CN110078502B - 一种提高8ysz硬度的方法 - Google Patents

一种提高8ysz硬度的方法 Download PDF

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CN110078502B
CN110078502B CN201910408957.2A CN201910408957A CN110078502B CN 110078502 B CN110078502 B CN 110078502B CN 201910408957 A CN201910408957 A CN 201910408957A CN 110078502 B CN110078502 B CN 110078502B
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8ysz
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林枞
周世勇
黄雨铭
吴啸
李含影
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Abstract

本发明公开了一种提高8YSZ陶瓷硬度的方法，该方法主要是通过初期加入液相介质来调节溶液的pH值，从而改变8YSZ粉体在溶液中的溶解度，为了增加溶解量的情况下，促进8YSZ初期烧结的溶解‑沉淀过程，从而增加8YSZ陶瓷的致密度和硬度，既简化了8YSZ制备中的烧结过程，相对于去离子水烧结的陶瓷，明显的进一步提高密度及硬度。而且，在电化学性能没有明显降低的情况下了完成了简化工艺、节约能源的目的。

Description

一种提高8YSZ硬度的方法
技术领域
本发明属于8YSZ陶瓷材料及冷烧技术的应用领域，具体涉及一种提高8YSZ陶瓷硬度的方法。
背景技术
ZrO2具有优良的耐热隔热性能、光学性能、电性能、机械性能以及化学稳定性，可用于热障涂层、绝缘层、耐磨、耐蚀涂层以及光电器件等，因而广泛用于航空航天、钢铁冶金、机械制造、光学、电学等领域。在常温、常压下，纯氧化锆共有三种晶态：单斜氧化锆(m-ZrO2)、四方氧化锆(t- ZrO2)和立方氧化锆(c-ZrO2)，这三种晶型在不同的温度范围能稳定存在，但若条件变化则其也会发生相互转化。8YSZ是一种立方相的氧化锆，在较高温度下有很好的离子导电性，其应用及研究一直是近年来的研究热点。8YSZ的烧结温度较高，达1400℃才能使8YSZ达到所需的致密度，在电池中起到传输氧离子、阻隔阴极和阳极的作用。提高8YSZ的密度和硬度，有利于提高其在使用过程中的使用寿命，同时也有助于提高制备过程中的成品率。通常需要提高烧结温度或者添加其他物质才能实现密度和硬度的提高。
本发明通过对8YSZ陶瓷工艺制备进行改进，利用酸性物质溶液作为初期烧结介质，从而促进对8YSZ粉体的溶解，得到密度更高，硬度更大的8YSZ陶瓷。酸性溶液的掺杂可以降低8YSZ的烧结温度，使其在较低温度下就能达到所需的致密度，并且增大晶粒尺寸，从而提高其硬度和电导率。
发明内容
由于YSZ陶瓷制备的成本比较高，在制备过程中，需要较高的烧结温度。所以，本发明的目的主要是在于提供一种新的8YSZ陶瓷成型方式，在减少烧结助剂使用的情况下，也简化了传统的造粒过程。并且保证8YSZ的致密度大幅度提升，同时YSZ陶瓷硬度也明显增加。该方法主要是通过初期加入液相来与粉体相互混合，从而利用水中的氢及氢氧根与锆氧键相互作用，并且使得粉体表面变得相对湿润。为了增加粉体与液体的相互作用，我们改变了液体的酸碱度，从而增加YSZ陶瓷的致密度和硬度，既简化了YSZ制备中的烧结过程，相对于传统烧结的陶瓷，明显的进一步提高密度及硬度。而且，在电化学性能没有明显降低的情况下了完成了简化工艺、节约能源的目的。
为了实现上述的技术目的，本发明的技术方案为：
一种提高8YSZ硬度的方法，包括以下步骤：
1）称取适量的酸性物质，滴入去离子水后，通过pH试纸调控，获得pH值为1-6的偏酸性溶液；
2）称取一定量的8YSZ粉末，加入酒精进行球磨后，在80℃下干燥，获得粒径均匀（150-200nm）的8YSZ粉体；
3）称取适量的8YSZ粉体，倒入研钵中，再滴入8YSZ粉体质量5%-20%的步骤1）中所制得的偏酸性溶液，混合研磨至均匀；
4）将步骤3）混合后的8YSZ粉体放入磨具中，置于液压机中，其中温度和压力分别设定为120-300℃和200-500MPa，进行压制成型，保压10-60min后得到8YSZ陶瓷生坯；
5）取出模具中的8YSZ陶瓷生坯，置于马弗炉中烧结2-10h，烧结温度设定为1100-1400℃，得到8YSZ陶瓷片；
6）将所得的8YSZ陶瓷片再次放入马弗炉中，让其在600-800℃下进行退火4小时，退火后即为陶瓷片成品。
步骤1）中的酸性物质为乙酸、甲酸、柠檬酸或硝酸。
本发明采用该技术方案后，可以使8YSZ在更低的温度下完成烧结，并且烧结后获得非常理想的机械强度。通过添加酸性物质，可以进一步提高机械强度。拓展8YSZ的应用范围。研究发现，8YSZ在加入酸性溶液后，经过初步加热加压，所获得的坯体密度会有大幅度的提升。溶液可以有效填补陶瓷中的孔隙，从而更加快速的完成烧结过程。陶瓷烧结温度大幅度降低，密度也明显提高，在不降低导电性的情况下，明显提高了8YSZ的强度。与现有的技术相比，该发明的有益效果为：
（1）通过该发明方法获得8YSZ生坯相对密度达到了65%以上，在1000℃~1200℃烧结下的致密度与传统的1400℃下的致密度还要高出很多，烧结后的相对密度可以达到95%以上。
（2）该方法制得的8YSZ有更好的机械强度和电导率，并且明显降低了烧结温度，使得8YSZ在SOFC的应用中有望实现三级共烧及提高SOFC的界面贴合性和电学性能。
附图说明
图1是实施例1-3以及对比例制得的YSZ陶瓷硬度对比图；
图2是实施例1-3及对比例制得的YSZ陶瓷的扫描电镜图。
具体实施方式
一种提高YSZ硬度的方法，包括以下步骤：
1）称取适量的酸性物质，滴入去离子水后，通过pH试纸调控，获得pH值为1-6的偏酸性溶液；
2）称取一定量的8YSZ粉末，加入酒精进行球磨后，在80℃下干燥，获得粒径均匀（150-200nm）的8YSZ粉体；
3）称取适量的8YSZ粉体，倒入研钵中，再滴入8YSZ粉体质量5%-20%的步骤1）中所制得的偏酸性溶液，混合研磨至均匀；
4）将湿润的8YSZ粉体放入磨具中，置于液压机中，其中温度和压力分别设定为120-300℃和200-500MPa，进行压制成型，保压10-60min后得到8YSZ陶瓷生坯；
5）取出模具中的8YSZ陶瓷生坯，置于马弗炉中烧结2-10h，烧结温度设定为1100-1400℃，得到8YSZ陶瓷片；
6）将所得的8YSZ陶瓷片再次放入马弗炉中，让其在600-800℃下进行退火4小时，退火后即为陶瓷片成品。
步骤1）中的酸性物质为乙酸、甲酸、柠檬酸或硝酸。
下面结合附图和具体实施方式对本发明做进一步的阐述：
实施例1
一种提高YSZ硬度的方法，包括以下步骤：
1）用量筒称取适量的乙酸，滴入去离子水后，通过pH试纸调控，获得pH值为3的乙酸溶液；
2）称取5g的8YSZ粉末，加入酒精进行球磨后，在80℃下干燥，获得粒径较为均匀（150-200nm）的8YSZ粉体；
3）称取0.3g的8YSZ粉体，倒入研钵中，再滴入8YSZ粉体质量20%的步骤1）中所制得的乙酸溶液，混合研磨至均匀；
4）将湿润的8YSZ粉体放入磨具中，置于液压机中，其中温度和压力分别设定为120℃和350MPa，进行压制成型，保压30min后得到8YSZ陶瓷生坯；
5）取出模具中的8YSZ陶瓷生坯，置于马弗炉中烧结4h，烧结温度设定为1200℃，得到8YSZ陶瓷片；
6）将所得的8YSZ陶瓷片再次放入马弗炉中，让其在600℃下进行退火4小时，退火后即为陶瓷片成品通过维氏硬度仪测得其硬度为11.5GPa，相对密度达到97.8%。
实施例2
一种提高YSZ硬度的方法，包括以下步骤：
1）用量筒称取适量的柠檬酸，滴入去离子水后，通过pH试纸调控，获得pH值为3的柠檬酸溶液；
2）称取5g的8YSZ粉末，加入酒精进行球磨后，在80℃下干燥，获得粒径较为均匀（150-200nm）的8YSZ粉体；
3）称取0.3g的8YSZ粉体，倒入研钵中，再滴入8YSZ粉体质量20%的步骤1）中所制得的柠檬酸溶液，混合研磨至均匀；
4）将湿润的8YSZ粉体放入磨具中，置于液压机中，其中温度和压力分别设定为150℃和350MPa，进行压制成型，保压20min后得到8YSZ陶瓷生坯；
5）取出模具中的8YSZ陶瓷生坯，置于马弗炉中烧结4h，烧结温度设定为1200℃，得到8YSZ陶瓷片；
6）将所得的8YSZ陶瓷片再次放入马弗炉中，让其在700℃下进行退火4小时，退火后即为陶瓷片成品通过维氏硬度仪测得其硬度为10.1GPa，相对密度达到95.8%。
实施例3
一种提高YSZ陶瓷硬度的方法，包括以下步骤：
1）用量筒称取适量的乙酸，滴入去离子水后，通过pH试纸调控，获得pH值为5的乙酸溶液；
2）称取5g的8YSZ粉末，加入酒精进行球磨后，在80℃下干燥，获得粒径较为均匀（150-200nm）的8YSZ粉体；
3）称取0.3g的8YSZ粉体，倒入研钵中，再滴入8YSZ粉体质量10%的步骤1）中所制得的乙酸溶液，混合研磨至均匀；
4）将湿润的8YSZ粉体放入磨具中，置于液压机中，其中温度和压力分别设定为120℃和350MPa，进行压制成型，保压30min后得到8YSZ陶瓷生坯；
5）取出模具中的8YSZ陶瓷生坯，置于马弗炉中烧结4h，烧结温度设定为1100℃，最终得到8YSZ陶瓷片；
6）将所得的8YSZ陶瓷片再次放入马弗炉中，让其在800℃下进行退火4小时，退火后即为陶瓷片成品通过维氏硬度仪测得其硬度为9.5GPa，相对密度达到93.9%。
对比例
一种提高YSZ硬度的方法，包括以下步骤：
1）用量筒称取适量的去离子水；
2）称取5g的8YSZ粉末，加入酒精进行球磨后，在80℃下干燥，获得粒径较为均匀（150-200nm）的8YSZ粉体；
3）称取0.3g的8YSZ粉体，倒入研钵中，再滴入8YSZ粉体质量20%的步骤1）中的去离子水，混合研磨至均匀；
4）将湿润的8YSZ粉体放入磨具中，置于液压机中，其中温度和压力分别设定为150℃和350MPa，进行压制成型，保压20min后得到8YSZ陶瓷生坯；
5）取出模具中的8YSZ陶瓷生坯，置于马弗炉中烧结4h，烧结温度设定为1200℃，得到8YSZ陶瓷片；
6）将所得的8YSZ陶瓷片再次放入马弗炉中，让其在700℃下进行退火4小时，退火后即为陶瓷片成品通过维氏硬度仪测得其硬度为8.1GPa，相对密度为82.5%.
图1反应了实例1-3及对比例中的硬度大小，说明了加入酸性物质有利于提高8YSZ陶瓷的硬度。
图2反应了实例1-3及对比例中陶瓷的致密度情况，可以看出8YSZ在加入酸性物质的情况下，密度有明显的提高。
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。

Claims (1)

1.一种提高8YSZ硬度的方法，其特征在于：其包括以下步骤：
1）称取适量的酸性物质，滴入去离子水后，通过pH试纸调控，获得pH值为1-6的偏酸性溶液；
2）称取一定量的8YSZ粉末，加入酒精进行球磨后，在80℃下干燥，获得粒径为150-200nm的8YSZ粉体；
3）称取适量的8YSZ粉体，倒入研钵中，再滴入8YSZ粉体质量5%-20%的步骤1）中所制得的偏酸性溶液，混合研磨至均匀；
4）将湿润的8YSZ粉体放入磨具中，置于液压机中，其中温度和压力分别设定为120-300℃和200-500MPa，进行压制成型，保压10-60min后得到8YSZ陶瓷生坯；
5）取出模具中的8YSZ陶瓷生坯，置于马弗炉中烧结2-10h，烧结温度设定为1100-1400℃，得到8YSZ陶瓷片；
6）将所得的8YSZ陶瓷片再次放入马弗炉中，让其在600-800℃下进行退火4小时，退火后即为陶瓷片成品；
步骤1）中的酸性物质为乙酸、甲酸、柠檬酸或硝酸。
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