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微波環(huán)行器用低維鐵氧體的制備及性能研究

發(fā)布時(shí)間:2018-05-18 08:20

  本文選題:微波環(huán)行器 + 鐵氧體薄膜 ; 參考:《電子科技大學(xué)》2016年博士論文


【摘要】:隨著電子信息和通訊技術(shù)的高速發(fā)展,電子器件不斷的向多功能、小型化發(fā)展,這對(duì)電子材料的篩選、制備以及設(shè)計(jì)提出了更高的要求。環(huán)行器屬于微波無(wú)源電子器件,利用鐵氧體材料的非互易性能,可實(shí)現(xiàn)對(duì)電磁信號(hào)傳播方向的調(diào)控。根據(jù)磁性器件的發(fā)展趨勢(shì),薄膜化、更多功能集成、工作頻率高頻化以及自偏置必將是磁性微波環(huán)行器的發(fā)展方向。六角M型鋇鐵氧體(BaFe_(12)O_(19),BaM)具有顯著的高單軸各向異性特性而被業(yè)界人員任命為未來(lái)環(huán)行器實(shí)現(xiàn)高頻以及自偏置的首選材料,同時(shí)釔鐵石榴石鐵氧體(Y3Fe5O12,YIG)具有顯著的低鐵磁共振線(xiàn)寬特性,因此低維BaM以及YIG的制備對(duì)實(shí)現(xiàn)環(huán)行器的小型化具有重要的意義。本論文的研究工作是圍繞著微波環(huán)行器用高飽和磁化強(qiáng)度、高磁晶各向異性場(chǎng)以及高矩形比的低維BaM材料以及低鐵磁共振線(xiàn)寬的低維YIG材料的制備進(jìn)行展開(kāi)。首先,分別在氧化鋁、氧化鎂以及硅基底上外延生長(zhǎng)BaM薄膜,通過(guò)測(cè)試設(shè)備對(duì)其微觀結(jié)構(gòu)以及磁性能進(jìn)行表征分析,探討薄膜的磁性能與沉積參數(shù)的關(guān)聯(lián)問(wèn)題,并最終擇出最佳薄膜沉積參數(shù)。其次在硅以及GGG基底上沉積制備亞微米厚度的YIG薄膜,探討鐵磁共振線(xiàn)寬擴(kuò)寬的機(jī)理問(wèn)題。然后嘗試在多孔硅掩模板里生長(zhǎng)鐵氧體納米線(xiàn)陣列膜,分析納米線(xiàn)的生長(zhǎng)機(jī)理及磁性能特性。最后利用脈沖激光沉積技術(shù)以及超薄氧化鋁掩模板(AAO)在不同襯底上制備二維鐵氧體納米點(diǎn)陣列膜,分析點(diǎn)陣的性能。主要內(nèi)容可分為以下四部分。1、BaM薄膜的制備以及性能的調(diào)控。(1)兩步燒結(jié)法制備致密性達(dá)到98.6%,且晶粒直徑僅為2.2mm的(33)a(44)靶材;((17))在氧化鋁基底上研究分析了沉積參數(shù)與薄膜微觀性能的關(guān)聯(lián)問(wèn)題,探討了薄膜微觀性能與磁性能的關(guān)聯(lián)問(wèn)題,并基于緩沖層Pt對(duì)薄膜的磁性能進(jìn)行調(diào)控研究。最終在20 nm厚的Pt以及最佳沉積參數(shù)下制備出具有357 emu/cm3的飽和磁化強(qiáng)度、16.5 kOe的單軸各向異性場(chǎng)以及不足20%的矩形比的BaM薄膜;(3)在氧化鎂基底上研究分析了退火溫度以及緩沖層Pt對(duì)BaM薄膜結(jié)構(gòu)以及磁性能的影響。研究緩沖層Pt在降低薄膜結(jié)晶溫度以及阻隔元素?cái)U(kuò)散方面的作用。并研究發(fā)現(xiàn)低溫長(zhǎng)時(shí)間退火處理在薄膜結(jié)晶性以及磁性能方面都有重要的改善作用。最終在20 nm-Pt的緩沖層上、950 oC-10 h的退火條件下制備出Ms高達(dá)358 emu/cm3,單軸各向異性場(chǎng)16.5 kOe,矩形比50.2%的BaM鐵氧體薄膜。(4)在硅基底上研究了緩沖層厚度對(duì)薄膜性能的影響,并最終在200nm-Pt緩沖層基礎(chǔ)上,900 oC-3 h的退火條件下得到BaM薄膜具有Ms高達(dá)317 emu/cm3,68.6%的矩形比以及15 kOe的單軸各向異性場(chǎng)。(5)通過(guò)對(duì)不同基底上的BaM薄膜進(jìn)行一階反轉(zhuǎn)曲線(xiàn)測(cè)試并對(duì)結(jié)果進(jìn)行分析對(duì)比,得到氧化鋁以及氧化鎂基底上得到的BaM薄膜以多疇晶粒結(jié)構(gòu)為主,而硅基底上的BaM薄膜以單疇晶粒結(jié)構(gòu)為主,并且晶粒之間的相互作用場(chǎng)大小滿(mǎn)足關(guān)系A(chǔ)l_2O_3MgOSi。2、YIG薄膜的的制備以及鐵磁共振線(xiàn)寬的研究。(1)采用分步燒結(jié)技術(shù)制備高質(zhì)量YIG靶材。(2)提出了采用多層緩沖層法,調(diào)控YIG薄膜的鐵磁共振特性。通過(guò)引入CeO2/YSZ以及三層(YAG/YAIG/YIG)低溫緩沖層,成功的將硅基底上YIG薄膜的鐵磁共振線(xiàn)寬降低到53 Oe,同時(shí)將YIG薄膜的最大無(wú)裂紋厚度提高到500 nm。(3)在GGG基底上研究制備亞微米級(jí)厚度的YIG薄膜,探討薄膜的鐵磁共振特性與薄膜微觀性能的關(guān)系問(wèn)題。通過(guò)鐵磁共振譜中的多峰以及與膜厚的關(guān)系問(wèn)題分析出薄膜內(nèi)存在擁有不同有效場(chǎng)的共振區(qū)域。并且通過(guò)不同磁場(chǎng)角度下共振譜得到亞微米級(jí)薄膜擁有7 Oe的本征鐵磁共振線(xiàn)寬以及最大25 Oe的非本征鐵磁共振線(xiàn)寬。3、鐵氧體納米線(xiàn)陣列膜的制備及其性能研究。(1)分別采用無(wú)電沉積銅顆粒法以及自組裝金點(diǎn)陣法制備多孔硅掩模板。并最終經(jīng)過(guò)兩步刻蝕出孔洞直徑與間距皆為500 nm的多孔硅掩模板。(2)利用溶膠凝膠法分別在多孔硅模板里生長(zhǎng)BaM以及鈷鐵氧體(CoFe2O_4,CFO)納米線(xiàn)陣列膜。微觀結(jié)構(gòu)顯示BaM以及CFO納米線(xiàn)陣列的直徑約為200 nm。磁性能上,BaM納米線(xiàn)陣列表現(xiàn)出各向同性特性,矯頑力以及矩形比分別為2560 Oe以及0.6。CFO納米線(xiàn)陣列也表現(xiàn)出各向同性特性,通過(guò)一階反轉(zhuǎn)曲線(xiàn)圖分析,矯頑力分布在1000 Oe出現(xiàn)的概率最高,納米線(xiàn)陣列之間存在一定的相互作用力。4、鐵氧體納米點(diǎn)陣膜的制備以及性能的研究。(1)YIG納米點(diǎn)陣膜的制備及磁性能的研究。分別在硅以及GGG基底上制備YIG納米點(diǎn)陣。微觀形貌上看,點(diǎn)陣的直徑與超薄AAO的直徑一致,大約在350 nm。YIG點(diǎn)陣具有比連續(xù)薄膜更大的矯頑力特性。YIG點(diǎn)陣的鐵磁共振譜出現(xiàn)多峰以及線(xiàn)寬展寬現(xiàn)象,可能源于納米點(diǎn)陣的微觀結(jié)構(gòu)的不均勻性和動(dòng)態(tài)磁化過(guò)程的非一致轉(zhuǎn)動(dòng)。(2)BaM點(diǎn)陣的制備及磁性能的研究。分別在硅以及氧化鋁基底上制備鋇鐵氧體點(diǎn)陣。X-射線(xiàn)衍射儀顯示氧化鋁基底上易獲得高取向點(diǎn)陣,點(diǎn)陣相比于連續(xù)薄膜具有更高的矩形比特性,同時(shí)一階反轉(zhuǎn)曲線(xiàn)圖顯示BaM點(diǎn)陣具有單疇特性。點(diǎn)陣具有顆粒間的相互作用力小于連續(xù)薄膜特性。
[Abstract]:With the rapid development of electronic information and communication technology, the electronic devices are constantly developing to multifunction and miniaturized. This has put forward higher requirements for the screening, preparation and design of electronic materials. The circulator is a microwave passive electronic device, and the non reciprocal properties of ferrite materials can be used to control the propagation direction of electromagnetic signals. According to the development trend of magnetic devices, thin film, more functional integration, high frequency frequency and self bias will certainly be the development direction of magnetic microwave circulators. The six angle M type barium ferrite (BaFe_ (12) O_ (19), BaM) has significant high uniaxial anisotropy and is appointed by industry personnel for high frequency and self bias of future circulators. The first choice material, while the yttrium ferric pomegranate ferrite (Y3Fe5O12, YIG) has a significant low ferromagnetic resonance linewidth characteristic, so the preparation of low dimensional BaM and YIG is of great significance for the realization of the miniaturization of the circulator. The research work of this paper is about the high saturation and magnetization of the microwave circulator, the high magnetic anisotropy field and the high moment. The preparation of low dimensional BaM material with shape ratio and low dimensional YIG material of low ferromagnetic resonance line width are carried out. First, BaM thin films are grown on alumina, Magnesium Oxide and silicon substrate respectively. The microstructure and magnetic properties of the thin films are characterized and analyzed by testing equipment. The relationship between the magnetic properties of thin films and the deposition parameters is discussed, and the most of them are discussed. The best thin film deposition parameters are selected. Secondly, the submicron thickness YIG film is deposited on the silicon and GGG substrates. The mechanism of the width expansion of the ferromagnetic resonance line is discussed. Then the ferrite nanowire array film is grown in the porous silicon mask, and the growth mechanism and magnetic properties of the nanowires are analyzed. Finally, the pulsed laser deposition is used. Technology and ultra-thin alumina mask (AAO) are used to prepare two-dimensional ferrite nanometers on different substrates and analyze the properties of the lattice. The main contents can be divided into four parts:.1, BaM film preparation and performance control. (1) two step sintering method is used to prepare 98.6% density, and the grain diameter is only 2.2mm (33) a (44) target; (17) in (17)) The relationship between the deposition parameters and the microstructure of the film was studied and analyzed on the alumina substrate. The relationship between the microstructure and magnetic properties was discussed. The magnetic properties of the films were regulated based on the buffer layer Pt. The saturation magnetization of 357 emu/cm3 was finally prepared under the 20 nm thick Pt and the optimum deposition parameters. 16.5 The uniaxial anisotropic field of kOe and the BaM thin film with a rectangular ratio of less than 20%; (3) the effects of annealing temperature and buffer layer Pt on the structure and magnetic properties of BaM films on the Magnesium Oxide substrate were investigated and analyzed. The effect of buffer layer Pt on the crystallization temperature of the film and the diffusion square surface of the barrier elements was studied. The treatment has an important improvement in the crystallinity and magnetic properties of the film. At 20 nm-Pt buffer layer and 950 oC-10 h annealing conditions, the effects of Ms as high as 358 emu/cm3, uniaxial anisotropy field 16.5 kOe, rectangular ratio 50.2% BaM ferrite film. (4) the effect of the thickness of buffer layer on the film properties is studied on the silicon substrate. Finally, on the basis of 200nm-Pt buffer layer, under the annealing condition of 900 oC-3 h, the BaM thin film has a rectangular ratio of up to 317 emu/cm3,68.6% and the uniaxial anisotropic field of 15 kOe. (5) the first order inversion curve of the BaM film on the different substrates is tested and the results are analyzed and compared, and the alumina and the Magnesium Oxide substrate are obtained. The BaM film is dominated by multi domain grain structure, and the BaM film on the silicon substrate is dominated by single domain crystal structure, and the interaction field between the grains satisfies the relationship Al_2O_3MgOSi.2, the preparation of the YIG film and the ferromagnetic resonance line width. (1) the high quality YIG target is prepared by the step sintering technology. (2) the application of the high quality YIG target is made. The ferromagnetic resonance characteristics of YIG films are regulated by the multilayer buffer layer method. By introducing CeO2/YSZ and three layer (YAG/YAIG/YIG) low temperature buffer layer, the ferromagnetic resonance line width of the YIG film on the silicon substrate is reduced to 53 Oe, and the maximum non crack thickness of the YIG film is raised to 500 nm. (3) to study the submicron thickness YIG on GGG substrate. The relationship between the ferromagnetic resonance characteristics of the film and the microstructure of the film is discussed. Through the multiple peaks in the ferromagnetic resonance spectrum and the relationship between the film thickness and the film thickness, the film has a resonant region with different effective fields. And the intrinsic ferromagnetic resonance of the submicron thin film with 7 Oe is obtained by the resonance spectrum of different magnetic fields. The line width and the maximum 25 Oe of the non intrinsic ferromagnetic resonance line width.3, the preparation and properties of the ferrite nanowire array film. (1) the porous silicon mask was prepared by the electroless copper particle method and the self assembled gold dot matrix method. The porous silicon mask with the diameter and spacing of the holes was 500 nm, and (2) using dissolution. BaM and cobalt ferrite (CoFe2O_4, CFO) nanowire arrays are grown in the porous silicon template respectively. The microstructure shows that the diameter of BaM and CFO nanowire arrays is about 200 nm. magnetic energy, the BaM nanowire array shows isotropic properties, the coercive force and the moment ratio are 2560 Oe and 0.6.CFO nanowire arrays respectively. According to the isotropic characteristics, the probability of the coercive force distribution at 1000 Oe is the highest by the first order reversal curve diagram. There is a certain interaction force.4 between the nanowire arrays, the preparation of the ferrite nano lattice film and the study of its properties. (1) the preparation and magnetic properties of the YIG nanometers are studied on silicon and GGG substrates, respectively. YIG nanometers are prepared. The micromorphology shows that the diameter of the lattice is in accordance with the diameter of the ultra-thin AAO. The ferromagnetic resonance spectrum of the ferromagnetic resonance spectrum of the.YIG lattice with greater coercivity than that of the continuous film appears at about 350 nm.YIG, which may arise from the inhomogeneity of the microstructures and the dynamic magnetization process of the nanolattice. Non uniform rotation. (2) the preparation and magnetic properties of BaM lattice. The barium ferrite lattice.X- ray diffractometer on silicon and alumina substrate shows high orientation lattice on the alumina substrate, and the lattice has a higher rectangular ratio than that of the continuous film. The first order reversal curve shows that the BaM lattice has a single domain at the same time. The lattice interaction between particles is smaller than that of continuous film.
【學(xué)位授予單位】:電子科技大學(xué)
【學(xué)位級(jí)別】:博士
【學(xué)位授予年份】:2016
【分類(lèi)號(hào)】:TM277;TN621

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