Nghiên cứu chế tạo vật liệu ag tio2, ag ni tio2 bằng phương pháp chiếu xạ tia co 60 ứng dụng làm xúc tác quang hóa phân hủy chất màu hữu cơ( luận án tiến sĩ kĩ thuật)

ĐẠI HỌC QUỐC GIA TP HỒ CHÍ MINH TRƯỜNG ĐẠI HỌC BÁCH KHOA VÕ THỊ THU NHƯ NGHIÊN CỨU CHẾ TẠO VẬT LIỆU Ag/TiO2, Ag-Ni/TiO2 BẰNG PHƯƠNG PHÁP CHIẾU XẠ TIA Co-60 ỨNG DỤNG LÀM XÚC TÁC QUANG HOÁ PHÂN HUỶ CHẤT MÀU HỮU CƠ LUẬN ÁN TIẾN SĨ KỸ THUẬT TP HỒ CHÍ MINH NĂM 2019 ĐẠI HỌC QUỐC GIA TP HCM TRƯỜNG ĐẠI HỌC BÁCH KHOA VÕ THỊ THU NHƯ NGHIÊN CỨU CHẾ TẠO VẬT LIỆU Ag/TiO2, Ag-Ni/TiO2 BẰNG PHƯƠNG PHÁP CHIẾU XẠ TIA Co-60 ỨNG DỤNG LÀM XÚC TÁC QUANG HOÁ PHÂN HUỶ CHẤT MÀU HỮU CƠ Chuyên ngành: Kỹ thuật hoá học Mã số chuyên ngành: 62520301 Phản biện độc lập 1: PGS TS Nguyễn Thị Phương Phong Phản biện độc lập 2: PGS TS Nguyễn Đình Thành Phản biện 1: PGS TS Phạm Nguyễn Kim Tuyến Phản biện 2: GS TS Phan Thanh Sơn Nam Phản biện 3: TS Bùi Duy Du NGƯỜI HƯỚNG DẪN: PGS.TS NGUYỄN QUỐC HIẾN PGS.TS ĐỖ QUANG MINH LỜI CAM ĐOAN Tác giả xin cam đoan cơng trình nghiên cứu thân tác giả Các kết nghiên cứu kết luận luận án trung thực, không chép từ nguồn hình thức Việc tham khảo nguồn tài liệu (nếu có) thực trích dẫn ghi nguồn tài liệu tham khảo quy định Tác giả luận án Chữ ký Võ Thị Thu Như i TÓM TẮT LUẬN ÁN Biến tính TiO2 kim loại có khả gia tăng hoạt tính xúc tác quang hóa TiO2, mở rộng vùng hoạt động TiO2 từ vùng tử ngoại đến khả kiến Các kết nghiên cứu cho thấy Ag, Au, Pt, Pd, Rh, Cu Ni kim loại biến tính vào TiO2 cho kết hoạt tính xúc tác quang TiO2 tốt Luận án chế tạo thành công vật liệu Ag/TiO2 phương pháp chiếu xạ tia Co-60 lần chế tạo thành công vật liệu TiO2 đồng biến tính Ag Ni với hỗ trợ xạ gamma từ nguồn Co-60 Đồng thời, xác định đặc trưng cấu trúc hoạt tính xúc tác quang hóa phân hủy chất hữu hai vật liệu Các vật liệu xúc tác Ag/TiO2 Ag-Ni/TiO2 điều chế sở TiO2 (P25) có kích thước hạt 20 - 40 nm phương pháp chiếu xạ tia Co-60 Thành phần pha, kích thước hạt, diện tích bề mặt riêng, lượng vùng cấm, lượng liên kết,…của vật liệu xác định phương pháp: nhiễu xạ tia X (XRD), kính hiển vi điện tử quét (SEM), kính hiển vi điện tử truyền qua (TEM), diện tích bề mặt BET, phổ tán sắc lượng tia X (EDX), phổ quang điện tử tia X (XPS),… Kết phân tích cấu trúc vật liệu Ag/TiO2 với hàm lượng Ag biến tính khoảng tỉ lệ khối lượng Ag/TiO2 từ 0,5 - 2,0% cho thấy vật liệu có cấu trúc pha TiO2 anatase rutile với kích thước 20 - 40 nm Ag kim loại kích thước khoảng 1- nm Năng lượng vùng cấm mẫu Ag/TiO2 (bằng 3,330; 3,312; 3,167 3,295 eV) thấp so với TiO2 ban đầu (bằng 3,348 eV) Kết phân tích cấu trúc mẫu vật liệu Ag-Ni/TiO2 với tỉ lệ khối lượng Ag/TiO2 Ni/TiO2 từ 0,75 – 3,0% cho thấy cấu trúc pha pha anatase rutile TiO2 ban đầu cịn Ag Ni kim loại với kích thước nano khoảng 1-3 nm, lượng vùng cấm mẫu Ag-Ni/TiO2 (bằng 3,180; 3,151; 3,123; 3,102; 3,024 eV) thấp so với mẫu TiO2 ban đầu Hoạt tính xúc tác quang hóa hai vật liệu chế tạo thể với hai chất hữu methyl red rhodamine B Kết cho thấy Ag/TiO2 Ag-Ni/TiO2 có hoạt tính xúc tác quang hố cao TiO2 ban đầu điều kiện phản ứng Nguyên nhân ii Ag/TiO2 có hoạt tính xúc tác quang hố cao TiO2 hạt nano Ag biến tính vào cấu trúc TiO2 hình thành nên mức lượng làm giảm lượng vùng cấm TiO2 TiO2 trở nên hoạt tính Ngồi hạt nano Ag cịn chất bắt giữ điện tử quang sinh, làm giảm khả tái hợp lỗ trống - điện tử quang sinh TiO2 biến tính đồng thời hai kim loại Ag Ni có hoạt tính xúc tác quang cao TiO2 Ag/TiO2 Vì hai kim loại Ag Ni làm chất bắt giữ điện tử quang sinh tốt trường hợp có Ag Do dẫn đến kết hiệu suất phân hủy quang hóa chất hữu vật liệu Ag-Ni/TiO2 cao Ag/TiO2 Các vật liệu Ag/TiO2 Ag-Ni/TiO2 chiếu sáng, điện tử vùng hóa trị bị kích thích dịch chuyển lên vùng dẫn, hình thành cặp điện tử - lỗ trống quang sinh (e- h+) Các điện tử quang sinh vùng dẫn lỗ trống quang sinh vùng hóa trị phản ứng oxy hố khử với chất hấp thụ bề mặt vật liệu Trong trường hợp này, điện tử quang sinh khử O2 tạo gốc O2- lỗ trống quang sinh oxy hóa H2O bề mặt chất xúc tác để tạo gốc •OH H2O + h+ → •OH + H+ O2 + e - → O2 Các phản ứng làm ngăn cản khả tái kết hợp điện tử lỗ trống quang sinh Các gốc oxy hố •OH, O2- có khả phân huỷ chất hữu ô nhiễm thành hợp chất trung gian cuối phân huỷ hoàn toàn thành CO2 H2O iii ABSTRACT TiO2 modified by metal can enhance the photocatalytic activity and extend the active region of TiO2 from ultraviolet to visible light Noble metals including Ag, Au, Pt, Pd, Rh, Cu and Ni have been reported to be very effective in enhancing photocatalysis of TiO2 This thesis studied the preparation and characterization of Ag/TiO2 photocatalysts by  irradiation method The first time, TiO2 were modified by Ag and Ni supported by  irradiation from the Co-60 source The resulted photocatalysts were further investigated the photocatalytic activity toward the degradation of organic compounds The Ag/TiO2 and Ag-Ni/TiO2 catalysts were prepared based on the commercial TiO2 substrates (P25) with size ranging from 20 - 40 nm by the assistance of Co-60 irradiation The characteristics of Ag nano/TiO2 material such as: crystal phase, particle size, specific surface area, band gap, binding energy… has been investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), BET surface area, the diffuse reflectance spectra (DRS), energy dispersive X-ray (EDX), X-ray photoemission spectroscopy (XPS) The modified Ag/TiO2 nanoparticles composing of 0.5 to 2.0 wt% of Ag in the composition revealed the co-existence of the TiO2 anatase and rutile phase with size of 20 - 40 nm and the Ag metallic phase with size of 1-3 nm The band gaps were of 3.330; 3.312; 3.167 and 3.295 eV which were lower than that of the pristine TiO2 substrates (3,348 eV) The characteristics of Ag-Ni/TiO2 material composing of 0.75 to 3.0 wt% of Ag and Ni in the composition indicated two phases of anatase and rutile of TiO2 and Ag and Ni metallic phase with size of 1-3 nm The band gap was of 3.180; 3.151; 3.123; 3.102 and 3.024 eV which were lower than that of TiO2 The photocatalytic activity of the obtained Ag/TiO2 and Ag-Ni/TiO2 nanoparticles prepared by the support of Co-60 irradiation was investigated toward the degradation of methyl red (MR) and rhodamine B (RB) in aqueous solution The results showed iv that both the Ag/TiO2 and Ag-Ni/TiO2 nanoparticles exhibited higher photocatalytic activities compared to that of the pristine TiO2 nanoparticles under the same controlled reaction condition The reason was attributed to the ability of nano-size doped metal in lowering the band gap energy and thus shifting the optical response to the visible light region In addition, the nano-size doped Ag particles also prevented the capacity of the instinct recombination of photogenerated electrons and holes inside the catalysts, thereby increasing the catalytic efficiency Noteworthy, the Ag/Ni modified TiO2 nanoparticles exhibited the highest photocatalytic activity compared to the Ag modified TiO2 and the pristine TiO2 under the same controlled reaction condition It was accounted for the synergetic ability of both Ag and Ni metals in capturing photogenerated eletrons better than in case of solely Ag modified TiO2 As a result, the Ag-Ni/TiO2 displayed the highest photocatalytic efficiency toward the organic compound degradation In principle, in the photocatalysts the electrons move from the valence band to the conduction band under light excitation, leading to the formation of electron – hole pairs, denoting as e- and h+ The e- is represented for the electron in the conduction band whereas the h+ is assigned to the electron vacancy in the valance band, respectively Both these entities can migrate to the catalyst surface where they can enter in redox reactions with other species presenting on the surface of the catalysts In most cases, h+ can react easily with surface bound H2O molecules to produce •OH radicals, whereas, e- can react with O2 molecules to form superoxide radical anions of oxygen H2O + h+ → •OH + H+ O2 + e - → O2 These reactions prevent the recombination of the generated electrons and the holes The •OH and O2- produced in the above manner can then react with the organic compounds to form other species and finally, decomposes into CO2 and H2O v LỜI CÁM ƠN Em xin bày tỏ lòng biết ơn sâu sắc đến PGS.TS Nguyễn Quốc Hiến PGS.TS Đỗ Quang Minh tận tình hướng dẫn giúp đỡ cho em hoàn thành Luận án Tiến sĩ Xin chân thành cảm ơn trung tâm Nghiên cứu Triển khai Cơng nghệ Bức xạ, phịng thí nghiệm Công nghệ Môi trường – trường Đại học Sư phạm Kỹ thuật Tp.HCM, Viện nghiên cứu hạt nhân Đà Lạt trường Đại học Bách Khoa Tp.HCM hỗ trợ trang thiết bị để giúp nghiên cứu thành công luận án Xin cảm ơn quý thầy cô bạn bè trường đại học Bách Khoa TP Hồ Chí Minh trường đại học Sư phạm Kỹ thuật TP Hồ Chí Minh giúp đỡ, khích lệ tơi hồn thành luận án Xin cảm ơn q thầy Hội đồng đánh giá Luận án Tiến sĩ, thầy phản biện độc lập góp ý quý giá, giúp chỉnh sửa luận án Xin bày tỏ lịng biết ơn đến gia đình ln an ủi, động viên, hỗ trợ mặt để tơi hồn thành luận án vi MỤC LỤC LỜI CAM ĐOAN .i TÓM TẮT LUẬN ÁN ii ABSTRACT iv LỜI CÁM ƠN vi MỤC LỤC vii DANH MỤC CÁC HÌNH ẢNH xi DANH MỤC BẢNG BIỂU xiv DANH MỤC CÁC TỪ VIẾT TẮT .xv MỞ ĐẦU CHƯƠNG TỔNG QUAN 1.1 Xúc tác quang hóa bán dẫn 1.2 Các vật liệu xúc tác quang hóa .6 1.3 Vật liệu xúc tác quang hóa TiO2 1.3.1 Cấu trúc pha tinh thể TiO2 tính chất TiO2 .8 1.3.2 TiO2 làm xúc tác quang hóa 10 1.3.2.1 Cơ chế phản ứng TiO2 làm chất xúc tác quang hóa .11 1.3.2.2 Các yếu tố ảnh hưởng đến khả xúc tác quang hóa TiO2 .12 1.2 Tổng quan vật liệu TiO2 biến tính 15 1.2.1 Cơ chế xúc tác quang hóa sở TiO2 biến tính 15 1.2.2 Các phương pháp biến tính TiO2 16 1.2.2.1 Phương pháp sol-gel .16 1.2.2.2 Phương pháp thủy nhiệt 17 1.2.2.3 Phương pháp nhũ tương .18 1.2.2.4 Phương pháp khử 19 1.2.3 Nguồn xạ, đơn vị đo xạ sở khoa học trình chiếu xạ chế tạo nano kim loại 20 1.2.3.1 Nguồn xạ gamma Co-60 20 1.2.3.2 Các đơn vị đo xạ 21 1.2.3.3 Các trình xảy chiếu xạ chế tạo vật liệu nano kim loại .22 vii 1.2.3.4 Xác định liều xạ khử kim loại .24 1.2.3.5 Áp dụng công nghệ xạ điều chế vật liệu nano .25 1.3 Tình hình nghiên cứu sử dụng TiO2 biến tính làm chất xúc tác quang hóa nước 27 1.4 Tình hình nghiên cứu sử dụng TiO2 biến tính làm chất xúc tác quang hóa giới 29 1.4.1 TiO2 biến tính với kim loại 29 1.4.2 TiO2 biến tính với phi kim 32 1.4.3 TiO2 biến tính đồng thời với nhiều nguyên tố 33 1.4.4 Vật liệu xúc tác quang hóa Ag/TiO2 34 1.4.5 Vật liệu xúc tác quang hóa Ag-Ni/TiO2 35 1.3 Hợp chất màu hữu methyl red rhodamine B 36 1.3.1 Rhodamine B .36 1.3.2 Methyl red 37 1.4 Hướng nghiên cứu luận án 39 CHƯƠNG THỰC NGHIỆM VÀ PHƯƠNG PHÁP NGHIÊN CỨU 41 Hóa chất vật liệu 41 2.2 Dụng cụ thiết bị thí nghiệm 41 2.3 Các quy trình chế tạo vật liệu .43 2.3.1 Quy trình chế tạo Ag/TiO2 phương pháp chiếu xạ .43 2.3.2 Quy trình chế tạo Ag-Ni/TiO2 phương pháp chiếu xạ 44 2.4 Các phương pháp phân tích tính chất vật liệu 45 2.4.1 Xác định cấu trúc tinh thể vật liệu 45 2.4.2 Hình thái kích thước hạt 46 2.4.3 Thành phần hóa học vi cấu trúc vật liệu 46 2.4.4 Năng lượng liên kết EB (eV) 47 2.4.5 Phổ khuếch tán phản xạ (DRS) lượng vùng cấm (Eg) 48 2.4.6 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làm xúc tác quang hóa phân huỷ chất màu hữu cơ? ?? nhằm tạo chất xúc tác quang mới,... HỌC BÁCH KHOA VÕ THỊ THU NHƯ NGHIÊN CỨU CHẾ TẠO VẬT LIỆU Ag/ TiO2, Ag- Ni/ TiO2 BẰNG PHƯƠNG PHÁP CHIẾU XẠ TIA ? ?Co- 60 ỨNG DỤNG LÀM XÚC TÁC QUANG HOÁ PHÂN HUỶ CHẤT MÀU HỮU CƠ Chuyên ngành: Kỹ thuật hoá... tính xúc tác vật liệu Ag/ TiO2 Ag- Ni/ TiO2 Ý nghĩa thực tiễn đề tài: Đề tài chế tạo tạo thành công vật liệu Ag/ TiO2 Ag- Ni/ TiO2 phương pháp chiếu xạ tia  từ nguồn Co- 60 Vật liệu chế tạo có hiệu ứng