CN112811897A - 一种压力传感器陶瓷材料及制备方法 - Google Patents
一种压力传感器陶瓷材料及制备方法 Download PDFInfo
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- CN112811897A CN112811897A CN202110028583.9A CN202110028583A CN112811897A CN 112811897 A CN112811897 A CN 112811897A CN 202110028583 A CN202110028583 A CN 202110028583A CN 112811897 A CN112811897 A CN 112811897A
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002105 nanoparticle Substances 0.000 claims abstract description 56
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 51
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 50
- 239000010432 diamond Substances 0.000 claims abstract description 50
- 239000000843 powder Substances 0.000 claims abstract description 41
- 239000002245 particle Substances 0.000 claims abstract description 19
- 239000011521 glass Substances 0.000 claims abstract description 15
- 239000013078 crystal Substances 0.000 claims abstract description 9
- 229920000642 polymer Polymers 0.000 claims abstract description 5
- 239000002243 precursor Substances 0.000 claims description 41
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- 238000002156 mixing Methods 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 33
- 238000010438 heat treatment Methods 0.000 claims description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 21
- 229910004247 CaCu Inorganic materials 0.000 claims description 19
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 18
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 17
- 239000012153 distilled water Substances 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 13
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 239000010949 copper Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 239000012298 atmosphere Substances 0.000 claims description 10
- 239000011575 calcium Substances 0.000 claims description 10
- 239000012300 argon atmosphere Substances 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 7
- 239000002033 PVDF binder Substances 0.000 claims description 6
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 6
- 150000003457 sulfones Chemical class 0.000 claims description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 5
- 229920001955 polyphenylene ether Polymers 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 4
- 239000012982 microporous membrane Substances 0.000 claims description 4
- 229910052706 scandium Inorganic materials 0.000 claims description 4
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 3
- 229910021592 Copper(II) chloride Inorganic materials 0.000 claims description 3
- 229910018057 ScCl3 Inorganic materials 0.000 claims description 3
- 229910008159 Zr(SO4)2 Inorganic materials 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- 229910052927 chalcanthite Inorganic materials 0.000 claims description 3
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 3
- 229910052602 gypsum Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 229910000346 scandium sulfate Inorganic materials 0.000 claims description 3
- 229910001631 strontium chloride Inorganic materials 0.000 claims description 3
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 claims description 3
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 2
- ZFFMLCVRJBZUDZ-UHFFFAOYSA-N 2,3-dimethylbutane Chemical group CC(C)C(C)C ZFFMLCVRJBZUDZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 2
- 229910003130 ZrOCl2·8H2O Inorganic materials 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000007822 coupling agent Substances 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- DFCYEXJMCFQPPA-UHFFFAOYSA-N scandium(III) nitrate Inorganic materials [Sc+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O DFCYEXJMCFQPPA-UHFFFAOYSA-N 0.000 claims description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 2
- 230000007547 defect Effects 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 4
- 239000012528 membrane Substances 0.000 abstract 1
- 238000001471 micro-filtration Methods 0.000 abstract 1
- 229910003211 Ni0.6Co0.4 Inorganic materials 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 6
- 229910002966 CaCu3Ti4O12 Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 125000004423 acyloxy group Chemical group 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N chromium(III) oxide Inorganic materials O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 2
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical group [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Polymers C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
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- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
- G01L9/12—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in capacitance, i.e. electric circuits therefor
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Abstract
本发明提供一种压力传感器陶瓷材料及其制备方法，包括以下成分：分子式为CaCu3‑ xMxTi4‑yScyO12的纳米陶瓷颗粒，其中0＜x≤1，0.2≤y≤0.8；分子式为B2O3的玻璃相纳米氧化物颗粒；AlN；BeO；聚甲基甲酰胺；多晶金刚石微粉；微滤膜聚合物；二甲基甲酰胺。本发明通过制备得到镀覆有10μm～20μm的AlN和BeO亚微米层的金刚石微粉，降低由于B2O3玻璃相纳米颗粒对CaCu3‑xMxTi4‑yScyO12进行梯度改性所带来的晶体结构均匀、各向同性的缺陷，进而有效降低了最终制备得到的所述陶瓷材料对抗冲击的应力集中，避免了晶界移动所带来的截面结合程度降低的缺陷。
Description
技术领域
本发明属于传感器陶瓷技术领域，具体涉及一种压力传感器陶瓷材料及制备方法。
背景技术
材料是人类生产和生活的物质基础，是人类进步与人类文明的标志。随着空间技术、光电技术、红外技术、传感技术、能源技术等新技术的出现、发展，要求材料必须有耐高温、抗腐蚀、耐磨等优越的性能，才能在比较苛刻的环境中使用。传统材料难以满足要求，开发和有效利用高性能材料已经成为材料科学发展的必然趋势。然而，现有技术中的陶瓷材料具有热膨胀系数低，导致散热能力较低，易引起消防安全隐含，且不满足现有市场上的片式化、小型化的传感器电子传感器陶瓷材料的要求。
发明内容
本发明针对上述缺陷，提供一种压力传感器陶瓷材料及制备方法。
本发明提供如下技术方案：一种压力传感器陶瓷材料，按重量组分计，包括以下成分
分子式为CaCu3-xMxTi4-yScyO12的纳米陶瓷颗粒45份～50份，其中0＜x≤1，0.2≤y≤0.8，所述M为Ni、Zr、Co、Sr；
分子式为B2O3的玻璃相纳米氧化物颗粒20份～25份，所述元素A为Er、Fe、Cr或Bi；
进一步地，所述CaCu3-xMxTi4-yScyO12纳米颗粒材料的制备方法包括以下步骤：
S1：将钙无机盐水合物、铜无机盐水合物和M元素无机盐水合物按照摩尔比为1:3-x:x溶于乙醇中，形成第一混合前驱体溶液；
S2：将硅烷偶联剂、钪无机盐水合物按照摩尔比为4-y:y溶于乙酰丙酮中，形成第二混合前驱体溶液；
S3：将所述S1步骤得到的第一混合前驱体溶液和所述S2步骤得到的第二混合前驱体溶液于95℃～105℃、200rpm～300rpm转速下搅拌15min，搅拌过程中滴加乙醇溶液，形成CaCu3-xMxTi4-yScyO12纳米前驱体凝胶；
S4：将所述步骤S3得到的CaCu3-xMxTi4-yScyO12纳米前驱体凝胶于氮气气体气氛中、150℃～160℃下干燥2h～2.5h后，采用行星球磨机研磨，得到CaCu3-xMxTi4-yScyO12纳米前驱体粉末；
S5：将所述CaCu3-xMxTi4-yScyO12纳米前驱体粉末于950℃～1150℃下煅烧1h～1.5h后，避免CaCu3-xMxTi4-yScyO12晶体生长，得到CaCu3-xMxTi4-yScyO12纳米颗粒。
进一步地，所述钛酸酯偶联剂为四异丙基二(二辛基亚磷酸酰氧基)钛酸酯、钛酸异丙酯、二(乙酰丙酮基)钛酸二异丙酯或正钛酸四丁酯中的一种或几种。
进一步地，所述铜无机盐水合物为Cu(NO3)2·3H2O、Cu(CH3COO)2·H2O、CuCl2·2H2O或CuSO4·5H2O；所述钙无机盐水合物为Ca(NO3)2·4H2O、Ca(CH3COO)2·H2O、CaSO4·2H2O或CaCl2·6H2O；
进一步地，所述M元素的水合物为Ni(NO3)2·6H2O、Ni(CH3COO)2·4H2O、NiSO4·6H2O、NiCl2·6H2O、Zr(NO3)3·5H2O、Zr(SO4)2·4H2O、ZrOCl2·8H2O、Co(NO3)2·6H2O、Co(CH3COO)2·4H2O、Co(SO4)2·7H2O、CoCl2·6H2O、Sr(CH3COO)2·2H2O或SrCl2·6H2O；所述钪无机盐水合物为ScCl3·6H2O、Sc2(SO4)3·8H2O、Sc(CH3COO)3·5H2O、Sc(NO3)3·H2O。
进一步地，所述S3步骤中滴加的乙醇溶液为含有乙醇的体积分数为20％～40％。
进一步地，所述多相金刚石微粉的粒径为15μm～25μm。
进一步地，所述微孔膜聚合物为聚苯醚砜、聚偏氟乙烯、聚磺化苯醚砜、聚四氟乙烯中的一种。
本发明还提供上述压力传感器陶瓷材料的制备方法，包括以下步骤：
M1：将所述重量组分的多晶金刚石微粉溶于浓度为10M～12M的浓NaOH溶液中，于100℃～110℃下煮沸后，采用蒸馏水清洗3次，然后浸没于浓度为2M～5M浓度的HCl，于超声波下振荡20min～30min后，得到预处理后的多晶金刚石微粉；
M2：将所述重量组分的AlN、所述重量组分的BeO与所述重量组分的聚甲基甲酰胺混合，于60℃～70℃下以180rpm～230rpm转速搅拌10min～15min；
M3：将所述M2步骤得到的混合物与所述M1步骤得到的预处理后的多晶金刚石微粉置于真空中，于10MPa～15MPa下于惰性气氛下抽真空，以20℃/min升温速率升温至350℃～400℃保温1.5h后，继续以20℃/min升温速率升温至950℃～1000℃保温2h～2.5h，得到镀覆有AlN和BeO掺杂的亚微米层的金刚石微粉，所述亚微米层为10μm～20μm；
M4：将所述重量组分的分子式为CaCu3-xMxTi4-yScyO12的纳米颗粒、所述重量组分的B2O3的玻璃相纳米氧化物颗粒与三分之一所述重量组分的二甲基甲酰胺混合，于50℃～70℃下、150rpm～200rpm转速下搅拌30min～45min，将得到的混合物于室温下静置10min后于3000rpm～4000rpm转速下离心5min～10min，将得到的沉淀于乙醇下清洗3次后，再于蒸馏水中清洗3次，得到B2O3纳米颗粒改性CaCu3-xMxTi4-yScyO12梯度纳米颗粒；
M5：将所述步骤M4得到的所述B2O3纳米颗粒改性CaCu3-xMxTi4-yScyO12梯度纳米颗粒与剩余三分之二所述重量组分的二甲基甲酰胺混合均匀后，与所述重量组分的微孔膜聚合物和所述步骤M3得到的镀覆有AlN和BeO掺杂的亚微米层的金刚石微粉混合，于55℃～75℃下、250rpm～300rpm转速下搅拌30min～45min，然后于氮气气流下、70℃～80℃下烘干，得到所述压力传感器陶瓷材料。
进一步地，所述M3步骤的中抽真空所使用的惰性气氛为氩气气氛，流量为160ml/min～200ml/min。
本发明的有益效果为：
1、通过利用多晶金刚石微粉和AlN、BeO经过聚甲基甲酰胺处理后，于真空惰性气氛高温下，制备得到镀覆有10μm～20μm的AlN和BeO亚微米层的金刚石微粉，多晶金刚石具有良好的机械强度，通过添加AlN和BeO能够增强最终的陶瓷复合材料的粘结强度，BeO在镀覆过程中能够将Be2+离子作为受主扩散至多晶金刚石微粉的境界，进而形成晶界势垒进而提高晶界势垒的高度，从而影响电性属性，降低由于B2O3玻璃相纳米颗粒对CaCu3-xMxTi4- yScyO12进行梯度改性所带来的晶体结构均匀、各向同性的缺陷，进而有效降低了最终制备得到的所述陶瓷材料对抗冲击的应力集中，能够进一步增强其机械性能，避免了晶界移动所带来的截面结合程度降低的缺陷。同时AlN最高可稳定到2200℃。室温强度高，且强度随温度的升高下降较慢。导热性好，热膨胀系数小，是良好的耐热冲击材料。抗熔融金属侵蚀的能力强，且其是良好的电绝缘体，介电性能优良，借助AlN和BeO镀覆多晶金刚石进一步增强了传感器陶瓷材料的绝缘性能并降低其热膨胀系数，使最终的陶瓷材料具有良好的绝缘性能和散热性能。
2、本发明通过自制备具有分子式为CaCu3-xMxTi4-yScyO12的纳米颗粒，利用Ni、Zr、Co、Sr对Cu进行取代掺杂通过制备过程中的钙无机盐水合物、铜无机盐水合物和M金属无机盐水合物的混合，M元素掺杂的前驱体溶液，进而抑制最终的CaCu3-xMxTi4-yScyO12的纳米颗粒的晶粒生长速度，进而可以得到致密的微观结构，降低了纳米颗粒的孔隙率，进而，能够改变CaCu3Ti4O12的空间结构，通过提高其各向异性场的方式提高了最终的CaCu3-xMxTi4- yScyO12的纳米颗粒的介电常数并降低其介电损耗；同时通过Sc元素对Ti进行掺杂取代，降低了Ti在空间内的空位，进而使制备的到的CaCu3-xMxTi4-yScyO12几何空间结构更有序，进而保证了其电位梯度，降低了其介电损耗和漏电流。
3、通过添加分子式为B2O3的玻璃相纳米颗粒，对分子式为CaCu3-xMxTi4-yScyO12的纳米颗粒进行改性包裹，进而提高CaCu3-xMxTi4-yScyO12的纳米颗粒的熔融焓，并且此种改性是具有梯度的改性，靠近内核CaCu3-xMxTi4-yScyO12的纳米颗粒的外壳B2O3玻璃相纳米颗粒的含量较低，随着远离内核CaCu3-xMxTi4-yScyO12的纳米颗粒，外壳B2O3玻璃相纳米颗粒逐渐升高，进而保证了提高其绝缘性能的同时，不会降低其介电常数，进而使最终获得的电容压敏传感器陶瓷材料具有高介电常数、低介电损耗的同时，具有高绝缘性能。
具体实施例方式
下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
本实施例提供的一种压力传感器陶瓷材料，按重量组分计，包括以下成分
其中，CaCu2(Ni0.6Co0.4)Ti3.8Sc0.2O12纳米颗粒材料的制备方法包括以下步骤：
S1：将Ca(CH3COO)2·H2O、Cu(CH3COO)2·H2O、Ni(CH3COO)2·4H2O和Co(CH3COO)2·4H2O按照摩尔比为1:2:0.6:0.4溶于乙醇中，形成第一混合前驱体溶液；
S2：将正钛酸四丁酯、Sc(CH3COO)3·5H2O按照摩尔比为3.8:0.2溶于乙酰丙酮中，形成第二混合前驱体溶液；
S3：将所述S1步骤得到的第一混合前驱体溶液和所述S2步骤得到的第二混合前驱体溶液于95℃下、200rpm转速下搅拌15min，搅拌过程中滴加体积分数为20％的乙醇溶液，形成CaCu2(Ni0.6Co0.4)Ti3.8Sc0.2O12纳米前驱体凝胶；
S4：将步骤S3得到的CaCu2(Ni0.6Co0.4)Ti3.8Sc0.2O12纳米前驱体凝胶于氮气气体气氛中、150℃下干燥2h后，采用行星球磨机研磨，得到CaCu2(Ni0.6Co0.4)Ti3.8Sc0.2O12纳米前驱体粉末；
S5：将CaCu2(Ni0.6Co0.4)Ti3.8Sc0.2O12纳米前驱体粉末于950℃下煅烧1h后，避免CaCu2(Ni0.6Co0.4)Ti3.8Sc0.2O12晶体生长，得到CaCu2(Ni0.6Co0.4)Ti3.8Sc0.2O12纳米颗粒。
本实施例还提供上述压力传感器陶瓷材料的制备方法，包括以下步骤：
M1：将10份的粒径为15μm的多晶金刚石微粉溶于浓度为10M的浓NaOH溶液中，于100℃下煮沸后，采用蒸馏水清洗3次，然后浸没于浓度为2M浓度的HCl，于超声波下振荡20min后，得到预处理后的多晶金刚石微粉；
M2：将15份的AlN、8的BeO与20份的聚甲基甲酰胺混合，于61℃下以180rpm转速搅拌10min；
M3：将M2步骤得到的混合物与M1步骤得到的预处理后的多晶金刚石微粉置于真空中，于10MPa下于流量为160ml/min的氩气气氛下抽真空，以20℃/min升温速率升温至350℃保温1.5h后，继续以20℃/min升温速率升温至950℃保温2h，得到镀覆有AlN和BeO掺杂的亚微米层的金刚石微粉，所述亚微米层为10μm；
M4：将45份的分子式为CaCu2(Ni0.6Co0.4)Ti3.8Sc0.2O12的纳米颗粒、所述重量组分的Er2O3的玻璃相纳米氧化物颗粒与6.67份的二甲基甲酰胺混合，于50℃下、150rpm转速下搅拌30min，将得到的混合物于室温下静置10min后于3000rpm转速下离心5min，将得到的沉淀于乙醇下清洗3次后，再于蒸馏水中清洗3次，得到Er2O3纳米颗粒改性CaCu2(Ni0.6Co0.4)Ti3.8Sc0.2O12梯度纳米颗粒；
M5：将步骤M4得到的所述Er2O3纳米颗粒改性CaCu2(Ni0.6Co0.4)Ti3.8Sc0.2O12梯度纳米颗粒与剩余13.33份的二甲基甲酰胺混合均匀后，与55份的聚偏氟乙烯和步骤M3得到的镀覆有AlN和BeO掺杂的亚微米层的金刚石微粉混合，于55℃下、250rpm转速下搅拌30min，然后于氮气气流下、70℃下烘干，得到压力传感器陶瓷材料。
实施例2
本实施例提供一种压力传感器陶瓷材料，按重量组分计，包括以下成分
其中，CaCu2.5Zr0.5Ti3.5Sc0.5O12纳米颗粒材料的制备方法包括以下步骤：
S1：将CaSO4·2H2O、CuSO4·5H2O、Zr(SO4)2·4H2O按照摩尔比为1:2.5:0.5溶于乙醇中，形成第一混合前驱体溶液；
S2：将四异丙基二(二辛基亚磷酸酰氧基)钛酸酯、Sc2(SO4)3·8H2O按照摩尔比为7:1溶于乙酰丙酮中，形成第二混合前驱体溶液；
S3：将S1步骤得到的第一混合前驱体溶液和S2步骤得到的第二混合前驱体溶液于105℃下、300rpm转速下搅拌15min，搅拌过程中滴加积分数为40％的乙醇溶液，形成CaCu2.5Zr0.5Ti3.5Sc0.5O12纳米前驱体凝胶；
S4：将步骤S3得到的CaCu2.5Zr0.5Ti3.5Sc0.5O12纳米前驱体凝胶于氮气气体气氛中、160℃下干燥2.5h后，采用行星球磨机研磨，得到CaCu2.5Zr0.5Ti3.5Sc0.5O12纳米前驱体粉末；
S5：将步骤S4得到的CaCu2.5Zr0.5Ti3.5Sc0.5O12纳米前驱体粉末于1150℃下煅烧1.5h后，避免CaCu2.5Zr0.5Ti3.5Sc0.5O12晶体生长，得到CaCu2.5Zr0.5Ti3.5Sc0.5O12纳米颗粒。
本实施例还提供上述压力传感器陶瓷材料的制备方法，包括以下步骤：
M1：将15份的粒径为20μm的多晶金刚石微粉溶于浓度为12M的浓NaOH溶液中，于110℃下煮沸后，采用蒸馏水清洗3次，然后浸没于浓度为5M浓度的HCl，于超声波下振荡30min后，得到预处理后的多晶金刚石微粉；
M2：将20份的AlN、12份的BeO与30份的聚甲基甲酰胺混合，于70℃下以230rpm转速搅拌15min；
M3：将M2步骤得到的混合物与M1步骤得到的预处理后的多晶金刚石微粉置于真空中，于15MPa下于流量为180ml/min的氩气气氛下抽真空，以20℃/min升温速率升温至400℃保温1.5h后，继续以20℃/min升温速率升温至1000℃保温2.5h，得到镀覆有AlN和BeO掺杂的亚微米层的金刚石微粉，所述亚微米层为15μm；
M4：将50份的分子式为CaCu2.5Zr0.5Ti3.5Sc0.5O12的纳米颗粒、25份的Bi2O3的玻璃相纳米氧化物颗粒与11.67份的二甲基甲酰胺混合，于70℃下、200rpm转速下搅拌45min，将得到的混合物于室温下静置10min后于4000rpm转速下离心10min，将得到的沉淀于乙醇下清洗3次后，再于蒸馏水中清洗3次，得到Bi2O3纳米颗粒改性CaCu2.5Zr0.5Ti3.5Sc0.5O12梯度纳米颗粒；
M5：将步骤M4得到的所述Bi2O3纳米颗粒改性CaCu2.5Zr0.5Ti3.5Sc0.5O12梯度纳米颗粒与剩余13.33份的二甲基甲酰胺混合均匀后，与65份的聚磺化苯醚砜和所述＝＝步骤M3得到的镀覆有AlN和BeO掺杂的亚微米层的金刚石微粉混合，于75℃下、300rpm转速下搅拌45min，然后于氮气气流下、80℃下烘干，得到压力传感器陶瓷材料。
10、根据权利要求9所述的一种压力传感器陶瓷材料的制备方法，其特征在于，所述M3步骤的中抽真空所使用的惰性气氛为氩气气氛，流量为160ml/min～200ml/min。
实施例3
本实施例提供的一种压力传感器陶瓷材料，按重量组分计，包括以下成分
其中，CaCu2.9Sr0.1Ti3.2Sc0.8O12纳米颗粒材料的制备方法包括以下步骤：
S1：将CaCl2·6H2O、CuCl2·2H2O和SrCl2·6H2O按照摩尔比为1:2.9:0.1溶于乙醇中，形成第一混合前驱体溶液；
S2：将二(乙酰丙酮基)钛酸二异丙酯、ScCl3·6H2O按照摩尔比为4:1溶于乙酰丙酮中，形成第二混合前驱体溶液；
S3：将S1步骤得到的第一混合前驱体溶液和S2步骤得到的第二混合前驱体溶液于100℃下、250rpm转速下搅拌15min，搅拌过程中滴加乙醇溶液，形成CaCu2.9Sr0.1Ti3.2Sc0.8O12纳米前驱体凝胶；
S4：将步骤S3得到的CaCu2.9Sr0.1Ti3.2Sc0.8O12纳米前驱体凝胶于氮气气体气氛中、155℃下干燥2.25h后，采用行星球磨机研磨，得到CaCu2.9Sr0.1Ti3.2Sc0.8O12纳米前驱体粉末；
S5：将所述CaCu2.9Sr0.1Ti3.2Sc0.8O12纳米前驱体粉末于1000℃下煅烧1.25h后，避免CaCu2.9Sr0.1Ti3.2Sc0.8O12晶体生长，得到CaCu2.9Sr0.1Ti3.2Sc0.8O12纳米颗粒。
本实施例还提供上述压力传感器陶瓷材料的制备方法，包括以下步骤：
M1：将12.5份的粒径为25μm的多晶金刚石微粉溶于浓度为11M的浓NaOH溶液中，于105℃下煮沸后，采用蒸馏水清洗3次，然后浸没于浓度为3.5M浓度的HCl，于超声波下振荡25min后，得到预处理后的多晶金刚石微粉；
M2：将17.5份的AlN、10份的BeO与所述重量组分的聚甲基甲酰胺混合，于65℃下以205rpm转速搅拌12min；
M3：将M2步骤得到的混合物与M1步骤得到的预处理后的多晶金刚石微粉置于真空中，于12.5MPa下于流量为200ml/min的氩气气氛下抽真空，以20℃/min升温速率升温至375℃保温1.5h后，继续以20℃/min升温速率升温至980℃保温2.25h，得到镀覆有AlN和BeO掺杂的亚微米层的金刚石微粉，所述亚微米层为20μm；
M4：将所述重量组分的分子式为CaCu2.9Sr0.1Ti3.2Sc0.8O12的纳米颗粒、22.5份的Cr2O3的玻璃相纳米氧化物颗粒与7.5份的的二甲基甲酰胺混合，于65℃下、175rpm转速下搅拌38min，将得到的混合物于室温下静置10min后于3500rpm转速下离心7.5min，将得到的沉淀于乙醇下清洗3次后，再于蒸馏水中清洗3次，得到Cr2O3纳米颗粒改性CaCu2.9Sr0.1Ti3.2Sc0.8O12梯度纳米颗粒；
M5：将步骤M4得到的所述Cr2O3纳米颗粒改性CaCu2.9Sr0.1Ti3.2Sc0.8O12梯度纳米颗粒与剩余15份的二甲基甲酰胺混合均匀后，与25份的聚苯醚砜、25份的聚四氟乙烯和步骤M3得到的镀覆有AlN和BeO掺杂的亚微米层的金刚石微粉混合，于65℃下、275rpm转速下搅拌37min，然后于氮气气流下、75℃下烘干，得到压力传感器陶瓷材料。
对比例1
本对比例与实施例1的区别在于，不采用AlN和BeO这两种成分，按重量组分计，包括以下成分：
进而在最后的制作步骤中，采用如下步骤：
M1：将10份的粒径为15μm的多晶金刚石微粉溶于浓度为10M的浓NaOH溶液中，于100℃下煮沸后，采用蒸馏水清洗3次，然后浸没于浓度为2M浓度的HCl，于超声波下振荡20min后，得到预处理后的多晶金刚石微粉；
M2：将M1步骤得到的混合物与20份的聚甲基甲酰胺混合，于61℃下以180rpm转速搅拌10min；
M3：将M2步骤得到的混合物与M1步骤得到的预处理后的多晶金刚石微粉置于真空中，于10MPa下于流量为160ml/min的氩气气氛下抽真空，以20℃/min升温速率升温至350℃保温1.5h后，继续以20℃/min升温速率升温至950℃保温2h，得到镀覆有AlN和BeO掺杂的亚微米层的金刚石微粉，所述亚微米层为10μm；
M4：将45份的分子式为CaCu2(Ni0.6Co0.4)Ti3.8Sc0.2O12的纳米颗粒、所述重量组分的Er2O3的玻璃相纳米氧化物颗粒与6.67份的二甲基甲酰胺混合，于50℃下、150rpm转速下搅拌30min，将得到的混合物于室温下静置10min后于3000rpm转速下离心5min，将得到的沉淀于乙醇下清洗3次后，再于蒸馏水中清洗3次，得到Er2O3纳米颗粒改性CaCu2(Ni0.6Co0.4)Ti3.8Sc0.2O12梯度纳米颗粒；
M5：将步骤M4得到的所述Er2O3纳米颗粒改性CaCu2(Ni0.6Co0.4)Ti3.8Sc0.2O12梯度纳米颗粒与剩余13.33份的二甲基甲酰胺混合均匀后，与55份的聚偏氟乙烯和步骤M3得到的镀覆有AlN和BeO掺杂的亚微米层的金刚石微粉混合，于55℃下、250rpm转速下搅拌30min，然后于氮气气流下、70℃下烘干，得到压力传感器陶瓷材料。
其中，分子式为CaCu2(Ni0.6Co0.4)Ti3.8Sc0.2O12的纳米颗粒的制备方法采用如实施例1中所述的方法进行。
对比例2
本对比例与实施例1的区别在于，不采用Er2O3的玻璃相纳米氧化物颗粒这一成分，按重量组分计，包括以下成分：
进而在最后的制作步骤中，采用如下步骤：
M1：将10份的粒径为15μm的多晶金刚石微粉溶于浓度为10M的浓NaOH溶液中，于100℃下煮沸后，采用蒸馏水清洗3次，然后浸没于浓度为2M浓度的HCl，于超声波下振荡20min后，得到预处理后的多晶金刚石微粉；
M2：将15份的AlN、8的BeO与20份的聚甲基甲酰胺混合，于61℃下以180rpm转速搅拌10min；
M3：将M2步骤得到的混合物与M1步骤得到的预处理后的多晶金刚石微粉置于真空中，于10MPa下于流量为160ml/min的氩气气氛下抽真空，以20℃/min升温速率升温至350℃保温1.5h后，继续以20℃/min升温速率升温至950℃保温2h，得到镀覆有AlN和BeO掺杂的亚微米层的金刚石微粉，所述亚微米层为10μm；
M4：将45份的分子式为CaCu2(Ni0.6Co0.4)Ti3.8Sc0.2O12的纳米颗粒与20份的二甲基甲酰胺混合均匀后，与55份的聚偏氟乙烯和步骤M3得到的镀覆有AlN和BeO掺杂的亚微米层的金刚石微粉混合，于55℃下、250rpm转速下搅拌30min，然后于氮气气流下、70℃下烘干，得到压力传感器陶瓷材料。
其中，分子式为CaCu2(Ni0.6Co0.4)Ti3.8Sc0.2O12的纳米颗粒的制备方法采用如实施例1中所述的方法进行。
对比例3
本对比例与实施例1的区别在于，采用CaCu3Ti4O12纳米颗粒替代自制备的CaCu2.5Ni0.5Ti4O12的纳米颗粒这一成分，按重量组分计，包括以下成分：
M1：将10份的粒径为15μm的多晶金刚石微粉溶于浓度为10M的浓NaOH溶液中，于100℃下煮沸后，采用蒸馏水清洗3次，然后浸没于浓度为2M浓度的HCl，于超声波下振荡20min后，得到预处理后的多晶金刚石微粉；
M2：将15份的AlN、8的BeO与20份的聚甲基甲酰胺混合，于61℃下以180rpm转速搅拌10min；
M3：将M2步骤得到的混合物与M1步骤得到的预处理后的多晶金刚石微粉置于真空中，于10MPa下于流量为160ml/min的氩气气氛下抽真空，以20℃/min升温速率升温至350℃保温1.5h后，继续以20℃/min升温速率升温至950℃保温2h，得到镀覆有AlN和BeO掺杂的亚微米层的金刚石微粉，所述亚微米层为10μm；
M4：将45份的分子式为CaCu3Ti4O12的纳米颗粒、所述重量组分的Er2O3的玻璃相纳米氧化物颗粒与6.67份的二甲基甲酰胺混合，于50℃下、150rpm转速下搅拌30min，将得到的混合物于室温下静置10min后于3000rpm转速下离心5min，将得到的沉淀于乙醇下清洗3次后，再于蒸馏水中清洗3次，得到Er2O3纳米颗粒改性CaCu3Ti4O12梯度纳米颗粒；
M5：将步骤M4得到的所述Er2O3纳米颗粒改性CaCu3Ti4O12梯度纳米颗粒与剩余13.33份的二甲基甲酰胺混合均匀后，与55份的聚偏氟乙烯和步骤M3得到的镀覆有AlN和BeO掺杂的亚微米层的金刚石微粉混合，于55℃下、250rpm转速下搅拌30min，然后于氮气气流下、70℃下烘干，得到压力传感器陶瓷材料。
测试例
测试实施例1-3以及对比例1-3的传感器陶瓷材料的机械强度、电阻率(代表绝缘性能)、孔隙率、介电常数、介电损耗、漏电流和热膨胀系数，结果如表1所示。
表1
虽然已经参考优选实施例对本发明进行了描述，但在不脱离本发明的范围的情况下，可以对其进行各种改进并且可以用等效物替换其中的成分及参数。尤其是，只要不存在技术方案的冲突，各个实施例中所提到的各项技术特征均可以任意方式组合起来。本发明并不局限于文中公开的特定实施例，而是包括落入权利要求的范围内的所有技术方案。
Claims (10)
1.一种压力传感器陶瓷材料，其特征在于，按重量组分计，包括以下成分
分子式为CaCu3-xMxTi4-yScyO12的纳米陶瓷颗粒45份～50份，其中0＜x≤1，0.2≤y≤0.8，所述M为Ni、Zr、Co、Sr；
分子式为B2O3的玻璃相纳米氧化物颗粒20份～25份，所述元素A为Er、Fe、Cr或Bi；
2.根据权利要求1所述的一种压力传感器陶瓷材料，其特征在于，所述CaCu3-xMxTi4- yScyO12纳米颗粒材料的制备方法包括以下步骤：
S1：将钙无机盐水合物、铜无机盐水合物和M元素无机盐水合物按照摩尔比为1:3-x:x溶于乙醇中，形成第一混合前驱体溶液；
S2：将硅烷偶联剂、钪无机盐水合物按照摩尔比为4-y:y溶于乙酰丙酮中，形成第二混合前驱体溶液；
S3：将所述S1步骤得到的第一混合前驱体溶液和所述S2步骤得到的第二混合前驱体溶液于95℃～105℃、200rpm～300rpm转速下搅拌15min，搅拌过程中滴加乙醇溶液，形成CaCu3-xMxTi4-yScyO12纳米前驱体凝胶；
S4：将所述步骤S3得到的CaCu3-xMxTi4-yScyO12纳米前驱体凝胶于氮气气体气氛中、150℃～160℃下干燥2h～2.5h后，采用行星球磨机研磨，得到CaCu3-xMxTi4-yScyO12纳米前驱体粉末；
S5：将所述CaCu3-xMxTi4-yScyO12纳米前驱体粉末于950℃～1150℃下煅烧1h～1.5h后，避免CaCu3-xMxTi4-yScyO12晶体生长，得到CaCu3-xMxTi4-yScyO12纳米颗粒。
3.根据权利要求2所述的一种压力传感器陶瓷材料，其特征在于，所述钛酸酯偶联剂为四异丙基二(二辛基亚磷酸酰氧基)钛酸酯、钛酸异丙酯、二(乙酰丙酮基)钛酸二异丙酯或正钛酸四丁酯中的一种或几种。
4.根据权利要求2所述的一种压力传感器陶瓷材料，其特征在于，所述铜无机盐水合物为Cu(NO3)2·3H2O、Cu(CH3COO)2·H2O、CuCl2·2H2O或CuSO4·5H2O；所述钙无机盐水合物为Ca(NO3)2·4H2O、Ca(CH3COO)2·H2O、CaSO4·2H2O或CaCl2·6H2O。
5.根据权利要求2所述的一种压力传感器陶瓷材料，其特征在于，所述M元素的水合物为Ni(NO3)2·6H2O、Ni(CH3COO)2·4H2O、NiSO4·6H2O、NiCl2·6H2O、Zr(NO3)3·5H2O、Zr(SO4)2·4H2O、ZrOCl2·8H2O、Co(NO3)2·6H2O、Co(CH3COO)2·4H2O、Co(SO4)2·7H2O、CoCl2·6H2O、Sr(CH3COO)2·2H2O或SrCl2·6H2O；所述钪无机盐水合物为ScCl3·6H2O、Sc2(SO4)3·8H2O、Sc(CH3COO)3·5H2O、Sc(NO3)3·H2O。
6.根据权利要求2所述的一种压力传感器陶瓷材料，其特征在于，所述S3步骤中滴加的乙醇溶液为含有乙醇的体积分数为20％～40％。
7.根据权利要求1所述的一种压力传感器陶瓷材料，其特征在于，所述多相金刚石微粉的粒径为15μm～25μm。
8.根据权利要求1所述的一种压力传感器陶瓷材料，其特征在于，所述微孔膜聚合物为聚苯醚砜、聚偏氟乙烯、聚磺化苯醚砜、聚四氟乙烯中的一种。
9.根据权利要求1-8任一所述的一种压力传感器陶瓷材料的制备方法，其特征在于，包括以下步骤：
M1：将所述重量组分的多晶金刚石微粉溶于浓度为10M～12M的浓NaOH溶液中，于100℃～110℃下煮沸后，采用蒸馏水清洗3次，然后浸没于浓度为2M～5M浓度的HCl，于超声波下振荡20min～30min后，得到预处理后的多晶金刚石微粉；
M2：将所述重量组分的AlN、所述重量组分的BeO与所述重量组分的聚甲基甲酰胺混合，于60℃～70℃下以180rpm～230rpm转速搅拌10min～15min；
M3：将所述M2步骤得到的混合物与所述M1步骤得到的预处理后的多晶金刚石微粉置于真空中，于10MPa～15MPa下于惰性气氛下抽真空，以20℃/min升温速率升温至350℃～400℃保温1.5h后，继续以20℃/min升温速率升温至950℃～1000℃保温2h～2.5h，得到镀覆有AlN和BeO掺杂的亚微米层的金刚石微粉，所述亚微米层为10μm～20μm；
M4：将所述重量组分的分子式为CaCu3-xMxTi4-yScyO12的纳米颗粒、所述重量组分的B2O3的玻璃相纳米氧化物颗粒与三分之一所述重量组分的二甲基甲酰胺混合，于50℃～70℃下、150rpm～200rpm转速下搅拌30min～45min，将得到的混合物于室温下静置10min后于3000rpm～4000rpm转速下离心5min～10min，将得到的沉淀于乙醇下清洗3次后，再于蒸馏水中清洗3次，得到B2O3纳米颗粒改性CaCu3-xMxTi4-yScyO12梯度纳米颗粒；
M5：将所述步骤M4得到的所述B2O3纳米颗粒改性CaCu3-xMxTi4-yScyO12梯度纳米颗粒与剩余三分之二所述重量组分的二甲基甲酰胺混合均匀后，与所述重量组分的微孔膜聚合物和所述步骤M3得到的镀覆有AlN和BeO掺杂的亚微米层的金刚石微粉混合，于55℃～75℃下、250rpm～300rpm转速下搅拌30min～45min，然后于氮气气流下、70℃～80℃下烘干，得到所述压力传感器陶瓷材料。
10.根据权利要求9所述的一种压力传感器陶瓷材料的制备方法，其特征在于，所述M3步骤的中抽真空所使用的惰性气氛为氩气气氛，流量为160ml/min～200ml/min。
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