CN108117385B - 一种大尺寸高耐电强度氧化钛基介质陶瓷材料及其制备方法和应用 - Google Patents

一种大尺寸高耐电强度氧化钛基介质陶瓷材料及其制备方法和应用 Download PDF

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CN108117385B
CN108117385B CN201711431333.XA CN201711431333A CN108117385B CN 108117385 B CN108117385 B CN 108117385B CN 201711431333 A CN201711431333 A CN 201711431333A CN 108117385 B CN108117385 B CN 108117385B
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陈莹
张文斌
李鑫
江峰
黄叶
董显林
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Shanghai Institute of Ceramics of CAS
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Abstract

本发明涉及一种大尺寸高耐电强度氧化钛基介质陶瓷材料及其制备方法和应用，所述氧化钛基介质陶瓷材料的组成配方包括：a CaTiO3+b SrTiO3+c TiO2+d Al2TiO5+e SiO2，其中a、b、c、d、e为各组分的摩尔百分比，15≤a≤35mol%，0≤b≤2mol%，30≤c≤84mol%，0.5≤d≤25 mol%，0.5≤e≤15 mol%，a+b+c+d+e=100 mol%。

Description

一种大尺寸高耐电强度氧化钛基介质陶瓷材料及其制备方法 和应用
技术领域
本发明涉及一种大尺寸高耐电强度氧化钛基介质陶瓷材料及其制备方法和应用，属于电子陶瓷材料技术领域。
背景技术
固态重复频率脉冲技术在军事(强脉冲激光、高功率微波、电磁脉冲武器等)、科学研究(粒子束惯性约束聚变、电子束加速器、强X射线技术等)、工业(化学工业、石油工业等)，以及生物医学和环境保护等诸多领域显示出十分诱人的应用前景。因此，固态传输介质受到国际科技界的广泛关注。
当前的固态传输介质有三种：有机物+陶瓷颗粒复合材料、玻璃陶瓷和陶瓷三种。有机物通常具有非常高的耐电强度(≥100kV/mm)，有机物+陶瓷颗粒复合材料也相应具有高的耐电强度，但因有机和无机材料界面不匹配同时存在热膨胀系数差异很大，其介电损耗很大，且介电性能随温度和频率变化明显。玻璃陶瓷虽然耐电强度和介电常数相对较高，但是存在介电性能和力学性能稳定性差、界面极化导致实际储能密度偏低等问题。陶瓷介质具有介电常数高且可调、介电损耗低、放电速度快、使用温度范围宽、耐腐蚀等优点，是固态传输介质的首先材料，但传统的陶瓷体系其耐电强度相对较低。如典型的TiO2陶瓷，常温下介电常数90，但其耐电强度只有25kV/mm，满足不了实际应用的需要。
发明内容
针对上述问题，本发明的目的在于提供一种兼具高耐电强度、适中介电常数、低介电损耗且介电性能随温度和频率稳定性好的介质陶瓷体系。
一方面，本发明提供了一种大尺寸高耐电强度氧化钛基介质陶瓷材料，所述氧化钛基介质陶瓷材料的组成配方包括：a CaTiO3+b SrTiO3+cTiO2+d Al2TiO5+e SiO2，其中a、b、c、d、e为各组分的摩尔百分比，15≤a≤35mol％，0≤b≤2mol％，30≤c≤84mol％，0.5≤d≤25mol％，0.5≤e≤15mol％，a+b+c+d+e＝100mol％。
本发明中，所述氧化钛基介质陶瓷材料的组成配方为：a CaTiO3+b SrTiO3+c TiO2+d Al2TiO5+e SiO2(15≤a≤35mol％，0≤b≤2mol％，30≤c≤84mol％，0.5≤d≤25mol％，0.5≤e≤15mol％)。CaTiO3、SrTiO3和TiO2陶瓷材料是当前最经典的三种材料，它们具有相当高的介电常数和较好的耐电强度。CaTiO3陶瓷介电常数～110，耐电强度20kV/mm；SrTiO3陶瓷介电常数～300，耐电强度10kV/mm；TiO2介电常数～90，耐电强度25kV/mm。Al2TiO5虽然介电常数不高，但力学强度很高，在氧化钛基的陶瓷基体中可以起到钉扎作用。SiO2的介电常数～4，其耐电强度非常高～480kV/mm，同时具有优异的介电频率稳定性，另外，它可作为烧结助剂，降低烧结温度，提高陶瓷的致密度和力学强度，从而增强陶瓷整体的耐电强度。这样利用氧化钛基材料的高的介电常数，氧化硅和钛酸铝低的介电常数，材料的介电常数可以实现在很宽范围内调节。通过改变这五种化合物的化学计量比结合最优热处理工艺，可望实现介电常数在宽范围内调节，耐电强度(抗电强度)高，且介电常数和介电损耗的温度、频率稳定性良好。介电常数的大小决定脉冲发生器输出的脉冲宽度，耐电强度决定了应用器件的最终加速场强和高压承受能力，良好的稳定性是保证脉冲输出波形稳定的必要条件，从而确保脉冲系统的正常运行。
较佳地，所述的氧化钛基介质陶瓷材料可至少实现一个维度上的尺寸≥300mm，优选为＞400mm。
较佳地，所述氧化钛基介质陶瓷材料的耐击穿强度为40～48kV/mm，介电常数在50～150可调，介电损耗＜0.003。
另一方面，本发明还提供了一种如上述的大尺寸高耐电强度氧化钛基介质陶瓷材料的制备方法，包括：
按照化学组成称取Ca源、Ti源、Sr源、Si源和Al源混合并进行预烧，得到混合粉体；
将粘结剂加入所得混合粉体中后喷雾造粒，并压制成型，得到生坯；
将所得生坯在1220～1350℃下进行烧结，得到所述大尺寸高耐电强度氧化钛基介质陶瓷材料。
较佳地，所述Ca源为CaO、CaCO3和CaTiO3中的至少一种，所述Ti源为TiO2、SrTiO3、AlTiO3、CaTiO3中的至少一种，所述Sr源为SrO、SrTiO3和SrCO3中的至少一种，所述Si源为SiO2，所述Al源为Al2O3或/和Al2TiO5。
较佳地，所述预烧的温度为1000℃～1150℃，时间为2～12小时。其中，预烧时间随配制粉体的质量增加而延长。
较佳地，所述混合粉体的粒径为0.2～1μm。
较佳地，所述粘结剂为聚乙烯醇、聚乙烯醇缩丁醛和甲基纤维素中的至少一种，加入量为混合粉体总质量的0.2～1wt％，优选为0.5～1wt％。较佳地，所述成型方式为等静压成型，所述等静压成型的压力为180～300MPa。
较佳地，所述烧结时间为2～24小时。
第三方面，本发明还提供了一种如上所述的尺寸高耐电强度氧化钛基介质陶瓷材料在制备小容量高频电容器中的应用。
第四方面，本发明还提供了一种如上所述的尺寸高耐电强度氧化钛基介质陶瓷材料在制备脉冲形成线中的应用。
与现有技术相比，本发明采用传统固相法制得了大尺寸(所述氧化钛基介质陶瓷材料在至少一个维度上的尺寸高达300mm，例如：长达300mm，宽达15mm，厚度达3mm的长方体)介质陶瓷材料，且所制得的介质陶瓷材料的耐击穿强度可达到48kV/mm，介电常数可达到50～250，介电损耗小于0.003，非常适用于制作小容量高频电容器，固态脉冲形成线，基板等，可应用于脉冲发生器、移相器、滤波器、振荡器、共振器及相控阵天线等电子设备；且所述材料具有频率稳定性好、耐高压、无铅环保、制备工艺简单等优点，具有显著性应用价值。
附图说明
图1为本发明实施例1-4制备的陶瓷微波性能标准片照片；
图2为本发明实施例1-4制备的陶瓷介电常数/介电损耗标准片照片；
图3为本发明实施例1-4制备的陶瓷介电强度标准片照片；
图4为本发明实施例1制备的长方体陶瓷片；
图5为本发明实施例1制备的陶瓷材料的断面抛光热腐蚀微观形貌图；
图6为本发明实施例1制备的陶瓷标准片的介电频谱图；
图7为本发明实施例1制备的长方体陶瓷片的介电频谱图；
图8为本发明实施例1制备的陶瓷标准片的介电强度随电压变化图；
图9为本发明实施例1制备的陶瓷标准片介电强度随厚度的变化图；
图10为本发明实施例2制备的陶瓷标准片的介电频谱图；
图11为本发明实施例3制备的陶瓷标准片的介电频谱图；
图12为本发明实施例4制备的陶瓷标准片的介电频谱图；
图13为本发明实施例1-4制备的陶瓷XRD图谱。
具体实施方式
以下通过下述实施方式进一步说明本发明，应理解，下述实施方式仅用于说明本发明，而非限制本发明。
本发明针对现有技术所存在的问题和市场需求，本发明了提供一种高电压下可供储能和脉冲成形的大尺寸氧化钛基介质陶瓷材料，包括如下组成配方：a CaTiO3+b SrTiO3+cTiO2+d Al2TiO5+e SiO2，其中a、b、c、d、e为各组分的摩尔百分比，15≤a≤35mol％，0≤b≤2mol％，30≤c≤84mol％，0.5≤d≤25mol％，0.5≤e≤15mol％，a+b+c+d+e＝100mol％。
本发明制备的氧化钛基介质陶瓷材料的耐击穿强度可达到40-48kV/mm，介电常数50～250可调，介电损耗小于0.003。且本发明制备的氧化钛基介质陶瓷材料在至少一个维度上的尺寸高达300mm。
以下示例性地说明本发明提供的氧化钛基介质陶瓷材料的制备方法。
按照氧化钛基介质陶瓷材料的化学组成称取Ca源、Ti源、Sr源、Si源和Al源并混合并进行预烧，得到混合粉体。其中氧化钛基介质陶瓷材料的化学组成包括(15～35)mol％CaTiO3+(0～2)mol％SrTiO3+(30～84)mol％TiO2+(0.5～25)mol％Al2TiO5+(0.5～15)mol％SiO2。所述预烧的温度1000℃～1150℃，时间为2～12小时。所得混合粉体的平均颗粒度为0.02～4μm。所述Ca源可为CaO、CaCO3和CaTiO3中的至少一种。所述Ti源可为TiO2、SrTiO3、Al2TiO5、CaTiO3中的至少一种。所述Sr源可为SrO、SrTiO3和SrCO3中的至少一种。所述Si源可为SiO2。所述Al源可为Al2O3或/和AlTiO3。
将粘结剂加入所得混合粉体中后喷雾造粒，并压制成型，得到生坯。所述粘结剂可为聚乙烯醇、聚乙烯醇缩丁醛和甲基纤维素中的至少一种，其加入量可为混合粉体总质量的0.2～5wt％，优选0.5～1wt％。所述成型方式可为等静压成型等。所述等静压成型的压力可为180～300MPa。作为一个示例，在混合粉体中加入粘结剂，进行喷雾造粒后在180～300MPa的压强下等静压成型的方式压制成生坯。
将制得的生坯在1220～1350℃下进行烧结，然后冷却到室温，即得所述的大尺寸的氧化钛基介质陶瓷材料。所述烧结时间可为2～24小时。
本发明采用传统固相法制备所述氧化钛基介质陶瓷材料，非常适用于制作小容量高频电容器，固态脉冲形成线，基板等，可应用于脉冲发生器、移相器、滤波器、振荡器、共振器及相控阵天线等电子设备；且所述材料还具有无铅环保、制备工艺简单等优点。
下面进一步例举实施例以详细说明本发明。同样应理解，以下实施例只用于对本发明进行进一步说明，不能理解为对本发明保护范围的限制，本领域的技术人员根据本发明的上述内容作出的一些非本质的改进和调整均属于本发明的保护范围。下述示例具体的工艺参数等也仅是合适范围中的一个示例，即本领域技术人员可以通过本文的说明做合适的范围内选择，而并非要限定于下文示例的具体数值。
实施例1
按25mol％CaTiO3+61mol％TiO2+8mol％Al2TiO5+6mol％SiO2配方称量CaCO3、TiO2、SiO2和Al2O3各组成原料，以水为介质、玛瑙球为磨介，湿法球磨12h后，出料、烘干，将得到的粉料在1100℃下预烧4h。再次进行湿法球磨，烘干后得到颗粒度为0.02～4μm的混合粉体；向所得混合粉体中加入重量为混合粉体总重量的0.8％聚乙烯醇(PVA)进行喷雾造粒，然后在200MPa的等静压下压制成生坯；将所得生坯在1250℃下烧结20h，然后自然冷却到室温，即得陶瓷块体；将所得陶瓷块体经切割、细磨加工，分别得到直径6mm×厚3mm和直径30mm×厚0.1～1mm的圆柱体陶瓷片，长300mm×宽15mm×厚3mm的长方体陶瓷片，将所得陶瓷片被银电极烧银后分别用于微波性能测试(如图1)，介电性能(如图2)，介电强度测试(如图3)和脉冲形成线(如图4)。图5为本实施例所得陶瓷材料的断面抛光腐蚀后微观形貌图，由图5可见：所得陶瓷材料的晶相混合均匀，致密，无裂纹。图6为本实施例中的陶瓷标准片(直径30mm，厚1mm)的介电频谱图，由图6可见：所得陶瓷材料在100Hz～1MHz频率范围，其介电常数在102左右，随频率基本不变；介电损耗小于0.003。图7为本实施例中的长方体陶瓷片(长300mm×宽15mm×厚3mm)的介电频谱图，由图7可见，所得陶瓷材料在100Hz～1MHz频率范围，其介电常数在113左右，随频率基本不变；介电损耗小于0.0012。表1为该实施例中的圆柱体陶瓷片(直径6mm×厚3mm)的微波性能测试数据。可以看出本陶瓷材料具有优异的频率特性，在7GHz介电常数依然不变，损耗很小。
表1为该实施例中的圆柱体陶瓷片(直径6mm×厚3mm)的微波性能测试数据：
Figure BDA0001524938330000051
。
图8为本实施例中的陶瓷标准片(直径30mm，厚1mm)的介电性能随电压的变化图，由图8可见。所得陶瓷材料在电场下介电性能稳定，随着电压的增加，其表征电容和损耗基本保持不变(电容～53.5pF，表征损耗～0.008)，实质为介电常数和介电损耗基本不变。图9为本实施例中的陶瓷介电强度随厚度的变化图，由图9可见：所得陶瓷材料随着厚度的剪薄，介电强度(Eb)呈非线性上升，从48kV/mm(@1mm)提高到90kV/mm(@0.1mm)。
实施例2
按22mol％CaTiO3+76.8mol％TiO2+0.2mol％SrTiO3+0.5mol％Al2TiO5+0.5mol％SiO2配方称量CaCO3、SrCO3、TiO2、SiO2和Al2O3各组成原料，以水为介质、玛瑙球为磨介，湿法球磨24h后，出料、烘干，将得到的粉料在1100℃下预烧4h；再次进行湿法球磨，烘干后得到颗粒度为0.2～2μm的混合粉体；向所得混合粉体中加入重量为混合粉体总重量的0.5％聚乙烯醇(PVA)进行喷雾造粒，然后在200MPa的等静压下压制成生坯；将所得生坯在1310℃下烧结6h，然后自然冷却到室温，即得陶瓷块体。
图10为本实施例中的陶瓷标准片(直径30mm，厚1mm)的介电频谱图，由图10可见：所得陶瓷材料在100Hz～1MHz频率范围，其介电常数和介电损耗基本不变，介电常数在137.5左右，介电损耗小于0.002。
实施例3
按29mol％CaTiO3+41mol％TiO2+12mol％Al2TiO5+18mol％SiO2配方称量CaCO3、TiO2、SiO2和Al2O3各组成原料，以水为介质、玛瑙球为磨介，湿法球磨24h后，出料、烘干，将得到的粉料在1100℃下预烧4h；再次进行湿法球磨，烘干后得到颗粒度为0.2～2μm的混合粉体；向所得混合粉体中加入重量为混合粉体总重量的0.8％聚乙烯醇(PVA)进行喷雾造粒，然后在200MPa的等静压下压制成生坯；将所得生坯在1220℃下烧结24h，然后自然冷却到室温，即得陶瓷块体。
图11为本实施例中的陶瓷标准片(直径30mm，厚1mm)的介电频谱图，由图11可见：所得陶瓷材料在100Hz～1MHz频率范围，其介电常数和介电损耗基本不变，介电常数在80左右，介电损耗小于0.003。
实施例4
按18mol％CaTiO3+49mol％TiO2+20mol％Al2TiO5+13mol％SiO2配方称量CaCO3、SrCO3、TiO2、SiO2和Al2O3各组成原料，以水为介质、玛瑙球为磨介，湿法球磨24h后，出料、烘干，将得到的粉料在1050℃下预烧4h；再次进行湿法球磨，烘干后得到颗粒度为0.2～2μm的混合粉体；向所得混合粉体中加入重量为混合粉体总重量的0.5％聚乙烯醇(PVA)进行喷雾造粒，然后在200MPa的等静压下压制成生坯；将所得生坯在1240℃下烧结6h，然后自然冷却到室温，即得陶瓷块体。
图12为本实施例中的陶瓷标准片(直径30mm，厚1mm)的介电频谱图，由图12可见：所得陶瓷材料在100Hz～1MHz频率范围，其介电常数和介电损耗基本不变，介电常数在70左右，介电损耗小于0.0025。
表2为上述实施例所得圆柱体陶瓷陶瓷片(直径30mm×厚1mm)的组分及在100Hz～1MHz频率范围时其介电常数和介电损耗，和耐电强度：
Figure BDA0001524938330000071
。
综上实验结果可见：本发明采用传统固相法可制得大尺寸(例如：长达300mm，宽达15mm，厚度达1mm的长方体)介质陶瓷材料，且所制得的介质陶瓷材料的耐击穿强度可达48kV/mm，介电常数50～250可调，介电损耗小于0.003，非常适用于制作小容量高频电容器，脉冲形成线，可应用于高功率微波、高功率激光和X光机的驱动源中的脉冲发生器或移相器、滤波器、振荡器、共振器及相控阵天线等器件；且所述材料具有频率稳定性好、耐高压、无铅环保、制备工艺简单等优点，具有显著性应用价值。
最后有必要在此说明的是：以上实施例只用于对本发明的技术方案作进一步详细地说明，不能理解为对本发明保护范围的限制，本领域的技术人员根据本发明的上述内容作出的一些非本质的改进和调整均属于本发明的保护范围。

Claims (9)

1.一种大尺寸高耐电强度氧化钛基介质陶瓷材料，其特征在于，所述氧化钛基介质陶瓷材料的组成配方由以下组成：a CaTiO3+b SrTiO3+c TiO2+d Al2TiO5+e SiO2，其中a、b、c、d、e为各组分的摩尔百分比，15≤a≤35mol%，0≤b≤2mol%，30≤c≤84mol%，0.5≤d≤25mol%，0.5≤e≤15 mol%，a+b+c+d+e=100 mol%；所述氧化钛基介质陶瓷材料的耐击穿强度为40～48 kV/mm，介电常数在50～150可调，介电损耗＜0.003。
2.根据权利要求1所述的氧化钛基介质陶瓷材料，其特征在于，所述的氧化钛基介质陶瓷材料在至少一个维度上的长度为≥300 mm。
3.一种如权利要求1或2所述的大尺寸高耐电强度氧化钛基介质陶瓷材料的制备方法，其特征在于，包括：
按照化学组成称取Ca源、Ti源、Sr源、Si源和Al源混合并进行预烧，得到混合粉体；
将粘结剂加入所得混合粉体中后喷雾造粒，并压制成型，得到生坯；
将所得生坯在1220～1350℃下进行烧结，得到所述大尺寸高耐电强度氧化钛基介质陶瓷材料。
4.根据权利要求3所述的制备方法，其特征在于，所述Ca源为CaO、CaCO3和CaTiO3中的至少一种，所述Ti源为TiO2、SrTiO3、Al2TiO5、CaTiO3中的至少一种，所述Sr源为SrO、SrTiO3和SrCO3中的至少一种，所述Si源为SiO2，所述Al源为Al2O3或/和Al2TiO5。
5.根据权利要求3所述的制备方法，其特征在于，所述预烧的温度为1000℃～1150℃，时间为2～12小时。
6.根据权利要求3所述的制备方法，其特征在于，所述粘结剂为聚乙烯醇、聚乙烯醇缩丁醛和甲基纤维素中的至少一种，加入量为混合粉体总质量的0.2～5wt%。
7.根据权利要求3-6中任一项所述的制备方法，其特征在于，烧结时间为2～24小时。
8.一种如权利要求1或2所述的大尺寸高耐电强度氧化钛基介质陶瓷材料在制备小容量高频电容器中的应用。
9.一种如权利要求1或2所述的大尺寸高耐电强度氧化钛基介质陶瓷材料在制备脉冲形成线中的应用。
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