(LUẬN án TIẾN sĩ) tổng hợp, biến tính vật liệu nano của một số nguyên tố đất hiếm và đánh giá hoạt tính xúc tác quang hóa

ĐẠI HỌC HUẾ TRƯỜNG ĐẠI HỌC KHOA HỌC LÊ HỮU TRINH TỔNG HỢP, BIẾN TÍNH VẬT LIỆU NANO CỦA MỘT SỐ NGUYÊN TỐ ĐẤT HIẾM VÀ ĐÁNH GIÁ HOẠT TÍNH XÚC TÁC QUANG HÓA LUẬN ÁN TIẾN SĨ HÓA LÝ THUYẾT VÀ HÓA LÝ HUẾ, NĂM 2022 LUAN VAN CHAT LUONG download : add luanvanchat@agmail.com ĐẠI HỌC HUẾ TRƯỜNG ĐẠI HỌC KHOA HỌC LÊ HỮU TRINH TỔNG HỢP, BIẾN TÍNH VẬT LIỆU NANO CỦA MỘT SỐ NGUYÊN TỐ ĐẤT HIẾM VÀ ĐÁNH GIÁ HOẠT TÍNH XÚC TÁC QUANG HĨA Ngành: HÓA LÝ THUYẾT VÀ HÓA LÝ Mã số: 944.01.19 LUẬN ÁN TIẾN SĨ HÓA LÝ THUYẾT VÀ HÓA LÝ Người hướng dẫn khoa học: GS.TS TRẦN THÁI HÒA PGS.TS NGUYỄN ĐỨC CƯỜNG HUẾ, NĂM 2022 LUAN VAN CHAT LUONG download : add luanvanchat@agmail.com LỜI CAM ĐOAN Tôi xin cam đoan cơng trình nghiên cứu riêng tôi, số liệu kết nghiên cứu nêu luận án trung thực, đồng tác giả cho phép sử dụng chưa công bố cơng trình khác Việc tham khảo nguồn tài liệu trích dẫn ghi nguồn tài liệu tham khảo quy định Tác giả luận án Lê Hữu Trinh i LUAN VAN CHAT LUONG download : add luanvanchat@agmail.com LỜI CẢM ƠN Trong suốt thời gian thực luận án, nhận nhiều quan tâm, giúp đỡ quý thầy cơ, gia đình bạn bè Với lịng biết ơn sâu sắc nhất, xin gửi đến quý thầy GS.TS Trần Thái Hòa, PGS.TS Nguyễn Đức Cường lời cám ơn chân thành, với tri thức tâm huyết mình, quý thầy truyền đạt vốn kiến thức quý báu cho suốt thời gian học tập-nghiên cứu Tơi xin trân trọng cảm ơn khoa Hóa học, mơn Hố Lý thuyết Hóa lý, phịng Đào tạo Sau đại học, Trường Đại học Khoa học - Đại học Huế tạo điều kiện thuận lợi cho tơi hồn thành luận án Cuối tơi xin bày tỏ lòng biết ơn sâu sắc đến người thân gia đình tơi, bạn bè gần xa dành cho tơi tình cảm, động viên, chia sẻ giúp đỡ suốt q trình tơi học tập nghiên cứu Tôi xin trân trọng cảm ơn! Thừa Thiên Huế, tháng năm 2022 Tác giả luận án Lê Hữu Trinh ii LUAN VAN CHAT LUONG download : add luanvanchat@agmail.com DANH MỤC CÁC KÝ HIỆU, CHỮ VIẾT TẮT Viết tắt Ý nghĩa tiếng Anh Ý nghĩa tiếng Việt BET Brunauer-Emmett-Teller Phương pháp Brunauer Emmett-Teller method CT Computed Tomography Chụp cắt lớp CR Red Congo Chất màu Công gô đỏ EDX Energy Dispersive X-ray Phổ tán sắc lượng tia X spectroscopy MB Methylene Blue Xanh metyl MRI Magetic Resonance Imaging Chụp cộng hưởng từ Ln Lanthanide Họ Lan tan RE Rare earth Đất IUPAC International Union of Pure Liên minh quốc tế Hoá học and Applied Chemistry Hoá học ứng dụng SEM Scanning electron Microscope Kính hiển vi điện tử quét TGA Thermogravimetry Analyse Phân tích nhiệt TEG Triethylene glycol HOCH₂CH₂OCH₂CH₂OCH₂CH₂OH TEM transmission electron Kính hiển vi điện tử truyền qua microscopy UV Ultraviolet Cực tím UV-VIS Ultraviolet Visible Diffuse Phổ UV – Vis phản xạ khuếch tán Reflectance Spectroscopy VB Valence band Vùng hóa trị VIS Visible light Ánh sáng nhìn thấy XPS X-ray photo electron Phổ quang điện tử tia X spectroscopy XRD X-ray diffraction Nhiễu xạ tia X iii LUAN VAN CHAT LUONG download : add luanvanchat@agmail.com MỤC LỤC LỜI CAM ĐOAN i LỜI CẢM ƠN ii DANH MỤC CÁC KÝ HIỆU, CHỮ VIẾT TẮT iii MỤC LỤC iv DANH MỤC CÁC BẢNG vi DANH MỤC CÁC HÌNH .vii MỞ ĐẦU CHƯƠNG I TỔNG QUAN TÀI LIỆU 1.1 Vật liệu nano oxit đất 1.2 Cấu trúc oxit đất 1.3 Tổng quan nano gadolini oxit 1.4 Tổng quan nano neodymi oxit 12 1.5 Tổng quan nano ceri oxit 14 1.6 Một số phương pháp hóa học điều chế vật liệu nano 17 1.6.1 Phương pháp thủy nhiệt 18 1.6.2 Phương pháp nhiệt dung môi 20 1.7 Q trình oxy hóa – khử nâng cao ứng dụng 23 1.7.1 Q trình oxy hóa – khử nâng cao 23 1.7.2 Ứng dụng vật liệu nano oxit đất xúc tác quang 26 CHƯƠNG NỘI DUNG VÀ PHƯƠNG PHÁP NGHIÊN CỨU 33 2.1 Mục tiêu 33 2.2 Nội dung nghiên cứu 33 2.3 Phương pháp nghiên cứu 33 2.3.1 Phương pháp tổng hợp vật liệu 33 2.3.3 Các phương pháp nghiên cứu đặc trưng vật liệu 39 2.4 Hóa chất thiết bị, dụng cụ 55 2.4.1 Hóa chất 55 CHƯƠNG III KẾT QUẢ VÀ THẢO LUẬN 56 iv LUAN VAN CHAT LUONG download : add luanvanchat@agmail.com 3.1 Vật liệu nano Nd2O3 56 3.2 Vật liệu nano CeO2 tính chất xúc tác quang 67 3.2.1 Đặc trưng vật liệu 68 3.3.2 Tính chất xúc tác quang vật liệu nano CeO2 71 3.3 Vật liệu nano Gd2O3 Gd(OH)3 75 3.3.1 Vật liệu nano Gd2O3 75 3.3.2 Vật liệu nano Gd(OH)3 tính chất xúc tác hệ UV/H2O2/Gd(OH)3 84 3.4 Biến tính vật liệu nano oxit đất 94 3.4.1 Vật liệu nano CeO2 dạng cầu phân cấp pha tạp Neodimium 94 3.4.2 Vật liệu nano Gd(OH)3 dạng que pha tạp với Neodimium 97 KẾT LUẬN 102 DANH MỤC CÁC CƠNG TRÌNH KHOA HỌC LIÊN QUAN ĐÃ CÔNG BỐ 104 TÀI LIỆU THAM KHẢO 106 v LUAN VAN CHAT LUONG download : add luanvanchat@agmail.com DANH MỤC CÁC BẢNG Bảng 1.1 Thống kê điều kiện điều chế số vật liệu nano nguyên tố đất [31] 22 Bảng 1.2 Một số cơng trình nghiên cứu phản ứng xúc tác quang Ceria 27 Bảng 1.3 Một số cơng trình nghiên cứu hoạt tính xúc tác quang xúc tác từ vật liệu ceria 30 Bảng 2.1 Một số điều kiện tổng hợp hạt nano Gd2O3 phương pháp polyol với hỗ trợ vi sóng 36 Bảng 2.2 Các loại hóa chất sử dụng 55 Bảng 3.2 Thành phần nguyên tố hạt nano Gd2O3 nung Gd2O3@TEG 80 Bảng 3.3 Thành phần nguyên tố mẫu Gd(OH)3 phân tích EDX 86 Bảng 3.4 Mức độ thời gian phân hủy CR hệ xúc tác UV/Gd(OH)3 91 Bảng 3.5 Mức độ thời gian phân hủy CR hệ xúc tác UV/ H2O2/Gd(OH)3 93 Bảng 3.6 Thành phần nguyên tố mẫu Nd-CeO2 96 Bảng 3.7 Đặc trưng tinh thể mẫu Gd(OH)3 Nd-Gd(OH)3 98 Bảng 3.8 Thành nguyên tố Nd Gd vật liệu Nd-Gd(OH)3 99 vi LUAN VAN CHAT LUONG download : add luanvanchat@agmail.com DANH MỤC CÁC HÌNH Hình 1.1 Cấu trúc tinh thể oxit đất hiếm: (a) Loại A RE2O3, (b) Loại B RE2O3, (c) Loại C RE2O3 (d) dạng florit REO2 [138] Hình 1.2 Giản đồ pha RE2O3 [127] Hình 1.3 Sơ đồ mức lượng Gd3+ [15] Hình 1.4 Một số hình ảnh MRI chuột động mạch chủ động mạch thận thời điểm phút trước tiêm (−5 phút) 15, 30, 45, 60, 90 120 phút sau tiêm phức PPI-MAL DS-DOTA (Gd) ([Gd3 +] = mg/mL−1 0,2 mL nước muối qua tĩnh mạch đuôi [64] Hình 1.5 Sơ đồ điều chế Nd2O3 có cấu trúc micro/nano [85] 13 Hình 1.6 Ảnh SEM TEM nano que CeO2 (aec), cầu rỗng CeO2 (def), khối lập phương CeO2 (gei) [35] 15 Hình 1.7 Cấu trúc mạng lưới tinh thể CeO2 tinh khiết (trái) pha tạp (phải) [70].16 Hình 1.8 Mức độ chuyển hóa CO xúc tác ceria pha tạp [117] 17 Hình 1.9 Ảnh TEM que nano La2O3 (a), Pr6O11 (b), Nd2O3 (c), Er2O3 (d) sau nung hydroxit tương ứng 600°C h [59] 19 Hình 1.10 Cơ chế trình oxy hóa khử nâng cao dị thể 25 Hình 1.11 Phân loại Quá trình Oxy hóa - khử nâng cao [152] 25 Hình 1.12 Hiệu xúc tác quang vật liệu Ln(OH)3 32 Hình 2.1 Sự phản xạ tia X mặt tinh thể 42 Hình 2.2 Sơ đồ nguyên lý máy chụp SEM 45 Hình 2.3 Sơ đồ nguyên lý máy chụp TEM 46 Hình 2.4 Nguyên lý phép phân tích EDX 48 Hình 2.5 Sơ đồ nguyên lý ghi nhận phổ EDS 49 Hình 2.6 Các kiểu đường hấp phụ-giải hấp đẳng nhiệt theo IUPAC 52 Hình 3.1 Ảnh hỗn hợp sau phản ứng nhiệt độ thủy nhiệt khác từ 120-180 oC 56 Hình 3.2 Ảnh TEM với độ phân giải khác Nd2O3 tổng hợp điều kiện khác nhau: (a, b) 120 oC, (c d) 140 oC, (e, f) 160 oC, (g, h) 180 oC 58 vii LUAN VAN CHAT LUONG download : add luanvanchat@agmail.com Hình 3.3 Ảnh TEM nano Nd2O3 tổng hợp 180 oC với thời gian nhiệt dung khác nhau: (a, b) 12 giờ, (c, d) 24 (e, f) 36 59 Hình 3.4 Cơ chế hình thành hạt nano Nd2O3 đơn phân tán phương pháp tổng hợp hai pha 60 Hình 3.5 Ảnh SEM với độ phân giải khác vật liệu Nd2O3 sau loại dung môi 61 Hình 3.6 Ảnh SEM (a, b), TEM (c) HRTEM (d) cấu trúc Nd2O3 dạng cầu phân cấp 62 Hình 3.7 Ảnh SEM (a, b) TEM (c, d) cấu trúc nano Nd2O3 dạng mạng lưới xốp.63 Hình 3.8 Giản đồ XRD Nd2O3 dạng mạng lưới xốp (a), cầu phân cấp (b).64 Hình 3.9 Phổ tán xạ lượng tia X Nd2O3 dạng cầu phân cấp (a) dạng mạng lưới xốp (b) 65 Hình 3.10 Đường đẳng nhiệt hấp phụ/giải hấp phụ N2 đường phân bố kích thước mao quản tương ứng vật liệu nano Nd2O3 dạng cầu (a) dạng mạng lưới (b) 66 Hình 3.11 Sơ đồ chế hình thành Nd2O3 cấu trúc nano phân cấp dạng cầu dạng mạng lưới 67 Hình 3.12 Giản đồ TG-DTG CeO2-80 trước nung 68 Hình 3.13 Giản đồ XRD CeO2-80 69 Hình 3.14 Ảnh SEM (a), (b) TEM (c), (d) CeO2-80 70 Hình 3.15 Ảnh SEM (a) TEM (b) mẫu CeO2-70 ảnh SEM (c) TEM (d) CeO2-90 70 Hình 3.16 Đường đẳng nhiệt hấp phụ/giải hấp phụ N2 (a) đường phân bố kích thước mao quản (b) mẫu CeO2-80 71 Hình 3.17 Phổ hấp thụ (a) đường chuẩn MB (b) 71 Hình 3.18 Phổ hấp thụ dung dịch MB sau 60 phút 72 Hình 3.19 Phổ hấp thụ dung dịch MB nồng độ (a) 5, (b) 10, (c) 15 (d) 20 ppm chiếu UV chất xúc tác CeO2-80 73 viii LUAN VAN CHAT LUONG download : add luanvanchat@agmail.com microwave-polyol method” The 3rd International Conference on Advanced Materials and Nanotechnology, October 2nd - 5th 2016, Hanoi, Vietnam Le Huu Trinh, Nguyen Duc Cuong, Tran Thai Hoa, Do Dang Trung, Nguyen Van Hieu “Synthesis and characterization of hierachical CeO2 spherical nanoparticles for photocatalytic degradation of methylene blue” VNU Journal of Science: Physics and Mathermatics (Đã nhận đăng) (2021) 105 LUAN VAN CHAT LUONG download : add luanvanchat@agmail.com TÀI LIỆU THAM KHẢO [1] Ahab A., Rohman F., Iskandar F., Haryanto F., and Arif I (2016), "ahA simple straightforward thermal decomposition synthesis of PEG-covered Gd2O3 (Gd2O3@ PEG) nanoparticles", Advanced Powder Technology, Vol.27, Iss.4, pp 1800-1805 [2] Ahrén M S r., Linnéa Klasson, Anna Soderlind, Fredrik Abrikossova, Natalia Skoglund, Caroline Bengtsson, Torbjörn Engström, Maria Käll, Per-Olov Uvdal, Kajsa (2010), "Synthesis and characterization of PEGylated Gd2O3 nanoparticles for MRI contrast enhancement", Langmuir, Vol.26, Iss.8, pp 5753-5762 [3] Akbari-Fakhrabadi A., Meruane V., Jamshidijam M., Gracia-Pinilla M., and Mangalaraja R V (2016), "Effect of rare earth dopants on structural and mechanical properties of nanoceria synthesized by combustion method", Materials Science and Engineering: A, Vol.649, pp 168-173 [4] Amoresi R A O., Regiane C Marana, Naiara L De Almeida, Priscila B Prata, Paloma S Zaghete, Maria A Longo, 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