CN108484175A - 一种导电陶瓷材料及其制备方法 - Google Patents
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Abstract
本发明公开了一种导电陶瓷材料,由如下重量份的组分制成:铁掺杂Zn‑Ti‑Zr‑O15‑25份、硼化硅15‑20份、蒙脱土10‑15份、氮化硼5‑10份、碳化钼5‑10份。所述的导电陶瓷材料的制备方法,包括如下步骤:S1、按比例称取铁掺杂Zn‑Ti‑Zr‑O、硼化硅、蒙脱土、氮化硼、碳化钼,并将上述组分用球磨机进行研磨混合得到混合物,再将混合物模压制坯;S2、将经过步骤S1制坯后的混合物高温烧结,得到导电陶瓷材料。本发明公开的导电陶瓷材料具有导电率好,耐高温能力强,使用寿命长,成本低廉的优点。
Description
技术领域
本发明涉及陶瓷材料技术领域,尤其涉及一种导电陶瓷材料及其制备方法。
背景技术
随着材料科学技术的飞速发展,导电陶瓷材料受到业内的广泛关注,其集金属电学性能和陶瓷结构特性于一身,具有类似金属导电性,同时又具有陶瓷的结构特征,如化学性质稳定、耐高温、寿命长、抗辐射、耐腐蚀、抗氧化等,被广泛应用于电极、气敏元件、铁电材料、超导材料等领域。
传统陶瓷是良好的绝缘体。由于其中原子的外层电子通常受到原子核的吸引力,被束缚在各自原子的周围,不能自由运动,从而使得传统陶瓷不导电。然而,在加热条件下,处于原子外层的电子可以获得足够的能量,以便克服原子核对它的吸引力,而成为可以自由运动的自由电子,这种陶瓷就变成导电陶瓷。现有的导电陶瓷材料导电率、耐高温的能力都远远达不到目前实际应用所需要的标准,其导电率及耐高温的能力有待进一步提高。同时,现有的导电陶瓷烧结温度较高,同时致密度较低。这些缺陷限制了导电陶瓷材料的进一步发展。
中国发明专利CN03139036.6中公开了一种导电陶瓷,通过在陶瓷基料中添加非金属导电材料,经高温烧制后得到中间层具有导电层的陶瓷材料,但该材料存在着电阻率不均匀,易吸潮,高温老化速度快的问题。
因此,开发一种在较宽的温度和湿度范围内具有稳定的物理和化学性能,导电率高,适于高温工作,且成本低廉的导电陶瓷材料符合市场需求,具有重要的市场价值和应用前景。
发明内容
为了克服现有技术中的缺陷,本发明提供一种导电陶瓷材料及其制备方法,该制备方法简单易行,原料易得,价格低廉,对设备和反应条件要求不高,适合大规模生产;通过所述制备方法制备得到的导电陶瓷材料克服了现有的导电陶瓷材料的导电率低、耐高温能力弱,电阻率不均匀,易吸潮,烧结温度较高,同时致密度较低的技术问题,具有导电率好,耐高温能力强,使用寿命长,成本低廉的优点。
为达到上述发明目的,本发明采用的技术方案是,一种导电陶瓷材料,由如下重量份的组分制成:铁掺杂Zn-Ti-Zr-O15-25份、硼化硅15-20份、蒙脱土10-15份、氮化硼5-10份、碳化钼5-10份。
优选地,所述铁掺杂Zn-Ti-Zr-O的制备方法,包括如下步骤:
1)将Zr(OH)4、Zn(CH3COO)2·2H2O、Ti(CH3COO)4、柠檬酸配制成浓度成溶液。将配制好的溶液经喷雾干燥仪合成前驱体粉末。再将前驱体于400-500℃空气中恒温预烧2-3h。再将产物研磨后置于850-950℃空气中煅烧10-12h,自然冷却后将产物研磨,过200-300目筛得Zn-Ti-Zr-O材料;
2)将经过步骤1)制备得到的Zn-Ti-Zr-O材料、质量分数为50-60%的HNO3溶液、Fe(NO3)3在80℃-100℃下水热反应12-15h,后置于90-100℃烘干混合物,研磨,过200-300目筛,并置于850-950℃下空气中烧结8-10h得到铁掺杂Zn-Ti-Zr-O。
较佳地,步骤1)中所述Zr(OH)4、Zn(CH3COO)2·2H2O、Ti(CH3COO)4、柠檬酸的质量比为(0.5-1):(1-2):0.5:(3-5)。
较佳地,步骤2)中所述Zn-Ti-Zr-O材料、HNO3溶液、Fe(NO3)3的质量比为(2-3):(5-10):1。
优选地,所述导电陶瓷材料的制备方法,包括如下步骤:
S1、按比例称取铁掺杂Zn-Ti-Zr-O、硼化硅、蒙脱土、氮化硼、碳化钼,并将上述组分用球磨机进行研磨混合得到混合物,再将混合物模压制坯;
S2、将经过步骤S1制坯后的混合物高温烧结,得到导电陶瓷材料。
进一步地,所述高温烧结温度为700-800℃,烧结时间4-6小时。
采用上述技术方案所产生的有益效果在于:
1)本发明提供的导电陶瓷材料的制备方法,工艺简单易行,原料易得,价格低廉,对设备和反应条件要求不高,适合大规模生产。
2)本发明提供的导电陶瓷材料,克服了现有的导电陶瓷材料的导电率低、耐高温能力弱,电阻率不均匀,易吸潮,烧结温度较高,同时致密度较低的技术问题,具有导电率好,耐高温能力强,温度适应范围广,使用寿命长,成本低廉的优点。
3)本发明提供的导电陶瓷材料,化学性能稳定,电阻率均匀,各原料分散及相容性好,不易吸潮和团聚,具有优异的导电性能和机械性能,且其耐磨、耐蚀、耐高温、抗氧化性、抗热冲击。
具体实施方式
为了使本技术领域人员更好地理解本发明的技术方案,并使本发明的上述特征、目的以及优点更加清晰易懂,下面结合实施例对本发明做进一步的说明。实施例仅用于说明本发明而不用于限制本发明的范围。
本发明下述实施例中所使用的原料购自摩贝商城。
实施例1
一种导电陶瓷材料,由如下重量份的组分制成:铁掺杂Zn-Ti-Zr-O15份、硼化硅15份、蒙脱土10份、氮化硼5份、碳化钼5份。
所述铁掺杂Zn-Ti-Zr-O的制备方法,包括如下步骤:
1)将Zr(OH)45g、Zn(CH3COO)2·2H2O10g、Ti(CH3COO)45g、柠檬酸30g配制成浓度成溶液。将配制好的溶液经喷雾干燥仪合成前驱体粉末。再将前驱体于400℃空气中恒温预烧2h。再将产物研磨后置于850℃空气中煅烧10h,自然冷却后将产物研磨,过200目筛得Zn-Ti-Zr-O材料;
2)将经过步骤1)制备得到的Zn-Ti-Zr-O材料10g、质量分数为50%的HNO3溶液25g、Fe(NO3)35g在80℃下水热反应12h,后置于90℃烘干混合物,研磨,过200目筛,并置于850℃下空气中烧结8h得到铁掺杂Zn-Ti-Zr-O。
所述导电陶瓷材料的制备方法,包括如下步骤:
S1、按比例称取铁掺杂Zn-Ti-Zr-O、硼化硅、蒙脱土、氮化硼、碳化钼,并将上述组分用球磨机进行研磨混合得到混合物,再将混合物模压制坯;
S2、将经过步骤S1制坯后的混合物高温烧结,得到导电陶瓷材料;所述高温烧结温度为700℃,烧结时间4小时。
实施例2
一种导电陶瓷材料,由如下重量份的组分制成:铁掺杂Zn-Ti-Zr-O17份、硼化硅17份、蒙脱土12份、氮化硼7份、碳化钼7份。
所述铁掺杂Zn-Ti-Zr-O的制备方法,包括如下步骤:
1)将Zr(OH)47g、Zn(CH3COO)2·2H2O12g、Ti(CH3COO)45g、柠檬酸35g配制成浓度成溶液。将配制好的溶液经喷雾干燥仪合成前驱体粉末。再将前驱体于420℃空气中恒温预烧2.3h。再将产物研磨后置于880℃空气中煅烧10.5h,自然冷却后将产物研磨,过220目筛得Zn-Ti-Zr-O材料;
2)将经过步骤1)制备得到的Zn-Ti-Zr-O材料12g、质量分数为52%的HNO3溶液30g、Fe(NO3)35g在85℃下水热反应13h,后置于93℃烘干混合物,研磨,过250目筛,并置于900℃下空气中烧结8.5h得到铁掺杂Zn-Ti-Zr-O。
所述导电陶瓷材料的制备方法,包括如下步骤:
S1、按比例称取铁掺杂Zn-Ti-Zr-O、硼化硅、蒙脱土、氮化硼、碳化钼,并将上述组分用球磨机进行研磨混合得到混合物,再将混合物模压制坯;
S2、将经过步骤S1制坯后的混合物高温烧结,得到导电陶瓷材料;所述高温烧结温度为750℃,烧结时间4.5小时。
实施例3
一种导电陶瓷材料,由如下重量份的组分制成:铁掺杂Zn-Ti-Zr-O20份、硼化硅18份、蒙脱土13份、氮化硼8份、碳化钼7份。
所述铁掺杂Zn-Ti-Zr-O的制备方法,包括如下步骤:
1)将Zr(OH)48.5g、Zn(CH3COO)2·2H2O15g、Ti(CH3COO)45g、柠檬酸40g配制成浓度成溶液。将配制好的溶液经喷雾干燥仪合成前驱体粉末。再将前驱体于460℃空气中恒温预烧2.6h。再将产物研磨后置于910℃空气中煅烧11h,自然冷却后将产物研磨,过280目筛得Zn-Ti-Zr-O材料;
2)将经过步骤1)制备得到的Zn-Ti-Zr-O材料13.5g、质量分数为56%的HNO3溶液35g、Fe(NO3)35g在90℃下水热反应14h,后置于97℃烘干混合物,研磨,过280目筛,并置于920℃下空气中烧结9h得到铁掺杂Zn-Ti-Zr-O。
所述导电陶瓷材料的制备方法,包括如下步骤:
S1、按比例称取铁掺杂Zn-Ti-Zr-O、硼化硅、蒙脱土、氮化硼、碳化钼,并将上述组分用球磨机进行研磨混合得到混合物,再将混合物模压制坯;
S2、将经过步骤S1制坯后的混合物高温烧结,得到导电陶瓷材料;所述高温烧结温度为760℃,烧结时间5小时。
实施例4
一种导电陶瓷材料,由如下重量份的组分制成:铁掺杂Zn-Ti-Zr-O22份、硼化硅19份、蒙脱土14份、氮化硼9份、碳化钼8份。
所述铁掺杂Zn-Ti-Zr-O的制备方法,包括如下步骤:
1)将Zr(OH)49g、Zn(CH3COO)2·2H2O18g、Ti(CH3COO)45g、柠檬酸45g配制成浓度成溶液。将配制好的溶液经喷雾干燥仪合成前驱体粉末。再将前驱体于450℃空气中恒温预烧2.8h。再将产物研磨后置于930℃空气中煅烧11.5h,自然冷却后将产物研磨,过280目筛得Zn-Ti-Zr-O材料;
2)将经过步骤1)制备得到的Zn-Ti-Zr-O材料14g、质量分数为58%的HNO3溶液45g、Fe(NO3)35g在95℃下水热反应14h,后置于98℃烘干混合物,研磨,过300目筛,并置于930℃下空气中烧结9.5h得到铁掺杂Zn-Ti-Zr-O。
所述导电陶瓷材料的制备方法,包括如下步骤:
S1、按比例称取铁掺杂Zn-Ti-Zr-O、硼化硅、蒙脱土、氮化硼、碳化钼,并将上述组分用球磨机进行研磨混合得到混合物,再将混合物模压制坯;
S2、将经过步骤S1制坯后的混合物高温烧结,得到导电陶瓷材料;所述高温烧结温度为780℃,烧结时间5.5小时。
实施例5
一种导电陶瓷材料,由如下重量份的组分制成:铁掺杂Zn-Ti-Zr-O25份、硼化硅20份、蒙脱土15份、氮化硼10份、碳化钼10份。
所述铁掺杂Zn-Ti-Zr-O的制备方法,包括如下步骤:
1)将Zr(OH)410g、Zn(CH3COO)2·2H2O20g、Ti(CH3COO)45g、柠檬酸50g配制成浓度成溶液。将配制好的溶液经喷雾干燥仪合成前驱体粉末。再将前驱体于500℃空气中恒温预烧3h。再将产物研磨后置于950℃空气中煅烧12h,自然冷却后将产物研磨,过300目筛得Zn-Ti-Zr-O材料;
2)将经过步骤1)制备得到的Zn-Ti-Zr-O材料15g、质量分数为60%的HNO3溶液50g、Fe(NO3)35g在100℃下水热反应15h,后置于100℃烘干混合物,研磨,过300目筛,并置于950℃下空气中烧结10h得到铁掺杂Zn-Ti-Zr-O。
所述导电陶瓷材料的制备方法,包括如下步骤:
S1、按比例称取铁掺杂Zn-Ti-Zr-O、硼化硅、蒙脱土、氮化硼、碳化钼,并将上述组分用球磨机进行研磨混合得到混合物,再将混合物模压制坯;
S2、将经过步骤S1制坯后的混合物高温烧结,得到导电陶瓷材料;所述高温烧结温度为800℃,烧结时间6小时。
对比例1
本例提供一种导电陶瓷材料,按照中国发明专利CN 105622099A实施例1的原料制备得到。
对比例2
本例提供一种导电陶瓷材料,原料和制备方法同实施例1,不同的是没有添加铁掺杂Zn-Ti-Zr-O。
对比例3
本例提供一种导电陶瓷材料,原料和制备方法同实施例1,不同的是没有添加硼化硅。
对比例4
本例提供一种导电陶瓷材料,原料和制备方法同实施例1,不同的是没有添加蒙脱土。
对比例5
本例提供一种导电陶瓷材料,原料和制备方法同实施例1,不同的是没有添加氮化硼。
对比例6
本例提供一种导电陶瓷材料,原料和制备方法同实施例1,不同的是没有添加碳化钼。
将实施例1-5和对比例1-6所述导电陶瓷材料样品进行性能测试,测试结果见表1,测试方法如下:
1)硬度:以49.03-980.7N的负荷,将相对面夹角为136°的方锥形金刚石压入陶瓷材料表面,保持规定的时间后,测量压痕对角线长度,再按公式来计算硬度的大小。
2)电导率:四探针测试仪实时采集两次组合模式下的测试数据,采集到的数据经计算机分析,从而得到所需的测试结果。
3)抗弯强度:按照GB/T6569-86测试方法测试。
4)断裂韧性:按照ASTMC1421-2001测试方法测试。
5)热膨胀系数:按照GB/T16535-1996测试方法测试。
表1导电陶瓷材料性能参数
从表1可见,本发明实施例公开的导电陶瓷材料,与现有技术中的导电陶瓷材料相比,具有更高的导电率,更优异的力学性能,且热膨胀系数更低。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (6)
1.一种导电陶瓷材料,其特征在于,由如下重量份的组分制成:铁掺杂Zn-Ti-Zr-O15-25份、硼化硅15-20份、蒙脱土10-15份、氮化硼5-10份、碳化钼5-10份。
2.根据权利要求1所述的导电陶瓷材料,其特征在于,所述铁掺杂Zn-Ti-Zr-O的制备方法,包括如下步骤:
1)将Zr(OH)4、Zn(CH3COO)2·2H2O、Ti(CH3COO)4、柠檬酸配制成浓度成溶液。将配制好的溶液经喷雾干燥仪合成前驱体粉末。再将前驱体于400-500℃空气中恒温预烧2-3h。再将产物研磨后置于850-950℃空气中煅烧10-12h,自然冷却后将产物研磨,过200-300目筛得Zn-Ti-Zr-O材料;
2)将经过步骤1)制备得到的Zn-Ti-Zr-O材料、质量分数为50-60%的HNO3溶液、Fe(NO3)3在80℃-100℃下水热反应12-15h,后置于90-100℃烘干混合物,研磨,过200-300目筛,并置于850-950℃下空气中烧结8-10h得到铁掺杂Zn-Ti-Zr-O。
3.根据权利要求2所述的导电陶瓷材料,其特征在于,步骤1)中所述Zr(OH)4、Zn(CH3COO)2·2H2O、Ti(CH3COO)4、柠檬酸的质量比为(0.5-1):(1-2):0.5:(3-5)。
4.根据权利要求2所述的导电陶瓷材料,其特征在于,步骤2)中所述Zn-Ti-Zr-O材料、HNO3溶液、Fe(NO3)3的质量比为(2-3):(5-10):1。
5.一种根据权利要求1-4任一项所述的导电陶瓷材料的制备方法,其特征在于,包括如下步骤:
S1、按比例称取铁掺杂Zn-Ti-Zr-O、硼化硅、蒙脱土、氮化硼、碳化钼,并将上述组分用球磨机进行研磨混合得到混合物,再将混合物模压制坯;
S2、将经过步骤S1制坯后的混合物高温烧结,得到导电陶瓷材料。
6.根据权利要求5所述的导电陶瓷材料的制备方法,其特征在于,所述高温烧结温度为700-800℃,烧结时间4-6小时。
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