CN112299845B - 一种高性能的陶瓷介质材料及其制备方法 - Google Patents

一种高性能的陶瓷介质材料及其制备方法 Download PDF

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CN112299845B
CN112299845B CN202011333420.3A CN202011333420A CN112299845B CN 112299845 B CN112299845 B CN 112299845B CN 202011333420 A CN202011333420 A CN 202011333420A CN 112299845 B CN112299845 B CN 112299845B
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黄景林
钟永全
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Xiamen Sanxing Electronics Co ltd
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Abstract

本发明涉及一种高性能的陶瓷介质材料及其制备方法，所述高性能的陶瓷介质材料由主成分和改性掺杂剂组成，所述主成分为BaTiO3；所述改性掺杂剂包括BaxSr1‑x(ZrySn1‑y)O3，x＝0.2～0.9,y＝0.1～0.8，Bi2Zr2O7，还包括下列组分中的三种或三种以上：ZnO、Al2O3、WO3、Nb2O5、ZrO2、Li2CO3、Nd2O3、Sm2O3或MnCO3。所述高性能的陶瓷介质材料的烧成温度1250～1320℃，介电常数15000～21000可调，介质损耗≦0.75％，抗电强度≧5KVAc/mm，温度特性变化率小于+20‑80％(‑25～85℃)，适用制作Y5V特性瓷介电容器。

Description

一种高性能的陶瓷介质材料及其制备方法
技术领域
本发明涉及陶瓷电容器制备技术，尤其是一种高性能的陶瓷介质材料及其制备方法。
背景技术
电容器是一类重要的无源电子器件，主要在电路中起到耦合、滤波、谐振、旁路、补偿等作用，是电子、通信及信息产业中所不可或缺的器件。根据构成材质，电容器可分为陶瓷电容、电解电容、薄膜电容等等。其中陶瓷电容器具有介质损耗低、绝缘电阻高、耐电强度高、稳定性及可靠性高应用更广泛等特点，而陶瓷介质材料又决定了陶瓷电容器的性能，是陶瓷电容器的核心材质。
瓷介电容器中使用的高介电常数(>20000)Y5V瓷介电容器介质材料目前仍存在介电常数、耐电强度及温度特性不能同时满足使用要求的现象。因此开发具有更高耐电强度及介电常数，更低容量温度变化率，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，是目前电子行业持续发展的重点之一。
发明内容
本发明的目的是为了克服现有技术的不足，提供一种高性能的陶瓷介质材料及其制备方法，具有烧成温度低、更高耐电强度及介电常数，更低容量温度变化率、可靠性高的优势。
本发明中，主成分BaTiO3，改性掺杂剂包括BaxSr1-x(ZrySn1-y)O3，其中x＝0.2～0.9，优选的，x＝0.3～0.5，或者x＝0.7～0.8；y＝0.1～0.8，优选的，y＝0.2～0.3，或者y＝0.4～0.6。还包括Bi2Zr2O7，以及下列组分中的三种或三种以上：ZnO、Al2O3、WO3、Nb2O5、ZrO2、Li2CO3、Nd2O3、Sm2O3或MnCO3。优选的，ZnO、Al2O3、ZrO2、Li2CO3和MnCO3为必选组分，WO3、Nb2O5、Nd2O3、Sm2O3为可选组分。
各组分按照重量百分比计，所述主成分占总重的80～90％，所述改性掺杂剂占总重的10～20％。优选的，所述主成分占总重的82～89％，所述改性掺杂剂占总重的11～18％，更优选的，所述主成分占总重的85～88％，所述改性掺杂剂占总重的12～15％。
所述高性能的陶瓷介质材料的制备方法中，BaTiO3可以商业购买获得，也可以自制，制备时按照以下方法获得：按结构式BaTiO3的化学计量比称量电子级的BaCO3、TiO2作为原料，将称量好的原料装入球磨罐中，加入去离子水进行研磨8～12小时，出料烘干、粉碎后在1200～1300℃下煅烧3～5小时，优选的，在1220～1280℃下煅烧2～3小时，合成BaTiO3。
Bi2Zr2O7可以商业购买获得，也可以自制，制备时按照以下方法获得：按结构式Bi2Zr2O7的化学计量比称量Bi2O3、ZrO2作为原料，将称量好的原料装入球磨罐中，加入去离子水进行研磨8～12小时，出料烘干、粉碎后在700～1050℃下煅烧2～3小时，优选的，在900～1000℃下煅烧2～3小时。
BaxSr1-x(ZrySn1-y)O3按照以下方法获得，按结构式BaxSr1-x(ZrySn1-y)O3的化学计量比称量电子级的BaCO3、SrCO3丶ZrO2、SnO2作为原料，将称量好的原料装入球磨罐中，加入去离子水进行研磨8～12小时，出料烘干、粉碎后在1200～1300℃下煅烧3～5小时，优选的，在1220～1280℃下煅烧3～5小时，合成BaxSr1-x(ZrySn1-y)O3烧块。
本发明中，以步骤A获得的BaTiO3作为主成分，再称量步骤B获得的BaxSr1-x(ZrySn1-y)O3烧块，以及步骤C获得的Bi2Zr2O7，以及下列组分中的三种或三种以上：ZnO、Al2O3、WO3、Nb2O5、ZrO2、Li2CO3、Nd2O3、Sm2O3或MnCO3作为改性掺杂剂，将称量好的物料装入球磨罐中，加入去离子水进行研磨，再加入聚乙烯醇溶液作为粘合剂进行干燥造粒获得所述的陶瓷介质材料。进一步的，将陶瓷介质材料进行高温烧结，可以获得陶瓷基片，烧结温度为1250～1320℃，保温2.5～3.5小时，优选的，烧结温度为1280～1300℃，
具体方案如下：
一种高性能的陶瓷介质材料，所述高性能的陶瓷介质材料由主成分和改性掺杂剂组成，其中，所述主成分为BaTiO3；
所述改性掺杂剂包括BaxSr1-x(ZrySn1-y)O3，其中x＝0.2～0.9，y＝0.1～0.8，以及Bi2Zr2O7，还包括下列组分中的三种或三种以上：ZnO、Al2O3、WO3、Nb2O5、ZrO2、Li2CO3、Nd2O3、Sm2O3或MnCO3。
进一步的，所述主成分占总重的80～90％，所述改性掺杂剂占总重的10～20％。
进一步的，所述改性掺杂剂包括BaxSr1-x(ZrySn1-y)O3，其中x＝0.6～0.9，y＝0.4～0.6。
进一步的，所述改性掺杂剂由以下组分组成：Ba0.9Sr0.1(Zr0.5Sn0.5)O3、Bi2Zr2O7、ZnO、Al2O3、ZrO2、Li2CO3和MnCO3。
进一步的，所述改性掺杂剂由以下组分组成：Ba0.9Sr0.1(Zr0.5Sn0.5)O3、Bi2Zr2O7、ZnO、Al2O3、ZrO2、Li2CO3和MnCO3，以及WO3、Nb2O5、Nd2O3、Sm2O3中至少一种。
进一步的，所述改性掺杂剂相对所述陶瓷介质材料按重量百分比计，由以下组分组成：BaxSr1-x(ZrySn1-y)O3 8～18％、Bi2Zr2O7 1～3％、ZnO 0.1～1.5％、Al2O3 0.01～0.3％、WO3 0～0.5％、Nb2O5 0～0.5％、ZrO2 0.1～0.3％、Li2CO3 0.01～0.05％、Nd2O3 0～0.75％、Sm2O3 0～0.75％和MnCO3 0.1～0.5％。
进一步的，所述改性掺杂剂相对所述陶瓷介质材料按重量百分比计，由以下组分组成：BaxSr1-x(ZrySn1-y)O3 8～10％、Bi2Zr2O7 1～3％、ZnO 1～1.5％、Al2O3 0.04～0.1％、WO3 0.2～0.5％、Nb2O5 0.1～0.4％、ZrO2 0.1～0.2％、Li2CO3 0.01～0.02％、Nd2O3 0～0.3％、Sm2O3 0～0.5％和MnCO3 0.1～0.3％。
本发明还保护所述高性能的陶瓷介质材料的制备方法，包括以下步骤：
A.获得BaTiO3；
B.按结构式BaxSr1-x(ZrySn1-y)O3的化学计量比称量BaCO3、SrCO3丶ZrO2、SnO2作为原料，将称量好的原料装入球磨罐中，加入去离子水进行研磨8～12小时，出料烘干、粉碎后在1200～1300℃下煅烧3～5小时合成BaxSr1-x(ZrySn1-y)O3烧块；
C.获得Bi2Zr2O7；
D.以步骤A获得的BaTiO3作为主成分，再称量步骤B获得的BaxSr1-x(ZrySn1-y)O3烧块，以及步骤C获得的Bi2Zr2O7，以及下列组分中的三种或三种以上：ZnO、Al2O3、WO3、Nb2O5、ZrO2、Li2CO3、Nd2O3、Sm2O3或MnCO3作为改性掺杂剂，将称量好的物料装入球磨罐中，加入去离子水进行研磨，再加入聚乙烯醇溶液作为粘合剂进行干燥造粒，获得所述的陶瓷介质材料。
进一步的，步骤A中BaTiO3按照以下方法获得，按结构式BaTiO3的化学计量比称量BaCO3、TiO2作为原料，将称量好的原料装入球磨罐中，加入去离子水进行研磨8～12小时，出料烘干、粉碎后在1200～1300℃下煅烧3～5小时；
步骤C中Bi2Zr2O7按照以下方法获得，按结构式Bi2Zr2O7的化学计量比称量Bi2O3、ZrO2作为原料，将称量好的原料装入球磨罐中，加入去离子水进行研磨8～12小时，出料烘干、粉碎后在700～1050℃下煅烧2～3小时。
本发明还保护一种陶瓷基片，所述陶瓷基片是将所述高性能的陶瓷介质材料，进行高温烧结得到，烧结温度为1250～1320℃，烧结时间为2.5～3.5小时。
一种陶瓷电元件，包含所述陶瓷基片。
有益效果：
本发明的瓷介电容器介质材料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BaTiO3、BaxSr1-x(ZrySn1-y)O3和Bi2Zr2O7，以及ZnO、Al2O3、WO3、Nb2O5、ZrO2、Li2CO3、Nd2O3、Sm2O3或MnCO3中的三种或三种以上的组分、含量的变化，陶瓷介质材料的介电常数可在15000～21000之间连续可调，能适应一定范围内的不同规格的Y5V特性瓷介电容器的制作要求，具有烧成温度低、更高耐电强度及合适的介电常数，更低容量温度变化率、可靠性高且环保的特点，是一种性能优越的瓷介电容器介质材料。
具体实施方式
下面将更详细地描述本发明的优选实施方式。虽然以下描述了本发明的优选实施方式，然而应该理解，可以以各种形式实现本发明而不应被这里阐述的实施方式所限制。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。在下面的实施例中，如未明确说明，“％”均指重量百分比。
实施例1
制备陶瓷介质材料，步骤如下：
A.按结构式BaTiO3的化学计量比称量电子级的BaCO3、TiO2作为原料，将称量好的原料装入球磨罐中，加入适量去离子水和氧化锆球进行研磨12小时，出料烘干、粉碎后在1250℃下煅烧3.5小时合成BaTiO3(简称BT)烧块；
B.按结构式Ba0.9Sr0.1(Zr0.5Sn0.5)O3的化学计量比称量电子级的BaCO3、SrCO3丶ZrO2、SnO2丶TiO2作为原料，将称量好的原料装入球磨罐中，加入适量去离子水和氧化锆球进行研磨12小时，出料烘干、粉碎后在1300℃下煅烧3.5小时合成Ba0.9Sr0.1(Zr0.5Sn0.5)O3(简称BSZS)烧块；
C.按结构式Bi2Zr2O7的化学计量比称量电子级的Bi2O3、丶ZrO2作为原料，将称量好的原料装入球磨罐中，加入适量去离子水和氧化锆球进行研磨8小时，出料烘干、粉碎后在1000℃下煅烧2.5小时合成Bi2Zr2O7(简称BZ)烧块；
D.按结构式BaTiO3(简称BT)烧块作为主成分，再称量Ba0.9Sr0.1(Zr0.5Sn0.5)O3(简称BSZS)、Bi2Zr2O7(简称BZ)烧块及ZnO、Al2O3、WO3、Nb2O5、ZrO2、Li2CO3、Nd2O3、Sm2O3、MnCO3作为改性掺杂剂，共计100％，各物质用量参见表1。将称量好的物料装入球磨罐中，加入适量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，再经加入聚乙烯醇溶液作为粘合剂进行干燥造粒，获得所述的陶瓷介质材料，材料经干压成型和烧结，烧结过程是8小时升温到1300℃，保温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，测试结果见表2。
实施例2-12
参照实施例中的方法制备材料，各物质用量见表1，测试结果见表2。
表1：陶瓷电容器介质材料组成表
表2：陶瓷电容器介质材料性能表
从表2可以看到，所述高性能的陶瓷介质材料的介电常数15000～21000可调,介质损耗≦0.75％，抗电强度≧5KVAc/mm，温度特性变化率符合Y5V标准，适用于制作Y5V特性瓷介电容器。
以上详细描述了本发明的优选实施方式，但是，本发明并不限于上述实施方式中的具体细节，在本发明的技术构思范围内，可以对本发明的技术方案进行多种简单变型，这些简单变型均属于本发明的保护范围。
另外需要说明的是，在上述具体实施方式中所描述的各个具体技术特征，在不矛盾的情况下，可以通过任何合适的方式进行组合。为了避免不必要的重复，本发明对各种可能的组合方式不再另行说明。
此外，本发明的各种不同的实施方式之间也可以进行任意组合，只要其不违背本发明的思想，其同样应当视为本发明所公开的内容。

Claims (6)

1.一种高性能的陶瓷介质材料，其特征在于：所述高性能的陶瓷介质材料由主成分和改性掺杂剂组成，所述主成分占总重的80～90％，所述改性掺杂剂占总重的10～20％，所述高性能的陶瓷介质材料的介电常数15000～21000可调，介质损耗≦0.75％，抗电强度≧5KVAc/mm，温度特性变化率符合Y5V标准，其中，所述主成分为BaTiO3；
所述改性掺杂剂包括BaxSr1-x(ZrySn1-y)O3，其中x＝0.2～0.9,y＝0.1～0.8，所述改性掺杂剂相对所述陶瓷介质材料按重量百分比计，由以下组分组成：BaxSr1-x(ZrySn1-y)O38～18％、Bi2Zr2O7 1～3％、ZnO 0.1～1.5％、Al2O30.01～0.3％、WO30～0.5％、Nb2O50～0.5％、ZrO2 0.1～0.3％、Li2CO3 0.01～0.05％、Nd2O3 0～0.75％、Sm2O3 0～0.75％和MnCO3 0.1～0.5％。
2.根据权利要求1所述高性能的陶瓷介质材料，其特征在于：所述改性掺杂剂包括BaxSr1-x(ZrySn1-y)O3，其中x＝0.6～0.9，y＝0.4～0.6。
3.一种权利要求1或2所述高性能的陶瓷介质材料的制备方法，其特征在于：包括以下步骤：
A.获得BaTiO3；
B.按结构式BaxSr1-x(ZrySn1-y)O3的化学计量比称量BaCO3、SrCO3丶ZrO2、SnO2作为原料，将称量好的原料装入球磨罐中，加入去离子水进行研磨8～12小时，出料烘干、粉碎后在1200～1300℃下煅烧3～5小时合成BaxSr1-x(ZrySn1-y)O3烧块；
C.获得Bi2Zr2O7；
D.以步骤A获得的BaTiO3作为主成分，再称量步骤B获得的BaxSr1-x(ZrySn1-y)O3烧块，以及步骤C获得的Bi2Zr2O7，以及下列组分：ZnO、Al2O3、WO3、Nb2O5、ZrO2、Li2CO3、Nd2O3、Sm2O3和MnCO3作为改性掺杂剂，将称量好的物料装入球磨罐中，加入去离子水进行研磨，再加入聚乙烯醇溶液进行干燥造粒，获得所述高性能的陶瓷介质材料。
4.根据权利要求3所述高性能的陶瓷介质材料的制备方法，其特征在于：步骤A中BaTiO3按照以下方法获得，按结构式BaTiO3的化学计量比称量BaCO3、TiO2作为原料，将称量好的原料装入球磨罐中，加入去离子水进行研磨8～12小时，出料烘干、粉碎后在1200～1300℃下煅烧3～5小时；
步骤C中Bi2Zr2O7按照以下方法获得，按结构式Bi2Zr2O7的化学计量比称量Bi2O3、ZrO2作为原料，将称量好的原料装入球磨罐中，加入去离子水进行研磨8～12小时，出料烘干、粉碎后在700～1050℃下煅烧2～3小时。
5.一种陶瓷基片，其特征在于：所述陶瓷基片是将权利要求1或2所述高性能的陶瓷介质材料，进行高温烧结得到，烧结温度为1250～1320℃，烧结时间为2.5～3.5小时。
6.一种陶瓷电元件，包含权利要求5所述陶瓷基片。
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