CN113999044B - 一种多孔陶瓷板及其制备方法 - Google Patents

一种多孔陶瓷板及其制备方法 Download PDF

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CN113999044B
CN113999044B CN202111337494.9A CN202111337494A CN113999044B CN 113999044 B CN113999044 B CN 113999044B CN 202111337494 A CN202111337494 A CN 202111337494A CN 113999044 B CN113999044 B CN 113999044B
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ceramic plate
porous ceramic
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CN113999044A (zh
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张昕
孙正斌
宋运运
裴亚星
刘勋
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Zhengzhou Research Institute for Abrasives and Grinding Co Ltd
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Abstract

本发明涉及一种防静电吸光多孔陶瓷板，其主要由下述重量百分比原料制成：三氧化二铬25‑62%，三氧化二铁24‑37%，氧化亚镍2‑29%，二氧化锰0‑14%，二氧化硅2‑16%，矿化剂0.6‑8%。本发明多孔陶瓷体积电阻率为106‑109Ω·cm，反射率不高于5%，气孔率为20‑50%，孔径为1‑50μm，具备防静电功能和低反射吸光功能，可减少对半导体晶圆、显示面板的静电伤害和对光学检测的曝光干扰。

Description

一种多孔陶瓷板及其制备方法
技术领域
本发明属于多孔陶瓷技术领域，具体涉及一种防静电吸光多孔陶瓷板及其制备方法。
背景技术
多孔陶瓷板在半导体、显示面板、光学元件等多行业里被用作吸附固定、气浮、运输的工作台，此外也可用作水处理、气体分离、燃料电池支撑体等。随着半导体晶圆和显示面板逐渐轻薄、尺寸增大，在工作台的使用过程中，会因为静电摩擦和静电释放产生异常电流，从而造成静电伤害以及大幅降低产品良率。而伴随着光学检测技术的发展，在工作台上方会设置各种光源，用来吸收干扰光线，减少曝光导致的检测误差。因此，对工作台的吸光性提出了更高的要求，要求多孔陶瓷为黑色吸光材质。
目前的多孔陶瓷板多为氧化铝和碳化硅材料，绝缘色浅，其体积电阻率为1010-1014Ω·cm，反射率高于40%，高的电阻值会引起静电伤害，而高的反射率会导致曝光干扰检测，无法满足工作台对多孔陶瓷防静电性能和低反射吸光性能的需求。因此，亟待研发低电阻率、低反射率的多孔陶瓷板。
发明内容
本发明目的在于克服现有技术缺陷，提供一种防静电吸光多孔陶瓷板，该多孔陶瓷体积电阻率为106-109Ω·cm，反射率不高于5%，气孔率为20-50%，孔径为1-50μm，具备防静电功能和低反射吸光功能，可减少对半导体晶圆、显示面板的静电伤害和对光学检测的曝光干扰。
本发明还提供了上述防静电吸光多孔陶瓷板的制备方法，该多孔陶瓷板的原材料成本低，制备工序简单，烧成温度低，适于大规模生产，低碳环保。
为实现上述目的，本发明采用如下技术方案：
一种防静电吸光多孔陶瓷板，其主要由下述重量百分比原料制成：三氧化二铬25-62%，三氧化二铁24-37%，氧化亚镍2-29%，二氧化锰0-14%，二氧化硅2-16%，矿化剂0.6-8%。
上述的防静电吸光多孔陶瓷板，进一步优选的，三氧化二铁+三氧化二铬的质量之和是氧化亚镍+二氧化锰的两倍以上。
上述的防静电吸光多孔陶瓷板，进一步优选的，三氧化二铁与三氧化二铬的质量比为0.5-1.2：1。
具体的，所述矿化剂可以为氧化钙、氧化钡、氧化硼、硝酸钾和氟化钠等中的一种或两种以上的混合物。
本发明还提供了上述防静电吸光多孔陶瓷板的制备方法，其包括如下步骤：
1）混合：按比例取各原料，倒入混合机中混合好后获得粉料，加入粉料重量5-20%的造孔剂、3-10%的临时粘结剂，在制粒机中完成制粉；
2）成型：将混合好的粉料倒入模具中压制成陶瓷板；
3）在空气或氧气气氛中进行烧结即得多孔陶瓷板。该多孔陶瓷板体积电阻率为106-109Ω·cm，反射率低于5%，气孔率为20-50%，孔径为1-50μm。
具体的，所述造孔剂可以为淀粉、碳粉、石墨、树脂粉、聚苯乙烯或聚甲基丙烯酸甲酯等。混合机可以为球磨机、高速混合机、三维混料机、V型混合机、方锥混合机、双锥混合机等。
具体的，所述临时粘结剂可以为羧甲基纤维素（CMC）或酚醛树脂。进一步的，为了提高混合效率，临时粘结剂优选以羧甲基纤维素水溶液或酚醛树脂液等形式加入。
进一步优选的，烧结过程具体为：300-1000min升温至450-600℃并保温100-300min，然后200-600min升温至1000-1250℃并保温60-240min，2000min以上缓慢降温至室温。
本发明多孔陶瓷板制备过程中，采用空气或氧气氧化气氛烧结是为了让各氧化物保持高价态，保证最终呈色，降低多孔陶瓷板的反射率，且造孔剂和临时粘结剂在氧化气氛中也能充分燃烧排出。450-600℃保温的目的是为了充分排出有机物。2000min以上缓慢降温的目的是为了防止开裂。
本发明的创新点和关键点在于多孔陶瓷板的配方（包括粉料的成分和比例，矿化剂的选择，造孔剂的成分和比例）以及制备过程中涉及的烧结气氛和烧结制度，这是实现防静电性能和吸光性能的关键。与现有技术相比，本发明的有益效果是：
1）与现有多孔陶瓷板相比，本发明的多孔陶瓷板体积电阻率为106-109Ω·cm，低于现有的1010-1014Ω·cm，具备防静电功能，可减少对半导体晶圆、显示面板等工件的静电伤害，提高了产品的良品率；
2）与现有多孔陶瓷板相比，本发明的多孔陶瓷板反射率不高于5%，远远低于现有的反射率40%，吸光性能大大提高，用于光学检测时，可吸收干扰光线，减少了曝光导致的检测误差，提高了检测效率。
附图说明
图1为实施例1制备所得多孔陶瓷板的SEM图；
图2为实施例2制备所得多孔陶瓷板的SEM图；
图3为实施例3制备所得多孔陶瓷板的SEM图。
具体实施方式
以下结合实施例对本发明的技术方案作进一步地详细介绍，但本发明的保护范围并不局限于此。
下述实施例中，所用原料均为可以直接购买的普通市售产品。三氧化二铬、三氧化二铁、氧化亚镍、二氧化锰、二氧化硅以及矿化剂均采用工业级99%含量的325目全过筛细粉。
实施例1
一种防静电吸光多孔陶瓷板，其主要由下述重量百分比原料制成：三氧化二铬52%，三氧化二铁26%，氧化亚镍2%，二氧化锰0%，二氧化硅16%，氧化钡2%，氟化钠2%。
本发明还提供了上述防静电吸光多孔陶瓷板的制备方法，其包括如下步骤：
1）混合：按比例取各原料，倒入混合机中混合好后获得粉料，加入粉料重量20%的淀粉造孔剂、粉料重量10%的临时粘结剂甲基纤维素水溶液（甲基纤维素水溶液的固含量为2wt%），在制粒机中完成制粉；
2）成型：将混合好的粉料倒入模具中压制成陶瓷板；
3）将制好的陶瓷板放入空气炉中进行烧结：烧结过程具体为：1000min升温至500℃并保温300min，然后200min升温至1000℃并保温200min，2100min缓慢降温至室温，制得防静电吸光多孔陶瓷板。
对制备所得防静电吸光多孔陶瓷板进行相关性能测定，结果显示：体积电阻率为107Ω·cm，反射率为5%，气孔率为49%，平均孔径为36μm。图1给出了实施例1制备所得多孔陶瓷板的SEM图；图中可以看出：陶瓷板内均匀分布着相互贯通的孔道，孔径范围经测量为15-45μm。
体积电阻率检测方法参考国标《GB/T 1410-2006 材料体积电阻率和表面电阻率实验方法》；反射率检测方法参考国标《GB/T 23981.1-2019 色漆和清漆遮盖力的测定》；气孔率和孔径检测方法参考国标《GB/T 21650.1-2008 压汞法和气体吸附法测定固体材料孔径分布和孔隙度》。
实施例2
一种防静电吸光多孔陶瓷板，其主要由下述重量百分比原料制成：三氧化二铬32%，三氧化二铁31%，氧化亚镍18%，二氧化锰9%，二氧化硅7%，氧化硼2%，氧化钙0.5%，硝酸钾0.5%。
本发明还提供了上述防静电吸光多孔陶瓷板的制备方法，其包括如下步骤：
1）混合：按比例取各原料，倒入混合机中混合好后获得粉料，加入粉料重量10%的淀粉造孔剂、粉料重量8%的临时粘结剂酚醛树脂液（树脂含量为50wt%），在制粒机中完成制粉；
2）成型：将混合好的粉料倒入模具中压制成陶瓷板；
3）将制好的陶瓷板放入空气炉中进行烧结：烧结过程具体为：800min升温至600℃并保温100min，600min升温至1100℃并保温150min，2300min缓慢降温至室温，制得防静电吸光多孔陶瓷板。
对制备所得防静电吸光多孔陶瓷板进行相关性能测定，结果显示：体积电阻率为106Ω·cm，反射率为4%，气孔率为37%，平均孔径为23μm。图2给出了实施例2制备所得多孔陶瓷板的SEM图；图中可以看出：陶瓷板内均匀分布着相互贯通的孔道，孔径范围经测量为10-35μm。
实施例3
一种防静电吸光多孔陶瓷板，其主要由下述重量百分比原料制成：三氧化二铬31%，三氧化二铁37%，氧化亚镍24%，二氧化锰5%，二氧化硅2%，氧化硼0.8%，氟化钠0.2%。
本发明还提供了上述防静电吸光多孔陶瓷板的制备方法，其包括如下步骤：
1）混合：按比例取各原料，倒入混合机中混合好后获得粉料，加入粉料重量5%的淀粉造孔剂、粉料重量5%的临时粘结剂羧甲基纤维素水溶液（甲基纤维素水溶液的固含量为2wt%），在制粒机中完成制粉；
2）成型：将混合好的粉料倒入模具中压制成陶瓷板；
3）将制好的陶瓷板放入空气炉中进行烧结：烧结过程具体为：300min升温至550℃并保温180min，350min升温至1250℃并保温100min，2400min缓慢降温至室温，制得防静电吸光多孔陶瓷板。
对制备所得防静电吸光多孔陶瓷板进行相关性能测定，结果显示：体积电阻率为108Ω·cm，反射率为5%，气孔率为24%，平均孔径为5μm。图3给出了实施例3制备所得多孔陶瓷板的SEM图；图中可以看出：陶瓷板内均匀分布着相互贯通的细小孔道，孔径范围经测量为3-10μm。
实施例4
与实施例1防静电吸光多孔陶瓷板不同之处在于：制备过程中选用造孔剂为石墨。
对制备所得防静电吸光多孔陶瓷板进行相关性能测定，结果显示：体积电阻率为106Ω·cm，反射率为2.8%，气孔率为48%，平均孔径为40μm。
实施例5
与实施例2防静电吸光多孔陶瓷板不同之处在于：制备过程中选用造孔剂为聚苯乙烯。
对制备所得防静电吸光多孔陶瓷板进行相关性能测定，结果显示：体积电阻率为108Ω·cm，反射率为3%，气孔率为36%，平均孔径为15μm。
实施例6
与实施例3防静电吸光多孔陶瓷板不同之处在于：制备过程中选用造孔剂为聚甲基丙烯酸甲酯。
对制备所得防静电吸光多孔陶瓷板进行相关性能测定，结果显示：体积电阻率为108Ω·cm，反射率为4%，气孔率为30%，平均孔径为5μm。
综上可以看出：本发明多孔陶瓷板体积电阻率为106-109Ω·cm，具备防静电功能，可减少对半导体晶圆、显示面板等工件的静电伤害；同时反射率不高于5%，吸光性能大大提高，用于光学检测时，可吸收干扰光线，减少了曝光导致的检测误差，提高了检测效率。

Claims (5)

1.一种多孔陶瓷板，其特征在于，主要由下述重量百分比原料制成：三氧化二铬25-62%，三氧化二铁24-37%，氧化亚镍2-29%，二氧化锰0-14%，二氧化硅2-16%，矿化剂0.6-8%；
所述矿化剂为氧化钙、氧化钡、氧化硼、硝酸钾和氟化钠中的一种或两种以上的混合物；
所述多孔陶瓷板还包括占上述原料总重量5-20%的造孔剂，所述造孔剂为淀粉、碳粉、石墨、聚苯乙烯或聚甲基丙烯酸甲酯。
2.如权利要求1所述的多孔陶瓷板，其特征在于，三氧化二铁+三氧化二铬的质量之和是氧化亚镍+二氧化锰的两倍以上。
3.如权利要求1或2所述的多孔陶瓷板，其特征在于，三氧化二铁与三氧化二铬的质量比为0.5-1.2：1。
4.权利要求1至3任一所述多孔陶瓷板的制备方法，其特征在于，包括如下步骤：
1）混合：按比例取各原料，倒入混合机中混合好后获得粉料，加入粉料重量5-20%的造孔剂、3-10%的临时粘结剂，在制粒机中完成制粉；
2）成型：将混合好的粉料倒入模具中压制成陶瓷板；
3）在空气或氧气气氛中进行烧结，烧结过程具体为：300-1000min升温至450-600℃并保温100-300min，然后200-600min升温至1000-1250℃并保温60-240min，经过2000min以上降温至室温。
5.如权利要求4所述多孔陶瓷板的制备方法，其特征在于，所述临时粘结剂为羧甲基纤维素或酚醛树脂。
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