CN111747745A - 一种5g滤波器用介质粉体及其制备方法 - Google Patents
一种5g滤波器用介质粉体及其制备方法 Download PDFInfo
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- CN111747745A CN111747745A CN202010431931.2A CN202010431931A CN111747745A CN 111747745 A CN111747745 A CN 111747745A CN 202010431931 A CN202010431931 A CN 202010431931A CN 111747745 A CN111747745 A CN 111747745A
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- 239000000843 powder Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 56
- 229910010252 TiO3 Inorganic materials 0.000 claims abstract description 38
- 239000000126 substance Substances 0.000 claims abstract description 24
- 239000000919 ceramic Substances 0.000 claims abstract description 14
- 239000013078 crystal Substances 0.000 claims abstract description 10
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 6
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 3
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 3
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 3
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 3
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 3
- 238000004891 communication Methods 0.000 claims abstract description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 3
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 3
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 3
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 3
- 229910052718 tin Inorganic materials 0.000 claims abstract description 3
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 3
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 62
- 239000002002 slurry Substances 0.000 claims description 45
- 238000002156 mixing Methods 0.000 claims description 38
- 238000000227 grinding Methods 0.000 claims description 32
- 239000008367 deionised water Substances 0.000 claims description 31
- 229910021641 deionized water Inorganic materials 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 30
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000000498 ball milling Methods 0.000 claims description 15
- 239000004576 sand Substances 0.000 claims description 15
- 239000004575 stone Substances 0.000 claims description 15
- 239000004408 titanium dioxide Substances 0.000 claims description 14
- 239000012071 phase Substances 0.000 claims description 11
- 239000007790 solid phase Substances 0.000 claims description 11
- 230000015572 biosynthetic process Effects 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000005469 granulation Methods 0.000 claims description 10
- 230000003179 granulation Effects 0.000 claims description 10
- 238000010298 pulverizing process Methods 0.000 claims description 10
- 239000007921 spray Substances 0.000 claims description 10
- 238000001694 spray drying Methods 0.000 claims description 10
- 238000003786 synthesis reaction Methods 0.000 claims description 10
- 239000010955 niobium Substances 0.000 claims description 9
- 239000011701 zinc Substances 0.000 claims description 9
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 230000001590 oxidative effect Effects 0.000 claims description 8
- 239000011575 calcium Substances 0.000 claims description 7
- 238000011049 filling Methods 0.000 claims description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 6
- 239000011777 magnesium Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 5
- 239000001095 magnesium carbonate Substances 0.000 claims description 5
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 4
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims description 4
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 4
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 4
- HFLAMWCKUFHSAZ-UHFFFAOYSA-N niobium dioxide Chemical compound O=[Nb]=O HFLAMWCKUFHSAZ-UHFFFAOYSA-N 0.000 claims description 4
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 4
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 3
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(II) oxide Inorganic materials [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 3
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 3
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 3
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 3
- 229910001954 samarium oxide Inorganic materials 0.000 claims description 3
- 229940075630 samarium oxide Drugs 0.000 claims description 3
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims description 3
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 3
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 claims description 3
- 229910021511 zinc hydroxide Inorganic materials 0.000 claims description 3
- 229940007718 zinc hydroxide Drugs 0.000 claims description 3
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 claims description 2
- QUEDYRXQWSDKKG-UHFFFAOYSA-M [O-2].[O-2].[V+5].[OH-] Chemical compound [O-2].[O-2].[V+5].[OH-] QUEDYRXQWSDKKG-UHFFFAOYSA-M 0.000 claims description 2
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims description 2
- 229910001863 barium hydroxide Inorganic materials 0.000 claims description 2
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- 229910021446 cobalt carbonate Inorganic materials 0.000 claims description 2
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 claims description 2
- IUYLTEAJCNAMJK-UHFFFAOYSA-N cobalt(2+);oxygen(2-) Chemical compound [O-2].[Co+2] IUYLTEAJCNAMJK-UHFFFAOYSA-N 0.000 claims description 2
- RDYMFSUJUZBWLH-UHFFFAOYSA-N endosulfan Chemical compound C12COS(=O)OCC2C2(Cl)C(Cl)=C(Cl)C1(Cl)C2(Cl)Cl RDYMFSUJUZBWLH-UHFFFAOYSA-N 0.000 claims description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 2
- 239000000347 magnesium hydroxide Substances 0.000 claims description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 2
- 229910001887 tin oxide Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 2
- 239000001393 triammonium citrate Substances 0.000 claims description 2
- 235000011046 triammonium citrate Nutrition 0.000 claims description 2
- 239000011667 zinc carbonate Substances 0.000 claims description 2
- 229910000010 zinc carbonate Inorganic materials 0.000 claims description 2
- 235000004416 zinc carbonate Nutrition 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 238000011068 loading method Methods 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000010295 mobile communication Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical compound [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 1
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- C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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Abstract
本发明公开的一种5G滤波器用介质粉体及其制备方法，该5G滤波器用介质粉体的化学结构式为(1‑z)A4M2O9‑zBxDyTiO3，由A4M2O9、BxDyTiO3两种晶相构成，z为BxDyTiO3相的摩尔分数，其中A为Mg、Zn中的一种，M为Sb、Ta、Nb、V中的一种，0.1<z<0.48；B为Ca、Sr、Ba中的一种，D为Sr、Sm、La、Ce、Nd、Sn、Co中的至少一种，0.5<x<0.9、y<1，x、y与B、D元素的化合价组合使BxDyTiO3总化合价代数和为零。本发明所述的一种5G滤波器用介质粉体及其制备方法，属于介质陶瓷原料制备技术领域，经验证本发明所述的介质陶瓷粉体具有介电常数可调、高品质因数、近零温漂的特点，应用于5G通信滤波器性能稳定，应用前景广泛、推广潜力较大。
Description
技术领域
本发明涉及一种介质粉体，尤其涉及到高品质因数、近零温漂的5G滤波器用介质粉体，属于介质陶瓷原料制备技术领域。
背景技术
根据全球移动通信系统协会(GSMA)最新发布的移动经济报告显示,全球通信运营商在202根据全球移动通信系统协会(GSMA)最新发布的移动经济报告显示，全球通信运营商在2020至2025年间至少将投入10270亿美元，其中80％将用于5G网络建设。介质陶瓷滤波器成为华为、中兴、三星等通信公司的首选。
介质陶瓷滤波器中的电磁波谐振发生在陶瓷介质材料内部，因此对于微波介质陶瓷材料的性能要求更高。陶瓷粉体的性能决定了介质滤波器的性能，粉体的配方与制备的难度较高。只有拥有好的材料配方才能获得在一定使用条件下的高Q值、低温漂的介质陶瓷，可以说获取性能优异的介质陶瓷粉体是陶瓷滤波器厂商的核心竞争力。
现有的微波介质陶瓷材料的介电常数在15～30之间连续可调，25℃的f*Q＞45000，具有良好的温度特性，在-40℃、25℃、110℃时的频率温度系数均接近零，温度稳定性高。但所述滤波器的Q×f0仍然偏低，已不能满足5G滤波器行业日益严格的要求，同时现有测试频率温度系数已打145℃，要求日趋严格；实质上要求组成陶瓷的微观晶相结构高度稳定。
发明内容
本发明的旨在提供一种高品质因数、近零温漂的5G滤波器用介质粉体及其制备方法。
为实现上述目的，本发明采取的技术方案为：
一种5G滤波器用介质粉体，该5G滤波器用介质粉体的化学结构式为(1-z)A4M2O9-zBxDyTiO3，由A4M2O9、BxDyTiO3两种晶相构成，z为BxDyTiO3相的摩尔分数，其中A为Mg、Zn中的一种，M为Sb、Ta、Nb、V中的一种，0.1<z<0.48；B为Ca、Sr、Ba中的一种，D为Sr、Sm、La、Ce、Nd、Sn、Co中的至少一种，0.5<x<0.9、y<1，x、y与B、D元素的化合价组合使BxDyTiO3总化合价代数和为零。
优选的，所述的5G通信滤波器用介质陶瓷粉体的化学结构式优选为0.74Mg4Ta2O9-0.26Ca0.8Sm0.4/3TiO3、0.82Mg4Ta2O9-0.18Ca0.5Sr0.5TiO3、0.80Mg4Nb2O9-0.20Ca0.6La0.8/3TiO3、0.87Mg4V2O9-0.13Sr0.95Co0.05TiO3、0.58Zn4Sb2O9-0.42Ba0.571Ce0.286TiO3中的一种。
优选的，该介质粉体的相对介电常数εr在18～21区间内可调，在-40℃、150℃温度下其谐振频率温度系数τf均可控制在-2ppm～2ppm，在25℃、10GHz下其品质因数Q×f0大于100000GHz；在10GHz下A4M2O9晶相的品质因数Q×f0>160000GHz，BxDyTiO3晶相的相对介电常数εr>100，在150℃下BxDyO3晶相谐振频率温度系数τf>200ppm。
一种5G滤波器用介质粉体的制备方法，包括以下步骤:
S1、合成A4M2O9：将含有A元素的原料、含有M元素的原料、有机助磨剂、去离子水加入至混合罐中混合均匀得浆料Ⅰ，然后将浆料Ⅰ转移至以氧化锆球石为研磨介质的砂磨机中研磨8～12h，至用激光粒度分析仪检测D50粒径小于0.20μm，采用喷雾干燥法将原料造粒并干燥，然后将干燥后的原料装入匣钵并放入电炉，在氧化气氛中按照100℃/h的升温速率升温至900℃～1000℃，然后在900℃～1000℃保温4h，冷却后取出得A4M2O9粉；
S2、合成BxDyTiO3：将含有B元素的原料、含有D元素的原料、二氧化钛、有机助磨剂、去离子水加入至混合罐中混合均匀得浆料Ⅱ，然后将浆料Ⅱ转移至以氧化锆球石为研磨介质的砂磨机中研磨8～12h，至用激光粒度分析仪检测D50粒径小于0.20μm，采用喷雾干燥法将原料造粒并干燥，然后将干燥后的原料装入匣钵并放入电炉，在氧化气氛中按照100℃/h的升温速率升温至900℃～1000℃，然后在900℃～1000℃保温4h，冷却后取出得BxDyTiO3粉；
S3、机械球磨法混合：将S1、S2步骤中获得的A4M2O9粉、BxDyTiO3粉按照(1-z)：z的摩尔比加入至卧式球磨罐中，加入去离子水、有机助磨剂、粘结剂混合均匀，即为浆料Ⅲ，然后加入氧化锆球石采用球料比为5:1球磨4-8h，将浆料Ⅲ转移至砂磨机中研磨8～12h，至用激光粒度分析仪检测D50粒径小于0.20μm，然后将浆料转移至离心型喷雾造粒塔中喷雾造粒，加筛控制颗粒粒径在80～120目，所得颗粒即为5G滤波器用介质粉体
优选的，所述步骤S1中含有A元素的原料为氢氧化镁、氢氧化锌、氧化镁、氧化锌、碳酸镁、碱式碳酸镁、碳酸锌、碳酸钴中的至少一种；含有M元素的原料为五氧化二铌、二氧化铌、三氧化二钒、五氧化二钒、五氧化二锑、三氧化二锑、五氧化二钽中的至少一种；含有A元素的原料与含有M元素的原料的加入量遵守加入A、M两种元素的摩尔比为2:1；所述的含有A元素的原料与含有M元素的原料为分析纯级，其粒径为0.5～1.2μm。
优选的，所述步骤S2中含有B元素的原料为碳酸锶、碳酸钡、碳酸钙、氢氧化钙、氢氧化钡、硫酸钡中的至少一种；含有D元素的原料为氧化钐、氧化镧、氧化钕、氧化锡、氧化铈、碳酸锶、氧化亚钴、四氧化三钴、三氧化二钴、中的至少一种；含有B元素的原料、含有D元素的原料、二氧化钛的加入量遵守B、D、Ti元素摩尔比为x：y:1的要求；其中0.5<x<1、y<1，x、y与B、D元素的化合价组合使BxDyTiO3总化合价代数和为零，所述的含有B元素的原料与含有D元素的原料为分析纯级，其粒径为0.5～1.2μm；所述的二氧化钛为分析纯二氧化钛，其粒径为0.5～1.2μm。
优选的，所述有机助磨剂为聚丙烯酸铵、柠檬酸三铵、司马化工CE-64、司马化工PC-67、日油型号AKM-0531中的至少一种；所述浆料Ⅰ、浆料Ⅱ、浆料Ⅲ的固相物质重量百分数均为15～20％，其中有机助磨剂的添加量为去离子水重量的0.2-0.5％；所述浆料Ⅲ中粘结剂优选为司马化工PAF635，浆料Ⅲ中粘结剂的添加量为去离子水重量的1-5％。
与现有技术相比，本发明具有如下有益效果：
本发明制备的5G滤波器用介质粉体，具有以下优点：
(1)本发明首次将A4M2O9晶相(高品质因数、负谐振频率温度系数)与BxDyTiO3混合(高介电常数、正高谐振频率温度系数)，使得介质粉体具有介电常数可调、高品质因数、近零温漂的特点；相对介电常数εr在18～21区间内可调，在-40℃、150℃温度下它的谐振频率温度系数τf均可控制在-2ppm～2ppm，在25℃、10GHz下它的品质因数Q×f0大于100000GHz；
(2)采用两步煅烧法制备构成介质粉体的两种晶相，由于煅烧前和混合前两种粉体的粒径都小于0.2微米，使介质粉体微观上更加均匀、规模生产的一致性好，烧结后的5G滤波器介质陶瓷收缩均匀、密度一致、微观晶相一致；由于具有0.2微米的粉体粒径，粉体不用添加其它助烧剂，其烧结温度控制在1250-1300℃即可。
具体实施方式
本发明结合以下实例对一种5G滤波器用介质粉体及其制备方法做进一步的描述；可以理解的是，此处所描述的具体实施例仅仅用于解释相关发明，而非对该发明的限定。
实施例1
一种高品质因数、近零温漂的5G滤波器用介质粉体ⅰ的化学结构式为：0.74Mg4Ta2O9-0.26Ca0.8Sm0.4/3TiO3，其制备方法，包括以下步骤：
(1)合成Mg4Ta2O9：首先分别称取摩尔比为4:1的分析纯的碳酸镁(中位粒径D50为0.6μm)、分析纯五氧化二钽(中位粒径D50为1.2μm)至混合罐中，然后加入去离子水配置成固相物质重量百分数均为15％的混合液，再加入去离子水重量0.2％的聚丙烯酸铵至混合罐中，搅拌混合均匀得浆料Ⅰ，然后将浆料Ⅰ转移至以氧化锆球石为研磨介质的砂磨机中研磨9h，至用激光粒度分析仪检测D50粒径小于0.20μm，采用喷雾干燥法将原料造粒并干燥，然后将干燥后的原料装入匣钵并放入电炉，在氧化气氛中按照100℃/h的升温速率升温至900℃，然后在900℃保温4h，冷却后取出得Mg4Ta2O9粉；
(2)合成Ca0.8Sm0.4/3TiO3：首先分别称取摩尔比为4.8:0.4的分析纯碳酸钙(中位粒径D50为0.5μm)、分析纯氧化钐(Sm2SO3)(中位粒径D50为1.2μm)、分析纯二氧化钛(中位粒径D50为0.5μm)至混合罐中，然后加入去离子水配置成固相物质重量百分数均为18％的混合液，再加入去离子水重量0.3％的PC-67至混合罐中，搅拌混合均匀得浆料Ⅱ，然后将浆料Ⅱ转移至以氧化锆球石为研磨介质的砂磨机中研磨12h，至用激光粒度分析仪检测D50粒径小于0.20μm，采用喷雾干燥法将原料造粒并干燥，然后将干燥后的原料装入匣钵并放入电炉，在氧化气氛中按照100℃/h的升温速率升温至1000℃，然后在1000℃保温4h，冷却后取出得Ca0.8Sm0.4/3TiO3粉；
(3)机械球磨法混合：将(1)(2)步中获得的Mg4Ta2O9粉、Ca0.8Sm0.4/3TiO3粉、按照0.74：0.26的摩尔比加入至卧式球磨罐中，加入去离子水配制成固相物质重量百分数均为16％的混合液，然后加入去离子水重量的0.5％的PC-67、去离子水重量的2％的PAF635混合均匀，即为浆料Ⅲ，然后加入氧化锆球石采用球料比为5:1球磨7h，将浆料Ⅲ转移至砂磨机中研磨8h，至用激光粒度分析仪检测D50粒径小于0.20μm，然后将浆料转移至离心型喷雾造粒塔中喷雾造粒，加筛控制颗粒粒径在80～120目，所得颗粒即为高品质因数、近零温漂的5G滤波器用介质粉体ⅰ。
实施例2
一种高品质因数、近零温漂的5G滤波器用介质粉体ⅱ的化学结构式为：0.58Zn4Sb2O9-0.42Ba0.571Ce0.286TiO3，其制备方法，包括以下步骤：
(1)合成Zn4Sb2O9：首先分别称取摩尔比为4:1的分析纯的氢氧化锌(中位粒径D50为1.2μm)、分析纯三氧化二锑(中位粒径D50为1.0μm)至混合罐中，然后加入去离子水配置成固相物质重量百分数均为20％的混合液，再加入去离子水重量0.5％的CE-64至混合罐中，搅拌混合均匀得浆料Ⅰ，然后将浆料Ⅰ转移至以氧化锆球石为研磨介质的砂磨机中研磨11h，至用激光粒度分析仪检测D50粒径小于0.20μm，采用喷雾干燥法将原料造粒并干燥，然后将干燥后的原料装入匣钵并放入电炉，在氧化气氛中按照100℃/h的升温速率升温至950℃，然后在950℃保温4h，冷却后取出得Zn4Sb2O9粉；
(2)合成Ba0.571Ce0.286TiO3：首先分别称取摩尔比为0.571:0.286：1的分析纯碳酸钡(中位粒径D50为0.5μm)、分析纯氧化铈(CeO2)(中位粒径D50为1.0μm)、分析纯二氧化钛(中位粒径D50为1.2μm)至混合罐中，然后加入去离子水配置成固相物质重量百分数均为17％的混合液，再加入去离子水重量0.1％的CE-64至混合罐中，搅拌混合均匀得浆料Ⅱ，然后将浆料Ⅱ转移至以氧化锆球石为研磨介质的砂磨机中研磨11h，至用激光粒度分析仪检测D50粒径小于0.20μm，采用喷雾干燥法将原料造粒并干燥，然后将干燥后的原料装入匣钵并放入电炉，在氧化气氛中按照100℃/h的升温速率升温至1000℃，然后在1000℃保温4h，冷却后取出得Ba0.571Ce0.286TiO3粉；
(3)机械球磨法混合：将(1)(2)步中获得的Zn4Sb2O9粉、Ba0.571Ce0.286TiO3粉按照0.58：0.42的摩尔比加入至卧式球磨罐中，加入去离子水配制成固相物质重量百分数均为18.5％的混合液，然后加入去离子水重量的0.5％的PC-67、去离子水重量的1％的PAF635混合均匀，即为浆料Ⅲ，然后加入氧化锆球石采用球料比为5:1球磨8h，将浆料Ⅲ转移至砂磨机中研磨8h，至用激光粒度分析仪检测D50粒径小于0.20μm，然后将浆料转移至离心型喷雾造粒塔中喷雾造粒，加筛控制颗粒粒径在80～120目，所得颗粒即为高品质因数、近零温漂的5G滤波器用介质粉体ⅱ。
实施例3
一种高品质因数、近零温漂的5G滤波器用介质粉体ⅲ的化学结构式为：0.61Zn4Nb2O9-0.39Ca0.5Co0.5TiO3，其制备方法，包括以下步骤：
(1)合成Zn4Nb2O9：首先分别称取摩尔比为4:1的分析纯的氧化锌(中位粒径D50为0.8μm)、分析纯五氧化二铌(中位粒径D50为1.1μm)至混合罐中，然后加入去离子水配置成固相物质重量百分数均为18％的混合液，再加入去离子水重量0.5％的日油型号AKM-0531助磨剂至混合罐中，搅拌混合均匀得浆料Ⅰ，然后将浆料Ⅰ转移至以氧化锆球石为研磨介质的砂磨机中研磨10h，至用激光粒度分析仪检测D50粒径小于0.20μm，采用喷雾干燥法将原料造粒并干燥，然后将干燥后的原料装入匣钵并放入电炉，在氧化气氛中按照100℃/h的升温速率升温至900℃，然后在900℃保温4h，冷却后取出得Zn4Nb2O9粉；
(2)合成Ca0.5Co0.5TiO3：首先分别称取摩尔比为0.5:0.5:1的分析纯碳酸钙(中位粒径D50为1.2μm)、分析纯氧化钴(CoO)(中位粒径D50为1.2μm)、分析纯二氧化钛(中位粒径D50为0.5μm)至混合罐中，然后加入去离子水配置成固相物质重量百分数均为19％的混合液，再加入去离子水重量0.3％的日油型号AKM-0531助磨剂至混合罐中，搅拌混合均匀得浆料Ⅱ，然后将浆料Ⅱ转移至以氧化锆球石为研磨介质的砂磨机中研磨11h，至用激光粒度分析仪检测D50粒径小于0.20μm，采用喷雾干燥法将原料造粒并干燥，然后将干燥后的原料装入匣钵并放入电炉，在氧化气氛中按照100℃/h的升温速率升温至900℃，然后在900℃保温4h，冷却后取出得Ca0.5Co0.5TiO3粉；
(3)机械球磨法混合：将(1)(2)步中获得的Zn4Nb2O9粉、Ca0.5Co0.5TiO3粉按照0.61：0.39的摩尔比加入至卧式球磨罐中，加入去离子水配制成固相物质重量百分数均为20％的混合液，然后加入去离子水重量的0.4％的PC-67、去离子水重量的3％的PAF635混合均匀，即为浆料Ⅲ，然后加入氧化锆球石采用球料比为5:1球磨5h，将浆料Ⅲ转移至砂磨机中研磨9h，至用激光粒度分析仪检测D50粒径小于0.20μm，然后将浆料转移至离心型喷雾造粒塔中喷雾造粒，加筛控制颗粒粒径在80～120目，所得颗粒即为高品质因数、近零温漂的5G滤波器用介质粉体ⅲ。
将实施例1-3中所述的Ca0.5Co0.5TiO3粉、Zn4Nb2O9粉、Ba0.571Ce0.286TiO3粉Zn4Sb2O9粉、Ca0.8Sm0.4/3TiO3粉、Mg4Ta2O9粉采用喷雾造粒塔造粒，然后采用干压法成型，然后以100℃/h升温至1500℃后在1500℃保温3h，烧结成测试尺寸样块，采用安捷伦E5071C ENA矢量网络分析仪，辅以介电常数测试仪、Q值测试工装，部分性能测试结果如下表：
将实施例1-3所述的5G滤波器用介质粉体采用干压法成型，然后以100℃/h升温至1000℃后再以50℃/h升温至1300℃，最后在1300℃保温4h，烧结成测试尺寸样块，采用安捷伦E5071C ENA矢量网络分析仪，辅以介电常数测试仪、Q值测试工装，测试实施例1-3所述的5G滤波器用介质粉体的介电性能，测试结果如下表：
尽管本发明已作了详细说明并引证了实施例，但对于本领域的普通技术人员，显然可以按照上述说明而做出的各种方案、修改和改动，都应该包括在权利要求的范围之内。
Claims (7)
1.一种5G滤波器用介质粉体，其特征在于：该5G滤波器用介质粉体的化学结构式为(1-z)A4M2O9-zBxDyTiO3，由A4M2O9、BxDyTiO3两种晶相构成，z为BxDyTiO3相的摩尔分数，其中A为Mg、Zn中的一种，M为Sb、Ta、Nb、V中的一种，0.1<z<0.48；B为Ca、Sr、Ba中的一种，D为Sr、Sm、La、Ce、Nd、Sn、Co中的至少一种，0.5<x<0.9、y<1，x、y与B、D元素的化合价组合使BxDyTiO3总化合价代数和为零。
2.根据权利要求1所述的一种5G滤波器用介质粉体，其特征在于：所述的5G通信滤波器用介质陶瓷粉体的化学结构式优选为0.74Mg4Ta2O9-0.26Ca0.8Sm0.4/3TiO3、0.82Mg4Ta2O9-0.18Ca0.5Sr0.5TiO3、0.80Mg4Nb2O9-0.20Ca0.6La0.8/3TiO3、0.87Mg4V2O9-0.13Sr0.95Co0.05TiO3、0.58Zn4Sb2O9-0.42Ba0.571Ce0.286TiO3中的一种。
3.根据权利要求1所述的一种5G滤波器用介质粉体，其特征在于：该介质粉体的相对介电常数εr在18～21区间内可调，在-40℃、150℃温度下其谐振频率温度系数τf均可控制在-2ppm～2ppm，在25℃、10GHz下其品质因数Q×f0大于100000GHz；在10GHz下A4M2O9晶相的品质因数Q×f0>160000GHz，BxDyTiO3晶相的相对介电常数εr>100，在150℃下BxDyO3晶相谐振频率温度系数τf>200ppm。
4.一种5G滤波器用介质粉体的制备方法，其特征在于，包括以下步骤:
S1、合成A4M2O9：将含有A元素的原料、含有M元素的原料、有机助磨剂、去离子水加入至混合罐中混合均匀得浆料Ⅰ，然后将浆料Ⅰ转移至以氧化锆球石为研磨介质的砂磨机中研磨8～12h，至用激光粒度分析仪检测D50粒径小于0.20μm，采用喷雾干燥法将原料造粒并干燥，然后将干燥后的原料装入匣钵并放入电炉，在氧化气氛中按照100℃/h的升温速率升温至900℃～1000℃，然后在900℃～1000℃保温4h，冷却后取出得A4M2O9粉；
S2、合成BxDyTiO3：将含有B元素的原料、含有D元素的原料、二氧化钛、有机助磨剂、去离子水加入至混合罐中混合均匀得浆料Ⅱ，然后将浆料Ⅱ转移至以氧化锆球石为研磨介质的砂磨机中研磨8～12h，至用激光粒度分析仪检测D50粒径小于0.20μm，采用喷雾干燥法将原料造粒并干燥，然后将干燥后的原料装入匣钵并放入电炉，在氧化气氛中按照100℃/h的升温速率升温至900℃～1000℃，然后在900℃～1000℃保温4h，冷却后取出得BxDyTiO3粉；
S3、机械球磨法混合：将S1、S2步骤中获得的A4M2O9粉、BxDyTiO3粉按照(1-z)：z的摩尔比加入至卧式球磨罐中，加入去离子水、有机助磨剂、粘结剂混合均匀，即为浆料Ⅲ，然后加入氧化锆球石采用球料比为5:1球磨4-8h，将浆料Ⅲ转移至砂磨机中研磨8～12h，至用激光粒度分析仪检测D50粒径小于0.20μm，然后将浆料转移至离心型喷雾造粒塔中喷雾造粒，加筛控制颗粒粒径在80～120目，所得颗粒即为5G滤波器用介质粉体。
5.根据权利要求4所述的一种5G滤波器用介质粉体的制备方法，其特征在于：所述步骤S1中含有A元素的原料为氢氧化镁、氢氧化锌、氧化镁、氧化锌、碳酸镁、碱式碳酸镁、碳酸锌、碳酸钴中的至少一种；含有M元素的原料为五氧化二铌、二氧化铌、三氧化二钒、五氧化二钒、五氧化二锑、三氧化二锑、五氧化二钽中的至少一种；含有A元素的原料与含有M元素的原料的加入量遵守加入A、M两种元素的摩尔比为2:1；所述的含有A元素的原料与含有M元素的原料为分析纯级，其粒径为0.5～1.2μm。
6.根据权利要求4所述的一种5G滤波器用介质粉体的制备方法，其特征在于：所述步骤S2中含有B元素的原料为碳酸锶、碳酸钡、碳酸钙、氢氧化钙、氢氧化钡、硫酸钡中的至少一种；含有D元素的原料为氧化钐、氧化镧、氧化钕、氧化锡、氧化铈、碳酸锶、氧化亚钴、四氧化三钴、三氧化二钴、中的至少一种；含有B元素的原料、含有D元素的原料、二氧化钛的加入量遵守B、D、Ti元素摩尔比为x：y:1的要求；其中0.5<x<1、y<1，x、y与B、D元素的化合价组合使BxDyTiO3总化合价代数和为零，所述的含有B元素的原料与含有D元素的原料为分析纯级，其粒径为0.5～1.2μm；所述的二氧化钛为分析纯二氧化钛，其粒径为0.5～1.2μm。
7.根据权利要求4所述的一种5G滤波器用介质粉体的制备方法，其特征在于：所述有机助磨剂为聚丙烯酸铵、柠檬酸三铵、司马化工CE-64、司马化工PC-67、日油型号AKM-0531中的至少一种；所述浆料Ⅰ、浆料Ⅱ、浆料Ⅲ的固相物质重量百分数均为15～20％，其中有机助磨剂的添加量为去离子水重量的0.2-0.5％；所述浆料Ⅲ中粘结剂优选为司马化工PAF635，浆料Ⅲ中粘结剂的添加量为去离子水重量的1-5％。
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