CN108503364A - 一种导电陶瓷电极材料及其制备方法 - Google Patents

一种导电陶瓷电极材料及其制备方法 Download PDF

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CN108503364A
CN108503364A CN201810363308.0A CN201810363308A CN108503364A CN 108503364 A CN108503364 A CN 108503364A CN 201810363308 A CN201810363308 A CN 201810363308A CN 108503364 A CN108503364 A CN 108503364A
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朱小红
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Hunan Chenli New Material Co Ltd
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Abstract

本发明公开了一种导电陶瓷电极材料及其制备方法，由以下重量份的组分制成：Ti‑Sn‑Zn‑Si‑N 15‑20份，氮化镓10‑15份，乙炔黑5‑10份，粘结剂2‑5份，碳化硼20‑25份，纳米二氧化硅5‑10份，硅化钼5‑10份，混合溶剂10‑15份。所述制备方法包括捏合、模压制坯、高温烧结步骤。本发明公开的导电陶瓷电极材料具有价格低廉，电导率高，耐磨抗腐蚀性能优异，导电性能、电化学性能和加工性能佳的优点。

Description

一种导电陶瓷电极材料及其制备方法
技术领域
本发明涉及电极材料技术领域，尤其涉及一种导电陶瓷电极材料及其制备方法。
背景技术
随着社会的进步及经济的发展，人们越来越关心日益严重的环境问题。水污染作为众多环境问题之一，由于其能直接影响人们的身体健康，引起了业内广泛关注。各种污水处理设备如雨后春笋般涌现，其中用于电渗透的设备是目前实现污泥高效脱水性价比比较高的设备，采用这种设备进行污泥脱水脱水速度快、效率高、有效避免了污泥中的各种污染物直接投入环境中对环境造成的严重污染。但是，这类设备采用的电极材料多为常规金属或金属涂层类电极材料，其电力学性能不高，耐磨、耐酸碱腐蚀性差，用于污泥脱水处理损耗大，寿命短。
导电陶瓷是众多陶瓷材料中的一种，其能实现离子导电、电子、空穴导电，具有化学性质稳定、耐高温、寿命长、抗辐射、耐腐蚀、抗氧化等优点，是电极材料的又一较佳选择。但现有的导电陶瓷或多或少存在导电率低、化学性质不稳定、耐高温性能差、价格昂贵、制备工艺复杂等缺陷。
因此，开发一种价格低廉、电导率低、耐磨抗腐蚀性能优异、具有较佳的导电性能和电化学性能的导电陶瓷电极材料符合市场需求，具有广泛是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电极材料及其制备方法，该制备方法简单易行，原料易得，价格低廉，对设备要求不高，适合工业化生产；通过所述制备方法制备得到的导电陶瓷电极材料克服了现有技术中传统电极材料耐腐蚀和耐磨性能差，电力学性能不高，使用寿命短的技术问题，也克服了现有导电陶瓷导电率低、电阻率不均匀，生产成本高，化学性能不稳定，耐高温性能差的技术问题，具有价格低廉，电导率高，耐磨抗腐蚀性能优异，导电性能、电化学性能和加工性能佳的优点。
为达到上述发明目的，本发明采用的技术方案是：一种导电陶瓷电极材料，由以下重量份的组分制成：Ti-Sn-Zn-Si-N 15-20份，氮化镓10-15份，乙炔黑5-10份，粘结剂2-5份，碳化硼20-25份，纳米二氧化硅5-10份，硅化钼5-10份，混合溶剂10-15份。
优选地，所述混合溶剂是异丙醇、水按质量比(3-5):1混合而成。
优选地，所述粘结剂选自淀粉、石蜡、羧甲基纤维素、聚乙烯醇、环氧树脂、乙烯-醋酸乙烯酯和水玻璃中的一种或几种。
优选地，所述Ti-Sn-Zn-Si-N的制备方法，包括如下步骤：
1)将金属锡粉、钛粉、硝酸锌、三正丁基叠氮化锡、纳米硅粉加入硬质合金球磨罐中球磨，得到混合粉；
2)将经过步骤1)球磨得到的混合粉加入带有程序升温装置的不锈钢高压釜中，保持高压釜内真空度≤0.08Pa，以6-10℃/min的加热速率将釜内温度程序升温到850-950℃，后保温3-5小时，自然冷却至室温，产物用蒸馏水洗涤4-8次，再用无水乙醇洗涤4-8次，最后置于真空干燥箱70-80℃下烘15-24小时，得到Ti-Sn-Zn-Si-N。
优选地，所述球磨时间为18-24小时，球磨速度为120-150转/分钟。
优选地，所述步骤1)中所述金属锡粉、钛粉、硝酸锌、三正丁基叠氮化锡、纳米硅粉的质量比为(1-2):1:(1-2):(0.3-0.5):(0.5-1)。
优选地，所述导电陶瓷电极材料的制备方法，包括如下步骤：
S1、按质量比称取Ti-Sn-Zn-Si-N、氮化镓、乙炔黑、粘结剂、碳化硼、纳米二氧化硅、硅化钼，并将上述组分用球磨机进行研磨混合得到混合物，再将混合物加入捏合机混合搅拌8-10小时，得到浆料；
S2、将经过步骤S1制备得到的浆料模压制坯，后常温固化10-15小时，得到胚料；
S3、将经过步骤S2制得的胚料在惰性气体氛围下高温烧结，得到导电陶瓷电极材料。
较佳地，所述高温烧结温度为950-1100℃，烧结时间为18-24小时。
较佳地，所述惰性气体选自氦气、氖气、氩气中的一种或几种。
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电极材料的制备方法，简单易行，原料易得，价格低廉，对设备要求不高，适合工业化生产。
2)本发明提供的导电陶瓷电极材料，克服了现有技术中传统电极材料耐腐蚀和耐磨性能差，电力学性能不高，使用寿命短的技术问题，也克服了现有导电陶瓷导电率低、电阻率不均匀，生产成本高，化学性能不稳定，耐高温性能差的技术问题，具有价格低廉，电导率高，耐磨、抗腐蚀性能和化学稳定性能优异，导电性能、电化学性能和加工性能佳的优点。
3)本发明提供的导电陶瓷电极材料，通过各组分合理的配伍，添加Ti-Sn-Zn-Si-N，同时掺入N、Si，有利于提高电学设备循环使用寿命和能量密度，引入纳米材料，有利于提高电极材料比表面积，提高电化学性能，降低导电陶瓷材料的热膨胀系数，避免了在使用时可能出现的爆瓷现象。
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述原料来自于上海泉昕进出口贸易有限公司。
实施例1
一种导电陶瓷电极材料，由以下重量份的组分制成：Ti-Sn-Zn-Si-N 15份，氮化镓10份，乙炔黑5份，淀粉2份，碳化硼20份，纳米二氧化硅5份，硅化钼5份，混合溶剂10份；所述混合溶剂是异丙醇、水按质量比3:1混合而成。
所述Ti-Sn-Zn-Si-N的制备方法，包括如下步骤：
1)将金属锡粉10g、钛粉10g、硝酸锌10g、三正丁基叠氮化锡3g、纳米硅粉5g加入硬质合金球磨罐中球磨，得到混合粉；所述球磨时间为18小时，球磨速度为120转/分钟；
2)将经过步骤1)球磨得到的混合粉加入带有程序升温装置的不锈钢高压釜中，保持高压釜内真空度≤0.08Pa，以6℃/min的加热速率将釜内温度程序升温到850℃，后保温3小时，自然冷却至室温，产物用蒸馏水洗涤4次，再用无水乙醇洗涤4次，最后置于真空干燥箱70℃下烘15小时，得到Ti-Sn-Zn-Si-N。
所述导电陶瓷电极材料的制备方法，包括如下步骤：
S1、按质量比称取Ti-Sn-Zn-Si-N、氮化镓、乙炔黑、淀粉、碳化硼、纳米二氧化硅、硅化钼，并将上述组分用球磨机进行研磨混合得到混合物，再将混合物加入捏合机混合搅拌8小时，得到浆料；
S2、将经过步骤S1制备得到的浆料模压制坯，后常温固化10小时，得到胚料；
S3、将经过步骤S2制得的胚料在氦气氛围下高温烧结，得到导电陶瓷电极材料；所述高温烧结温度为950℃，烧结时间为18小时。
实施例2
一种导电陶瓷电极材料，由以下重量份的组分制成：Ti-Sn-Zn-Si-N 17份，氮化镓12份，乙炔黑7份，石蜡3份，碳化硼22份，纳米二氧化硅7份，硅化钼6份，混合溶剂12份；所述混合溶剂是异丙醇、水按质量比4:1混合而成。
所述Ti-Sn-Zn-Si-N的制备方法，包括如下步骤：
1)将金属锡粉12g、钛粉10g、硝酸锌12g、三正丁基叠氮化锡3.5g、纳米硅粉5.5g加入硬质合金球磨罐中球磨，得到混合粉；所述球磨时间为20小时，球磨速度为130转/分钟；
2)将经过步骤1)球磨得到的混合粉加入带有程序升温装置的不锈钢高压釜中，保持高压釜内真空度≤0.08Pa，以7℃/min的加热速率将釜内温度程序升温到890℃，后保温3.5小时，自然冷却至室温，产物用蒸馏水洗涤5次，再用无水乙醇洗涤5次，最后置于真空干燥箱73℃下烘17小时，得到Ti-Sn-Zn-Si-N。
所述导电陶瓷电极材料的制备方法，包括如下步骤：
S1、按质量比称取Ti-Sn-Zn-Si-N、氮化镓、乙炔黑、石蜡、碳化硼、纳米二氧化硅、硅化钼，并将上述组分用球磨机进行研磨混合得到混合物，再将混合物加入捏合机混合搅拌8.5小时，得到浆料；
S2、将经过步骤S1制备得到的浆料模压制坯，后常温固化12小时，得到胚料；
S3、将经过步骤S2制得的胚料在氖气氛围下高温烧结，得到导电陶瓷电极材料；所述高温烧结温度为1000℃，烧结时间为20小时。
实施例3
一种导电陶瓷电极材料，由以下重量份的组分制成：Ti-Sn-Zn-Si-N 18份，氮化镓13份，乙炔黑8份，羧甲基纤维素4份，碳化硼23份，纳米二氧化硅8份，硅化钼8份，混合溶剂13份；所述混合溶剂是异丙醇、水按质量比5:1混合而成。
所述Ti-Sn-Zn-Si-N的制备方法，包括如下步骤：
1)将金属锡粉15g、钛粉10g、硝酸锌16g、三正丁基叠氮化锡4g、纳米硅粉8g加入硬质合金球磨罐中球磨，得到混合粉；所述球磨时间为21小时，球磨速度为135转/分钟；
2)将经过步骤1)球磨得到的混合粉加入带有程序升温装置的不锈钢高压釜中，保持高压釜内真空度≤0.08Pa，以8℃/min的加热速率将釜内温度程序升温到910℃，后保温4小时，自然冷却至室温，产物用蒸馏水洗涤6次，再用无水乙醇洗涤6次，最后置于真空干燥箱76℃下烘20小时，得到Ti-Sn-Zn-Si-N。
所述导电陶瓷电极材料的制备方法，包括如下步骤：
S1、按质量比称取Ti-Sn-Zn-Si-N、氮化镓、乙炔黑、羧甲基纤维素、碳化硼、纳米二氧化硅、硅化钼，并将上述组分用球磨机进行研磨混合得到混合物，再将混合物加入捏合机混合搅拌9小时，得到浆料；
S2、将经过步骤S1制备得到的浆料模压制坯，后常温固化13.5小时，得到胚料；
S3、将经过步骤S2制得的胚料在氩气氛围下高温烧结，得到导电陶瓷电极材料；所述高温烧结温度为1020℃，烧结时间为22小时。
实施例4
一种导电陶瓷电极材料，由以下重量份的组分制成：Ti-Sn-Zn-Si-N 19份，氮化镓14份，乙炔黑9份，粘结剂4份，碳化硼24份，纳米二氧化硅9份，硅化钼9份，混合溶剂14份；所述混合溶剂是异丙醇、水按质量比4:1混合而成；所述粘结剂是聚乙烯醇、环氧树脂、乙烯-醋酸乙烯酯按质量比1:2:3混合而成的混合物。
所述Ti-Sn-Zn-Si-N的制备方法，包括如下步骤：
1)将金属锡粉18g、钛粉10g、硝酸锌19g、三正丁基叠氮化锡4.5g、纳米硅粉9g加入硬质合金球磨罐中球磨，得到混合粉；所述球磨时间为23小时，球磨速度为145转/分钟。
2)将经过步骤1)球磨得到的混合粉加入带有程序升温装置的不锈钢高压釜中，保持高压釜内真空度≤0.08Pa，以9℃/min的加热速率将釜内温度程序升温到940℃，后保温4.5小时，自然冷却至室温，产物用蒸馏水洗涤7次，再用无水乙醇洗涤7次，最后置于真空干燥箱79℃下烘23小时，得到Ti-Sn-Zn-Si-N。
所述导电陶瓷电极材料的制备方法，包括如下步骤：
S1、按质量比称取Ti-Sn-Zn-Si-N、氮化镓、乙炔黑、粘结剂、碳化硼、纳米二氧化硅、硅化钼，并将上述组分用球磨机进行研磨混合得到混合物，再将混合物加入捏合机混合搅拌9小时，得到浆料；
S2、将经过步骤S1制备得到的浆料模压制坯，后常温固化14小时，得到胚料；
S3、将经过步骤S2制得的胚料在氦气氛围下高温烧结，得到导电陶瓷电极材料。
较佳地，所述高温烧结温度为1050℃，烧结时间为23小时。
实施例5
一种导电陶瓷电极材料，由以下重量份的组分制成：Ti-Sn-Zn-Si-N 20份，氮化镓15份，乙炔黑10份，水玻璃5份，碳化硼25份，纳米二氧化硅10份，硅化钼10份，混合溶剂15份；所述混合溶剂是异丙醇、水按质量比5:1混合而成。
所述Ti-Sn-Zn-Si-N的制备方法，包括如下步骤：
1)将金属锡粉20g、钛粉10g、硝酸锌20g、三正丁基叠氮化锡5g、纳米硅粉10g加入硬质合金球磨罐中球磨，得到混合粉；所述球磨时间为24小时，球磨速度为150转/分钟；
2)将经过步骤1)球磨得到的混合粉加入带有程序升温装置的不锈钢高压釜中，保持高压釜内真空度≤0.08Pa，以10℃/min的加热速率将釜内温度程序升温到950℃，后保温5小时，自然冷却至室温，产物用蒸馏水洗涤8次，再用无水乙醇洗涤8次，最后置于真空干燥箱80℃下烘24小时，得到Ti-Sn-Zn-Si-N。
所述导电陶瓷电极材料的制备方法，包括如下步骤：
S1、按质量比称取Ti-Sn-Zn-Si-N、氮化镓、乙炔黑、水玻璃、碳化硼、纳米二氧化硅、硅化钼，并将上述组分用球磨机进行研磨混合得到混合物，再将混合物加入捏合机混合搅拌10小时，得到浆料；
S2、将经过步骤S1制备得到的浆料模压制坯，后常温固化15小时，得到胚料；
S3、将经过步骤S2制得的胚料在氖气氛围下高温烧结，得到导电陶瓷电极材料；所述高温烧结温度为1100℃，烧结时间为24小时。
对比例
本例提供一种导电陶瓷电极材料，按照中国发明专利201610042815.5实施例1的原料及制备方法制备得到。
对上述实施例1-5以及对比例所得所述导电陶瓷电极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导电陶瓷电极材料性能参数
从表1可见，本发明实施例公开的导电陶瓷电极材料，与现有技术中的导电陶瓷电极材料相比，具有更高的导电率，更大的硬度，更优异的抗弯强度和断裂韧性，且热膨胀系数更低。
以上显示和描述了本发明的基本原理、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的范围内。本发明要求的保护范围由所附的权利要求书及其等同物界定。

Claims (9)

1.一种导电陶瓷电极材料，其特征在于，由以下重量份的组分制成：Ti-Sn-Zn-Si-N15-20份，氮化镓10-15份，乙炔黑5-10份，粘结剂2-5份，碳化硼20-25份，纳米二氧化硅5-10份，硅化钼5-10份，混合溶剂10-15份。
2.根据权利要求1所述的导电陶瓷电极材料，其特征在于，所述混合溶剂是异丙醇、水按质量比(3-5):1混合而成。
3.根据权利要求1所述的导电陶瓷电极材料，其特征在于，所述粘结剂选自淀粉、石蜡、羧甲基纤维素、聚乙烯醇、环氧树脂、乙烯-醋酸乙烯酯和水玻璃中的一种或几种。
4.根据权利要求1所述的导电陶瓷电极材料，其特征在于，所述Ti-Sn-Zn-Si-N的制备方法，包括如下步骤：
1)将金属锡粉、钛粉、硝酸锌、三正丁基叠氮化锡、纳米硅粉加入硬质合金球磨罐中球磨，得到混合粉；
2)将经过步骤1)球磨得到的混合粉加入高压釜中，保持高压釜内真空度≤0.08Pa，以6-10℃/min的加热速率将釜内温度程序升温到850-950℃，后保温3-5小时，自然冷却至室温，产物用蒸馏水洗涤4-8次，再用无水乙醇洗涤4-8次，最后置于真空干燥箱70-80℃下烘15-24小时，得到Ti-Sn-Zn-Si-N。
5.根据权利要求4所述的导电陶瓷电极材料，其特征在于，所述球磨时间为18-24小时，球磨速度为120-150转/分钟。
6.根据权利要求4所述的导电陶瓷电极材料，其特征在于，所述步骤1)中所述金属锡粉、钛粉、硝酸锌、三正丁基叠氮化锡、纳米硅粉的质量比为(1-2):1:(1-2):(0.3-0.5):(0.5-1)。
7.一种如权利要求1-6任一项所述的导电陶瓷电极材料的制备方法，其特征在于，包括如下步骤：
S1、按质量比称取Ti-Sn-Zn-Si-N、氮化镓、乙炔黑、粘结剂、碳化硼、纳米二氧化硅、硅化钼，并将上述组分用球磨机进行研磨混合得到混合物，再将混合物加入捏合机混合搅拌8-10小时，得到浆料；
S2、将经过步骤S1制备得到的浆料模压制坯，后常温固化10-15小时，得到胚料；
S3、将经过步骤S2制得的胚料在惰性气体氛围下高温烧结，得到导电陶瓷电极材料。
8.根据权利要求7所述的一种导电陶瓷电极材料的制备方法，其特征在于，所述高温烧结温度为950-1100℃，烧结时间为18-24小时。
9.根据权利要求7所述的一种导电陶瓷电极材料的制备方法，其特征在于，所述惰性气体选自氦气、氖气、氩气中的一种或几种。
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CN105523761A (zh) * 2016-01-22 2016-04-27 江苏联合金陶特种材料科技有限公司 一种污水污泥处理用耐蚀导电陶瓷电极材料及其制备方法

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CN109545580A (zh) * 2018-12-01 2019-03-29 韩德军 一种超级电容器用电极及其制备方法
CN110372368A (zh) * 2019-07-29 2019-10-25 浙江爱鑫电子科技有限公司 一种增强型高导电陶瓷电极材料及其制备方法
CN114195490A (zh) * 2021-12-31 2022-03-18 武汉中维创发工业研究院有限公司 陶瓷电阻的制备方法、陶瓷电阻及电子电路器件
CN114195490B (zh) * 2021-12-31 2023-11-28 维达力实业(深圳)有限公司 陶瓷电阻的制备方法、陶瓷电阻及电子电路器件

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