I HC QUC GIA H NI TRNG I HC KHOA HC T NHIấN V MINH THNH NGHIấN CU CH TO COMPOZIT CACBON-CACBON CHA CT SI NG NANO CACBON NH HNG NG DNG TRONG CễNG NGH K THUT CAO LUN N TIN S: NGNH HO HC H Ni - 2016 I HC QUC GIA H NI TRNG I HC KHOA HC T NHIấN V Minh Thnh NGHIấN CU CH TO COMPOZIT CACBON-CACBON CHA CT SI NG NANO CACBON NH HNG NG DNG TRONG CễNG NGH K THUT CAO Chuyờn ngnh: Hoỏ lớ thuyt v húa lớ Mó s: 62 44 01 19 LUN N TIN S: NGNH HO HC NGI HNG DN KHOA HC: PGS TS Lờ Kim Long GS TS Nguyn c Ngha LI CM N Lun ỏn ny c thc hin v hon thnh ti B mụn Hoỏ lý, Khoa Hoỏ hc, i Hc Khoa hc T nhiờn, i hc Quc gia H Ni v Vin Hoỏ hc-Vt liu, Vin Khoa hc v Cụng ngh Quõn s, B Quc phũng Xin by t lũng bit n sõu sc n PGS.TS Lờ Kim Long, GS.TS Nguyn c Ngha, nhng ngi Thy ó nh hng khoa hc v tn tỡnh hng dn sut thi gian hc v thc hin lun ỏn ny Xin chõn thnh cm n B mụn Hoỏ lý, Khoa Hoỏ hc, i hc Khoa hc T nhiờn; i hc Giỏo dc, i hc Quc gia H Ni; Trung tõm Phỏt trin Cụng ngh cao, Vin Hn lõm Khoa hc v Cụng ngh Vit Nam; Vin Hoỏ hc-Vt liu; Phũng Gm-Kim loi-Hp kim; Phũng Hoỏ lý/Vin Hoỏ hc-Vt liu; cỏc ng nghip, ng ó giỳp v to iu kin nghiờn cu thun li cho tỏc gi thi gian thc hin lun ỏn Xin chõn thnh cm n PGS TS ng Vn ng, KS Phan Vn Bỏ, TS Nguyn Mnh Tng, ThS H Ngc Minh, TS Lờ Vn Th, TS Ngụ Quc Dng, ThS Ngụ Minh Tin, ThS on Tun Anh, ThS Ngụ Cao Long, KS Phm Tun Anh ó cựng tỏc gi tin hnh nhng thớ nghim ch to mu v tho lun úng gúp ý kin cho lun ỏn Cui cựng, xin gi li cm n ti gia ỡnh, ngi thõn, bn bố ó ng viờn, c v tụi hon thnh bn lun ỏn ny Nghiờn cu sinh V Minh Thnh i LI CAM OAN Tụi xin cam oan õy l cụng trỡnh nghiờn cu ca riờng tụi Cỏc s liu, kt qu c nờu lun ỏn l trung thc v cha c cụng b bt k cụng trỡnh no khỏc Nghiờn cu sinh V Minh Thnh ii MC LC LI CM N i LI CAM OAN ii MC LC iii DANH MC CC Kí HIU, CC CH VIT TT vi DANH MC BNG BIU vii DANH MC HèNH V viii M U CHNG TNG QUAN Error! Bookmark not defined 1.1 Tỡnh hỡnh nghiờn cu v ng dng vt liu compozit cacbon-cacbon trờn th gii v nc Error! Bookmark not defined 1.2 Vt liu compozit cacbon-cacbon Error! Bookmark not defined 1.2.1 Thnh phn compozit cacbon-cacbon Error! Bookmark not defined 1.2.1.1 ng nano cacbon (Carbon nanotubes-CNT)Error! Bookmark not defined 1.2.1.2 Si cacbon Error! Bookmark not defined 1.2.1.3 Vt liu nn cacbon Error! Bookmark not defined 1.2.2 Cu trỳc vt liu compozit cacbon-cacbonError! Bookmark not defined 1.2.3 Tớnh cht vt liu compozit cacbon-cacbonError! Bookmark not defined 1.3 Cụng ngh ch to vt liu compozit cacbon-cacbonError! Bookmark not defined 1.3.1 Phng phỏp pha khớ Error! Bookmark not defined 1.3.2 Phng phỏp pha lng Error! Bookmark not defined 1.3.3 Phng phỏp kt hp Error! Bookmark not defined 1.4 To mng ph chu nhit, chng xúi mũn cho compozit cacbon-cacbonError! Bookmark n CHNG I TNG V PHNG PHP NGHIấN CUError! Bookmark not def 2.1 Nguyờn vt liu, hoỏ cht Error! Bookmark not defined 2.2 Thit b Error! Bookmark not defined 2.2.1 Thit b ch to Error! Bookmark not defined 2.2.2 Thit b phõn tớch Error! Bookmark not defined iii 2.3 Thc nghim Error! Bookmark not defined 2.3.1 Bin tớnh b mt CNT Error! Bookmark not defined 2.3.2 X lý nhit b mt si cacbon Error! Bookmark not defined 2.3.3 S ch bt graphit Error! Bookmark not defined 2.3.4 Tng hp nha nn phenolformaldehit dng novolacError! Bookmark not defined 2.3.5 Ch to compozit cacbon-cacbon Error! Bookmark not defined 2.3.6 Ph chng oxi hoỏ b mt nhit caoError! Bookmark not defined 2.4 Phng phỏp nghiờn cu Error! Bookmark not defined 2.4.1 Phng phỏp hin vi in t quột ph tỏn sc nng lng tia X (SEMEDX) v kớnh hin vi in t quột phỏt x trng (FESEM)Error! Bookmark not define 2.4.2 Phng phỏp hin vi in t truyn qua (TEM)Error! Bookmark not defined 2.4.3 Phng phỏp phõn tớch nhit (DSC/TGA)Error! Bookmark not defined 2.4.4 Phng phỏp ph hng ngoi (FT-IR) Error! Bookmark not defined 2.4.5 Phng phỏp nhiu x Rnghen (XRD) Error! Bookmark not defined 2.4.6 Phng phỏp phõn tớch c ht Error! Bookmark not defined 2.4.7 Phng phỏp cõn thy tnh Error! Bookmark not defined 2.4.8 Phng phỏp xỏc nh tớnh cht c hc ca vt liuError! Bookmark not defined 2.4.9 Kim tra kh nng chu sc nhit v xúi mũn ca vt liuError! Bookmark not def CHNG KT QU V THO LUN Error! Bookmark not defined 3.1 Kho sỏt v bin tớnh nguyờn liu u Error! Bookmark not defined 3.1.1 Kho sỏt v bin tớnh ng nano cacbon Error! Bookmark not defined 3.1.2 Kho sỏt tớnh cht ca si cacbon Error! Bookmark not defined 3.1.3 Kho sỏt tớnh cht ca bt graphit Error! Bookmark not defined 3.1.4 Tng hp v kho sỏt nha nn phenolformaldehit dng novolac (PF)Error! Bookm 3.2 Ch to compozit cacbon-cacbon Error! Bookmark not defined 3.2.1 Nghiờn cu ch to compozit trờn c s bt graphit, vi cacbon, CNTbt v nha PF Error! Bookmark not defined 3.2.1.1 nh hng ca hm lng nha PFError! Bookmark not defined 3.2.1.2 nh hng ca hm lng CNTbt Error! Bookmark not defined 3.2.1.3 nh hng ca ỏp lc ộp Error! Bookmark not defined iv 3.2.1.4 nh hng ca thi gian ộp Error! Bookmark not defined 3.2.2 Nghiờn cu quỏ trỡnh nhit phõn compozitError! Bookmark not defined 3.2.2.1 nh hng ca nhit Error! Bookmark not defined 3.2.2.2 nh hng ca tc nõng nhit Error! Bookmark not defined 3.2.2.3 nh hng ca thi gian nhit phõnError! defined Bookmark not 3.2.3 Nghiờn cu quỏ trỡnh thm cacbon t pha hiError! Bookmark not defined 3.2.3.1 nh hng ca nhit CVI Error! Bookmark not defined 3.2.3.2 nh hng ca thi gian CVI Error! Bookmark not defined 3.2.3.3 nh hng ca lu lng khớ Error! Bookmark not defined 3.2.3.4 nh hng ca hm lng CNT Error! Bookmark not defined 3.2.4 nh hng ca quỏ trỡnh x lý nhit n tớnh cht ca CCCError! Bookmark not d 3.2.5 To lp ph chng xúi mũn cho compozit cacbon-cacbonError! Bookmark not de 3.2.6 Kt qu th nghim thc t Error! Bookmark not defined KT LUN V KIN NGH Error! Bookmark not defined TI LIU THAM KHO 13 v DANH MC CC Kí HIU, CC CH VIT TT CCC Compozit cacbon-cacbon CCC0 Compozit cacbon-cacbon khụng cha ng cha CNTbt CCCCNT Compozit cacbon-cacbon cha ng cha CNTbt Cf Si cacbon CNT ng nano cacbon CNTbt ng nano cacbon bin tớnh CVD Quỏ trỡnh lng ng hoỏ hc t pha hi CVI Quỏ trỡnh thm cacbon t pha hi DTA Phõn tớch nhit vi sai F Formaldehit FESEM Kớnh hin vi in t quột phỏt x trng IR Ph hng ngoi MWCNT ng nano cacbon a tng P Phenol PAN Polyacrylonitril PF Phenolformaldehit SEM-EDX Kớnh hin vi in t quột-ph tỏn sc nng lng tia X SWCNT ng nano cacbon n tng XLN X lý nhit X-ray Nhiu x tia-X h xp h, % kớn xp kớn, % tng xp tng, % bk T trng biu kin vi DANH MC BNG BIU Bng 1.1 Tớnh cht c hc ca CNT v mt s vt liu thụng dngError! Bookmark not de Bng 1.2 S ph thuc tớnh cht ca pirocacbon vo nhit lng ngError! Bookmark no Bng 1.3 Tớnh cht nn cacbon trờn c s hc ớn thu c 900CError! Bookmark not de Bng 1.4 Tớnh cht ca mt s vt liu compozit cacbon-cacbonError! Bookmark not defin Bng 1.5 Tớnh cht ca compozit cacbon-cacbon ch to bng cỏc phng phỏp to pha nn khỏc Error! Bookmark not defined Bng 1.6 Mt s lp ph lng ng theo cụng ngh CVDError! Bookmark not defined Bng 1.7 Mt s tớnh cht v c tớnh ca ZrC Error! Bookmark not defined Bng 3.1 Phi liu cỏc mu compozit cú thnh phn nha PF thay iError! Bookmark not Bng 3.2 T trng biu kin, xp h, xp kớn ca cỏc mu compozit.Error! Bookmark Bng 3.3 Phi liu cỏc mu compozit cú thnh phn CNTbt thay iError! Bookmark not d Bng 3.4 T trng biu kin, xp h, xp kớn ca cỏc mu compozitError! Bookmark no Bng 3.5 Ch nhit phõn cỏc mu compozit Error! Bookmark not defined Bng 3.6 Ch nhit phõn cỏc mu compozit Error! Bookmark not defined Bng 3.7 Ch nhit phõn cỏc mu compozit Error! Bookmark not defined Bng 3.8 Mt s tớnh cht ca cỏc mu CCC2CNT trc v sau XLNError! Bookmark no Bng 3.9 Tớnh cht ca CCC0 trc v sau x lý nhit chu kError! Bookmark not de Bng 3.10 cng t vi ca mng ZrC Error! Bookmark not defined vii DANH MC HèNH V Hỡnh 1.1 S tng hp CNT bng phng phỏp CVD trờn xỳc tỏc kim loiError! Bookm Hỡnh 1.2 S quỏ trỡnh bin tớnh CNT bng axitError! Bookmark not defined Hỡnh 1.3 Ch to CNT polyme nanocompozit theo phng phỏp trựng hp In-situError! Bookm Hỡnh 1.4 Ch to CNT polyme nanocompozit theo phng phỏp trn hp dung mụi Error! Bookmark not defined Hỡnh 1.5 S quỏ trỡnh cacbon húa vi nhng phng ỏn kộo cng si khỏc nhauError! Bookm Hỡnh 1.6 Tng quan gia gii hn bn B v mụ un n hi E ca si cacbon trờn c s xenlulo Error! Bookmark not defined Hỡnh 1.7 S ph thuc ca gii hn bn kộo B v mụ un n hi ca si cacbon trờn c s hc ớn vo nhit x lý nhit Error! Bookmark not defined Hỡnh 1.8 S thay i gim lng theo nhit vi tc nung si khỏc nhau: - 0,5; - 15; - 2; - 4; - 8; - 25C/phỳtError! Bookmark not defined Hỡnh 1.9 S ph thuc lng riờng pirocacbon vo nhit b mt lng ngError! Bookm Hỡnh 1.10 S ph thuc lng riờng ca hc ớn vo nhit húa mmError! Bookmark n Hỡnh 1.11 S ph thuc lng riờng v nht ca hc ớn vo nhit húa mm khỏc (1-65C; 2-83C; 3-145C) vo nhit nungError! Bookmark not defined Hỡnh 1.12 Cu trỳc vt liu compozit cacbon-cacbonError! Bookmark not defined Hỡnh 1.13 S ph thuc bn kộo ca compozit cacbon-cacbon 3D vo nhit (1 - theo hng x; - theo hng z) Error! Bookmark not defined Hỡnh 1.14 S ph thuc ca h s dón n nhit (a) v dn nhit (b) ca vt liu compozit cacbon-cacbon 3D vo nhit (1 - lý thuyt; - thc nghim)Error! Bookmark not d Hỡnh 1.15 S chung ch to vt liu compozit cacbon-cacbonError! Bookmark not defi Hỡnh 1.16 S bung lũ phng phỏp ng nhit thu lng pirocacbonError! Bookmark not Hỡnh 1.17 S bung lũ phng phỏp gim nhit lng ng pirocacbon Error! Bookmark not defined Hỡnh 1.18 Chu k cacbon húa (a) v graphit húa (b) c trngError! Bookmark not define Hỡnh 1.19 Quỏ trỡnh hỡnh thnh lp ph bng cụng ngh CVDError! Bookmark not define Hỡnh 1.20 Thang im chy ca mt s hp chtError! 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(1998), , - .. , 318-382 c (Buranov I M., Vorobei V B (1998), Cụng ngh cỏc kt cu tờn la v hng khụng v tr t vt liu compozit, NXB "MGTU Bauman N E.", trang 318-392) 140 .., .., . (1994), - , , , 68-82 c (Bushuev Yu G, Persin M I, Sokolov V A (1994), S tay vt liu compozit cacbon-cacbon, NXB "Luyn kim", trang 68-82) 141 (1988), , , , 319-323 (Lyubin Dj (1988), S tay vt liu compozit, NXB "Ch to mỏy", trang 319-323) 142 ., (2007), , , , "-", 176-183 (Meleshko A I, Polivnhikov C P (2007), Cacbon, si cacbon, compozit cacbon, NXB "SAINZ-PRESS", trang 176-183) 143 (1988), : ., : , 125-133 (Fitzer E (1988), Si cacbon v compozit ca chỳng: bn dch t ting Anh, NXB "Hũa Bỡnh", trang 125-133) 144 . (2009), , 216226 (Tshurik A G (2009), Vt liu cacbon nhõn to, NXB "Perm", trang 216-226) 28 [...]... chí Khoa học công nghệ quân sự số 8, tr.113-117 3 Nguyễn Đức Nghĩa (2007), Hóa học Nano- Công nghệ nền và vật liệu nguồn, NXB Khoa học tự nhiên và công nghệ, Hà Nội 4 Nguyễn Hoa Thịnh, Nguyễn Đình Đức (2001), Vật liệu composite - Cơ học và công nghệ, NXB Khoa học và kỹ thuật 5 Lê Quốc Trung, Vũ Đình Khiêm, Ngô Cao Long, Lê Văn Thụ (2010), Công nghệ nano – Công nghệ của thể kỷ XXI, NXB Công an Nhân... Khôi (2005), Nghiên cứu công nghệ chế tạo màng mỏng giả kim cƣơng và ống nano cacbon bằng phƣơng pháp lắng đọng hóa học (CVD) và phƣơng pháp lắng đọng hóa học kết hợp sóng micromet (MWCVD), Báo cáo tổng kết đề tài NCKH&CN cấp Viện Khoa học và Công nghệ Việt Nam 2 Hồ Ngọc Minh, Trần Nhƣ Thọ (2010), “Một số kết quả nghiên cứu độ bền ở nhiệt độ cao của vật liệu compozit phenolic/vải cacbon, sử dụng làm vật... lửa đẩy chế tạo bằng CCC đƣợc phủ ZrC trƣớc và sau thử nghiệm Error! Bookmark not defined Hình 2.1 Sơ đồ khối quá trình chế tạo mẫu vật liệu compozit cacbon- cacbonError! Bookmark Hình 2.2 Sơ đồ công nghệ nhiệt phân Error! Bookmark not defined Hình 2.3 Sơ đồ công nghệ CVI Error! Bookmark not defined Hình 2.4 Sơ đồ công nghệ graphit hóa Error! Bookmark not defined Hình 2.5 Sơ đồ công nghệ tổng... nhiệt trong môi trƣờng không khí của CNT ban đầu (a) và CNT biến tính (b) Error! Bookmark not defined Hình 3.7 Trạng thái của CNT trƣớc và sau biến tính với thời gian sa lắng khác nhau Error! Bookmark not defined Hình 3.8 Hình ảnh vải và sợi cacbon sử dụng để nghiên cứu chế tạo compozit cacbon- cacbon Error! Bookmark not defined Hình 3.9 Giản đồ phân tích nhiệt lƣợng vi sai của mẫu sợi. .. liệu compozit, NXB "Chế tạo máy", trang 319-323) 142 Мелешко А И., Половников С П (2007), Углерод, углеродные волокна, углеродные композиты, Москва "САЙНС-ПРЕСС", 176-183 с (Meleshko A I, Polivnhikov C P (2007), Cacbon, sợi cacbon, compozit cacbon, NXB "SAINZ-PRESS", trang 176-183) 143 Фитцер Э (1988), Углеродные волокна и композиты: пер с англ., Москва: Мир, 125-133 с (Fitzer E (1988), Sợi cacbon và compozit. .. electrical properties of aligned carbon nanotube/carbon matrix composites", Carbon 75, pp 307-313 Tiếng Nga 138 Бервено А (2002), Создание новых углерод-углеродных композиционных 27 материалов с применением углеродных нанотрубок, Москва, Из-во МГТУ им.Н.Э Баумана, 160-255 c (Berveno A (2002), Chế tạo vật liệu compozit cacbon- cacbon thế hệ mới sử dụng ống nano cacbon, NXB "MGTU Bauman N E.", trang 160-255)... 300; 400; 500; 600 và 700oC trong môi trƣờng không khíError! Bookmark not Hình 3.12 Ảnh FESEM bề mặt gẫy của compozit G-CF-CNT/P đƣợc chế tạo từ sợi cacbon ban đầu (Cf), và xử lý ở 300; 400; 500; 600 và 700oCError! Bookmark not defined Hình 3.13 Bột graphit dùng gia cƣờng chế tạo compozit cacbon- cacbonError! Bookmark no Hình 3.14 Ảnh SEM bột graphit với độ phóng đại khác nhauError! Bookmark not defined... nhiệt lƣợng vi sai của mẫu sợi cacbon trong môi trƣờng không khí Error! Bookmark not defined Hình 3.10 Ảnh FESEM bề mặt của sợi cacbon trƣớc xử lý (Cf), xử lý ở 300; 400; 500; 600 và 700oC trong môi trƣờng không khí Error! Bookmark not defined Hình 3.11 Phổ phân tích thành phần hoá học bề mặt của sợi cacbon trƣớc xử lý (Cf), xử lý ở 300; 400; 500; 600 và 700oC trong môi trƣờng không khíError!... c (Buranov I M., Vorobei V B (1998), Công nghệ các kết cấu tên lửa và hàng không vũ trụ từ vật liệu compozit, NXB "MGTU Bauman N E.", trang 318-392) 140 Бушуев Ю.Г., Персин М.И., Соколоь В.А (1994), Углерод-углеродные композиционные материалы Справочник, Москва, “Металлугия”, 68-82 c (Bushuev Yu G, Persin M I, Sokolov V A (1994), Sổ tay vật liệu compozit cacbon- cacbon, NXB "Luyện kim", trang 68-82)... nanotubes grafted on carbon fibres", Composites Part A 71, pp 168-175 30 Guixiang D., Chang S., Jianghong Z., Shouai F., Zhenping Z (2008), "Solidphase transformation of glass-like carbon nanoparticles into nanotubes and the related mechanism", Carbon 46, pp 92-98 31 Han S.J., Kim B., Suh K.D (2007), “Electrical properties of a composite film of poly(acrylonitrile) nanoparticles coated with carbon nanotubes”,