Luận án Tiến sĩ Nghiên cứu các cơ chế đốt nóng từ trong hệ hạt nano ferit spinel M1XZNXFE2O4 (M = MN, CO)

GI O V OT O VI N HÀN LÂM KHO H V NG NGH VI T N M HỌC VIỆN KHOA HỌC VÀ CÔNG NGHỆ PHẠM HỒNG NAM NGHIÊN CỨU CÁC CƠ CHẾ ĐỐT NÓNG TỪ TRONG HỆ HẠT NANO FERIT SPINEL M1-xZnxFe2O4 (M = Mn, Co) huyên ngành: Vật liệu điện tử Mã số: 62.44.01.23 LUẬN ÁN TIẾN SĨ KHOA HỌC VẬT LIỆU Hà Nội - 2018 GI O V OT O VI N H N L M KHO H V NG NGH VI T N M HỌC VIỆN KHOA HỌC VÀ CÔNG NGHỆ PHẠM HỒNG NAM NGHIÊN CỨU CÁC CƠ CHẾ ĐỐT NÓNG TỪ TRONG HỆ HẠT NANO FERIT SPINEL M1-xZnxFe2O4 (M = Mn, Co) huyên ngành: Vật liệu điện tử Mã số: 62.44.01.23 LUẬN ÁN TIẾN SĨ KHOA HỌC VẬT LIỆU NGƢỜI HƢỚNG DẪN KHOA HỌC: PGS.TS ĐỖ HÙNG MẠNH PGS.TS PHẠM THANH PHONG Hà Nội - 2018 LỜI CẢM ƠN Lời đầu tiên, tơi xin bày tỏ lịng biết ơn sâu sắc tới PGS.TS ỗ Hùng Mạnh PGS.TS Phạm Thanh Phong, người Thầy dành cho tơi động viên, giúp đỡ tận tình định hướng khoa học hiệu suốt trình thực luận án Tôi xin cảm ơn bảo, giúp đỡ khích lệ GS.TSKH Nguyễn Xuân Phúc, PGS.TS Trần ại Lâm, TS Hà Phương Thư TS Lê Trọng Lư dành cho năm qua Tôi xin đư c cảm ơn cộng tác giúp đỡ đầy hiệu N S ỗ Khánh Tùng, N S Lưu Hữu Nguyên, N Lê Thị Thanh Tâm cán Phòng Vật liệu nano y sinh, Phòng Vật lý vật liệu từ siêu dẫn - Viện Khoa học vật liệu (VKHVL) - Viện Hàn lâm Khoa học ông nghệ Việt Nam (VHLKH NVN), nơi tơi hồn thành luận án Tơi xin đư c gửi lời cảm ơn chân thành tới GS Nguyễn Thị Kim Thanh TS Lê ức Tùng, ại học London, Vương quốc Khoa Vật lý, Trường iện nh, PGS Phan Mạnh Hưởng, ại học Nam Florida, Mỹ cán thuộc iện tử, Trường ộ Môn ại học asque (UPV/EHU), Tây an Nha h p tác nghiên cứu giúp đỡ thực số phép đo quý báu Tôi xin đư c gửi lời cảm ơn tới học viên ộ môn Mô phôi Tế bào thuộc Khoa Sinh học Trường ại học Khoa học Tự nhiên ( HKHTN) - ại học Quốc gia Hà Nội ( HQGHN) h p tác nghiên cứu ứng dụng y sinh Tôi xin trân trọng cảm ơn giúp đỡ tạo điều kiện thuận l i sở đào tạo Học viện Khoa học ông nghệ VKHVL - VHLKH NVN, quan mà công tác, trình thực luận án Luận án đư c hỗ tr kinh phí ề tài cấp sở mã số S L02.16 (Viện Khoa học vật liệu), đề tài nghiên cứu định hướng ứng dụng mã số TNCCB- HƯ -2012-G/08 (N FOSTE ), đề tài h p tác quốc tế F 2386-14-10025 FA2386-17-1-4042 ( O R ), đề tài nghiên cứu mã số103.02– 2015.74 (Nafosted) Luận án đư c thực Phòng Vật liệu nano y sinh Phòng Vật lý vật liệu từ siêu dẫn (VKHVL, VHLKH NVN); Phòng Kỹ thuật i iện- iện tử (Viện Kỹ thuật nhiệt đới, VHLKH NVN) Khoa sinh học, Trường HKHTN, HQGHN Sau cùng, muốn gửi tới tất người thân gia đình bạn bè lời cảm ơn chân thành hính tin yêu mong đ i gia đình bạn bè tạo động lực cho thực thành công luận án Tác giả luận án Phạm Hồng Nam ii LỜI CAM ĐOAN Tôi xin cam đoan công trình nghiên cứu riêng tơi ác số liệu, kết nêu luận án đư c trích dẫn lại từ báo đư c xuất cộng ác số liệu, kết trung thực chưa đư c cơng bố cơng trình khác Tác giả luận án Phạm Hồng Nam iii DANH MỤC CÁC KÝ HIỆU VÀ CHỮ VIẾT TẮT I DANH MỤC CÁC KÝ HIỆU a : Hằng số mạng A : Phân mạng tứ diện A1 : A2 : Nội hệ hạt nano A3 : Năng lư ng chu trình từ hóa B : Phân mạng bát diện C : Nhiệt dung riêng c : Nồng độ hạt từ E : Năng lư ng dị hướng Ea : Năng lư ng kích hoạt dx : Mật độ khối lư ng D : Kích thước hạt Dc : Kích thước tới hạn đơn đơmen DFESEM : Kích thước từ ảnh FESEM DTEM : Kích thước tử ảnh TEM DSP : Kích thước siêu thuận từ DXRD : Kích thước từ giản đổ XR f : Tần số fo : Tần số tiêu chuẩn H : HA : Trường dị hướng Hc : Lực kháng từ Hmax : Từ trường lớn Hmin : Từ trường nhỏ K : Hằng số dị hướng Keff : Hằng số dị hướng hiệu dụng ộ lớn tương tác trao đổi ường độ từ trường iv KV : Hằng số dị hướng từ tinh thể KS : Hằng số dị hướng bề mặt kB : Hằng số Boltzmann L : Hàm Langevin m : Khối lư ng M : Từ độ M(0) : Từ độ 0K Me2+ : Mr : Từ dư Ms : Từ độ bão hòa Ms( ) : Từ độ vật liệu khối n : Số hạt đơn vị thể tích P : ơng suất Phys : ông suất tổn hao từ trễ Q : Nhiệt lư ng thu vào T : Nhiệt độ TB : Nhiệt độ khóa Tb : Nhiệt độ bão hịa TC : Nhiệt độ urie To : Nhiệt độ hiệu dụng T1 : Thời gian hồi phục spin-mạng T2 : Thời gian hồi phục spin-spin ΔT : t : Thời gian V : Thể tích hạt Vopt : Thể tích tối ưu hạt W : Năng lư ng từ hóa  ác kim loại hóa trị 2+ ộ biến thiên nhiệt độ : ộ dài tương quan : ộ nhớt chất lỏng từ v : ộ lớn tương tác trao đổi  : Khối lư ng riêng 0 : χ’ : Phần thực độ cảm từ xoay chiều χ’‘ : Phần ảo độ cảm từ xoay chiều ộ từ thẩm chân không : Thời gian hồi phục hiệu dụng : Thờ gian hồi phục rown τm : Thời gian hồi phục đặc trưng phép đo hồi phục : Thời gian hồi phục Neél : Thời gian hồi phục đặc trưng ω0 : Tần số Larmor II DANH MỤC CÁC CHỮ VIẾT TẮT Tiếng Anh Tiếng Việt EDX : Energy dispersive X-ray EHT : Exogenous heating FC : Field cooled FESEM : Field Phổ tán xạ lư ng tia X ốt nóng ngồi Làm lạnh có từ trường emission scanning Kính hiển vi điện tử quét phát xạ electron microscope trường Phổ hồng ngoại phân giải Fourier FTIR : Fourier-transform infrared ILP : Intrinsic loss of power ISPM : Interacting superparamagnetic Siêu thuận từ tương tác LRT : Linear response theory Lý thuyết đáp ứng tuyến tính MHT : Magnetic hyperthermia Nhiệt từ trị MRI : Magnetic resonance imaging Ảnh cộng hưởng từ hạt nhân NA : Neél Arrhenius Luật Neél Arrhenius OA : Oleic acid OLA : Oleylamine PMAO : Poly(maleic ông suất tổn hao nội anhydride-alt-1- vi octadecene) Physical property measurement Hệ đo tính chất vật lý PPMS : SPM : SQUID : SLP : SLPHC : SLPLRT : SLPmax : ông suất tổn hao cực đại SLPTN : ông suất tổn hao thực nghiệm SW : Stoner-Wohlfarth TEM : Transmission electron system Siêu thuận từ Superparamagnetic Superconducting quantum interference device Giao thoa kế lư ng tử siêu dẫn ông suất tổn hao riêng Specific loss power ông suất tổn hao sau hiệu chỉnh ông suất tổn hao theo lý thuyết đáp ứng tuyến tính Hiển vi điện tử truyền qua microscope TGA : Thermo gravimetric analysis Phân tích nhiệt vi lư ng XRD : X-ray difraction Nhiễu xạ tia X VF : Vogel-Fulcher Luật Vogel-Fulcher VSM : ZFC : Vibrating sample magnetometer Hệ từ kế mẫu rung Làm lạnh không từ trường Zero field cooled vii DANH MỤC CÁC HÌNH VẼ VÀ ĐỒ THỊ Hình 1.1 ấu trúc tinh thể vật liệu ferit spinel Hình 1.2 Một số cấu hình phân bố ion mạng spinel, phân mạng ion kim loại vị trí tứ diện bát diện, vịng trịn lớn ion ơxy Hình 1.3 Mơmen từ bão hịa K ferit spinel Hình 1.4 Mơmen từ bão hịa K ferit spinel Me2+Fe2O4 phụ thuộc vào nồng độ Zn2+, đường nét liền số liệu thực nghiệm, đường nét đứt kết tính theo cơng thức lý thuyết (1.3) Hình 1.5 Cơ chế đảo từ hệ hạt nano Hình 1.6 ác đường từ độ phụ thuộc nhiệt độ MnFe2O4 theo hai kiểu F ZFC Hình 1.7 Sự phụ thuộc mơmen từ vào từ trường H (a) H/T (b) nhiệt độ khác hạt nano Fe có kích thước = 4,4 nm Hình 1.8 Lực kháng từ phụ thuộc vào kích thước hạt Hình 1.9 ường M(H) với kích thước khác (a) phụ thuộc lực kháng từ vào kích thước hệ hạt nano Fe3O4 300 K (b) Hình 1.10 ường M(H) với kích thước khác (a) phụ thuộc lực kháng từ vào kích thước mẫu o0,4Fe2,6O3 (b) Hình 1.11 ường cong từ hóa tinh thể Fe (a) Co (b) theo phương khác Hình 1.12 Sự phụ thuộc Ms vào nồng độ pha tạp Zn2+ hệ nano (ZnxM1−x)Fe2O4 (M = Fe, Mn) Hình 1.13 Kết làm khớp phụ thuộc 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