HAp) 1.2.1 Tớnh cht ca HAp 1.2.1.1 Tớnh cht vt lý 1.2.1.2 Tớnh cht hoỏ hc 11 1.2.1.3 Tớnh cht sinh hc 12 1.2.2 Cỏc phng phỏp tng hp HAp 14 1.2.2.1 Dng bt 14 1.2.2.2 HAp dng xp v gm xp 15 1.2.2.3 HAp dng compozit 16 1.2.2.4 HAp dng mng 17 a Phng phỏp vt lý 17 b Phng phỏp in húa 19 1.2.3 Th nghim dung dch mụ phng dch c th ngi iii (SBF) 25 1.2.4 Vai trũ v ng dng ca HAp 30 1.2.4.1 ng dng ca HAp bt 31 1.2.4.2 ng dng ca HAp dng gm xp 31 1.2.4.3 ng dng ca HAp dng composit 31 1.2.4.4 ng dng ca HAp dng mng 32 1.2.4 Tỡnh hỡnh nghiờn cu nc 34 CHNG 2: IU KIN V PHNG PHP THC NGHIM 38 2.1 Húa cht v iu kin thc nghim 38 2.1.1 Húa cht 38 2.1.2 Tng hp mng TiN bng phng phỳn x magnetron mt chiu 38 2.1.3 Tng hp in húa HAp trờn nn TKG316L 39 2.1.4 Tng hp in húa HAp trờn nn TiN/TKG316L 39 2.1.5 Th nghim dung dch SBF 40 2.2 Cỏc phng phỏp nghiờn cu 41 2.2.1 Cỏc phng phỏp in húa 41 2.2.1.1 Phng phỏp quột th ng 41 2.2.1.2 Phng phỏp th tnh (in th ỏp t) 42 2.2.1.3 Phng phỏp o in th mch h theo thi gian 42 2.2.1.4 Phng phỏp tng tr in húa 42 2.2.2 Cỏc phng phỏp phõn tớch 43 2.2.2.1 Phng phỏp ph hng ngoi (IR) 43 2.2.2.2 Kớnh hin vi in t quột (SEM) 43 2.2.2.3 Tỏn x nng lng tia X (EDX) 43 2.2.2.4 Nhiu x tia X (XRD) 44 2.2.2.5 Kớnh hin vi lc nguyờn t (AFM) 44 iv 2.2.3 Cỏc phng phỏp o tớnh cht c lý ca mng TiN v mng HAp 44 2.2.3.1 cng Vickers 44 2.2.3.2 o búng ca mng TiN 45 2.2.3.3 o mi mũn ca mng TiN 45 2.2.3.4 o bn va p ca mng TiN 46 2.2.3.5 Modul n hi ca mng TiN 46 2.2.3.6 bn un ca mng TiN 46 2.2.3.7 o bỏm dớnh ca mng HAp 47 2.2.3.8 o chiu dy ca mng HAp 47 2.2.4 Chun H2O2 47 CHNG KT QU THO LUN 48 3.1 Tng hp v c trng ca mng HAp/TKG316L 48 3.1.1 nh hng ca nng dung dch 48 3.1.2 nh hng ca khong quột th 51 3.1.3 nh hng ca H2O2 54 3.1.4 nh hng ca nhit 57 3.1.5 nh hng ca s ln quột th 62 3.1.6 nh hng ca tc quột 65 3.1.7 Xỏc nh thnh phn, chiu dy v g gh b mt ca mng HAp 68 3.2 Tng hp v c trng ca mng HAp/TiN/TKG316L 70 3.2.1 c trng ca nn TiN/TKG316L 70 3.2.1.1 Phõn tớch hỡnh thỏi cu trỳc v thnh phn 70 3.2.1.2 Tớnh cht c lý ca vt liu TiN/TKG316L 72 a cng 72 b bn va p 73 v c búng 74 d bn mi mũn 74 e Mụ un n hi 75 f bn un 75 3.2.2 Kho sỏt cỏc yu t nh hng n quỏ trỡnh n quỏ trỡnh tng hp HAp trờn nn TiN/TKG316L 76 3.2.2.1 nh hng ca nng H2O2 76 3.2.2.2 nh hng ca in th tng hp 81 3.2.2.3 nh hng ca nhit 83 3.2.2.4 nh hng ca pH . 88 3.2.2.5 nh hng ca thi gian tng hp 90 3.2.2.6 Phõn tớch chiu dy, g gh b mt v thnh phn ca mng HAp 3.3 Th nghim vt liu TKG316L, 92 HAp/TKG316L, TiN/TKG316L V HAp/TiN/TKG316L dung dch mụ phng dch c th ngi 94 3.3.1 Xỏc nh pH ca dung dch SBF theo thi gian ngõm 94 3.3.2 in th mch h 96 3.3.3 o in tr phõn cc 99 3.3.4 Tng tr in húa 103 3.3.5 Xỏc nh tn hao lng ca mu ngõm SBF 105 3.3.6 Phõn tớch c trng húa lý ca mng apatit hỡnh thnh dung dch SBF 106 KT LUN CHUNG 112 NHNG ểNG GểP MI CA LUN N 113 DANH MC CC CễNG TRèNH KHOA HC CễNG B 114 TI LIU THAM KHO 115 vi DANH MC CC Kí HIU V CH VIT TT AFM ASTM CVD DCPD DC DLC dE/dt EDX Eocp, Eo Ecorr Eb Ep HAp HAp/TKG316L : : : : : : : : : : : : : : HAp/TiN/TKG316L : HV Icorr IR ISO PLA PLA/HAp PVD Ra Ru Rp RF SEM : : : : : : : : : : : : Kớnh hin vi lc nguyờn t Tiờu chun vt liu ca M Phng phỏp lng ng hi húa hc icanxi phosphat ihydrat (CaHPO4.2H2O) Phỳn x phúng in mt chiu Cacbon vụ nh hỡnh cú tớnh cht ging kim cng S bin i in th theo thi gian Tỏn x nng lng tia X in th mch h in th n mũn in th phúng in in th th ng Hydroxyapatit Mng hydroxyapatit ph trờn nn thộp khụng g 316L Mng hydroxyapatit ph trờn nn t hp ca mng titan nitrua ph trờn nn thộp khụng g 316L cng Vickers Mt dũng n mũn Ph hng ngoi T chc tiờu chun húa quc t Polyaxit lactic Compozit ca polyaxit lactic v hydroxyapatit Phng phỏp lng ng hi vt lý Thụng s nhỏm b mt bn un in tr phõn cc Phỳn x phúng in xoay chiu Kớnh hin vi in t quột vii SBF SCE TKG316L TiN TiN/TKG316L TEM V/SCE XRD Z .cm o C : : : : : : : : : : : Dung dch mụ phng dch c th ngi in cc so sỏnh calomen bóo hũa Thộp khụng g 316L Titan nitrua Mng titan nitrua ph trờn nn thộp khụng g 316L Kớnh hin vi in t truyn qua n v in th so vi in cc calomen Nhiu x tia X Mụ un tng tr n v 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