CN108129145B - 一种x7r陶瓷电容器介质材料及其制备方法 - Google Patents
一种x7r陶瓷电容器介质材料及其制备方法 Download PDFInfo
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- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 88
- 239000003989 dielectric material Substances 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002019 doping agent Substances 0.000 claims abstract description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910004481 Ta2O3 Inorganic materials 0.000 claims abstract description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 10
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 10
- 239000011656 manganese carbonate Substances 0.000 claims abstract description 10
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims abstract description 10
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 10
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 8
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 8
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 8
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 8
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 8
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 60
- 238000000227 grinding Methods 0.000 claims description 43
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 33
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 31
- 239000008367 deionised water Substances 0.000 claims description 30
- 229910021641 deionized water Inorganic materials 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000002994 raw material Substances 0.000 claims description 28
- 239000002002 slurry Substances 0.000 claims description 27
- 238000000498 ball milling Methods 0.000 claims description 26
- 238000005303 weighing Methods 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 18
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 17
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 17
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims description 17
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 16
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 16
- 239000003990 capacitor Substances 0.000 claims description 15
- 239000012856 weighed raw material Substances 0.000 claims description 15
- 229910015802 BaSr Inorganic materials 0.000 claims description 14
- 238000003825 pressing Methods 0.000 claims description 14
- 239000004576 sand Substances 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 4
- 238000010304 firing Methods 0.000 abstract description 17
- 230000008859 change Effects 0.000 abstract description 9
- 239000000919 ceramic Substances 0.000 description 42
- 239000000758 substrate Substances 0.000 description 25
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 24
- 239000004332 silver Substances 0.000 description 24
- 229910052709 silver Inorganic materials 0.000 description 24
- 238000000465 moulding Methods 0.000 description 12
- 238000004321 preservation Methods 0.000 description 12
- 230000001680 brushing effect Effects 0.000 description 11
- 238000012360 testing method Methods 0.000 description 11
- 238000007599 discharging Methods 0.000 description 6
- 238000011161 development Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 229910002370 SrTiO3 Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical group [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000007613 environmental effect Effects 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
- 238000011056 performance test Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
本发明涉及一种X7R陶瓷电容器介质材料及其制备方法，其包括主成分BaSrxCa1‑xTi2O6，其中0.35≤x≤0.85和改性掺杂剂，所述的改性掺杂剂是纳米级或亚纳米级ZnO、SiO2、Al2O3、Dy2O3、Nb2O5、Ta2O3、Li2CO3、TiO2、MnCO3中的两种或两种以上。本发明所述的X7R陶瓷电容器介质材料烧成温度1050～1150℃，介电常数800～1200,介质损耗≦0.5％，抗电强度≧9KVAc/mm，温度特性变化率(‑55～125℃)<±15％,适用于制作高可靠性X7R陶瓷电容器。
Description
技术领域
本发明涉及电子材料与器件技术领域，尤其是一种X7R陶瓷电容器介质材料及其制备方法。
背景技术
近年来，随着电子行业的不断发展，目前市场上(特别是手机充电器等)，对瓷介电容器的质量要求越来越高,既要小型化亦要可靠性高.研发生产高可靠性及小型化瓷介电容器要解决的关键技术问题就是开发高性能的瓷介电容器用介质材料，而目前国内相应的材料逐渐难以满足发展要求。因此开发具有更高耐电强度，更低介质损耗，更宽使用温度范围，可靠性高的瓷介电容器介质材料的制备技术，并实现产业化，是目前国内电子行业持续发展的重点之一。
电容器中的介质材料不一样，其极化类型就不一样，相应地其对电场变化的响应速度和极化率亦不一样。在相同的体积下的容量就不同，随之带来的电容器的介质损耗、容量稳定性等也就不同。介质材料按容量的温度稳定性可以划分为两类，即Ⅰ类陶瓷电容器和Ⅱ类陶瓷电容器，NPO属于Ⅰ类陶瓷，Ⅰ类陶瓷电容器的介电常数一般小于100，其电气性能稳定，基本上不随温度、电压、时间的改变而变化，属超稳定、低损耗的电容器介质材料，常用于对稳定性、可靠性要求较高的高频、超高频、甚高频的场合。X7R、X5R、Y5V、Z5U等都属于Ⅱ类陶瓷。Ⅱ类陶瓷电容器的介电常数一般大于1000，其电气性能较稳定，适用于隔直、耦合、旁路及对可靠性要求较高的中、低频场合，以及对容量稳定性和损耗要求不高的场合。
Ⅱ类陶瓷电容器中的X7R电容器被称为温度稳定型的陶瓷电容器。当温度在-55℃到+125℃时其容量变化一般在15％左右，此时电容器容量变化是非线性的，X7R电容器主要应用于要求不高的工业应用，而且当电压变化时其容量变化是可以接受的条件下。它的主要特点是在相同的体积下电容量可以做的比较大。
发明专利CN104193328B公开了一种陶瓷介质材料，主相为钛酸钡，副料为SrTiO3，还包括改性添加剂和烧结助溶剂，其在-25～+85℃温度特性变化率在20％左右，其使用环境温度范围窄，可靠性低，不满足高品质要求的市场要求。
发明内容
本发明所要解决的问题是克服现有技术存在的不足，提供一种X7R陶瓷电容器介质材料及其制备方法，与国内同类X7R陶瓷电容器介质材料产品相比，具有烧成温度低、介质损耗低、使用环境温度范围宽、抗电强度高、可靠性高的优势。适应产品小型化及高品质要求的市场需求，降低后续产品应用领域的生产运行成本。
具体方案如下：
一种X7R陶瓷电容器介质材料，包括主成分和改性掺杂剂，所述的主成分是BaSrxCa1-xTi2O6，其中0.35≤x≤0.85；所述的改性掺杂剂是纳米级或亚纳米级ZnO、SiO2、Al2O3、Dy2O3、Nb2O5、Ta2O3、Li2CO3、TiO2、MnCO3中的两种或两种以上。
进一步的，所述的X7R陶瓷电容器介质材料由所述的主成分和所述的改性掺杂剂组成。
进一步的，所述的X7R陶瓷电容器介质材料中，所述的主成分占总重86～97％，所述的改性掺杂剂占总重3～14％。
进一步的，所述的改性掺杂剂由占所述X7R陶瓷电容器介质材料总重的以下原料组成：ZnO为0.5～2％、SiO2为0～1％、Al2O3为0～1％、Dy2O3为0～0.5％、Nb2O5为0.1～1％、Ta2O3为0.1～1.5％、Li2CO3为0.1～1％、TiO2为1～5％、MnCO3为0.1～1％。
进一步的，所述的X7R陶瓷电容器介质材料按重量百分比由以下原料组成：BaSr0.5Ca0.5Ti2O6为92.5％，ZnO为1％、SiO2为1％、Al2O3为1％、Dy2O3为0.5％、Nb2O5为1.25％、Ta2O3为0.25％、Li2CO3为0.5％、TiO2为1.5％、MnCO3为0.5％。
进一步的，所述的主成分的制备方法为：按结构式BaSrxCa1-xTi2O6的化学计量比称量BaCO3、SrCO3、CaCO3、TiO2作为原料，其中0.35≤x≤0.85，将称量好的原料装入球磨罐中，加入去离子水和氧化锆球进行研磨8～12小时，出料烘干、粉碎后在1250～1350℃下煅烧3～5小时得到BaSrxCa1-xTi2O6。
本发明还保护所述的X7R陶瓷电容器介质材料的用途，用于制备X7R陶瓷电容器。
进一步的，所述的X7R陶瓷电容器介质材料干压成型后，6～10小时内升温到1050～1150℃，之后在1050～1150℃烧结2.5～3.5小时得到X7R陶瓷电容器介质。
本发明还保护所述的X7R陶瓷电容器介质材料的制备方法，包括以下步骤：
1)按结构式BaSrxCa1-xTi2O6的化学计量比称量BaCO3、SrCO3、CaCO3、TiO2作为原料，其中0.35≤x≤0.85，将称量好的原料装入球磨罐中，加入去离子水和氧化锆球进行研磨8～12小时，出料烘干、粉碎后煅烧得到BaSrxCa1-xTi2O6；
2)将上步得到的BaSrxCa1-xTi2O6作为主成分，再称量纳米级或亚纳米级ZnO、SiO2、Al2O3、Dy2O3、Nb2O5、Ta2O3、Li2CO3、TiO2、MnCO3中的两种或两种以上作为改性掺杂剂，将称量好的物料装入球磨罐中，加入去离子水和氧化锆球用进行研磨成浆料后再加入超细砂磨机中研磨，再加入聚乙烯醇的水溶液进行干燥造粒后得到所述的X7R陶瓷电容器介质材料。
进一步的，所述步骤1)中煅烧的温度为1250～1350℃，煅烧的时间为3～5小时；
任选的，所述步骤2)中所述的主成分占总重86～97％，所述的改性掺杂剂占总重3～14％，所述的聚乙烯醇的水溶液的用量为总重的0.1～1％。
有益效果：本发明所述的X7R陶瓷电容器介质材料烧成温度1050～1150℃，介电常数800～1200,介质损耗≦0.5％，抗电强度≧9KVAc/mm，温度特性变化率(-55～125℃)<±15％，适用于制作高可靠性X7R陶瓷电容器介质陶瓷体。本发明采用了固相反应合成技术，重现性好，符合环保要求，并且通过调整BaSrxCa1-xTi2O6中SrCO3、CaCO3及纳米级或亚纳米级ZnO、SiO2、Al2O3、Dy2O3、Nb2O5、Ta2O3、Li2CO3、TiO2、MnCO3改性掺杂剂含量的变化，陶瓷介质材料的介电常数可在800～1200之间连续可调，能适应一定范围内的不同K值的X7R瓷介电容器陶瓷介质材料的制作要求，具有烧成温度低、介质损耗低、使用环境温度范围宽、抗电强度高、可靠性高的特点，是一种性能优越的瓷介电容器陶瓷介质材料。
具体实施方式
下面结合实施例对本发明技术方案作进一步阐述。实施例中未注明具体技术或条件者，按照本领域内的文献所描述的技术或条件或者按照产品说明书进行。所用试剂或仪器未注明生产厂商者，均为可以通过市购获得的常规产品。
本发明中X7R陶瓷电容器介质材料的主成分是BaSrxCa1-xTi2O6，其中0.35≤x≤0.85，实施例中以x＝0.5为例。
实施例1
X7R陶瓷电容器介质材料的制备方法如下：
1)按结构式BaSr0.5Ca0.5Ti2O6的化学计量比称量BaCO3、SrCO3、CaCO3、TiO2作为原料，将称量好的原料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球进行研磨10小时，出料烘干、粉碎后在1290℃下煅烧3小时得到BaSr0.5Ca0.5Ti2O6；
2)将上步得到的BaSr0.5Ca0.5Ti2O6作为主成分，按照表1再称量改性掺杂剂，将称量好的各物料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球用进行研磨成浆料后再加入超细砂磨机中研磨，再加入总重5％的聚乙烯醇的水溶液(质量浓度10％)进行干燥造粒后得到所述的X7R陶瓷电容器介质材料。
将所得的X7R陶瓷电容器介质材料干压成型后，8小时内升温到1150℃后保温烧结2.5小时得到陶瓷基片，在烧制后的陶瓷基片上刷银浆，在810℃烧15min，制得银电极，测试各项电性能。其介电性能参数测试见表2。
表1各材料用量表(按重量％)
表2性能检测结果表
实施例2
X7R陶瓷电容器介质材料的制备方法如下：
1)按结构式BaSr0.5Ca0.5Ti2O6的化学计量比称量BaCO3、SrCO3、CaCO3、TiO2作为原料，将称量好的原料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球进行研磨10小时，出料烘干、粉碎后在1300℃下煅烧3小时得到BaSr0.5Ca0.5Ti2O6；
2)将上步得到的BaSr0.5Ca0.5Ti2O8作为主成分，按照表1再称量改性掺杂剂，将称量好的各物料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球用进行研磨成浆料后再加入超细砂磨机中研磨，再加入总重10％的聚乙烯醇的水溶液(质量浓度10％)进行干燥造粒后得到所述的X7R陶瓷电容器介质材料。
将所得的X7R陶瓷电容器介质材料干压成型后，10小时内升温到1150℃后保温烧结3小时得到陶瓷基片，在烧制后的陶瓷基片上刷银浆，在810℃烧15min，制得银电极，测试各项电性能。其介电性能参数测试见表2。
实施例3
X7R陶瓷电容器介质材料的制备方法如下：
1)按结构式BaSr0.5Ca0.5Ti2O6的化学计量比称量BaCO3、SrCO3、CaCO3、TiO2作为原料，将称量好的原料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球进行研磨12小时，出料烘干、粉碎后在1250℃下煅烧5小时得到BaSr0.5Ca0.5Ti2O6；
2)将上步得到的BaSr0.5Ca0.5Ti2O6作为主成分，按照表1再称量改性掺杂剂，将称量好的各物料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球用进行研磨成浆料后再加入超细砂磨机中研磨，再加入总重10％的聚乙烯醇的水溶液(质量浓度10％)进行干燥造粒后得到所述的X7R陶瓷电容器介质材料。
将所得的X7R陶瓷电容器介质材料干压成型后，6小时内升温到1110℃后保温烧结3小时得到陶瓷基片，在烧制后的陶瓷基片上刷银浆，在810℃烧15min，制得银电极，测试各项电性能。其介电性能参数测试见表2。
实施例4
X7R陶瓷电容器介质材料的制备方法如下：
1)按结构式BaSr0.5Ca0.5Ti2O6的化学计量比称量BaCO3、SrCO3、CaCO3、TiO2作为原料，将称量好的原料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球进行研磨8小时，出料烘干、粉碎后在1350℃下煅烧3小时得到BaSr0.5Ca0.5Ti2O6；
2)将上步得到的BaSr0.5Ca0.5Ti2O6作为主成分，按照表1再称量改性掺杂剂，将称量好的各物料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球用进行研磨成浆料后再加入超细砂磨机中研磨，再加入总重10％的聚乙烯醇的水溶液(质量浓度10％)进行干燥造粒后得到所述的X7R陶瓷电容器介质材料。
将所得的X7R陶瓷电容器介质材料干压成型后，10小时内升温到1150℃后保温烧结2.5小时得到陶瓷基片，在烧制后的陶瓷基片上刷银浆，在810℃烧15min，制得银电极，测试各项电性能。其介电性能参数测试见表2。
实施例5
X7R陶瓷电容器介质材料的制备方法如下：
1)按结构式BaSr0.5Ca0.5Ti2O6的化学计量比称量BaCO3、SrCO3、CaCO3、TiO2作为原料，将称量好的原料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球进行研磨8小时，出料烘干、粉碎后在1250℃下煅烧3小时得到BaSr0.5Ca0.5Ti2O6；
2)将上步得到的BaSr0.5Ca0.5Ti2O6作为主成分，按照表1再称量改性掺杂剂，将称量好的各物料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球用进行研磨成浆料后再加入超细砂磨机中研磨，再加入总重10％的聚乙烯醇的水溶液(质量浓度10％)进行干燥造粒后得到所述的X7R陶瓷电容器介质材料。
将所得的X7R陶瓷电容器介质材料干压成型后，10小时内升温到1050℃后保温烧结3.5小时得到陶瓷基片，在烧制后的陶瓷基片上刷银浆，在810℃烧15min，制得银电极，测试各项电性能。其介电性能参数测试见表2。
实施例6
X7R陶瓷电容器介质材料的制备方法如下：
1)按结构式BaSr0.5Ca0.5Ti2O6的化学计量比称量BaCO3、SrCO3、CaCO3、TiO2作为原料，将称量好的原料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球进行研磨8小时，出料烘干、粉碎后在1250℃下煅烧5小时得到BaSr0.5Ca0.5Ti2O6；
2)将上步得到的BaSr0.5Ca0.5Ti2O6作为主成分，按照表1再称量改性掺杂剂，将称量好的各物料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球用进行研磨成浆料后再加入超细砂磨机中研磨，再加入总重10％的聚乙烯醇的水溶液(质量浓度10％)进行干燥造粒后得到所述的X7R陶瓷电容器介质材料。
将所得的X7R陶瓷电容器介质材料干压成型后，6小时内升温到1150℃后保温烧结2.5小时得到陶瓷基片，在烧制后的陶瓷基片上刷银浆，在810℃烧15min，制得银电极，测试各项电性能。其介电性能参数测试见表2。
实施例7
X7R陶瓷电容器介质材料的制备方法如下：
1)按结构式BaSr0.5Ca0.5Ti2O6的化学计量比称量BaCO3、SrCO3、CaCO3、TiO2作为原料，将称量好的原料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球进行研磨11小时，出料烘干、粉碎后在1310℃下煅烧4.5小时得到BaSr0.5Ca0.5Ti2O6；
2)将上步得到的BaSr0.5Ca0.5Ti2O6作为主成分，按照表1再称量改性掺杂剂，将称量好的各物料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球用进行研磨成浆料后再加入超细砂磨机中研磨，再加入总重10％的聚乙烯醇的水溶液(质量浓度10％)进行干燥造粒后得到所述的X7R陶瓷电容器介质材料。
将所得的X7R陶瓷电容器介质材料干压成型后，6小时内升温到1090℃后保温烧结3小时得到陶瓷基片，在烧制后的陶瓷基片上刷银浆，在810℃烧15min，制得银电极，测试各项电性能，其介电性能参数测试见表2。
实施例8
X7R陶瓷电容器介质材料的制备方法如下：
1)按结构式BaSr0.5Ca0.5Ti2O6的化学计量比称量BaCO3、SrCO3、CaCO3、TiO2作为原料，将称量好的原料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球进行研磨11小时，出料烘干、粉碎后在1290℃下煅烧3.5小时得到BaSr0.5Ca0.5Ti2O6；
2)将上步得到的BaSr0.5Ca0.5Ti2O8作为主成分，按照表1再称量改性掺杂剂，将称量好的各物料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球用进行研磨成浆料后再加入超细砂磨机中研磨，再加入总重8％的聚乙烯醇的水溶液(质量浓度10％)进行干燥造粒后得到所述的X7R陶瓷电容器介质材料。
将所得的X7R陶瓷电容器介质材料干压成型后，7小时内升温到1060℃后保温烧结3.2小时得到陶瓷基片，在烧制后的陶瓷基片上刷银浆，在810℃烧15min，制得银电极，测试各项电性能，其介电性能参数测试见表2。
实施例9
X7R陶瓷电容器介质材料的制备方法如下：
1)按结构式BaSr0.5Ca0.5Ti2O6的化学计量比称量BaCO3、SrCO3、CaCO3、TiO2作为原料，将称量好的原料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球进行研磨9小时，出料烘干、粉碎后在1280℃下煅烧4小时得到BaSr0.5Ca0.5Ti2O6；
2)将上步得到的BaSr0.5Ca0.5Ti2O6作为主成分，按照表1再称量改性掺杂剂，将称量好的各物料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球用进行研磨成浆料后再加入超细砂磨机中研磨，再加入总重5％的聚乙烯醇的水溶液(质量浓度10％)进行干燥造粒后得到所述的X7R陶瓷电容器介质材料。
将所得的X7R陶瓷电容器介质材料干压成型后，9小时内升温到1100℃后保温烧结3小时得到陶瓷基片，在烧制后的陶瓷基片上刷银浆，在810℃烧15min，制得银电极，测试各项电性能，
其介电性能参数测试见表2。
实施例10
X7R陶瓷电容器介质材料的制备方法如下：
1)按结构式BaSr0.5Ca0.5Ti2O6的化学计量比称量BaCO3、SrCO3、CaCO3、TiO2作为原料，将称量好的原料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球进行研磨10小时，出料烘干、粉碎后在1300℃下煅烧4小时得到BaSr0.5Ca0.5Ti2O6；
2)将上步得到的BaSr0.5Ca0.5Ti2O6作为主成分，按照表1再称量改性掺杂剂，将称量好的各物料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球用进行研磨成浆料后再加入超细砂磨机中研磨，再加入总重10％的聚乙烯醇的水溶液(质量浓度10％)进行干燥造粒后得到所述的X7R陶瓷电容器介质材料。
将所得的X7R陶瓷电容器介质材料干压成型后，7小时内升温到1100℃后保温烧结3小时得到陶瓷基片，在烧制后的陶瓷基片上刷银浆，在810℃烧15min，制得银电极，测试各项电性能,其介电性能参数测试见表2。
实施例11
X7R陶瓷电容器介质材料的制备方法如下：
1)按结构式BaSr0.5Ca0.5Ti2O6的化学计量比称量BaCO3、SrCO3、CaCO3、TiO2作为原料，将称量好的原料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球进行研磨12小时，出料烘干、粉碎后在1350℃下煅烧3小时得到BaSr0.5Ca0.5Ti2O6；
2)将上步得到的BaSr0.5Ca0.5Ti2O6作为主成分，按照表1再称量改性掺杂剂，将称量好的各物料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球用进行研磨成浆料后再加入超细砂磨机中研磨，再加入总重10％的聚乙烯醇的水溶液(质量浓度10％)进行干燥造粒后得到所述的X7R陶瓷电容器介质材料。
将所得的X7R陶瓷电容器介质材料干压成型后，6小时内升温到1050℃后保温烧结3.5小时得到陶瓷基片，在烧制后的陶瓷基片上刷银浆，在810℃烧15min，制得银电极，测试各项电性能,其介电性能参数测试见表2。
实施例12
X7R陶瓷电容器介质材料的制备方法如下：
1)按结构式BaSr0.5Ca0.5Ti2O6的化学计量比称量BaCO3、SrCO3、CaCO3、TiO2作为原料，将称量好的原料装入球磨罐中，加入去离子水(占总重10％)和氧化锆球进行研磨8小时，出料烘干、粉碎后在1250℃下煅烧5小时得到BaSr0.5Ca0.5Ti2O6；
2)将上步得到的BaSr0.5Ca0.5Ti2O6作为主成分，按照表1再称量改性掺杂剂，将称量好的各物料装入球磨罐中，加入去离子水(占总重50％)和氧化锆球用进行研磨成浆料后再加入超细砂磨机中研磨，再加入总重10％的聚乙烯醇的水溶液(质量浓度10％)进行干燥造粒后得到所述的X7R陶瓷电容器介质材料。
将所得的X7R陶瓷电容器介质材料干压成型后，10小时内升温到1150℃后保温烧结2.5小时得到陶瓷基片，在烧制后的陶瓷基片上刷银浆，在810℃烧15min，制得银电极，测试各项电性能,其介电性能参数测试见表2。
从上述实施例可以看出，本发明所述的X7R陶瓷电容器介质材料烧成温度1050～1150℃，介电常数800～1200,介质损耗≦0.5％，抗电强度≧9KVAc/mm，温度特性变化率(-55～125℃)<±15％,且介电常数可在800～1200之间连续可调，能适应一定范围内的不同K值的X7R瓷介电容器陶瓷介质材料的制作要求，具有烧成温度低、介质损耗低、使用环境温度范围宽、抗电强度高、可靠性高的特点，是一种性能优越的X7R陶瓷电容器介质材料。
尽管上面已经示出和描述了本发明的实施例，可以理解的是，上述实施例是示例性的，不能理解为对本发明的限制，本领域的普通技术人员在不脱离本发明的原理和宗旨的情况下在本发明的范围内可以对上述实施例进行变化、修改、替换和变型。
Claims (8)
1.一种X7R陶瓷电容器介质材料，包括主成分和改性掺杂剂，其特征在于：所述的主成分是BaSrxCa1-xTi2O6，其中0.35≤x≤0.85；所述的改性掺杂剂是纳米级或亚纳米级ZnO、SiO2、Al2O3、Dy2O3、Nb2O5、Ta2O3、Li2CO3、 TiO2、MnCO3；所述的X7R陶瓷电容器介质材料由所述的主成分和所述的改性掺杂剂组成，其中，所述的主成分占总重86~95%，所述的改性掺杂剂占总重5～14%；所述的改性掺杂剂由占所述X7R陶瓷电容器介质材料总重的以下原料组成：ZnO为0.5～2%、SiO2为0.25～1%、Al2O3为0.25～1%、Dy2O3为0.25～0.5%、Nb2O5为0.1～1%、Ta2O3为0.1～1.5%、Li2CO3为0.1～1%、 TiO2为1～5% 、MnCO3为0.1～1%。
2.根据权利要求1所述的X7R陶瓷电容器介质材料，其特征在于：所述的X7R陶瓷电容器介质材料按重量百分比由以下原料组成：BaSr0.5Ca0.5Ti2O6 为92.5%，ZnO为1%、SiO2为1%、Al2O3为1%、Dy2O3为0.5%、Nb2O5为1%、Ta2O3为0.25%、Li2CO3为0.5%、TiO2为1.5%、MnCO3为0.5%。
3.根据权利要求1所述的X7R陶瓷电容器介质材料，其特征在于：所述的主成分的制备方法为：按结构式BaSrxCa1-xTi2O6的化学计量比称量BaCO3、SrCO3、CaCO3、TiO2作为原料，其中0.35≤x≤0.85，将称量好的原料装入球磨罐中，加入去离子水和氧化锆球进行研磨8～12小时，出料烘干、粉碎后在1250～1350℃下煅烧3～5小时得到BaSrxCa1-xTi2O6。
4.权利要求1或2所述的X7R陶瓷电容器介质材料的用途，用于制备X7R陶瓷电容器。
5.根据权利要求4所述的X7R陶瓷电容器介质材料的用途，其特征在于：所述的X7R陶瓷电容器介质材料干压成型后，6～10小时内升温到1050～1150℃，之后在1050～1150℃烧结2.5～3.5小时得到X7R陶瓷电容器介质。
6.一种权利要求1或2所述的X7R陶瓷电容器介质材料的制备方法，其特征在于：包括以下步骤：
1）按结构式BaSrxCa1-xTi2O6的化学计量比称量BaCO3、SrCO3、CaCO3、TiO2作为原料，其中0.35≤x≤0.85，将称量好的原料装入球磨罐中，加入去离子水和氧化锆球进行研磨8～12小时，出料烘干、粉碎后煅烧得到BaSrxCa1-xTi2O6；
2）将上步得到的BaSrxCa1-xTi2O6作为主成分，再称量纳米级或亚纳米级ZnO、SiO2、Al2O3、Dy2O3、Nb2O5、Ta2O3、Li2CO3、 TiO2、MnCO3作为改性掺杂剂，将称量好的物料装入球磨罐中，加入去离子水和氧化锆球进行研磨成浆料后再加入超细砂磨机中研磨，再加入聚乙烯醇的水溶液进行干燥造粒后得到所述的X7R陶瓷电容器介质材料。
7.根据权利要求6所述的X7R陶瓷电容器介质材料的制备方法，其特征在于：所述步骤1）中煅烧的温度为1250～1350℃，煅烧的时间为3～5小时。
8.根据权利要求6所述的X7R陶瓷电容器介质材料的制备方法，其特征在于：所述步骤2）中所述的聚乙烯醇的水溶液的用量为总重的0.1~1%。
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