Ổn định quy trình chế tạo màng áp điện PZT với chất lượng cao bằng phương pháp quay phủ solgel.

LI LI CAM CM OAN N tiờnõy tụi xin by t lũng kớnh trng v riờng bit n scsnht n dn PGS.TS TụiLi camu oan: l cụng trỡnh nghiờn cu ca tụisõu di hng ca V Ngc v TS Nguyn Minh,c nhng ngi tỡnho hng dn, t PGS TS Hựng V Ngc Hựng v TS.c Nguyn Minh, thcThy hinó titn Vin to Quc giỳp v toVt mi iu kin ITIMS, thun liTrng cho tụii thi gianH thc hin lun v Khoa hc liu Vin hcsut Bỏch Khoa Ni Cỏc s ỏn liuCỏc v Thy thc s l nhng nh khoa hc mu mc, luụn quan tõm, ng viờn v khớch l tụi kt qu lun ỏn l hon ton trung thc v cha tng c cụng b bt k gp khú khn c cụng vic v cuc sng, cựng hc trũ chia s c tht bi cụng trỡnh no ln thnh cụng Cỏc Thy ó truyn cho tụi ng lc v nim hnh phỳc ln lao luc ỏn nghiờn cu v khỏm phỏ khoa hc, bit vt qua khú khn hon thnh Tỏclun ỏn nghiờn cu vi cỏc Thy, tụi hc cỏc Thy tinh thn tn ty vi hc trũ v nghiờm tỳc nghiờn cu khoa hc, hin ti v tng lai Tụi xin trõn trng cm n B Giỏo dc v o to, Trng i hc Bỏch Khoa H ni, Vin o to Quc t v Khoa hc Vt liu (ITIMS), Trng i hc Lõm nghip ó to iu kin thun li v thi gian, vt cht cng nh tinh thn tụi thc hin PGS TS V N H N T Q lun ỏn C Tụi xin cm n PGS TS Trnh Quang Thụng, TS Chu Mnh Hong, TS V Thu Hin, Th S Nguyn Thanh Hng, ThS Phm Ngc Tho, C nhõn Nguyn Ti ó thng xuyờn quan tõm v ng viờn cng nh ó cú nhiu bn lun khoa hc v ý kin úng gúp quý giỏ cho tụi quỏ trỡnh thc hin lun ỏn Tụi xin cm n th cỏn b B mụn Vt lý, Khoa C in v cụng trỡnh, Trng i hc Lõm nghip ó ng viờn, chia s v giỳp tụi sut thi gian qua Tụi cng xin c cm n bn bố, ng nghip v ngi thõn ó ng viờn, giỳp tụi tụi cú iu kin thc hin lun ỏn Cui cựng, tụi xin gi ti nhng ngi thõn yờu gia ỡnh nh ca tụi lũng bit n vt ngoi gii hn ca ngụn t S ng viờn, h tr v hy sinh thm lng ca chng, con, anh em thc s th hin nhng tỡnh cm vụ giỏ, l ngun ng lc tinh thn vụ cựng mnh m giỳp tụi kiờn trỡ vt qua khú khn, tr ngi i n thnh cụng Mong rng hai Bo Ngõn Nguyt Anh s n lc hc hn na ti thnh cụng trờn ng hc H Ni, ngy thỏng nm 20 Tỏc gi iii MC LC Trang LI CAM OAN i LI CM N ii DANH MC CC Kí HIU vi BNG DANH MC THUT NG viii DANH MC CC BNG xi DANH MC CC HèNH NH, TH xii GI I THIU LUN N M N í 3.1 ngh a khoa hc 3.2 Nhng úng gúp mi ca lun ỏn B CHNG L C S Lí THUYT 1.1.1 Phõn cc t phỏt 1.1.1.1 Tớnh i xng 1.1.1.2 Hin tng st in 1.1.1.3 Hin tng phn st in 1.1.1.4 Hin tng in 1.1.1.5 Hin tng ỏp in 1.1.2 Lý thuyt chuyn pha st in Ginzburg-Landau 10 1.1.3 Gii thiu vt liu st in 14 1.1.4 ụ men st in 16 1.1.4.1 S hỡnh thnh ụ men 16 1.1.4.2 Cu tr c ụ men t nh ca vt liu mng mng 18 1.1.4.3 Phõn b v c t phõn cc 19 1.1.4.4 Chuyn vỏch ụ men st in 20 1.1.5 Hin tng ghim ụ men 21 T PZT 22 1.2.1 nh hng ca thnh phn pha 22 1.2.2 S ph thuc vo nh hng ca mng 25 1.2.3 B dy, lp tip x c v kớch thc ht 28 iii 1.2.4 Chuyn ng ụ men (Hỡnh thnh ụ men/ hỡnh thnh v dch chuyn vỏch ụ men) 31 1.2.5 Tớnh cht mi 33 1.2.6 nh hng ca cu tr c d lp n tớnh cht ca mng mng PZT 34 1.2.7 nh hng ca cht n cu tr c, tớnh cht ca mng mng PZT 35 M K CHNG PZT 40 41 CễNG NGH CH TO V CC PHNG PHP NGHIấN CU 43 P PZT 43 2.1.1 Tng quan v phng phỏp ch to sol-gel 43 2.1.2 Ch to mng mng PZT bng phng phỏp quay ph sol-gel 45 2.1.2.1 Vt liu to sol 45 2.1.2.2 Quy trỡnh cụng ngh sol-gel ch to mng mng PZT 45 2.1.2.3 Quay ph to mng 46 P 47 2.2.1 Phng phỏp xỏc nh cu tr c ca mng mng 47 2.2.1.1 Nhiu x tia X (XRD) 47 2.2.1.2 Cỏc phng phỏp xỏc nh hỡnh thỏi cu tr c b mt 48 2.2.2 Cỏc phng phỏp kho sỏt tớnh cht st in - ỏp in 49 2.2.2.1 Phng phỏp kho sỏt tớnh cht st in 49 2.2.2.2 Phng phỏp kho sỏt tớnh cht in mụi 51 2.2.2.3 Phng phỏp kho sỏt tớnh cht ỏp in 52 C 54 2.3.1 Phng phỏp n mũn khụ 57 2.3.2 Phng phỏp n mũn t 57 K 57 CHNG NGHIấN CU TNH CHT CA MNG MNG SOL-GEL PZT 59 T PZT 59 3.1.1 nh hng ca nhit 59 3.1.2 nh hng ca chiu dy mng mng PZT 63 N K PZT rỳ 67 77 CHNG NGHIấN CU NH HNG CA PHA TP Fe3+ v Nb5+ N TNH CHT CA MNG MNG PZT 79 4.1 Fe3+ iv PZT, PFZT/PZT 79 4.1.1 nh hng ca Fe3+ n tớnh cht ca mng mng PZT 79 4.1.2 nh hng ca Fe3+ n tớnh cht ca mng mng d lp PFZT/PZT 84 K Nb5+ PZT 86 91 CHNG NGHIấN CU NG DNG CH TO LINH KIN PIEZOMEMS 93 rỡ ũ 95 5.1.1 n mũn lp in cc 95 5.1.2 n mũn mng mng PZT 97 L b r 101 5.2.1 Linh kin cm bin kiu rung 101 5.2.1.1 Kt qu ch to linh kin dng rung 101 5.2.1.2 Kho sỏt tớnh cht ca linh kin 105 5.2.2 Linh kin dng mng chn 108 5.2.2.1 Kt qu ch to linh kin dng mng chn 108 5.2.2.2 Kho sỏt tớnh cht ca mng chn 109 K C b rờ r 112 118 KT LUN CHUNG 120 XUT: 121 TI LIU THAM KHO 123 v DANH MC CC Kí HIU K N xf rng ca mt na ng cong tn s cng hng c bn (Fundamental resonance frequency curve) x , x0 Hng s in mụi mụi trng v chõn khụng x in tr sut ca mng x x Dung sai A Din tớch bn t C in dung D Khong cỏch gia hai bn t (b dy ca mng) dijk Mụun ỏp in E, ED cm in mụi in trng ngoi, in trng kh phõn cc Ej Thnh phn ca v ct cng in trng fr Giỏ tr ng vi nh ca ng cong tn s cng hng k H s liờn kt in c k Hng s Boltzmann k15 H s liờn kt xon k31 H s liờn kt ngang k33 H s liờn kt theo chiu dy kij Cỏc thnh phn ca h s liờn kt in c kp H s liờn kt b mt kt H s liờn kt theo chiu di Np , Nt Hng s tn s cỏc mode dao ng theo bỏn kớnh v theo chiu dy (Hz.m) PFZT Pb([Zr0.52Ti0.48]Fe)O3 Pr, Ps phõn cc d, bóo hũa Q H s phm cht Qe phm cht cng hng in Qm phm cht c R RA, RB, RO RS in tr thun ca mng mng PZT Bỏn kớnh cation Pb2+, cation Zr4+/Ti4+, anion O2in tr dõy ni vi sE , sD Sut n hi tng ng vi iu kin in trng khụng i v mt in tớch khụng i (10-12 m2/N) Sjk Thnh phn ca Tenx bin dng T Nhit tuyt i T tan x Nhit (C, K) Tang gúc tn hao Tc Nhit Curie TC Nhit chuyn pha (C, K) Tjk Thnh phn ca Tenx ng sut Tm Nhit ng vi hng s in mụi cc i (C, K) U in th vii BNG DANH MC THUT NG T N A space-charge model Mụ hỡnh vựng khụng gian in tớch Actuators Linh kin chp hnh AF Antiferroelectric phase (pha khụng st in hay pha cht) AFM Atomic Force Microscopy (kớnh hin vi lc nguyờn t) Antibody Phn dựng gn kt Antigen Cht cn phõn tớch Ar-beam dry etching n mũn khụ bng chựm tia Ar Atomic concentration Nng nguyờn t Cantilever length Chiu di linh kin Chrome mask Lp mt l Chrome Coil Cun lũ xo CSD Chemical solution deposition (dung dch húa hc) CVD Chemical vapor deposition (phng phỏp lng ng t pha hi) Dipole Lng cc st in Displacement dch chuyn Downward displacement dch chuyn theo chiu xung di DRIE Deep reactive-ion etching (thit b quang khc) DTA Differential Thermal Analysis (phõn tớch nhit vi sai) Effective area Phm vi hot ng ca linh kin Etch rate Tc n mũn Ferroelectric domain ụ men st in Ferroelectric phase Pha st in Ferroelectric Random Acces Memory (b nh truy cp ngu FRAM nhiờn st in) Field Emission Scanning Electron Microscopy (phng phỏp FE-SEM chp nh hin vi in t qu t phỏt x trng) Gas pressure p sut khớ viii Gas pressure p sut khớ Heterolayers Cu tr c d lp Hydrochloric acid A xớt HCl Hydrofluoric acid A xớt HF Inert passivation layer Lp th ng tr In-plane transverse H s bin dng mng cỏc lp phõn biờn th ng piezo coefficient Interfacial passive layers Lp phõn biờn th ng Mask Mt n bo v MBE Molecular beam epitaxy (phng phỏp epitaxy chựm phõn t) Membrane Linh kin dng mng chn MEMS Micro Electro Mechanial Systems (h thng vi c in t) MHDA Phõn t 16-Mercaptohexadecanoic a xớt (HS-(CH2)15-COOH) Microactuator Vi chp hnh Microscope nh hin vi quang hc Microsensor Vi cm bin MPB Morphotropic Phase Boundary (biờn pha hỡnh thỏi) P40 Pb(Zr0.4Ti0.6)O3 P60 Pb(Zr0.6Ti0.4)O3 Paraelectric cubic Pha khụng st in lp phng PFZT Pb([Zr0.52Ti0.48]Fe)O3 Photoresist Lp bo v Piezo Lp hot ng Piezoresponse force microscopy (kớnh hin vi lc hi ỏp ỏp PFM in) Piezoelectric cantilever Thanh rung ỏp in PNZT Pb(Zr0.52Ti0.48)1-xNbxO3 Polarization loop ng cong in tr Prostate-specific antigen (mt cht gõy bnh ung th PSA ngi) Pyrochlore A2B2O7 Pyrochlore phase (pha thiu chỡ) PZT Loi gm, mng cú cụng thc Pb(TixZr1-x)O3 ix Rhombohedral Cu tr c trc thoi Residue Cht cn SAM Self-assembled monolayers (phn t lp rỏp n lp) SEM Scaning Electro Microscopy (hin vi in t qu t) Sensors Linh kin c dng cm bin Silicon cantilever- beam Linh kin dng rung Silicon membrane Linh kin dng mng chn SOI Silicon on Insulators (phin Silic dng SOI) Sputter time Thi gian tỏn x SRO SrRuO3 TEM Hin vi in t truyn qua Tetragonal Cu tr c t giỏc X-ray 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627-632 143 144 [...]... công màng áp điện có các cấu trúc và tính chất đặc trưng như mong muốn Cấu trúc và tính chất của màng áp điện phụ thuộc vào nhiều yếu tố khác nhau như phương pháp chế tạo, lớp tiếp xúc, lớp điện cực hay sự pha tạp ion Hiện nay có nhiều phương pháp được sử dụng trong việc chế tạo màng áp điện theo cả hai phương pháp: phương pháp vật lý và phương pháp hóa học Các phương pháp vật lý bao gồm phương pháp. .. như sau: o Ổn định quy trình chế tạo màng áp điện PZT với chất lượng cao bằng phương pháp quay phủ sol-gel o Tích hợp màng PZT vào thanh rung silic nhằm chế tạo các linh kiện cảm biến với kích thước micro-mét o Định hướng ứng dụng của linh kiện cảm biến trong việc phát hiện các hợp chất cần phân tích trong l nh vực y - sinh học Luận án được nghiên cứu bằng phương pháp thực nghiệm, kết hợp với phân tích... 178], phương pháp bốc bay xung laser (PLD) [220, 210, 125, 53, 135] và phương pháp lắng đọng chùm phân tử epitaxy (MBE) [238] Trong số các phương pháp hóa học có phương pháp lắng đọng pha hơi hợp chất kim loạihữu cơ (MOCVD) [32, 249], phương pháp lắng đọng hơi hóa học bằng plasma (PECVD) [73, 72] và phương pháp quay phủ sol-gel [245, 75, 8, 78, 216] Trong các phương pháp này thì phương pháp quay phủ. .. (d31,f) của thanh rung áp điện trên cơ sở màng mỏng PZT chế tạo bằng phương pháp quay phủ solgel Chiều rộng của các thanh rung là 100 µm 107 5.19 Sự phụ thuộc của hệ số phẩm chất Q vào chiều dài của thanh rung áp điện trên cơ sở màng mỏng PZT chế tạo bằng phương pháp phương pháp quay phủ sol-gel Chiều rộng của các thanh rung là 100 µm 107 5.20 Cấu tr c và mặt cắt ngang của linh kiện dạng màng chắn 108 5.21... trong quá trình chế tạo linh liện thanh rung bằng phương pháp quang khắc 104 5.16 (a) Đường cong sắt điện - điện áp (P-E) và (b) dòng điện (switching current) – điện áp, của cấu tr c dạng tụ điện và thanh rung 105 5.17 a) Ảnh hiển vi quang học và (b) độ dịch chuyển của thanh rung áp điện với màng mỏng PZT được chế tạo bằng phương pháp quay phủ sol-gel 105 5.18 Ảnh hưởng của chiều dài đến hệ số áp điện ngang... là phương pháp yêu cầu thiết bị đơn giản, rẻ tiền và có thể dễ dàng thay đổi thành phần màng cũng như phù hợp với điều kiện công nghệ hiện nay ở Việt Nam Tuy nhiên nhược điểm của phương pháp này là mật độ kết khối thấp và màng thường bị nứt gẫy trong quá trình chế tạo 1 Trong luận án này, màng sắt điện – áp điện PZT đã được chế tạo trên đế silic bằng phương pháp quay phủ sol-gel Quy trình công nghệ chế. .. chế tạo màng PZT đã được tối ưu hóa, trên cơ sở kế thừa và phát triển các kết quả của các nghiên cứu trước, nhằm thu được các màng có chất lượng với độ ổn định cao Màng sau khi chế tạo có mật độ kết khối cao và không bị nứt gẫy Việc cải thiện các tính chất sắt điện và áp điện của màng được nghiên cứu thông qua việc chế tạo màng với cấu trúc dị lớp (các lớp màng PZT có thành phần khác nhau được quay phủ. .. 5 Việc chế tạo thành công linh kiện cảm biến khối lượng với kích thước micro-m t trên cơ sở màng áp điện PZT sẽ gi p cho việc triển khai nghiên cứu phát hiện các hợp chất sinh học, đặc biệt là các phân tử chất gây ra bệnh ung thư ở người u Các vấn đề mới đặt ra trong nghiên cứu này là: (1) Chế tạo màng PZT bằng phương pháp quay phủ sol-gel (phương pháp hóa học) có chất lượng tốt và độ lặp lại cao, cho... tiếp xúc sắt điện – sắt điện (với thành phần khác nhau), ứng suất kéo trong cấu trúc giảm đi và cùng với sự hình thành một thế điện áp nội tại lớp tiếp x c đã làm tăng khả năng quay của các domain sắt điện Màng PZT sau đó được sử dụng trong việc chế tạo các linh kiện cảm biến khối lượng trên cơ sở các thanh rung áp điện Thanh rung áp điện, với kích thước micro-m t được chế tạo bằng phương pháp quang khắc,... trưng sắt điện – điện áp (P-E) của màng PZT với cấu tr c đa lớp và dị lớp 72 3.20 Ảnh hưởng của cấu tr c đa lớp và dị lớp đến (a) mômen sắt điện dư Pr và (b) hệ số áp điện d33 của màng mỏng PZT 73 3.21 Ảnh hưởng của chiều dày màng đến (a) mômen sắt điện dư Pr và (b) hệ số áp điện d33, của màng mỏng PZT với cấu tr c đa lớp và dị lớp xen kẽ 74 3.22 (a) Đường cong điện môi – điện áp và (b) Hằng số điện môi