CN113321496A - 复合微波介质陶瓷材料及其制备方法 - Google Patents
复合微波介质陶瓷材料及其制备方法 Download PDFInfo
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- CN113321496A CN113321496A CN202110742895.6A CN202110742895A CN113321496A CN 113321496 A CN113321496 A CN 113321496A CN 202110742895 A CN202110742895 A CN 202110742895A CN 113321496 A CN113321496 A CN 113321496A
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- dielectric ceramic
- ceramic material
- microwave dielectric
- composite
- titanate
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- 239000002131 composite material Substances 0.000 title claims abstract description 76
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000000498 ball milling Methods 0.000 claims abstract description 37
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000654 additive Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 230000000996 additive effect Effects 0.000 claims abstract description 20
- 239000002270 dispersing agent Substances 0.000 claims abstract description 16
- 238000000227 grinding Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000010304 firing Methods 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 61
- 239000000919 ceramic Substances 0.000 claims description 35
- 238000001354 calcination Methods 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 17
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 14
- 229910052726 zirconium Inorganic materials 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 12
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 11
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 10
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 9
- 238000007873 sieving Methods 0.000 claims description 9
- 229910002113 barium titanate Inorganic materials 0.000 claims description 7
- 239000011777 magnesium Substances 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 229920002125 Sokalan® Polymers 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical group [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 6
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 6
- 239000000391 magnesium silicate Substances 0.000 claims description 6
- 229910052919 magnesium silicate Inorganic materials 0.000 claims description 6
- 235000019792 magnesium silicate Nutrition 0.000 claims description 6
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000004584 polyacrylic acid Substances 0.000 claims description 5
- VAWSWDPVUFTPQO-UHFFFAOYSA-N calcium strontium Chemical compound [Ca].[Sr] VAWSWDPVUFTPQO-UHFFFAOYSA-N 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 239000004110 Zinc silicate Substances 0.000 claims description 3
- 229910052878 cordierite Inorganic materials 0.000 claims description 3
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052634 enstatite Inorganic materials 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- BBCCCLINBSELLX-UHFFFAOYSA-N magnesium;dihydroxy(oxo)silane Chemical compound [Mg+2].O[Si](O)=O BBCCCLINBSELLX-UHFFFAOYSA-N 0.000 claims description 3
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 3
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 229910052882 wollastonite Inorganic materials 0.000 claims description 3
- 239000010456 wollastonite Substances 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- XSMMCTCMFDWXIX-UHFFFAOYSA-N zinc silicate Chemical compound [Zn+2].[O-][Si]([O-])=O XSMMCTCMFDWXIX-UHFFFAOYSA-N 0.000 claims description 3
- 235000019352 zinc silicate Nutrition 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims 2
- 229910052454 barium strontium titanate Inorganic materials 0.000 claims 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims 1
- 239000013078 crystal Substances 0.000 description 9
- 239000002002 slurry Substances 0.000 description 9
- 238000003825 pressing Methods 0.000 description 7
- 239000004677 Nylon Substances 0.000 description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 6
- 229920001778 nylon Polymers 0.000 description 6
- ZADYMNAVLSWLEQ-UHFFFAOYSA-N magnesium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[Mg+2].[Si+4] ZADYMNAVLSWLEQ-UHFFFAOYSA-N 0.000 description 5
- 229910003080 TiO4 Inorganic materials 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910000484 niobium oxide Inorganic materials 0.000 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 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 3
- 229910001948 sodium oxide Inorganic materials 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- WOIHABYNKOEWFG-UHFFFAOYSA-N [Sr].[Ba] Chemical compound [Sr].[Ba] WOIHABYNKOEWFG-UHFFFAOYSA-N 0.000 description 2
- WEUCVIBPSSMHJG-UHFFFAOYSA-N calcium titanate Chemical compound [O-2].[O-2].[O-2].[Ca+2].[Ti+4] WEUCVIBPSSMHJG-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910017676 MgTiO3 Inorganic materials 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
Abstract
本发明属于微波介质陶瓷材料领域，尤其是一种复合微波介质陶瓷材料及其制备方法。本发明为解决目前微波介质陶瓷材料品质因数较差，稳定性不高，烧结温度高的问题，提供了一种复合微波介质陶瓷材料及其制备方法。所述复合微波介质陶瓷材料的主要成分包含摩尔比为0.01～0.4:1的钛酸盐和硅酸盐，以及占总质量3～12％的添加剂。制备方法主要是将分散剂与钛酸盐和硅酸盐分别混合后，采用球磨工艺后研磨，再加入和添加剂，烧制成复合微波介质陶瓷材料。本方法通过调整复合介电陶瓷材料中钛酸盐的占比，实现了介电性能灵活可调的目的。所得微波介质陶瓷材料，微波介电损耗较低，在10GHz频率下，Q×F值可稳定达到60000以上。
Description
技术领域
本发明属于微波介质陶瓷材料领域，尤其是一种复合微波介质陶瓷材料及其制备方法。
背景技术
微波介质陶瓷材料可用来制作介质基板、介质天线、介质谐振器、等微波器件，具有损耗小、稳定性高、体积小等特点，这些特点满足了通信微波电路对元器件的性能要求。
其中，钛酸盐体系微波介质陶瓷材料，具有优异的介电性能，且原料丰富、价格低廉。目前市面上存在很多该体系的粉体，各有异同，普遍存在的介电性能(尤其是品质因数)差、烧结温度高、稳定性和一致性差等缺点。例如纯Mg2TiO4的微波介电陶瓷粉体，存在有两个缺点制约其广泛应用。第一个是其烧成温度过高，达到1450℃～1470℃，且焙烧温度较窄(5～10℃)，因此烧成温度较难控制，只要稍微烧过几度，就会使Mg2TiO4晶粒长大，气孔增大，从而降低材料第二个是Mg2TiO4的谐振频率温度系数为-50ppm/℃，制约了其直接应用；纯MgTiO3陶瓷的烧结致密化温度有所降低，在1450℃左右，τf值比Mg2TiO4容易调节，并且原料来源丰富，成本较低廉。但是，相对来说MgTiO3陶瓷的烧结致密化温度依然很高，εr值偏低，τf的绝对值偏大。
因此，需要开发一种介电性能好，稳定性高，烧结温度低的微波介质陶瓷材料。
发明内容
本发明要解决的技术问题是：目前微波介质陶瓷材料品质因数较差，稳定性不高，烧结温度高的问题。
本发明针对上述技术问题采用的技术方案是：提供一种复合微波介质陶瓷材料及其制备方法。
本发明首先提供了一种复合微波介质陶瓷材料，所述材料的原料包含钛酸盐和硅酸盐；其中，钛酸盐和硅酸盐摩尔比为0.01～0.4:1。
进一步地，所述钛酸盐为钛酸镁、钛酸钙、钛酸锶钙、钛酸钡或钛酸锶钡中的至少一种；所述的硅酸盐为硅酸锌、硅酸镁、堇青石、硅灰石或顽辉石中的至少一种。
进一步地，所述复合微波介质陶瓷材料的原料还包含添加剂。
进一步地，所述添加剂为低熔点氧化物和/或碳酸盐；优选地，所述低熔点氧化物为锂、钠、锌或硅的氧化物中的至少一种；所述碳酸盐为碳酸锂和/或碳酸钠。
进一步地，所述添加剂占所述复合微波介质陶瓷材料总质量的3～12％。
本发明还提供了一种复合微波介质陶瓷材料的制备方法，包括如下步骤：
a.制备钛酸盐粉体：将钛酸盐与水形成的混合物，磨合后干燥、过筛，将所得筛下物煅烧后冷却至室温，得钛酸盐粉体；
b.制备硅酸盐粉体：将硅酸盐与水形成的混合物，磨合后干燥、过筛，将所得筛下物煅烧后冷却至室温，得硅酸盐粉体；
c.制备复合陶瓷粉体：将钛酸盐粉体和硅酸盐粉体按摩尔比例为0.01～0.4:1混合，得到复合陶瓷粉体；
d.烧制复合微波介质陶瓷：将复合陶瓷粉体与水形成的混合物，磨合后干燥、过筛；将所得筛下物煅烧，即得复合微波介质陶瓷材料。
进一步地，所述磨合采用球磨工艺。
进一步地，所述球磨工艺使用的是Φ3锆球。
进一步地，所述球磨工艺中球磨的转速为280～420r/min。
进一步地，所述球磨工艺中球磨时间为16～30h。
进一步地，钛酸盐/硅酸盐/复合陶瓷粉体、锆球、水的质量比为1:2～4:1.5～3.5。
进一步地，磨合前向混合物中加入分散剂。
进一步地，分散剂为分子量7万～400万的聚丙烯酸、氨基磺酸或马来酸酐中的任一种；分散剂制成质量分数为3％～10％的水溶液。
进一步地，分散剂添加量为每300g混合物加入1～5mL分散剂水溶液。
进一步地，所述筛的目数是200～300目。
进一步地，步骤a中煅烧温度为1050～1350℃。
进一步地，步骤b中煅烧温度为1050～1400℃。
进一步地，步骤d中煅烧温度为1300～1380℃。
进一步地，步骤a、b、d所述的锻造过程按照2～4℃/min升温。
进一步地，步骤a、b、d所述的煅烧结束后保温3～5h，随炉降温至室温。
进一步地，步骤d中，在磨合之前还要加入添加剂。
进一步地，所述添加剂是低熔点氧化物和/或碳酸盐。
进一步地，所述添加剂占复合陶瓷粉体总质量的3～12％。
进一步地，所述复合微波介质陶瓷材料在煅烧前压制成型，压制成型前加入聚乙烯醇；所述聚乙烯醇的添加量为混合物总质量的5～6％。
本发明的有益效果为：本发明以钛酸盐为基础，引入硅酸盐材料，配以添加剂降低烧结温度，降低损耗以及调整温度频率系数，完成钛酸盐材料体系的复合掺杂改性，改善了整体烧结特性，通过调整复合介电陶瓷材料中钛酸盐的占比，实现了介电性能灵活可调的目的。本发明所涉及的粉体微波介电损耗较低，10GHz频率下测试，Q×F值可稳定达到60000以上。本发明微波介电性能灵活可调，工艺简便且重复性好，利于大规模批产。
具体实施方式
本发明提供了一种复合微波介质陶瓷材料及其制备方法。
具体地，本发明首先提供了一种复合微波介质陶瓷材料，所述材料的原料包含钛酸盐和硅酸盐；其中，钛酸盐和硅酸盐摩尔比为0.01～0.4:1。
其中，所述钛酸盐为钛酸镁、钛酸钙、钛酸锶钙、钛酸钡、钛酸锶钡中的至少一种；所述的硅酸盐为硅酸锌、硅酸镁，堇青石、硅灰石、顽辉石中的至少一种。
所述复合微波介质陶瓷材料中还含有添加剂；所述添加剂为低熔点氧化物和碳酸盐中的至少一种；所述低熔点氧化物为锂、钠、锌、硅的氧化物中的至少一种；所述碳酸盐为碳酸锂和/或碳酸钠；两种添加剂的总含量占总质量的3～12％。低熔点氧化物的含量过低或者未添加低熔点氧化物，不仅会导致陶瓷材料烧结温度高，还不利于相关相的形成和材料制作过程中的控制。碳酸盐的存在能保证复合介质陶瓷材料的致密度。
然后，本发明还提供了一种复合微波介质陶瓷材料的制备方法，步骤如下：
a.制备钛酸盐粉体：将钛酸盐与水形成的混合物，磨合后干燥、过筛，将所得筛下物煅烧后冷却至室温，得钛酸盐粉体；
b.制备硅酸盐粉体：将硅酸盐与水形成的混合物，磨合后干燥、过筛，将所得筛下物煅烧后冷却至室温，得硅酸盐粉体；
c.制备复合陶瓷粉体：将钛酸盐粉体和硅酸盐粉体按摩尔比例为0.01～0.4:1混合，得到复合陶瓷粉体；
d.烧制复合微波介质陶瓷：将复合陶瓷粉体与水形成的混合物，磨合后干燥、过筛；将所得筛下物煅烧，即得复合微波介质陶瓷材料。
进一步地，若磨合前的混合物混合不均匀，则向混合物中加入分散剂；所述分散剂是指包括聚丙烯酸类(分子量7万-400万)、氨基磺酸、马来酸酐中的任一种，配成质量分数为3％～10％的水溶液；分散剂添加量为每300g混合物加入1～5mL分散剂水溶液。
进一步地，所述磨合采用的是球磨工艺；使用的是Φ3锆球；所述球磨工艺中，球磨的转速为280～420r/min，球磨时间为16～30h；以此保证球磨前的混合物能彻底混合均匀，有利于提高复合介质陶瓷材料的致密度。
进一步地，所述干燥条件是80～120℃，干燥8～24h。
进一步地，步骤a中煅烧温度为1050～1350℃；步骤b中煅烧温度为1050～1400℃；步骤d所述煅烧温度为1300～1380℃；步骤a、b、d的煅烧都按2～4℃/分钟升温至指定范围，然后保温3～5小时，随炉降温至室温。a、b步骤中的温度均为各自盐类粉体的预烧温度，目的是通过预烧，得到陶瓷晶相，利于陶瓷的合成。因为所需复合陶瓷粉体的主晶相由a、b步骤中的得到的两晶相组成，若不经预烧，混合后直接煅烧，则或造成晶相掺杂(如过程中形成其他晶相、所需晶相不足等)，从而大幅度影响最终复合陶瓷材料的性能。d步骤中，煅烧工艺参数会直接影响材料烧结过程中的晶相的形成，晶相的变化。若温度过高过低均会影响成品粉体的性能，从而得不到复合陶瓷材料。
进一步地，本方法所述筛的目数是200～300目，用于保证混合物的均匀性，有利于提高最终所得复合陶瓷材料的烧结致密度。
进一步地，步骤d中，在磨合之前还要加入添加剂；所述添加剂是低熔点氧化物和碳酸盐中的至少一种；添加剂的添加量是复合陶瓷粉体总质量3～12％。添加剂的加入不仅进一步促进球磨前的混合物混合均匀，而且其中的碳酸盐还能保证复合陶瓷材料的烧结致密度。
进一步地，步骤d中，所述复合微波介质陶瓷材料在煅烧前压制成型，压制成型前加入聚乙烯醇；所述聚乙烯醇的添加量为混合物总质量的5～6％。聚乙烯醇的作用是为了利于造粒和压制，有利于复合陶瓷材料的烧结致密度。
进一步地，所述压制过程，压力范围是8～10MPa，压制所得复合介质陶瓷材料是直径为Φ12，高度4.5mm的圆柱形坯体。
进一步地，所得复合微波陶瓷材料，微波介电常数为：17～21，Q×F值：>60000@10GH，频率温漂系数(25℃∽85℃)：±10ppm/℃。
以下通过实施例对本发明作进一步的解释和说明。
实施例1
称取钛酸锶钙200g，Φ3锆球800g，去离子水600g，用2升行星尼龙罐球磨。球磨转速360r/min，球磨时间24h。磨合完成后用200目网纱过滤料浆，在110℃下干燥；将过筛的钛酸盐混合物在1350℃下煅烧后冷却至室温，得钛酸盐粉体；
称取硅酸镁100g，Φ3锆球400g，去离子水300g，用500ml行星尼龙罐球磨。球磨转速320r/min，球磨时间18h。磨合完成后用200目网纱过滤料浆，在110℃下干燥；将过筛的钛酸盐混合物煅烧后冷却至室温，得硅酸盐粉体；
将钛酸盐粉体175g和硅酸盐粉体25g混合，得到复合陶瓷粉体；
取复合陶瓷粉体200g与锆球800g和水600g混合，加入氧化纳2g、氧化铌2g、氧化锰2g、氧化锌2g，碳酸锂4g，聚丙烯酸类1.5ml采用球磨工艺磨合材料；球磨完成，用200目网纱过滤料浆，在110℃下干燥。
向干燥的复合陶瓷粉体中加入10g聚乙烯醇，在8～10MPa下压制成直径Φ12，高度约4.5mm的圆柱坯体。将圆柱坯体置入冶炼炉中，按2℃/分钟升温至1350℃，保温3小时，随炉降温至室温，烧结致密的圆柱瓷体，即复合介质陶瓷材料。用矢量网络分析仪与封闭金属腔测试，测试结果为Q×F值@10GHz 65828.3，介电常数18.56，瓷体密度3.70.g/cm3。
实施例2
称取钛酸钡200g，Φ3锆球800g，去离子水600g，用2升行星尼龙罐球磨。球磨转速360r/min，球磨时间24h。磨合完成后用200目网纱过滤料浆，在110℃下干燥；将过筛的钛酸盐混合物在1350℃下煅烧后冷却至室温，得钛酸盐粉体；
称取硅酸镁100g，Φ3锆球400g，去离子水300g，用500ml行星尼龙罐球磨。球磨转速320r/min，球磨时间18h。磨合完成后用200目网纱过滤料浆，在110℃下干燥；将过筛的钛酸盐混合物煅烧后冷却至室温，得硅酸盐粉体；
将钛酸盐粉体150g和硅酸盐粉体50g混合，得到复合陶瓷粉体；
取复合陶瓷粉体200g与锆球800g和水600g混合，加入氧化纳4g、氧化铌0.5g、氧化锰1g、氧化锌0.5g、碳酸锂4g，聚丙烯酸类2.5ml采用球磨工艺磨合材料；球磨完成，用200目网纱过滤料浆，在110℃下干燥。
向干燥的复合陶瓷粉体中加入10g聚乙烯醇，混匀，在8～10MPa下压制成直径Φ12，高度约4.5mm的圆柱坯体。将圆柱坯体置入冶炼炉中，按2℃/分钟升温至1350℃，保温3小时，随炉降温至室温，烧结致密的圆柱瓷体，即复合介质陶瓷材料。用矢量网络分析仪与封闭金属腔测试，测试结果为Q×F值@10GHz 68451.2，介电常数19.78，瓷体密度3.69.g/cm3。
对比例1不采用本发明所述工艺参数
称取钛酸钡200g，Φ3锆球800g，去离子水600g，用2升行星尼龙罐球磨。球磨转速360r/min，球磨时间24h。磨合完成后用200目网纱过滤料浆，在110℃下干燥；将过筛的钛酸盐混合物在1350℃下煅烧后冷却至室温，得钛酸盐粉体；
称取硅酸镁200g，Φ3锆球800g，去离子水600g，用2升行星尼龙罐球磨。球磨转速320r/min，球磨时间18h。磨合完成后用200目网纱过滤料浆，在110℃下干燥；将过筛的钛酸盐混合物煅烧后冷却至室温，得硅酸盐粉体；
将钛酸盐粉体100g和硅酸盐粉体100g混合，得到复合陶瓷粉体；
取复合陶瓷粉体200g与锆球800g和水600g混合，加入氧化纳8g、氧化铌4g、氧化锰4g、氧化锌1g、碳酸锂1g，聚丙烯酸类2.5ml采用球磨工艺磨合材料；球磨完成，用200目网纱过滤料浆，在110℃下干燥。
向干燥的复合陶瓷粉体中加入10g聚乙烯醇溶液，混匀，在8～10MPa下压制成直径Φ12，高度约4.5mm的圆柱坯体。将圆柱坯体置入冶炼炉中，按2℃/分钟升温至1350℃，保温3小时，随炉降温至室温，烧结致密的圆柱瓷体，即复合介质陶瓷材料。用矢量网络分析仪与封闭金属腔测试，测试结果为Q×F值@10GHz 32463.8，介电常数15.77，瓷体密度3.43.g/cm3。
Claims (10)
1.复合微波介质陶瓷材料，其特征在于，所述材料的原料包含钛酸盐和硅酸盐；其中，钛酸盐和硅酸盐摩尔比为0.01～0.4:1。
2.根据权利要求1所述的复合微波介质陶瓷材料，其特征在于，所述钛酸盐为钛酸镁、钛酸钙、钛酸锶钙、钛酸钡或钛酸锶钡中的至少一种；所述硅酸盐为硅酸锌、硅酸镁、堇青石、硅灰石或顽辉石中的至少一种。
3.根据权利要求1或2所述的复合微波介质陶瓷材料，其特征在于，所述复合微波介质陶瓷材料的原料还包含添加剂；
进一步地，所述添加剂为低熔点氧化物和/或碳酸盐；优选地，所述低熔点氧化物为锂、钠、锌或硅的氧化物中的至少一种；所述碳酸盐为碳酸锂和/或碳酸钠；
进一步地，所述添加剂占所述复合微波介质陶瓷材料总质量的3～12％。
4.复合微波介质陶瓷材料的制备方法，其特征在于，包括如下步骤：
a.制备钛酸盐粉体：将钛酸盐与水形成的混合物磨合后干燥、过筛，将所得筛下物煅烧后冷却至室温，得钛酸盐粉体；
b.制备硅酸盐粉体：将硅酸盐与水形成的混合物磨合后干燥、过筛，将所得筛下物煅烧后冷却至室温，得硅酸盐粉体；
c.制备复合陶瓷粉体：将钛酸盐粉体和硅酸盐粉体按摩尔比0.01～0.4:1混合，得复合陶瓷粉体；
d.烧制复合微波介质陶瓷：将复合陶瓷粉体与水形成的混合物，磨合后干燥、过筛；将所得筛下物煅烧，即得复合微波介质陶瓷材料。
5.根据权利要求4所述的复合微波介质陶瓷材料的制备方法，其特征在于，所述磨合采用球磨工艺；所述球磨工艺至少满足下列条件中的至少一项：
使用Φ3锆球；
球磨的转速为280～420r/min；
球磨时间为16～30h；
钛酸盐/硅酸盐/复合陶瓷粉体、锆球、水的质量比为1:2～4:1.5～3.5。
6.根据权利要求4或5所述的复合微波介质陶瓷材料的制备方法，其特征在于，磨合前向混合物中加入分散剂；所述分散剂满足下列条件中的至少一项：
分散剂为分子量7万～400万的聚丙烯酸、氨基磺酸或马来酸酐中的任一种；分散剂制成质量分数为3％～10％的水溶液；
分散剂添加量为每300g混合物加入1～5mL分散剂水溶液。
7.根据权利要求4～6任一项所述的复合微波介质陶瓷材料的制备方法，其特征在于，所述筛的目数是200～300目。
8.根据权利要求4～7任一项所述的复合微波介质陶瓷材料的制备方法，其特征在于，所述煅烧满足下列条件中的至少一项：
步骤a中煅烧温度为1050～1350℃；
步骤b中煅烧温度为1050～1400℃；
步骤d中煅烧温度为1300～1380℃；
按照2～4℃/min升温；
煅烧结束后保温3～5h，随炉降温至室温。
9.根据权利要求4～8任一项所述的复合微波介质陶瓷材料的制备方法，其特征在于，步骤d中，在磨合之前还要加入添加剂；所述添加剂满足下列条件中的至少一项：
添加剂是低熔点氧化物和/或碳酸盐；
添加剂的添加量是复合陶瓷粉体总质量的3～12％。
10.根据权利要求4～9任一项所述的复合微波介质陶瓷材料的制备方法，其特征在于，所述复合微波介质陶瓷材料在煅烧前压制成型，压制成型前加入聚乙烯醇；进一步地，所述聚乙烯醇的添加量为混合物总质量的5～6％。
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