六角M型钡铁氧体材料的低温烧结与基本磁性能研究
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摘要
本文的工作围绕毫米波旋磁铁氧体器件用的六角BaM铁氧体材料这一主题而展开,旨在通过采用陶瓷工艺,经过掺杂和工艺调整,制备研究适于LTCF技术要求的微波铁氧体器件用M型钡铁氧体材料,研究材料结构与性能的关系;物相与工艺参数的关系;高频磁性能与配方、材料结构及工艺的关系;低温烧结的机理;通过精细制粉及助烧剂的添加以期研制出一种符合微波铁氧体器件性能要求又符合LTCF工艺技术要求的六角铁氧体材料。
在材料研制方面,采用氧化物(固相反应)法研制了一种实用的低温共烧M型Ba铁氧体材料。首先明确了M型铁氧体配方设计的基本原则,并在此基础上详细研究了材料结构与性能的关系、物相与工艺参数的关系、高频磁性能与配方、材料结构及工艺的关系;确定最佳的工艺参数;研究了掺杂Bi_2O_3等物质对M型铁氧体材料电磁性能的影响,证实掺杂助烧剂可以显著的降低材料的烧结温度;又研究了不同的离子(如ZnTi、CoTi等)取代对材料性能的影响。最后在一次球磨6小时、预烧温度1100℃、Bi_2O_3掺杂量为3wt%或V_2O_5的掺杂量为0.75%、二次球磨时间为9小时、在900℃烧结后制得了不同参数的M型铁氧体材料。通过对钡铁氧体掺杂实现了低温烧结,由于M型钡铁氧体具有的高磁晶各向异性内场,降低烧结温度使其有望实现通过LTCF(低温共烧铁氧体)技术研制片式化的微波/毫米波旋磁器件。
The work of this paper surround millimeter-wave gyromagnetic ferrite component’s hex-ferrite to expand, Using the ceramics and adjusting the adulteration and technology, M-type Ba ferrite material for microwave ferrite component was prepared in order to fit the LTCF(low temperature co-fire ferrite) technology. The research include: the relation of material structure and performance; the relation of microstructures and technics parameter; the relation of high frequency magnetic properties and compositions、material structure and technology; the mechanism of low temperature sinter. Through fine milling and adding dopants, one kind of applicable low temperature co-fired M-type Ba ferrite material was prepared in order to fit the LTCF technology.
In the part of experiments investigations, one kind of applicable low temperature co-fired M-type Ba ferrite material was prepared by the oxide method (solid-phase reaction). At first the basic principle of the compositions was defined, In this foundation, the relation of material structure and performance;the relation of microstructures and technics parameter; the relation of high frequency magnetic properties and compositions、material structure and technology was studied, Effect of adding Bi2O3 on the electromagnetic properties of Ba ferrite was investigated, it showed that adding this dopants can reduce the sintering temperature of Ba ferrite material evidently. The improvement on the electromagnetic properties of Ba ferrite by controling different ion substitute(such as ZnTi、CoTi) were studied also. Finally, the high performance Ba ferrite material was prepared on the condition of first milling is 6 hours, calcining at 1100℃, adding 3.0wt%Bi_2O_3 or 0.75wt% V_2O_5, second milling for 9h, sintering at 900℃. Through adding the dopant, low temperature of M-type ferrite was obtained. Because M-type Ba ferrite has high anisotropy inner field, the decrease of the ferrite sintering temperature makes the slice millimeter wave component through LTCF technology to become possible.
在材料研制方面,采用氧化物(固相反应)法研制了一种实用的低温共烧M型Ba铁氧体材料。首先明确了M型铁氧体配方设计的基本原则,并在此基础上详细研究了材料结构与性能的关系、物相与工艺参数的关系、高频磁性能与配方、材料结构及工艺的关系;确定最佳的工艺参数;研究了掺杂Bi_2O_3等物质对M型铁氧体材料电磁性能的影响,证实掺杂助烧剂可以显著的降低材料的烧结温度;又研究了不同的离子(如ZnTi、CoTi等)取代对材料性能的影响。最后在一次球磨6小时、预烧温度1100℃、Bi_2O_3掺杂量为3wt%或V_2O_5的掺杂量为0.75%、二次球磨时间为9小时、在900℃烧结后制得了不同参数的M型铁氧体材料。通过对钡铁氧体掺杂实现了低温烧结,由于M型钡铁氧体具有的高磁晶各向异性内场,降低烧结温度使其有望实现通过LTCF(低温共烧铁氧体)技术研制片式化的微波/毫米波旋磁器件。
The work of this paper surround millimeter-wave gyromagnetic ferrite component’s hex-ferrite to expand, Using the ceramics and adjusting the adulteration and technology, M-type Ba ferrite material for microwave ferrite component was prepared in order to fit the LTCF(low temperature co-fire ferrite) technology. The research include: the relation of material structure and performance; the relation of microstructures and technics parameter; the relation of high frequency magnetic properties and compositions、material structure and technology; the mechanism of low temperature sinter. Through fine milling and adding dopants, one kind of applicable low temperature co-fired M-type Ba ferrite material was prepared in order to fit the LTCF technology.
In the part of experiments investigations, one kind of applicable low temperature co-fired M-type Ba ferrite material was prepared by the oxide method (solid-phase reaction). At first the basic principle of the compositions was defined, In this foundation, the relation of material structure and performance;the relation of microstructures and technics parameter; the relation of high frequency magnetic properties and compositions、material structure and technology was studied, Effect of adding Bi2O3 on the electromagnetic properties of Ba ferrite was investigated, it showed that adding this dopants can reduce the sintering temperature of Ba ferrite material evidently. The improvement on the electromagnetic properties of Ba ferrite by controling different ion substitute(such as ZnTi、CoTi) were studied also. Finally, the high performance Ba ferrite material was prepared on the condition of first milling is 6 hours, calcining at 1100℃, adding 3.0wt%Bi_2O_3 or 0.75wt% V_2O_5, second milling for 9h, sintering at 900℃. Through adding the dopant, low temperature of M-type ferrite was obtained. Because M-type Ba ferrite has high anisotropy inner field, the decrease of the ferrite sintering temperature makes the slice millimeter wave component through LTCF technology to become possible.
引文
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[2] M. Pal, P. Brahma. Magnetic properties of Ba hexaferrites doped with bismuth oxide, Journal Magnetism and Magnetic Materials 147 (1995) 208-212
[3] A. Huanosta-Tera, R. de Lira-Hueso, O.Perez-Orta, S.A. Palomares-Sanchez, S. Ponce-Castaneda and M. Mirabal-Garcia, ELECTRIC CHARACTEIZATION OF (Sr, Sr-Ba,Ba) M-TYPE FERRITES BY AC MEASUREMENTS, Scripta mater. 42 (2000) 603~607
[4]冯全源,任朗. BaAl x Fe1 2 ? xO19铁氧体的微波特性[J].磁性材料及器件,1999.30(6):6-7,51
[5] E.Rezlescu, L.Rezlescu, P.D. Popa, N.Rezlescu, BaFe1 2 O1 9 fine crystals dispersed in a glassy matrix: magnetic and structural properties, Materials Science and Engineering ,A 375-377(2004)1269-1272
[6] Ping Xu, Xijiang Han, Hongtao Zhao, Zhihua Liang, Jiufu Wang, Effect of stoichiometry on the phase formation and magnetic properties of BaFe1 2 O1 9 nanoparticles by reverse micelle technique, Materials Letters xx (2007) xxx-xxx
[7] T. Kagotani, D.Fujiwara, S.Sugimoto, K.Inomata, M.Homma, Enhancement of GHz electromagnetic wave absorption characteristics in aligned M-type barium ferrite Ba1 ? x Lax Znx Fe1 2? x ? y (M e0 .5 Mn0 .5 ) yO1 9( x = 0.0 ? 0.5; y = 1.0 ? 3.0, Me : Zr, Sn) by metal substitution, Journal of Magnetism and Magnetic Materials 272-276 (2004) e1813-e1815
[8] Han-Shin Cho M-Hexaferrites with Planar Magnetic Anisotropy and Their Application to High-Frequency Microwave Absorbers. Transaction on magnetics Vol 35 No 5 Sep 1999
[9] L.Wane, A.Bessaudou, F.Cosset, et al. Thick barium hexaferrite (BaM) films prepared by electron-beam evaporation for microwave application[J]. Journal of Magnetism and Magnetic Materia1s,2000.211:309-313
[10] M.R.Meshram, Nawal K. Agrawal, Bharoti Sinha, P.S.Misra, Characterization of M-type barium hexagonal ferrite-based wide band microwave absorber, Journal of Magnetism and Magnetic Materials 271 (2004) 207-214
[11] O.Kubo, T.Ido and H.Yokoyama. Properties of Ba ferrite particles for perpendicular magneticrecording media[J]. IEEE Transactions on Magnetics,1982.MAG-18(6):1122-1124
[12] G. Turilli, F. Licci, A.Paoluzi, et al. NiTi substituted hexaferrites for magnetic recording[J]. IEEE Transactions on Magnetics, 1988.24(4):2146-2149
[13] C.Wang, F.Wei, M.Lu, et al. Structure and magnetic properties of Zn-Ti-substituted Ba-ferrite particles for magnetic recording[J]. Journal of Magnetism and Magnetic Materials,1998.183 241-246
[14] S. Rosler, P.Wartewig, H.Langbein. Synthesis and characterization of hexagonal ferrites Ba ( ZnTi )x Fe1 2 ? 2 xO19(0
[16]何水校.低温共烧铁氧体无源集成技术及其应用.磁性材料与器件,2003,29(5):4
[17]何水校,杨思勇. LTCF技术及其发展趋势.第六届国内外磁学与磁性材料发展及应用技术交流会议论文集:31-35
[18]贾利军,张怀武.添加Y 3+、Mn 2+对Z型软磁铁氧体结构与性能的影响磁性材料与器件2003年6月
[19]贾利军,张怀武,钟智勇.等,平面Z型软磁铁氧体频率特性的研究功能材料与器件学报Vol. 8,No.4 Dec. ,2002
[20]黄永杰,兰中文.磁性材料.成都:电子科技大学出版社,1993
[21]钟文定,铁磁学[M],科学出版社, 1987
[22] Zhang Haijun, Liu Zhichao, Ma Chengliang, Yao Xi, Zhang Liangying,“Complex permittivity, permeability, and microwave absorption of Zn- and Ti-substituted barium ferrite by citrate sol-gel process”, Materials Science and Engineering B96 (2002) 289-295
[23] P.Braun. The crystal structures of a new group of ferromagnetic compounds[J]. Philips Research. Report, 1957.12.491-548
[24]谢天,李晓红,逯迈,等,高密度磁记录用ZnTi替代钡铁氧体材料的温度特性研究[J].磁性材料与器件,2000.31(2):1~4,23
[25]张海军,姚熹,张良莹,等. BaM、BaCoTiM、BaZnTiM的柠檬酸溶胶-凝胶合成及其微波介电性能、磁性能研究[J].功能材料,2003.34(3):269-271
[26] Han-Shin Cho . M-Hexaferrites with Planar Magnetic Anisotropy and Their Application to High-Frequency Microwave Absorbers, Transactions on magnetics Vol 35 No5 Sep 1999
[27] C.Wang,F.Wei,M.Lu, et al. Structure and magnetic properties of ZnTi-substituted Ba-ferrite particles for magnetic recording[J]. Journal of Magnetism and MagneticMaterials,1998.183:241-246
[28] AUTISSER D,PODEMBSKI A,JACQU IOD C M Microwave properties of M and Z type hexaferrites [J] J Phys IV,1977,7:409-412
[29] Q.Feng and J.Lang. Microwave properties of Zn-Ti-substituted M-type barium hexaferrites[J]. IEEE Transaction on Magnetics, 2002.38(2):1391-1394
[30]冯全源, Ba ( ZnTi )x Fe1 2 ? 2 xO19铁氧体旋磁特性[J].磁性材料与器件, 2001.32(3):1-5
[31] O.Kubo,T.Ido and H.Yokoyama.“Properties of Ba ferrite particles for prependicular magnetic recording media[J].”IEEE Transactions on Magnetics,1982.MAG-18(6):1122-1124
[32] I.Nedkov, A.Petkov, V.Karpov. Microwave absorption in Sc- and CoTi-substituted Ba hexaferrite powders[J]. IEEE Transactions on Magnetics,1990.26(5):1483-1484
[33] Z.Simsa, S.Lego, R.Gerber, et al. Faraday rotation in cobalt- and titanium-subtituted barium hexaferrite[J], Journal of Magnetism and Magnetic Materials.1992,104-107:403-404
[34] Z.Simsa, S.Lego, R.Gerber, et al. Cation distribution in Co-Ti-substituted barium hexaferrites:a consistent model[J]. Journal of Magnetism and Magnetic Materials,1995.140-144:2103-2104
[35] J.Williams, J.Adetunji, M.Gregori. Mossbauer spectroscopic determination of magnetic moments of Fe 3+ and Co 2+ in substituted barium hexaferrite, Ba (C o, Ti )x Fe1 2 ? 2 xO19[J]. Journal of Magnetism and Magnetic Materials,2000.220:124-128
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