Nghiên cứu chế tạo vật liệu nano lai trên cơ sở hạt nano bạc và nano cacbon định hướng ứng dụng trong kháng khuẩn và cảm biến quang SERS

BỘ GIÁO DỤC VÀ ĐÀO TẠO TRƯỜNG ĐẠI HỌC BÁCH KHOA HÀ NỘI NGÔ XUÂN ĐINH NGHIÊN CỨU CHẾ TẠO VẬT LIỆU NANO LAI TRÊN CƠ SỞ HẠT NANO BẠC VÀ NANO CARBON ĐỊNH HƯỚNG ỨNG DỤNG TRONG KHÁNG KHUẨN VÀ CẢM BIẾN QUANG SERS LUẬN ÁN TIẾN SĨ KHOA HỌC VẬT LIỆU Hà Nội - 2017 BỘ GIÁO DỤC VÀ ĐÀO TẠO TRƯỜNG ĐẠI HỌC BÁCH KHOA HÀ NỘI NGÔ XUÂN ĐINH NGHIÊN CỨU CHẾ TẠO VẬT LIỆU NANO LAI TRÊN CƠ SỞ HẠT NANO BẠC VÀ NANO CARBON ĐỊNH HƯỚNG ỨNG DỤNG TRONG KHÁNG KHUẨN VÀ CẢM BIẾN QUANG SERS Chuyên ngành: Vật liệu điện tử Mã số: 62440123 LUẬN ÁN TIẾN SĨ KHOA HỌC VẬT LIỆU NGƯỜI HƯỚNG DẪN KHOA HỌC: PGS TS LÊ ANH TUẤN PGS TS NGUYỄN VĂN QUY Hà Nội - 2017 LỜI CẢM ƠN Lời đầu tiên, xin bày tỏ lòng kính trọng biết ơn sâu sắc đến thầy hướng dẫn: PGS TS Lê Anh Tuấn PGS TS Nguyễn Văn Quy hết lòng quan tâm hướng dẫn, dìu dắt tơi suốt q trình thực luận án tiến sĩ tạo điều kiện thuận lợi, giúp đỡ kể vật chất lẫn tinh thần cho học tập cơng việc để hồn thành tốt luận án Tôi xin chân thành cảm ơn TS Trần Quang Huy, Viện Vệ sinh dịch tễ trung ương tạo điều kiện giúp đỡ thời gian thực luận án Tôi xin gửi lời cảm ơn tới Thầy Cô, anh chị, bạn đồng nghiệp Viện tiên tiến Khoa học Công nghệ Trường Đại học Bách Khoa Hà Nội giúp đỡ, tạo điều kiện để tơi hồn thành luận án Lời cuối cùng, tơi xin gửi lời cảm ơn đến tồn thể gia đình, bạn bè đồng nghiệp động viên, chia hỗ trợ để tơi hồn thành luận án Tác giả Ngô Xuân Đinh i LỜI CAM ĐOAN Tác giả xin cam đoan cơng trình nghiên riêng tác giả hướng dẫn PGS TS Lê Anh Tuấn PGS TS Nguyễn Văn Quy Các kết luận án trung thực chưa cơng bố cơng trình khác Hà nội, ngày tháng năm 2017 TM Tập thể hướng dẫn Tác giả PGS TS Lê Anh Tuấn Ngô Xuân Đinh ii MỤC LỤC Lời cảm ơn………………………………………………………………………………… i Lời cam đoan……………………………………………………………………………… ii Mục lục…………………………………………………………………………………… iii Danh mục kí hiệu chữ viết tắt………………………………………………………vii Danh mục bảng biểu………………………………………………………………………viii Danh mục hình vẽ đồ thị………………………………………………………………… ix MỞ ĐẦU Chương 1: TỔNG QUAN 1.1 Hạt nano bạc (Ag-NPs) 1.1.1 Các phương pháp tổng hợp hạt nano bạc 1.1.1.1 Phương pháp hóa học 1.1.1.2 Phương pháp vật lý 10 1.1.1.3 Phương pháp sinh học 11 1.1.2 Tính chất hạt nano bạc 16 1.1.2.1 Hoạt tính kháng khuẩn, kháng nấm, diệt virut 16 1.2.2.2 Tính chất quang 18 1.1.3 Một số ứng dụng hạt nano bạc 20 1.1.3.1 Ứng dụng cho màng lọc nước, lọc khí khử trùng 21 1.1.3.2 Ứng dụng cảm biến 21 1.2 Các vật liệu nano carbon 24 1.2.1 Ống nano carbon (CNTs) 24 1.2.1.1 Các phương pháp chế tạo CNTs 25 1.2.1.2 Tính chất CNTs 26 1.2.1.3 Một số ứng dụng CNTs 28 1.2.2 Graphene oxit (GO) 29 1.2.2.1 Các phương pháp chế tạo GO 30 1.2.2.2 Tính chất GO 30 1.2.2.3 Một số ứng dụng GO 32 1.3 Vật liệu nano lai hạt nano bạc nano carbon (Ag-nC) 33 iii 1.3.1 Giới thiệu 33 1.3.2 Chế tạo vật liệu nano lai Ag-nC 34 1.3.2.1 Chế tạo vật liệu nano lai Ag/CNTs 34 1.3.2.2 Chế tạo vật liệu nano lai Ag/GO 35 1.3.3 Tính chất tiềm ứng dụng vật liệu nano lai Ag-nC 38 1.3.3.1 Tính chất diệt vi sinh vật ứng dụng khử trùng 38 1.3.3.2 Tính chất quang ứng dụng cho cảm biến SERS 39 1.3.3.3 Một số tính chất ứng dụng khác 40 1.4 Kết luận chương 42 Chương Vật liệu nano lai Ag/MWCNTs 43 2.1 Mở đầu 43 2.2 Thực nghiệm phương pháp nghiên cứu 44 2.2.1 Hóa chất dụng cụ thí nghiệm 44 2.2.2 Chế tạo hạt nano bạc theo phương pháp quang hóa 44 2.2.3 Chế tạo Ag/MWCNTs theo quy trình bước sử dụng phương pháp hóa học 46 2.2.3.1 Biến tính ống nano carbon (MWCNTs) 46 2.2.3.2 Khử ion phức bạc bề mặt MWCNTs-biến tính 47 2.2.4 Các phương pháp nghiên cứu phân tích 48 2.3 Cấu trúc tính chất hạt nano bạc (Ag-NPs) 50 2.3.1 Ảnh hưởng nguồn xạ 50 2.3.2 Ảnh hưởng pH dung dịch 54 2.3.3 Ảnh hưởng chất hoạt động bề mặt 57 2.4 Cấu trúc tính chất vật liệu nano lai Ag/MWCNTs 61 2.4.1 Sự hình thành hạt nano bạc ống nano carbon biến tính (f-MWCNTs) ……………………………………………………………………………………61 2.4.2 Ảnh hưởng pH dung dịch đến hình thành vật liệu nano lai Ag/MWCNTs ……………………………………………………………………………………66 2.4.3 Ảnh hưởng chất hoạt động bề mặt đến hình thành vật liệu nano lai Ag/MWCNTs 69 Chương Vật liệu nano lai Ag/GO 73 3.1 Mở đầu 73 iv 3.2 Cấu trúc tính chất vật liệu nano lai Ag/GO chế tạo theo phương pháp quang hóa …………………………………………………………… 74 3.2.1 Thực nghiệm 74 3.2.1.1 Hóa chất thiết bị sử dụng 74 3.2.1.2 Quy trình chế tạo GO 74 3.2.1.3 Quy trình chế tạo vật liệu nano lai Ag/GO 75 3.2.1.4 Các phương pháp nghiên cứu 76 3.2.2 Đặc trưng cấu trúc tính chất Ag/GO 77 3.3 Cấu trúc tính chất vật liệu lai Ag/GO chế tạo theo phương pháp thủy nhiệt … 83 3.3.1 Thực nghiệm 83 3.3.1.1 Hóa chất thiết bị sử dụng 83 3.3.1.2 Quy trình chế tạo vật liệu nano lai Ag/GO 83 3.3.1.3 Các phương pháp nghiên cứu 85 3.3.2 Đặc trưng cấu trúc tính chất Ag/GO chế tạo theo phương pháp thủy nhiệt 85 3.4 Kết luận chương 90 Chương Đánh giá khả ứng dụng vật liệu nano lai kháng khuẩn cảm biến quang SERS 91 4.1 Mở đầu 91 4.2 Thử nghiệm ứng dụng vật liệu nano lai kháng khuẩn 92 4.2.1 Phương pháp thực nghiệm 92 4.2.1.1 Phương pháp khoanh giấy (vòng vơ khuẩn) 92 4.2.1.2 Kĩ thuật lát cắt siêu mỏng hiển vi điện tử 92 4.2.2 Hoạt tính kháng khuẩn 94 4.2.3 Cơ chế kháng khuẩn 97 4.2.3.1 Tương tác Ag-NPs với tế bào vi khuẩn 97 4.2.3.2 Tương tác Ag/MWCNTs với tế bào vi khuẩn 100 4.2.3.3 Tương tác GO với tế bào vi khuẩn 103 4.2.3.4 Tương tác Ag/GO với tế bào vi khuẩn 105 4.3 Thử nghiệm ứng dụng vật liệu nano lai cảm biến quang SERS 107 4.3.1 Phương pháp thực nghiệm 107 4.3.2 Phát chất màu hữu dung dịch nước 108 v 4.3.2.1 Đặc trưng SERS hạt nano bạc 108 4.3.2.2 Đặc trưng SERS vật liệu nano lai Ag/MWCNTs 109 4.3.2.3 Đặc trưng SERS vật liệu nano lai Ag/GO 111 4.3.3 Hệ số tăng cường 112 4.4 Kết luận chương 116 KẾT LUẬN VÀ KIẾN NGHỊ 117 TÀI LIỆU THAM KHẢO 119 DANH MỤC CÁC CÔNG TRÌNH ĐÃ CƠNG BỐ CỦA LUẬN ÁN 136 vi DANH MỤC CÁC KÍ HIỆU VÀ CHỮ VIẾT TẮT Ag-NPs: Hạt nano bạc Ag/MWCNTs Vật liệu lai hạt nano bạc ống nano carbon đa tường Ag/GO Vật liệu lai hạt nano bạc graphene oxit Ag-nC Vật liệu lai hạt nano bạc vật liệu nano carbon EDX Phổ tán xạ tia X TEM Hiển vi điện tử truyền qua HRTEM Hiển vi điện tử truyền qua phân giải cao SAED Nhiễu xạ điện tử chọn lọc vùng FTIR Phổ hồng ngoại biến đổi Fourier UV-vis Phổ hấp thụ dải UV ánh sáng nhìn thấy SERS Hiệu ứng tăng cường tán xạ Raman bề mặt (Surface-Enhanced Raman Scattering) CE Tăng cường hóa học ME Tăng cường trường điện từ MB Chất màu Xanh methylene E coli Vi khuẩn Escherichia coli S aureus Vi khuẩn tụ cầu vàng (Staphylococcus aureus) PVP Polyvinyl pyrrolidone XRD Nhiễu xạ tia X EF Hệ số tăng cường tán xạ Raman SD Độ lệch chuẩn tương đối vii DANH MỤC BẢNG BIỂU Bảng 1.1 Bảng tổng hợp phương pháp chế tạo hạt nano bạc 14 Bảng 1.2 Tính chất tiềm ứng dụng hạt nano bạc 23 Bảng 1.3 Các phương pháp chế tạo khả ứng dụng vật liệu nano lai Ag-nC 37 Bảng 2.1 Tổng hợp điều kiện chế tạo mẫu Ag-NPs 46 Bảng 2.2 Tổng hợp điều kiện chế tạo mẫu Ag/MWCNTs 48 Bảng 2.3 So sánh thông số khả ứng dụng vật liệu nano lai Ag/MWCNTs chế tạo theo phương pháp khác 71 Bảng 3.1 Bảng tổng hợp điều kiện chế tạo mẫu Ag/GO phương pháp thủy nhiệt 84 Bảng 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DỤC VÀ ĐÀO TẠO TRƯỜNG ĐẠI HỌC BÁCH KHOA HÀ NỘI NGÔ XUÂN ĐINH NGHIÊN CỨU CHẾ TẠO VẬT LIỆU NANO LAI TRÊN CƠ SỞ HẠT NANO BẠC VÀ NANO CARBON ĐỊNH HƯỚNG ỨNG DỤNG TRONG KHÁNG KHUẨN VÀ CẢM BIẾN QUANG SERS. .. đó, định hướng nghiên cứu luận án Nghiên cứu chế tạo vật liệu nano lai sở hạt nano bạc nano carbon định hướng ứng dụng kháng khuẩn cảm biến quang SERS Mục tiêu luận án Với đề tài nghiên cứu. .. dự kiến trên, mục tiêu luận án đặt là: - Nghiên cứu chế tạo vật liệu nano lai Ag-nC khảo sát tính chất chúng - Định hướng ứng dụng hệ vật liệu nano lai chế tạo kháng khuẩn cảm biến quang SERS Nội