(Luận án tiến sĩ) chế tạo, nghiên cứu các tính chất từ và khả năng sinh nhiệt của một số hệ nano nền fe3o4

BỘ GIÁO DỤC VÀ ĐÀO TẠO VIỆN HÀN LÂM KHOA HỌC VÀ CÔNG NGHỆ VIỆT NAM HỌC VIỆN KHOA HỌC VÀ CÔNG NGHỆ - Lê Thị Hồng Phong n CHẾ TẠO, NGHIÊN CỨU CÁC TÍNH CHẤT TỪ VÀ KHẢ NĂNG SINH NHIỆT CỦA MỘT SỐ HỆ NANO NỀN Fe3O4 LUẬN ÁN TIẾN SĨ KHOA HỌC VẬT LIỆU Hà Nội – 2023 BỘ GIÁO DỤC VÀ ĐÀO TẠO VIỆN HÀN LÂM KHOA HỌC VÀ CÔNG NGHỆ VIỆT NAM HỌC VIỆN KHOA HỌC VÀ CÔNG NGHỆ - Lê Thị Hồng Phong CHẾ TẠO, NGHIÊN CỨU CÁC TÍNH CHẤT TỪ VÀ KHẢ NĂNG SINH NHIỆT CỦA MỘT SỐ HỆ HẠT NANO NỀN Fe3O4 Chuyên ngành: Vật liệu điện tử n Mã số: 9.44.01.23 LUẬN ÁN TIẾN SĨ KHOA HỌC VẬT LIỆU NGƯỜI HƯỚNG DẪN KHOA HỌC: PGS.TS Đỗ Hùng Mạnh PGS.TS Phạm Thanh Phong Hà Nội – 2023 i LỜI CẢM ƠN Lời đầu tiên, tơi xin bày tỏ lịng biết ơn sâu sắc tới PGS.TS Đỗ Hùng Mạnh PGS.TS Phạm Thanh Phong, người Thầy dành cho định hướng khoa học hiệu quả, động viên, giúp đỡ tận tình suốt trình thực luận án Tơi xin bày tỏ lịng kính trọng gửi lời cảm ơn sâu sắc cho bảo, định hướng khích lệ GS TSKH Nguyễn Xuân Phúc từ năm bắt đầu thực luận án Tôi xin gửi lời cảm ơn chân thành tới TS Vũ Hồng Kỳ, TS Nguyễn Thị Ngọc Anh, TS Phạm Hoài Linh giúp đỡ nhiệt tình bàn luận quý báu giai đoạn hoàn thiện luận án Cảm ơn cộng tác giúp đỡ TS Phạm Hồng Nam, TS Vương Thị Kim Oanh, ThS Tạ Ngọc Bách nghiên cứu thực nghiệm phân tích kết Tôi xin gửi lời cảm ơn chân thành đến PGS.TS Nguyễn Thanh Tùng, TS Đỗ Khánh Tùng, TS Ngô Thị Hồng Lê, NCS Nguyễn Thị Mai Những lời động viên, khích lệ giúp đỡ nhiệt tình anh chị em suốt thời gian thực luận án giúp tơi có thêm n nhiều động lực, vượt qua giai đoạn khó khăn để hồn tất chương trình học nghiên cứu sinh Tơi xin gửi lời cảm ơn tới đồng nghiệp thuộc Phòng Vật lý vật liệu từ siêu dẫn Phòng Hiển vi điện tử - Viện Khoa học vật liệu giúp đỡ nhiệt tình tạo điều kiện suốt thời gian thực luận án Tôi xin gửi lời cảm ơn tới GS Nguyễn Thị Kim Thanh, TS Lê Đức Tùng, Dr Stefanos Mourdikoudis công tác Đại học Luân Đôn (UCL) – Vương quốc Anh hỗ trợ giúp đỡ thời gian thực tập trao đổi nghiên cứu Phịng thí nghiệm vật liệu nano từ tính sinh học chăm sóc sức khỏe thuộc UCL Tôi xin gửi lời cảm ơn tới nhóm nghiên cứu TSKH Ivan Skorvanek thuộc Viện Vật lý thực nghiệm – Viện Hàn lâm Khoa học Slovakia, nhóm nghiên cứu GS Trần Vĩnh Hùng – Viện Nhiệt độ thấp Nghiên cứu cấu trúc – Viện Hàn lâm khoa học Ba Lan phép đo từ nhiệt độ thấp, từ trường cao Mossbauer bàn luận khoa học sâu sắc q trình hợp tác nghiên cứu ii Tơi xin trân trọng cảm ơn giúp đỡ tạo điều kiện thuận lợi sở đào tạo Học viện Khoa học Công nghệ, đặc biệt Viện Khoa học vật liệu, quan mà công tác, trình thực luận án Luận án hỗ trợ kinh phí dự án hợp tác ba bên nhóm nghiên cứu GS TSKH Nguyễn Xuân Phúc – Viện Khoa học vật liệu với nhóm nghiên cứu GS Nguyễn Thị Kim Thanh - Trường Đại học Luân Đôn GS Srinivas Sridhah – Trường đại học Đông Bắc – Hoa Kỳ tài trợ Văn phịng nghiên cứu phát triển khơng gian vũ trụ châu Á (AOARD) với mã số: FA2386, đề tài Hợp tác quốc tế cấp Viện Hàn lâm Khoa học công nghệ Việt Nam (VAST) mã số: QTSK01.01/20-21 QTPL01.01/20-21, nhiệm vụ thuộc chương trình hỗ trợ Nghiên cứu viên cao cấp (VAST) mã số: NVCC04.08/21-21, đề tài thuộc chương trình phát triển Vật lý với mã số: KHCBVL.02/21-22, nhiệm vụ khoa học công nghệ theo Nghị định thư với Nhật Bản mã số: NĐT.88.JP/20 Lời cảm ơn sau xin dành cho yêu thương, mong đợi chồng, hai hỗ trợ, cổ vũ tất người thân yêu gia đình nội, ngoại bạn bè thân thiết Những nguồn lực tinh thần lớn lao giúp con/em/chị/mẹ có thêm nhiều động lực để hồn thành luận án n Tác giả luận án Lê Thị Hồng Phong iii LỜI CAM ĐOAN Tôi xin cam đoan cơng trình nghiên cứu riêng tơi hướng dẫn khoa học PGS.TS Đỗ Hùng Mạnh PGS.TS Phạm Thanh Phong Các số liệu, kết nêu luận án trích dẫn lại từ báo xuất cộng Các số liệu, kết trung thực chưa công bố cơng trình khác Tác giả luận án n Lê Thị Hồng Phong iv DANH MỤC KÝ HIỆU VÀ CHỮ VIẾT TẮT Danh mục ký hiệu viết tắt : Hằng số mạng Bhf : Trường siêu tinh tế C : Nhiệt dung riêng E : Năng lượng dị hướng Ea : Năng lượng kích hoạt dx : Mật độ khối lượng D : Kích thước hạt Dc : Kích thước tới hạn đơn đơmen DFESEM : Kích thước từ ảnh FESEM DTEM : Kích thước từ ảnh TEM DSP : Kích thước siêu thuận từ DXRD : Kích thước tinh thể xác định từ giản đổ XRD f : Tần số fo : Tần số tiêu chuẩn H : Cường độ từ trường HA : Trường dị hướng Hac : Cường độ từ trường xoay chiều HC : Lực kháng từ HK : Từ trường dị hướng Hmax : Từ trường lớn Hmin : Từ trường nhỏ K : Hằng số dị hướng Keff : Hằng số dị hướng hiệu dụng KV : Hằng số dị hướng từ tinh thể KS : Hằng số dị hướng bề mặt kB : Hằng số Boltzmann m : Khối lượng M : Từ độ M (0) : Từ độ K n a v : Từ độ dư MS : Từ độ bão hòa n : Số hạt đơn vị thể tích P : Cơng suất Pf : Cơng suất tổn hao dịng điện xốy Fuco Ph : Công suất tổn hao từ trễ PL : Tổng công suất tổn hao Pr : Công suất tổn hao hồi phục rSP : Kích thước siêu thuận từ rSD : Kích thước đơn men T : Nhiệt độ TB : Nhiệt độ khóa Tb : Nhiệt độ bão hòa TC : Nhiệt độ Curie To : Nhiệt độ hiệu dụng TV : Nhiệt độ chuyển pha Verwey ΔT : Độ biến thiên nhiệt độ ∆Eq : Tách mức tứ cực điện ∆EM : Tách mức từ Zeeman t : Thời gian V : Thể tích hạt VH : Thể tích động học Vopt : Thể tích tối ưu hạt W : Năng lượng từ hóa ẟ : Dịch chuyển đồng phân η : Độ nhớt c : Khối lượng riêng 0 : Độ từ thẩm chân không χ’ : Phần thực độ cảm từ xoay chiều χ’’ : Phần ảo độ cảm từ xoay chiều τ : Thời gian hồi phục n Mr vi τB : Thời gian hồi phục Brown τeff : Thời gian hồi phục hiệu dụng τm : Thời gian hồi phục đặc trưng 𝜏𝑁 : Thời gian hồi phục Neél τ0 : Thời gian hồi phục đặc trưng ω0 : Tần số Larmor Danh mục chữ viết tắt Tiếng Anh Tiếng Việt AC : Alternating Current Dòng điện xoay chiều EC : Exchange Coupling Liên kết trao đổi Energy Dispersive X-ray Phổ tán xạ lượng tia X EDX ESC : Enhanced Spin Canting Nghiêng spin tăng cường FC : Field cooled n Làm lạnh có từ trường Field scanning Kính hiển vi điện tử quét phát xạ FESEM : emission electron microscope trường FM : Ferrimagnetism Feri từ ILP : Intrinsic loss power Công suất tổn hao nội LRT : Linear response theory Lý thuyết đáp ứng tuyến tính LSPR : MHT Localized surface plasmon Cộng hưởng plasmon bề mặt cục resonance : Magnetic hyperthermia Nhiệt từ trị MIH : Magnetic Inductive Heating Đốt nóng cảm ứng từ MNPs : Magnetic nanoparticles Các hạt nano từ MRI : Magnetic resonance imaging Ảnh cộng hưởng từ NPs : Nanoparticles Các hạt nano PPMS : SAR : Specific Absoption Rate Tốc độ hấp thụ riêng SHP : Specific Heating Power Cơng suất đốt nóng riêng Physical property measurement system Hệ đo tính chất vật lý vii SPM : Superparamagnetic SQUID : SW : Stoner-Wohlfarth TEM : Transmission electron Superconducting Siêu thuận từ quantum interference device Giao thoa kế lượng tử siêu dẫn Mơ hình mơ tả trạng thái từ hạt nano từ dị hướng Hiển vi điện tử truyền qua microscope VSM : Vibrating sample magnetometer Hệ từ kế mẫu rung XRD : X-ray difraction Nhiễu xạ tia X ZFC : Zero Field cooled Làm lạnh khơng có từ trường n viii DANH MỤC CÁC HÌNH VẼ VÀ ĐỒ THỊ Hình 1.1 Cấu trúc tinh thể ferit spinel Hình 1.2 Cấu trúc spinel đảo tinh thể Fe3O4 Hình 1.3 Cấu hình cặp ion ferit spinel với khoảng cách góc tối ưu cho tương tác từ hiệu Hình 1.4 (a) Đường cong từ trễ M(H) cho hạt nano Fe3O4 siêu thuận từ (màu xanh) sắt từ (màu cam) (b) mối quan hệ lực kháng từ với kích thước hạt trạng thái từ tính vật liệu nano Fe3O4 Hình 1.5 Lực kháng từ, HC (a) từ độ bão hòa, MS (b) phụ thuộc vào kích thước hạt hạt nano Fe3O4 hình cầu Hình 1.6 ( a) Đường cong ZFC hạt nano Fe3O4 hình dạng khác từ trường 50 Oe (b) Đường cong từ hóa ban đầu hạt nano Fe3O4 với hình dạng khác Hình 1.7 (a) Sơ đồ chế sinh nhiệt hạt nano từ đặt từ trường xoay chiều bao gồm: Các trình quay spin (hồi phục Néel) n quay hạt (hồi phục Brown) trạng thái siêu thuận từ tổn hao trễ trạng thái sắt từ (b) Kết tính SAR phụ thuộc kích thước hạt với tổn hao từ trễ tổn hao hồi phục Hình 1.8 Giá trị SAR thực nghiệm (điểm màu xanh) theo lý thuyết LRT phụ thuộc kích thước hạt nano Fe3O4 Hình 1.9 Giá trị SAR phụ thuộc kích thước hạt cường độ từ trường khác (184 - 625 Oe) hạt nano Fe3O4 Hình 1.10 Giá trị SAR phụ thuộc kích thước hạt Fe3O4 dạng hình cầu hình lập phương nồng độ mg/ml môi trường nước tần số 300 kHz từ trường thay đổi – 800 Oe Hình 1.11 Giá trị SAR phụ thuộc cường độ từ trường hạt nano Fe3O4 hình cầu, hình lập phương dạng với thể tích ~ 2000 nm3 Hình 1.12 (a) Đường cong nhiệt độ phụ thuộc thời gian đặt từ trường chất lỏng chứa hạt nano Fe3O4 với hình dạng khác với nồng độ 110 TÀI LIỆU THAM KHẢO M D Nguyen, H V Tran, S Xu, and T R Lee, “Fe3O4 nanoparticles: Structures, synthesis, magnetic properties, surface functionalization, and emerging applications,” Applied Sciences (Switzerland), vol 11, no 23 2021 doi: 10.3390/app112311301 [2] F G da Silva, J Depeyrot, A F C Campos, R Aquino, D Fiorani, and D Peddis, “Structural and Magnetic Properties of Spinel Ferrite Nanoparticles,” J Nanosci Nanotechnol., vol 19, no 8, pp 4888–4902, 2019, doi: 10.1166/jnn.2019.16877 [3] K K Kefeni, T A M Msagati, T T Nkambule, and B B Mamba, “Spinel ferrite nanoparticles 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