CN108751998B - 一种氮化硅结合碳化硅陶瓷过滤器及其制备方法 - Google Patents

一种氮化硅结合碳化硅陶瓷过滤器及其制备方法 Download PDF

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CN108751998B
CN108751998B CN201810598516.9A CN201810598516A CN108751998B CN 108751998 B CN108751998 B CN 108751998B CN 201810598516 A CN201810598516 A CN 201810598516A CN 108751998 B CN108751998 B CN 108751998B
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silicon carbide
ceramic filter
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silicon nitride
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李秋南
王惠民
夏志强
吴急涛
黄涛
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Hanjiang Hongyuan Xiangyang Silicon Carbide Special Ceramics Co ltd
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Abstract

本发明公开了一种氮化硅结合碳化硅陶瓷过滤器及其制备方法，该陶瓷过滤器由一定配比的碳化硅砂、高岭土、金属硅粉、添加剂和结合剂制备而成。其制备方法为：1、将高岭土、金属硅粉和添加剂进行球磨，得到小料；2、将结合剂加入碳化硅中，混合均匀，加入小料，混匀，得到混合物料；3、将混合物料进行困料，再混合均匀，得到颗粒料；4、将颗粒料加入模具中压制成型，得到多孔湿坯；5、将湿坯烘干，得到干坯；6、将干坯置于氮化炉中烧结，得到一次烧结品；7、将一次烧结品浸入金属硅粉悬浮液中，取出后继续烧结。该陶瓷过滤器颗粒结合强度高，不掉渣；耐高温；抗热冲击性能和热稳定性能良好；过滤精度高；开孔率高，气孔直径分布集中。该方法简单，操作方便，制备成本低。

Description

一种氮化硅结合碳化硅陶瓷过滤器及其制备方法
技术领域
本发明涉及陶瓷过滤技术领域，具体涉及一种氮化硅结合碳化硅陶瓷过滤器及其制备方法。
背景技术
在铝精炼行业中，常用的板式过滤器为泡沫陶瓷过滤器，泡沫陶瓷过滤器的基本材质有氧化铝，氧化锆和氧化钇，碳化硅三大类。
对于氧化铝类泡沫过滤器而言，其主要问题是耐高温性差、抗热冲击性能差、热稳定性能差和过滤精度低，以30PPI(泡沫过滤器型号)泡沫过滤器为例，对10μm以下的颗粒的过滤能力只有30％，完全达不到精密铝制品过滤要求。
对于氧化锆和氧化钇类泡沫过滤器而言，其主要问题是价格较高，加工时对人体有伤害。如中国专利“一种氧化钇泡沫陶瓷过滤器”(201010511259.4)，该陶瓷过滤器的耐高温性好、强度高和过滤性能好，但其制作工艺复杂，而且氧化钇价格高。
目前，研发较多的是碳化硅类陶瓷过滤器，如中国专利“一种碳化硅陶瓷过滤板”(201410704684.3)，其优点是采用三层结构，具有更加合理的孔梯度，孔径可调，过滤时不易堵塞，其缺点是并未强调其高温时的稳定性，且工艺过于复杂，制备成本相对较高。
发明内容
为了解决现有技术存在的问题，本发明提供了一种氮化硅结合碳化硅陶瓷过滤器的制备方法，该陶瓷过滤板颗粒结合强度高，不掉渣；耐高温；抗热冲击性能和热稳定性能良好，过滤精度高，开孔率高，气孔直径分布集中。
该制作方法简单，操作方便，制备成本低。
实现本发明上述目的所采用的技术方案为：
一种氮化硅结合碳化硅陶瓷过滤器，由以下质量分数的原料制备而成：碳化硅砂75-85％；高岭土1-2％；金属硅粉5-12％；添加剂1-2％；结合剂7-14％。
进一步，所述碳化硅砂的粒度范围为4-50目。
进一步，所述的结合剂的制备方法为：先将结合剂原料和水按质量比为1:10-20的比例混合，再用水浴法进行溶解。
进一步，所述的结合剂原料为聚乙烯醇、糊精、硅酸钠、磺化木质素、羧甲基纤维素、海藻酸盐中的一种或者多种。
进一步，所述的添加剂为钇稳定氧化锆、氧化钇、氮化铝、氧化铝、碳化硼、氮化硼中的一种或多种。
一种氮化硅结合碳化硅陶瓷过滤器的制备方法，包括如下步骤：
1、将高岭土、金属硅粉、添加剂进行干法球磨，球磨至粒径为不大于20μm，得到小料；
2、将粗碳化硅砂加入混合机中，然后加入结合剂，混合均匀，再加入混合粉末后混合均匀，得到混合物料；
3、将混合物料进行困料24-72小时，困料温度为25-40℃，困料结束后，混合均匀，得到湿润的颗粒料；
4、将颗粒料加入模具中，用半干压成型法压制成型，得到多孔湿坯；
5、将湿坯放入烘箱中，在110-180℃下烘干，得到干坯；
6、将干坯置于氮化炉中，以30-100℃/h的速率进行升温，先升温至1000-1200℃，保温1.5-2.5小时，接着升温至1400-1500℃，继续保温1.5-2.5小时，再自然冷却至室温，得到一次烧结品；
7、将一次烧结品浸入金属硅粉悬浮液中，3-8分钟后取出，接着在110-180℃下烘干，得到干燥品；
8、将干燥品置于氮化炉中，以30-100℃/h的速率进行升温，先升温至1000-1200℃，保温1.5-2.5小时，接着升温至1400-1500℃，继续保温1.5-2.5h，再自然冷却至室温，得到所述的碳化硅陶瓷过滤器。
进一步，金属硅粉悬浮液的配制方法为：将金属硅粉与水按1:5-15的比例混合，搅拌均匀。
与现有技术相比，本发明的有益效果和优点在于：
1、该氮化硅结合碳化硅陶瓷过滤器颗粒结合强度高，不掉渣；开孔率高，气孔直径分布集中；过滤速度快，过滤精度高，气孔直径分布集中。
2、该氮化硅结合碳化硅陶瓷过滤器耐高温，且耐腐蚀，适用于1450℃以下的高温工作环境，适用于有色金属铸造精炼过滤，也可用于固相分离领域。
3、该氮化硅结合碳化硅陶瓷过滤器制作工艺简单，制作过程中，分两次烧结，保证产品强度，同时还不会因产生过多纤维状氮化硅而堵塞气孔，保证其孔径大小，进而保证过滤速度。
4、该氮化硅结合碳化硅陶瓷过滤器通过改变碳化硅砂的粒度分布，制成气孔直径不一样的产品，从而获得过滤速度及过滤精度不同的产品。
附图说明
图1为实施例1制备的氮化硅结合碳化硅陶瓷过滤板的过滤效能测试结果图。
图2为实施例4制备的氮化硅结合碳化硅陶瓷过滤板的孔径分布图。
具体实施方式
下面结合具体实施例对本发明进行详细说明。
实施例1
一种氮化硅结合碳化硅陶瓷过滤板，由以下质量分数的原料制备而成：
Figure BDA0001692396890000031
结合剂的制备方法为：先将聚乙烯醇、硅酸钠、木质素磺酸钠和水按2:1:2:75的质量比混合，再在水浴(100℃)中进行溶解。
上述的氮化硅结合碳化硅陶瓷过滤板的制作方法是：
1、将高岭土、金属硅粉、钇稳定氧化锆和碳化硼放入球磨机中，球磨24小时，球磨至小于15μm，得到小料；
2、将粗碳化硅砂加入混合机中，然后加入结合剂，混合均匀，再加入小料后混合均匀，得到粗碳化硅砂外包细粉的混合物料；
3、将混合物料进行困料48小时，困料温度为30℃，困料结束后，混合均匀，得到湿润的颗粒料
4、将颗粒料加入模具中，用半干压成型法压制成型，得到板状的多孔湿坯；
5、将湿坯放入烘箱中，在150℃下烘2小时，得到板状干坯；
6、将干坯置于氮化炉中，以50℃/h的速率进行升温，先升温至1100℃，保温2小时，接着升温至1450℃，继续保温2小时，再自然冷却至室温，得到一次烧结品；
7、将金属硅粉与水按质量比为1:10的比例混合，搅拌均匀，得到金属硅粉悬浮液，将一次烧结品浸入金属硅粉悬浮液中，5分钟后取出，接着在150℃下烘2小时，得到干燥品；
8、将干燥品置于氮化炉中，以50℃/h的速率进行升温，先升温至1100℃，保温2小时，接着升温至1450℃，继续保温2小时，再自然冷却至室温，得到所述的碳化硅陶瓷过滤板。
实施例2-4
实施例2-4与实施例1的制作方法相同，原料配方中仅碳化硅砂的粒度不同，实施例2-4的原料配方如下表1所示：
表1实施例2-4的原料配方
Figure BDA0001692396890000041
将实施例1-4制作的氮化硅结合碳化硅陶瓷过滤板进行测试，测试其抗折强度、气孔率、中值孔径过水速度和过铝液速度，测试结果见下表2：
表2实施例1-4的碳化硅陶瓷过滤板的性能
Figure BDA0001692396890000042
由表2可知，本发明的氮化硅结合碳化硅陶瓷过滤板常温和高温下的强度高，气孔率高，过水速度和过铝液速度大。
将实施例1制备的氮化硅结合碳化硅陶瓷过滤板进行过滤效能测试，所得结果如图1所示，由图1可知，与传统泡沫陶瓷30PPI相比，实施例1制备的氮化硅结合碳化硅陶瓷过滤的过滤性能的优势明显，当固体颗粒物的直径达到50μm以上，实施例制备的陶瓷过滤板的过滤比例大于95％，过滤效果非常好。
将实施例4制备的氮化硅结合碳化硅陶瓷过滤板进行孔径测试，其孔径分布图如图2所示，由图2可知，实施例2制备的氮化硅结合碳化硅陶瓷过滤板的孔径比较集中，集中在400-800μm之间。

Claims (6)

1.一种氮化硅结合碳化硅陶瓷过滤器的制备方法，其特征在于，由以下质量分数的原料制备而成：碳化硅砂75-85%，高岭土1-2%，金属硅粉 5-12%，添加剂 1-2%，结合剂 7-14%；包括如下步骤：
1.1、将高岭土、金属硅粉、添加剂进行干法球磨，球磨至粒径为不大于20μm，得到小料；
1.2、将碳化硅砂加入混合机中，然后加入结合剂，混合均匀，再加入小料后混合均匀，得到混合物料；
1.3、将混合物料进行困料24 -72小时，困料温度25-40℃，困料结束后，混合均匀，得到湿润的颗粒料；
1.4、将颗粒料加入模具中，用半干压成型法压制成型，得到多孔湿坯；
1.5、将湿坯放入烘箱中，在110-180℃下烘干，得到干坯；
1.6、将干坯置于氮化炉中，以30-100℃/h的速率进行升温，先升温至1000-1200℃，保温1.5-2.5小时，接着升温至1400-1500℃，继续保温1.5-2.5小时，再自然冷却至室温，得到一次烧结品；
1.7、将一次烧结品浸入金属硅粉悬浮液中，3-8分钟后取出，接着在110-180℃下烘干，得到干燥品；
1.8、将干燥品置于氮化炉中，以30-100℃/h的速率进行升温，先升温至1000-1200℃，保温1.5-2.5小时，接着升温至1400-1500℃，继续保温1.5-2.5h，再自然冷却至室温，得到所述的碳化硅陶瓷过滤器。
2.根据权利要求1所述的氮化硅结合碳化硅陶瓷过滤器的制备方法，其特征在于：金属硅粉悬浮液的制备方法为：将金属硅粉与水按1:5-15的比例混合，搅拌均匀。
3.根据权利要求1所述的制备方法所制得氮化硅结合碳化硅陶瓷过滤器，其特征在于：所述碳化硅砂的粒度范围为4-50目。
4.根据权利要求3所述的氮化硅结合碳化硅陶瓷过滤器，其特征在于所述的结合剂的制备方法为：先将结合剂原料和水按质量比为1:10-20的比例混合，再用水浴法进行溶解。
5.根据权利要求3所述的氮化硅结合碳化硅陶瓷过滤器，其特征在于：所述的结合剂原料为聚乙烯醇、糊精、硅酸钠、磺化木质素、羧甲基纤维素、海藻酸盐中的一种或者多种。
6.根据权利要求3所述的氮化硅结合碳化硅陶瓷过滤器，其特征在于：所述的添加剂为钇稳定氧化锆、氧化钇、氮化铝、氧化铝、碳化硼、氮化硼中的一种或多种。
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