CN107226696A - X7R型BaTiO3基电容器陶瓷材料及其制备方法 - Google Patents

X7R型BaTiO3基电容器陶瓷材料及其制备方法 Download PDF

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CN107226696A
CN107226696A CN201710358505.9A CN201710358505A CN107226696A CN 107226696 A CN107226696 A CN 107226696A CN 201710358505 A CN201710358505 A CN 201710358505A CN 107226696 A CN107226696 A CN 107226696A
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孙华君
胡伟
高文秋
董海泉
尹长霞
廖园富
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Shandong Wei Breaking Electronic Technology Co Ltd
Zibo Advanced High Tech Industrial Development Zone Advanced Ceramics Research Institute
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Zibo Advanced High Tech Industrial Development Zone Advanced Ceramics Research Institute
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Abstract

本发明属于电子信息技术领域，具体涉及一种X7R型BaTiO3基电容器陶瓷材料及其制备方法。包括以下质量份数的原料：BaTiO394～97份、CaZrO31.5～3份、Ta2O50.5～1份、Nb2O51～1.5份、MnCO30.1～0.3份和MgO 0.2～0.5份。本发明在‑55℃～125℃范围内满足容温变化率≤15％，具有较高的介电常数、低的介电损耗且环境友好、烧结范围宽、性能重复性好。本发明还提供其制备方法，配方简单可调、烧结范围宽、性能重复性好、成本低、易于工业化生产。

Description

X7R型BaTiO3基电容器陶瓷材料及其制备方法
技术领域
本发明属于电子信息技术领域，具体涉及一种X7R型BaTiO3基电容器陶瓷材料及其制备方法。
背景技术
随着信息技术的迅猛发展，整机产业制备如以平板显示、手机以及汽车等为代表的新型电子产品的不断涌现，使其对电容器的性能要求更加严格。片式多层陶瓷电容器(Multilayer Ceramic Capacitor，MLCC)具有体积小、比容量大、抗湿性好、等效串联电阻小、高可靠和耐高温等优点，从而成为目前使用量最大、发展速度最快的片式元器件之一。X7R型MLCC是指电容器在测试频率1KHz、测试电压1V下，满足-55～125℃区间内容温变化率≤15％，介电损耗≤2.0％。主要分为三大类：(a)铅系弛豫类铁电材料；(b)BaTiO3系材料；(c)铅系和BaTiO3系复合材料。由于铅存在严重的环境污染问题，使得BaTiO3基电容器陶瓷材料受到了广泛的关注并具有广阔的应用前景。
BaTiO3在室温下具有较低的介电常数，主要通过添加Nb、Ta、Co、Zn、Sm、Mn、Mg、Dy、Yb等元素来改性BaTiO3基陶瓷材料，其烧结温度一般较高(＞1300℃)。为了降低烧结温度，通常用低温玻璃、二氧化硅和氧化硼等作为烧结助剂，其中低温玻璃的制备工艺复杂且周期较长，而且会造成材料的介电损耗变大。目前X7R型MLCC材料的制备方法存在制备工艺复杂、介电常数较低和损耗偏大的问题。
发明内容
针对现有技术的不足，本发明的目的是提供一种X7R型BaTiO3基电容器陶瓷材料，在-55℃～125℃范围内满足容温变化率≤15％，具有较高的介电常数、低的介电损耗且环境友好、烧结范围宽、性能重复性好，本发明还提供其制备方法，工艺简单，成本低，易于工业化生产。
本发明所述的X7R型BaTiO3基电容器陶瓷材料，包括以下质量份数的原料：
本发明所述的X7R型BaTiO3基电容器陶瓷材料的制备方法，包括以下步骤：
(1)将BaTiO3粉体、CaZrO3粉体与Ta2O5、Nb2O5、MnCO3、MgO混合，与去离子水混合球磨后烘干，得到陶瓷粉末；
(2)在陶瓷粉末中加入粘结剂，造粒、过筛、压片、排胶，随后烧结、保温，得到陶瓷样品，抛光后制得X7R型BaTiO3基电容器陶瓷材料。
其中：
BaTiO3粉体的制备方法为：将BaCO3和TiO2按照BaTiO3的化学计量比1:1配料，与去离子水混合球磨后烘干，然后升温至1100～1150℃煅烧3～5小时，随炉冷却，制得BaTiO3粉体。BaTiO3粉体的制备方法中的升温速率为2～5℃/分钟。
CaZrO3粉体的制备方法为：将CaCO3和ZrO2按照CaZrO3的化学计量比1:1配料，与去离子水混合球磨后烘干，然后升温至1400～1450℃煅烧3～5小时，随炉冷却，制得CaZrO3粉体。CaZrO3粉体的制备方法中的升温速率为2～5℃/分钟。
通过采用上述方法制备的BaTiO3粉体、CaZrO3粉体，在高温段的温度稳定性更好。
球磨时间为4～12小时。
粘结剂添加质量为陶瓷粉末的4％～7％。
粘结剂为PVA粘结剂，浓度为3～5wt％。
步骤(2)中过筛后的粒径≤150μm。
步骤(2)中的烧结为升温至1200～1280℃烧结；保温为保温2～4小时。
步骤(2)中的排胶温度为600～700℃，升温速率为1～2℃/分钟，保温时间2小时。
制备得到的X7R型BaTiO3基电容器陶瓷材料可以制备银电极，用小毛刷在陶瓷的上下表面涂银浆，在烘箱中100℃下烘干，最后在马弗炉中500℃烧结30分钟，制得产品。
综上所述，本发明具有以下优点：
(1)通过同时添加Ta2O5和Nb2O5改善陶瓷材料的容温变化率，同时增宽了烧结温度范围(1200～1280℃)。
(2)通过添加CaZrO3和MgO提高陶瓷材料125℃处的介电常数，并降低高温端介电损耗。
(3)本发明所述的X7R型BaTiO3基电容器陶瓷材料介电损耗低，室温下介电损耗为0.0085～0.0110。
(4)本发明所述的材料体系不含铅，属于环境友好型，具有良好的应用前景；且制备方法工艺简单、可控，便于工业化生产。
(5)本发明所述的材料在-55℃～125℃范围内满足容温变化率≤15％，具有较高的介电常数、低的介电损耗且环境友好、烧结范围宽、性能重复性好。
(6)本发明还提供其制备方法，配方简单可调、烧结范围宽、性能重复性好、工艺简单、成本低、易于工业化生产。
附图说明
图1是实施例1制备的X7R型BaTiO3基电容器陶瓷材料的XRD图谱；
图2是实施例1制备的X7R型BaTiO3基电容器陶瓷材料的SEM图谱；
图3是实施例1制备的X7R型BaTiO3基电容器陶瓷材料在1KHz时的介电常数和介电损耗随温度的变化图谱；
图4是实施例1制备的X7R型BaTiO3基电容器陶瓷材料在1KHz时的容温变化率(以25℃为基准)随温度的变化图。
具体实施方式
下面结合实施例对本发明做进一步说明。
实施例1
(1)将BaCO3和TiO2按照BaTiO3的化学计量比1:1配料，与去离子水混合球磨6小时后烘干，然后升温至1100℃煅烧4小时，随炉冷却，制得BaTiO3粉体；
(2)将CaCO3和ZrO2按照CaZrO3的化学计量比1:1配料，与去离子水混合球磨6小时后烘干，然后升温至1420℃煅烧4小时，随炉冷却，制得CaZrO3粉体；
(3)将BaTiO3、CaZrO3、Ta2O5、Nb2O5、MnCO3、MgO按质量比96：2：0.7：1：0.2：0.3配料，与去离子水混合球磨4小时后烘干，得到陶瓷粉末。
(4)将步骤(3)得到的陶瓷粉末外加质量比5％的PVA粘结剂，造粒、过筛、压片，制得直径为12mm、厚度1mm～1.5mm的陶瓷胚体。陶瓷胚体在600℃下保温2小时排胶，随后升温至1240℃烧结，保温3小时，抛光后得到X7R型BaTiO3基电容器陶瓷材料。
将实施例1制备的X7R型BaTiO3基电容器陶瓷材料样品抛光后进行XRD测试，XRD图谱如图1所示，分析表明：其结构为完整的立方钙钛矿结构，没有发现杂峰。
将实施例1制备的X7R型BaTiO3基电容器陶瓷材料样品热处理后进行SEM测试，SEM图谱如图2所示，分析表明：陶瓷材料的微观结构致密度较好，晶粒尺寸较小，约为300nm。
将实施例1制备的X7R型BaTiO3基电容器陶瓷材料样品抛光制备银电极后测试其介电性能，得到其1KHz下介电常数和介电损耗随温度的变化图谱(图3)和容温变化率(以25℃为基准)随温度的变化图(图4)，图4中虚线内为容温变化率不超过±15％的范围。由图3和图4可以得到：本发明的陶瓷材料在-55～125℃的温度范围内具有优良的温度稳定性(ΔC/C25℃<11％)，符合X7R型多层陶瓷电容器材料的要求；在-55～125℃温度范围内的介电损耗较低，其中25℃的介电常数和介电损耗分别为3039和0.0089。
实施例2
(1)将BaCO3和TiO2按照BaTiO3的化学计量比1:1配料，与去离子水混合球磨6小时后烘干，然后升温至1125℃煅烧4小时，随炉冷却，制得BaTiO3粉体；
(2)将CaCO3和ZrO2按照CaZrO3的化学计量比1:1配料，与去离子水混合球磨6小时后烘干，然后升温至1400℃煅烧4小时，随炉冷却，制得CaZrO3粉体；
(3)将BaTiO3、CaZrO3、Ta2O5、Nb2O5、MnCO3、MgO按质量比95：3：0.6：1：0.1：0.2配料，与去离子水混合球磨8小时后烘干，得到陶瓷粉末。
(4)将步骤(3)得到的陶瓷粉末外加质量比3％的PVA粘结剂，造粒、过筛、压片，制得直径为12mm、厚度1mm～1.5mm的陶瓷胚体。陶瓷胚体在650℃下保温2小时排胶，随后升温至1220℃烧结，保温4小时，得到X7R型BaTiO3基电容器陶瓷材料。
实施例3
(1)将BaCO3和TiO2按照BaTiO3的化学计量比1:1配料，与去离子水混合球磨6小时后烘干，然后升温至1150℃煅烧4小时，随炉冷却，制得BaTiO3粉体；
(2)将CaCO3和ZrO2按照CaZrO3的化学计量比1:1配料，与去离子水混合球磨6小时后烘干，然后升温至1450℃煅烧4小时，随炉冷却，制得CaZrO3粉体；
(3)将BaTiO3、CaZrO3、Ta2O5、Nb2O5、MnCO3、MgO按质量比96：1.5：0.8：1.2：0.3：0.5配料，与去离子水混合球磨12小时后烘干，得到陶瓷粉末。
(4)将步骤(3)得到的陶瓷粉末外加质量比4％的PVA粘结剂，造粒、过筛、压片，制得直径为12mm、厚度1mm～1.5mm的陶瓷胚体。陶瓷胚体在600℃下保温2小时排胶，随后升温至1260℃烧结，保温2小时，得到X7R型BaTiO3基电容器陶瓷材料。
对实施例2和实施例3制备的X7R型BaTiO3基电容器陶瓷材料在25℃和1KHz条件下进行介电性能测试，结果如表1所示。
表1

Claims (9)

1.一种X7R型BaTiO3基电容器陶瓷材料，其特征在于：包括以下质量份数原料：
2.一种权利要求1所述的X7R型BaTiO3基电容器陶瓷材料的制备方法，其特征在于：包括以下步骤：
(1)将BaTiO3粉体、CaZrO3粉体与Ta2O5、Nb2O5、MnCO3、MgO混合，与去离子水混合球磨后烘干，得到陶瓷粉末；
(2)在陶瓷粉末中加入粘结剂，造粒、过筛、压片、排胶，随后烧结、保温，得到陶瓷样品，抛光后制得X7R型BaTiO3基电容器陶瓷材料。
3.根据权利要求2所述的X7R型BaTiO3基电容器陶瓷材料的制备方法，其特征在于：
BaTiO3粉体的制备方法为：将BaCO3和TiO2按照BaTiO3的化学计量比1:1配料，与去离子水混合球磨后烘干，然后升温至1100～1150℃煅烧3～5小时，随炉冷却，制得BaTiO3粉体；
CaZrO3粉体的制备方法为：将CaCO3和ZrO2按照CaZrO3的化学计量比1:1配料，与去离子水混合球磨后烘干，然后升温至1400～1450℃煅烧3～5小时，随炉冷却，制得CaZrO3粉体。
4.根据权利要求3所述的X7R型BaTiO3基电容器陶瓷材料的制备方法，其特征在于：BaTiO3粉体的制备方法中的升温速率为2～5℃/分钟；CaZrO3粉体的制备方法中的升温速率为2～5℃/分钟。
5.根据权利要求2、3或4所述的X7R型BaTiO3基电容器陶瓷材料的制备方法，其特征在于：球磨时间为4～12小时。
6.根据权利要求2、3或4所述的X7R型BaTiO3基电容器陶瓷材料的制备方法，其特征在于：粘结剂添加质量为陶瓷粉末的4％～7％。
7.根据权利要求2、3或4所述的X7R型BaTiO3基电容器陶瓷材料的制备方法，其特征在于：粘结剂为PVA粘结剂，浓度为3～5wt％。
8.根据权利要求2、3或4所述的X7R型BaTiO3基电容器陶瓷材料的制备方法，其特征在于：步骤(2)中的烧结为升温至1200～1280℃烧结；保温为保温2～4小时。
9.根据权利要求2、3或4所述的X7R型BaTiO3基电容器陶瓷材料的制备方法，其特征在于：步骤(2)中的排胶温度为600～700℃，升温速率为1～2℃/分钟，保温时间2小时。
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