CN114409397B - 一种低tcr陶瓷芯片电阻及其材料和制备 - Google Patents

一种低tcr陶瓷芯片电阻及其材料和制备 Download PDF

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CN114409397B
CN114409397B CN202210085460.3A CN202210085460A CN114409397B CN 114409397 B CN114409397 B CN 114409397B CN 202210085460 A CN202210085460 A CN 202210085460A CN 114409397 B CN114409397 B CN 114409397B
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李志成
方超
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Abstract

本发明涉及一种低TCR陶瓷电阻材料，该陶瓷电阻材料的化学通式为(Sn1‑xSbxO2)(Bi8TiO14)y(Sb2O3)w，其中0.03≤x≤0.07，0＜y≤0.2，0≤w≤0.1。本发明还涉及一种低TCR陶瓷芯片电阻及其制备方法，所述低TCR陶瓷芯片电阻包括瓷体和设于瓷体两表面的电极，所述瓷体采用所述陶瓷电阻材料。本发明所述陶瓷电阻材料的原料来源广且成本低，制得电阻的室温电阻率可调节，电阻温度系数小。

Description

一种低TCR陶瓷芯片电阻及其材料和制备
技术领域
本发明涉及电阻材料技术领域，特别是涉及一种低TCR陶瓷芯片电阻、电阻材料及其制备。
背景技术
精密电阻要求电阻的阻值误差、电阻的热稳定性(温度系数)、电阻器的分布参数(分布电容和分布电感)等项指标均达到一定标准的电阻器。精密电阻按材料分，有金属膜精密电阻、线绕精密电阻和金属箔精密电阻几类，但这些精密电阻的制造工艺要求严格，生产成本高。
普通的厚膜电阻元件和薄膜电阻元件虽然在制造工艺和成本上有优势，但往往不具备较小的电阻温度系数，在温度变化的环境中使用时难以保持稳定的电性能。
发明内容
基于此，本发明提供一种低TCR陶瓷电阻材料，其原料来源广且成本低，制得电阻的室温电阻率可调节，电阻温度系数小，该陶瓷电阻材料适合制备陶瓷电阻元件、厚膜电阻元件、薄膜电阻元件等。
本发明采取的技术方案如下：
一种低TCR陶瓷电阻材料，其化学通式为(Sn1-xSbxO2)(Bi8TiO14)y(Sb2O3)w，其中0.03≤x≤0.07，0＜y≤0.2，0≤w≤0.1。
进一步，所述陶瓷电阻材料由Sn1-xSbxO2粉体、Bi8TiO14粉体和含Sb元素的原料粉体按配比混合后通过烧结制成。
进一步，所述烧结的条件为：在烧结温度1200～1400℃下保温3～10小时。
本发明还提供一种低TCR陶瓷芯片电阻，包括瓷体和设于瓷体相对两面的电极，所述瓷体采用所述的陶瓷电阻材料。
进一步，所述电极为银电极。
进一步，所述陶瓷芯片电阻的尺寸大小为0.5mm×1.0mm×1.0mm。
本发明还提供所述陶瓷芯片电阻的制备方法，包括以下步骤：
(1)分别制备Sn1-xSbxO2粉体、Bi8TiO14粉体和含Sb元素的原料粉体；
(2)按配比称取制得的Sn1-xSbxO2粉体、Bi8TiO14粉体和含Sb元素的原料粉体，经过球磨混合和干燥后，得到混合干燥粉料；
(3)对混合干燥粉料冷等静压，制得坯体；
(4)将坯体烧结，得到陶瓷块体；
(5)对陶瓷坯体切片，得到陶瓷片；
(6)在陶瓷片上印刷电极；
(7)对印刷有电极的陶瓷片划切，得到单个的陶瓷芯片电阻。
进一步，步骤(2)中，干燥温度为100～250℃。
进一步，步骤(3)中，冷等静压的压强为300MPa。
进一步，步骤(4)中，烧结温度为1200～1400℃，保温时间为3～10小时。
本发明的低电阻温度系数(TCR)陶瓷电阻材料的化学组成包含Sn、Sb、Bi和Ti四种元素的氧化物，配方中x的比例是用来调节电阻温度系数的，不能过大或者过小，y是用来调节电阻率的，由于Bi8TiO14的电阻率很大，所以添加量不能很多。采用所述陶瓷电阻材料的电阻通过球磨-煅烧-球磨-成型-烧结-切片的陶瓷制备工艺制成，所制得的低TCR陶瓷芯片电阻的室温电阻率ρ25＝54Ω·mm～730Ω·mm，电阻温度系数TCR＝-76ppm/℃～156ppm/℃。
本发明所设计的低温度系数陶瓷电阻材料配方，具有原料来源广、原料成本低的优点，所制得电阻的室温电阻率可调节，电阻温度系数小，适合制备陶瓷电阻元件、厚膜电阻元件、薄膜电阻元件等。
为了更好地理解和实施，下面结合附图详细说明本发明。
附图说明
图1为本发明实施例1-4的电阻材料的电阻率-温度变化图。
具体实施方式
本发明提供的低TCR陶瓷电阻材料，其化学通式如下：
(Sn1-xSbxO2)(Bi8TiO14)y(Sb2O3)w，其中0.03≤x≤0.07，0＜y≤0.2，0≤w≤0.1。
具体地，所述陶瓷电阻材料由Sn1-xSbxO2粉体、Bi8TiO14粉体和含Sb元素的原料粉体按配比混合后通过烧结制成。
本发明的低TCR陶瓷芯片电阻，包括瓷体和设于瓷体相对两表面的电极，所述瓷体采用上述陶瓷电阻材料。所述电极可以为银电极。
所述TCR陶瓷芯片电阻的制备方法，包括以下步骤：
(1)分别制备Sn1-xSbxO2粉体、Bi8TiO14粉体和含Sb元素的原料粉体；
(2)按配比称取制得的Sn1-xSbxO2粉体、Bi8TiO14粉体和含Sb元素的原料粉体，经过球磨混合和干燥后，得到混合干燥粉料；
(3)对混合干燥粉料冷等静压，制得坯体；
(4)将坯体烧结，得到陶瓷块体；
(5)对陶瓷坯体切片，得到陶瓷片；
(6)在陶瓷片上印刷电极；
(7)对印刷有电极的陶瓷片划切，得到单个的陶瓷芯片电阻。
具体按如下步骤制备所述TCR陶瓷芯片电阻：
步骤1：按Sn1-xSbxO2(其中，0.03≤x≤0.07)化合物组成，分别称取含Sn、Sb元素的原料进行球磨混合，在100～250℃温度下烘干，得到干燥粉体。
步骤2：将步骤1得到的粉料进行煅烧得到Sn1-xSbxO2粉体，煅烧温度为800～1100℃，保温3～10小时。
步骤3：按Bi8TiO14化合物组成，分别称取含Bi、Ti元素的原料进行球磨混合，在100～250℃温度下烘干，得到干燥粉体；
步骤4：将步骤3得到的粉料进行煅烧得到Bi8TiO14粉体，煅烧温度为600～700℃，保温3～10小时。
步骤5：按照成分组成(Sn1-xSbxO2)(Bi8TiO14)y(Sb2O3)w，其中0.03≤x≤0.07，0＜y≤0.2，0≤w≤0.1，称取步骤2得到的Sn1-xSbxO2、步骤4得到的Bi8TiO14和含Sb元素的原料；
步骤6：将步骤5配料称取的物料进行球磨混合，在100～250℃温度下干燥，得到混合干燥粉料；
步骤7：通过冷等静压方式将步骤6得到的粉料制成尺寸为50mm×50mm×15mm的坯体，其中，冷等静压的压力为300MPa。
步骤8：将步骤7制得的坯体进行烧结，得到陶瓷块体，烧结温度为1200～1400℃，保温3～10小时。
步骤9：将步骤8得到的陶瓷块体进行切片，得到厚度为0.5mm的陶瓷片；
步骤10：利用丝网印刷方法在步骤9得到的陶瓷片上印刷银浆，然后通过烧结固化银电极；
步骤11：对步骤10得到的含银电极陶瓷片进行划切，得到单个的陶瓷芯片电阻，其尺寸大小为0.5mm×1.0mm×1.0mm。
其中，所述含Sn、Sb、Bi、Ti元素的原料分别为单质、氧化物、无机盐或有机盐中的一种。
经检测，所制得的低TCR陶瓷芯片电阻的室温电阻率ρ25＝54Ω·mm～730Ω·mm，电阻温度系数TCR＝-76ppm/℃～156ppm/℃。
实施例1
本实施例中陶瓷电阻材料的组成为(Sn0.94Sb0.06O2)(Bi8TiO14)。
实施例2
本实施例中陶瓷电阻材料的组成为(Sn0.94Sb0.06O2)(Bi8TiO14)0.007。
实施例3
本实施例中陶瓷电阻材料的组成为(Sn0.94Sb0.06O2)(Bi8TiO14)0.007(Sb2O3)0.007。
实施例4
本实施例中陶瓷电阻材料的组成为(Sn0.94Sb0.06O2)(Bi8TiO14)0.007(Sb2O3)0.003。
根据前述的具体制备步骤，按照实施例1-4的陶瓷电阻材料配方分别制得相同尺寸规格的陶瓷芯片电阻，测试这些陶瓷芯片电阻的电阻率随温度的变化，结果如图1所示，由该图可见，本发明采取特定配方制成的陶瓷芯片电阻，具有较小的电阻温度系数，在温度变化的环境中使用可以保持稳定的电性能，而且通过调整配方中的元素比例，可方便、有效地调节电阻的电阻率。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。

Claims (10)

1.一种低TCR陶瓷电阻材料，其特征在于，化学通式为(Sn1-xSbxO2)(Bi8TiO14)y(Sb2O3)w，其中0.03≤x≤0.07，0＜y≤0.2，0≤w≤0.1。
2.根据权利要求1所述的陶瓷电阻材料，其特征在于，由Sn1-xSbxO2粉体、Bi8TiO14粉体和含Sb元素的原料粉体按配比混合后通过烧结制成。
3.根据权利要求2所述的陶瓷电阻材料，其特征在于，所述烧结的条件为：在烧结温度1200～1400℃下保温3～10小时。
4.一种低TCR陶瓷芯片电阻，包括瓷体和设于瓷体两表面的电极，其特征在于，所述瓷体采用权利要求1所述的陶瓷电阻材料。
5.根据权利要求4所述的陶瓷芯片电阻，其特征在于，所述电极为银电极。
6.根据权利要求4或5所述的陶瓷芯片电阻，其特征在于，尺寸大小为0.5mm×1.0mm×1.0mm。
7.权利要求4所述的低TCR陶瓷芯片电阻的制备方法，其特征在于，包括以下步骤：
(1)分别制备Sn1-xSbxO2粉体、Bi8TiO14粉体和含Sb元素的原料粉体；
(2)按配比称取制得的Sn1-xSbxO2粉体、Bi8TiO14粉体和含Sb元素的原料粉体，经过球磨混合和干燥后，得到混合干燥粉料；
(3)对混合干燥粉料冷等静压，制得坯体；
(4)将坯体烧结，得到陶瓷块体；
(5)对陶瓷坯体切片，得到陶瓷片；
(6)在陶瓷片上印刷电极；
(7)对印刷有电极的陶瓷片划切，得到单个的陶瓷芯片电阻。
8.根据权利要求7所述的制备方法，其特征在于：步骤(2)中，干燥温度为100～250℃。
9.根据权利要求7所述的制备方法，其特征在于：步骤(3)中，冷等静压的压强为300MPa。
10.根据权利要求7-9任一项所述的制备方法，其特征在于：步骤(4)中，烧结温度为1200～1400℃，保温时间为3～10小时。
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