Nghiên cứu tính chất nhạy khí của vật liệu nano ôxít sắt sử dụng vi cân tinh thể thạch anh.

Nghiên cứu tính chất nhạy khí của vật liệu nano ôxít sắt sử dụng vi cân tinh thể thạch anh.Nghiên cứu tính chất nhạy khí của vật liệu nano ôxít sắt sử dụng vi cân tinh thể thạch anh.Nghiên cứu tính chất nhạy khí của vật liệu nano ôxít sắt sử dụng vi cân tinh thể thạch anh.Nghiên cứu tính chất nhạy khí của vật liệu nano ôxít sắt sử dụng vi cân tinh thể thạch anh.Nghiên cứu tính chất nhạy khí của vật liệu nano ôxít sắt sử dụng vi cân tinh thể thạch anh.

BỘ GIÁO DỤC VÀ ĐÀO TẠO TRƯỜNG ĐẠI HỌC BÁCH KHOA HÀ NỘI NGUYỄN THÀNH VINH NGHIÊN CỨU TÍNH CHẤT NHẠY KHÍ CỦA VẬT LIỆU NANO Ơ-XÍT SẮT SỬ DỤNG VI CÂN TINH THỂ THẠCH ANH LUẬN ÁN TIẾN SĨ KHOA HỌC VẬT LIỆU HÀ NỘI, 2021 BỘ GIÁO DỤC VÀ ĐÀO TẠO TRƯỜNG ĐẠI HỌC BÁCH KHOA HÀ NỘI NGUYỄN THÀNH VINH NGHIÊN CỨU TÍNH CHẤT NHẠY KHÍ CỦA VẬT LIỆU NANO Ơ-XÍT SẮT SỬ DỤNG VI CÂN TINH THỂ THẠCH ANH Ngành: Khoa học vật liệu Mã ngành: 9440122 LUẬN ÁN TIẾN SĨ KHOA HỌC VẬT LIỆU NGƯỜI HƯỚNG DẪN KHOA HỌC PGS TS Nguyễn Văn Quy GS TS Lê Anh Tuấn LỜI CẢM ƠN Lời em xin gửi lời cảm ơn sâu sắc đến PGS TS Nguyễn Văn Quy – Viện Đào tạo Quốc tế Khoa học vật liệu (ITIMS) – Đại học Bách Khoa Hà Nội, GS TS Lê Anh Tuấn – Viện Nghiên cứu nano – Đại học Phenikaa Các thầy tận tình giúp đỡ hướng dẫn em suốt trình làm học tập hoàn thành luận án Em xin chân thành cảm ơn thầy cô giáo, anh chị em NCS, học viên cao học Viện đào tạo Quốc tế Khoa học vật liệu (ITIMS), nhóm nghiên cứu NEB (ITIMS – AIST – Phenikaa University), nhóm iSensor (ITIMS) giúp đỡ em nhiều công tác chun mơn, đóng góp nhiều ý kiến tận tình q trình học, giúp em hồn thành luận án Đồng thời, xin chân thành cảm ơn giúp đỡ chuyên môn công tác giảng dạy, chế độ người lao động Ban giám hiệu, tập thể sử phạm nhà trường đặc biệt anh chị em đồng nghiệp Bộ môn Vật lý công nghệ – Khoa Khoa học ứng dụng – Trường Đại học Công nghệ GTVT, giúp tơi hồn thành luận án Cuối không phần quan trọng, xin cảm ơn thành viên gia đình tơi bên mang lại cho động lực để hồn thành q trình học tập nghiên cứu khoa học Nghiên cứu sinh 10 11 12 13 Nguyễn Thành Vinh 14 LỜI CAM ĐOAN 15 16 Tơi xin cảm đoan luận án cơng trình nghiên cứu bảo khoa học tập thể hướng dẫn Luận án khơng có chép tài liệu, cơng trình nghiên cứu người khác mà khơng có trích dẫn danh mục tài liệu tham khảo Những kết luận án chưa cơng bố hình thức ngồi tơi tập thể hướng dẫn Tơi xin chịu hoàn toàn trách nhiệm trước nhà trường lời cam đoan 17 18 19 20 27 28 29 dẫn 22 24 25 26 PGS TS Nguyễn Văn Quy Nghiên cứu sinh 30 31 32 33 21 Thay mặt tập thể hướng 23 Hà Nội, ngày …… tháng… năm…… 34 Nguyễn Thành Vinh 35 MỤC LỤC 36 LỜI CẢM ƠN LỜI CAM ĐOAN 37 D ANH MỤC CÁC KÍ HIỆU VÀ CHỮ VIẾT TẮT iv 38 D ANH MỤC CÁC BẢNG vi 39 DA NH MỤC CÁC HÌNH VẼ ĐỒ THỊ vii 40 M Ở ĐẦU 1 Lý chọn đề tài Mục tiêu luận án 3 Nội dung nghiên cứu Đối tượng phạm vi nghiên cứu Phương pháp nghiên cứu Ý nghĩa khoa học đóng góp thực tiễn luận án Tính luận án Bố cục luận án 41 C HƯƠNG 1: TỔNG QUAN 1.1.Tổng quan vi cân tinh thể thạch anh (QCM) 1.1.1 Hiệu ứng áp điện 1.1.2 Vi cân tinh thể thạch anh 1.2 Tổng quan ứng dụng QCM cảm biến khí 12 1.2.1 Giới thiệu cảm biến khí 12 1.2.2 Cảm biến QCM nguyên lý hoạt động 13 1.2.3 Cơ chế nhạy khí cảm biến QCM 17 1.3 Tổng quan vật liệu nhạy khí cảm biến QCM 19 1.3.1 Vật liệu nhóm cacbon 19 1.3.2 Vật liệu polymer vật liệu hữu 22 1.3.3 Khung hữu kim loại 25 1.3.4 Vật liệu nano ô-xít kim loại bán dẫn chất vô 27 1.4 Tổng quan vật liệu ô-xít sắt 29 1.4.1 Phương pháp chế tạo vật liệu nano ô-xít sắt 29 1.4.2 Vật liệu nano ơ-xít sắt ứng dụng lĩnh vực cảm biến môi trường31 1.4.3 Tổng quan cấu trúc vật liệu nano ơ-xít ơ-xít – hydroxit sắt 36 1.5 Kết luận chương 38 42 C HƯƠNG 2: CHẾ TẠO, KHẢO SÁT TÍNH CHẤT VẬT LIỆU NANO Ơ-XÍT SẮT VÀ LỚP CẢM NHẬN TRÊN ĐIỆN CỰC QCM 39 2.1 Tổng hợp vật liệu nano ơ-xít sắt 39 43 .2.1 Tổng hợp hạt nano (NPs) ơ-xít sắt 39 44 .2.1 Tổng hợp nano (NRs) ơ-xít sắt 42 2.2 Nghiên cứu phương pháp khảo sát tính chất hóa - lý vật liệu .43 2.2.1 Phương pháp phân tích cấu trúc thành phần mẫu 43 2.2.2 Phương pháp phân tích Rietveld 45 2.2.3 Phương pháp khảo sát kính hiển vi điện tử quét (SEM) kính hiển vi điện tử truyền qua (TEM) 45 2.2.4 Phương pháp đo từ tính vật liệu từ kế mẫu rung (VSM) 46 2.2.5.Phương pháp đo phổ hồng ngoại biến đổi Fourier phổ tán xạ Raman 47 2.2.6 Phương pháp đo diện tích bề mặt phân bố kích thước lỗ rỗng 48 2.3 Chế tạo lớp cảm nhận nano ơ-xít sắt điện cực QCM khảo sát đo khí 49 2.3.1 Chế tạo lớp cảm nhận nano ơ-xít sắt điện cực QCM .49 2.3.2 Quy trình khảo sát đo khí 52 45 2.4 Kết luận Chương 54 46 C HƯƠNG 3: ĐẶC TRƯNG NHẠY KHÍ CỦA CÁC HẠT NANO Ơ-XÍT SẮT SỬ DỤNG CẢM BIẾN QCM 55 3.1 Khảo sát cấu trúc, hình thái tính chất hóa lý hạt nano ơ-xít sắt 55 3.1.1 Khảo sát đặc trưng cấu trúc hạt nano ơ-xít sắt .55 3.1.2 Khảo sát hình thái tính chất hóa lý vật liệu hạt nano ơ-xít sắt 61 3.2 Khảo sát đặc trưng nhạy khí cảm biến QCM phủ hạt nano Fe3O4, γ-Fe2O3 (QP200) α-Fe2O3 67 3.2.1 Khảo sát khả nhận biết khí cảm biến QCM phủ hạt nano Fe3O4 67 3.2.2 So sánh đặc trưng nhạy khí SO2 cảm biến QCM phủ hạt nano Fe3O4, γ-Fe2O3 (QP200) α-Fe2O3 68 3.2.3 Khảo sát đặc trưng nhạy khí SO2 cảm biến sử dụng hạt nano γ-Fe2O3 (QP200) 72 3.3 Ảnh hưởng ion [Fe3+] [Fe2+] tính chất nhạy khí SO2 hạt nano γ-Fe2O3 phủ điện cực QCM 74 3.3.1 Khảo sát đặc trưng nhạy khí SO2 cảm biến QCM phủ hạt nano γ-Fe2O3 chế tạo từ tiền chất khác 74 3.3.2 Khảo sát đặc trưng nhạy khí chọn lọc, ổn định ảnh hưởng độ ẩm đến tính chất nhạy khí cảm biến Q3 79 3.4 Kết luận Chương 81 47 C HƯƠNG 4: ĐẶC TRƯNG NHẠY KHÍ CỦA THANH NANO Ơ-XÍT SẮT SỬ DỤNG CẢM BIẾN QCM 83 4.1 Khảo sát cấu trúc, hình thái tính chất vật liệu nano ơ-xít sắt .83 4.1.1 Vật liệu nano Fe3O4/α-FeOOH 83 4.1.2 So sánh cấu trúc, hình thái tính chất nano Fe3O4/αFeOOH, γ-Fe2O3 α-Fe2O3 86 4.2 Khảo sát đặc trưng nhạy khí cảm biến sử dụng nano Fe3O4/α-FeOOH 90 4.2.1 Các đặc trưng nhạy khí SO2, NO2, CO .90 4.2.2 Khảo sát ảnh hưởng khí CO nồng độ cao đến đặc trưng nhạy khí cảm biến Fe3O4/α-FeOOH 95 4.3 Khảo sát đặc trưng nhạy khí SO2 cảm biến sử dụng nano Fe3O4/α-FeOOH, γ-Fe2O3 α-Fe2O3 106 4.3.1 So sánh đặc trưng nhạy khí 106 4.3.2 Đề xuất chế nhạy khí SO2 nano ơ-xít sắt .110 4.3.3 Ảnh hưởng độ ẩm đến khả nhận biết khí SO2 111 4.3.4 Tính chọn lọc SO2 cảm biến sử dụng nano γ-Fe2O3 113 4.4 Kết luận Chương 117 4.4.1 KẾT LUẬN VÀ KIẾN NGHỊ 119 4.4.2 TUY ỂN TẬP CÁC CƠNG TRÌNH ĐÃ CƠNG BỐ CỦA LUẬN ÁN 121 4.4.3 TÀI LIỆU THAM KHẢO 122 4.4.4 DANH MỤC CÁC KÍ HIỆU VÀ CHỮ VIẾT TẮT 4.4.5 4.4.7 4.4.6 Kí hiệu 4.4.9 Tên tiếng Anh 4.4.10.Ý STT nghĩa 4.4.8 viết tắt 4.4.11 4.4.12 4.4.13 Zero4.4.14 Không chiều 0D Dimensional 4.4.15 4.4.16 4.4.17 One4.4.18 Một chiều 1D Dimensional 4.4.19 4.4.20 4.4.21 Two4.4.22 Hai chiều 2D Dimensional 4.4.23 4.4.24 4.4.25 Three4.4.26 Ba chiều 3D Dimensional 4.4.29 Advanced 4.4.31 Viện Tiên tiến Khoa 4.4.27 4.4.28 Institute for học Công AIST 4.4.30 Science and 4.4.32 nghệ Technology 4.4.33 4.4.34 4.4.35 Brunauer – 4.4.36 Phương pháp đo diện BET Emmett – Teller tích bề mặt 4.4.40 Phương pháp đo phân 4.4.37 4.4.38 4.4.39 Barrett – bố kích BJH Joyner - Halenda 4.4.41 thước lỗ rỗng 4.4.42 4.4.43 4.4.44 Carbon 4.4.45 Ống nano cacbon CNT nanotube 4.4.48 Multi wall 4.4.46 4.4.47 4.4.50 Ống nano cacbon đa carbon MWCNT lớp 4.4.49 nanotubes 4.4.51 4.4.52 4.4.53 Concentration 4.4.54 Nồng độ 10 Con 4.4.55 4.4.56 4.4.57 Dionized Water 4.4.58 Nước khử ion 11 DI 4.4.61 X-ray Energy 4.4.59 4.4.60 4.4.63 Phổ tán sắc Dispersion 12 EDX lượng tia X 4.4.62 Spectroscopy 4.4.66 Fourier 4.4.64 4.4.65 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NGUYỄN THÀNH VINH NGHIÊN CỨU TÍNH CHẤT NHẠY KHÍ CỦA VẬT LIỆU NANO Ơ-XÍT SẮT SỬ DỤNG VI CÂN TINH THỂ THẠCH ANH Ngành: Khoa học vật liệu Mã ngành: 9440122 LUẬN ÁN TIẾN SĨ KHOA HỌC VẬT LIỆU NGƯỜI... phân tích ưu điểm linh kiện QCM vật liệu nano ơ-xít sắt trên, lựa chọn đề tài: ? ?Nghiên cứu tính chất nhạy khí vật liệu nano ơ-xít sắt sử dụng vi cân tinh thể thạch anh” 2 Mục tiêu luận án 4.4.259... HƯƠNG 4: ĐẶC TRƯNG NHẠY KHÍ CỦA THANH NANO Ơ-XÍT SẮT SỬ DỤNG CẢM BIẾN QCM 83 4.1 Khảo sát cấu trúc, hình thái tính chất vật liệu nano ơ-xít sắt .83 4.1.1 Vật liệu nano Fe3O4/α-FeOOH