CN105461310A - 一种凝胶注模成型异形陶瓷坯体的制备方法 - Google Patents
一种凝胶注模成型异形陶瓷坯体的制备方法 Download PDFInfo
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Abstract
本发明一种凝胶注模成型异形陶瓷坯体的制备方法，以去离子水为溶剂，将粘结剂、助剂和分散剂加入去离子水中，搅拌10-30min，制得溶液，所述的分散剂、粘结剂、助剂和去离子水的质量比为（0.15-1.5）：（1-3）：（0.45-0.9）：100，向上述溶液中加入陶瓷粉体，陶瓷粉体和去离子水的质量比为（160-650）：100，球磨，将得到的浆料在真空条件下除气，制得陶瓷浆料，将得到的陶瓷浆料注入模具中，在30-80℃条件下固化，然后脱模、干燥，制得凝胶注模成型异形陶瓷坯体。本发明的制备方法有机物总量低，生产成本低，容易控制，陶瓷素坯强度高，表面光滑，完好光洁，尤其适用于复杂形状陶瓷部件的成型。
Description
技术领域
本发明属于陶瓷制备技术领域，涉及一种异形陶瓷坯体的制备方法，具体来说是一种凝胶注模成型陶瓷坯体的制备方法。
背景技术
陶瓷坯体成型是陶瓷材料制备工艺中的一个关键环节，成型过程造成的缺陷往往很难在其后的烧结工艺中予以消除，所以它直接影响材料的结构和性能。传统的成型工艺(如干压成型)很难制备异形形状的陶瓷部件；而普通注浆成型只限于薄壁陶瓷部件，对于厚壁陶瓷坯体内部存在密度梯度，烧成时容易产生缺陷和开裂。
20世纪90年代以来，许多科研机构致力于新型胶态成型技术的研究，取得了一定的进展。其中最为成功的例子是美国橡树岭实验室于1991年提出的注凝成型技术。该工艺利用有机单体聚合反应形成的三维网络凝胶，使陶瓷浆料固化成具有相当强度的坯体。该工艺适用于多种陶瓷体系，获得的坯体强度高，均匀性好，可进行机械加工。另“制备陶瓷生坯的方法”(CN1705545A)通过模具给生坯加热制备坯体，使溶剂从生坯中脱离出来至生坯表面和模具之间形成溶剂膜，易于脱模，制备的坯体表面光滑、外观无损伤；“一种陶瓷坯体增强剂及应用”(CN103420680)以羧甲基纤维素钠、膨润土和焦磷酸钠不同配比制成的增强剂制备陶瓷坯体，所制备的陶瓷坯体强度高、易于成型，提高粉体的结合性能，改善坯体在输送线上的振动、变形等问题；“水溶性环氧树脂原位固化制备陶瓷坯体的方法”(CN1864961A)以聚乙烯亚胺或二丙三胺和水溶性的环氧树脂原位固化制备陶瓷坯体，所制备的陶瓷坯体强度高和韧性好，用于氧化物陶瓷、非氧化物陶瓷或复合陶瓷的成型。但是以上方法存在很明显的不足:
⑴、由于空气中的氧气会阻碍聚合反应，因此坯体表面聚合反应不完全，干燥后会剥落，无法制备出完好的陶瓷坯体。为了克服表面氧气的阻聚，目前采用的方法是在惰性气氛保护下进行固化。这样不但设备要求大大提高，而且工艺复杂，难以推广应用。
⑵、所用的有机物用量较大，且毒性较大，如单体丙烯酰胺、亚甲基双丙烯酰胺、固化剂聚乙烯亚胺对眼睛、皮肤、呼吸道和黏膜都有刺激作用，会危害操作人员的健康；同时烧结过程中有机物的燃烧产生大量的废气，对环境污染严重，更加使得该工艺不易被接受。
⑶、此类方法制备过程中有机物用量比较大，成本比较高，不适于规模化生产。而其它一些新型胶态成型技术(如直接凝固成型、温度诱导絮凝成型)因为只适用于少数陶瓷体系，而且所得坯体强度低，难以推广产业化。
发明内容
针对现有技术中的上述技术问题，本发明提供了一种凝胶注模成型陶瓷坯体的制备方法，所述的这种凝胶注模成型陶瓷坯体的制备方法解决了现有技术中的制备陶瓷坯体的方法工艺复杂、成本高、坯体强度低、对环境污染严重的技术问题。
本发明提供了一种凝胶注模成型异形陶瓷坯体的制备方法，包括下列步骤：
1)以去离子水为溶剂，将粘结剂、助剂和分散剂加入去离子水中，搅拌10-30min，制得溶液，其中，分散剂、粘结剂、助剂和去离子水的质量比为(0.15-1.5)：(0.5-3)：(0.45-0.9)：100；所述分散剂为柠檬酸三铵、聚乙二醇、或者聚丙烯酸及其共聚物中的任意一种，上述物质的纯度为98.50％-99.00％；所述助剂为硅溶胶、或者稀土氧化物中的任意一种，上述物质的纯度为30.00％-50.00％；所述粘结剂为羧甲基纤维素-甲基丙烯酸甲酯接枝共聚物、聚维酮、或者TDE-85环氧树脂中的任意一种，上述物质的纯度为98.00％-99.00％；
2)向上述溶液中加入陶瓷粉体，球磨0.5-1.5h，对得到的浆料在真空条件下除气5～20min；其中，陶瓷粉体和去离子水的质量比为(160-650)：100；所述陶瓷粉体为氧化铝粉体、氧化锆粉体、碳化硅粉体、或者SiC/SiO2复合粉体中的任意一种；
3)将得到的陶瓷浆料注入模具中，在30-80℃条件下固化2-5h，然后脱模，干燥，制得凝胶注模成型异形构件的陶瓷坯体。
最后，将干燥后的素坯进行预烧和无压烧结制得异形陶瓷。
进一步的，所述的模具为由金属、玻璃、橡胶、或者塑料制成的不透水模具中的任意一种。
进一步的，所述干燥是在湿度大于40％的室温下干燥。
本发明的制备方法由于采用了低于现有技术中分散剂、粘结剂、助剂总含量，即有机物的总量与去离子水的质量比为(1.1-5.4):100，大大降低了有机物的用量。更进一步，本发明的制备方法由于采用了与现有技术不同的分散剂、粘结剂、助剂，因而该技术适于氧化物粉体、非氧化物粉体或它们复合粉体不同类型及异形形状陶瓷的成型，所得坯体表面光滑、强度高，且强度较常用的丙烯酰胺体系和水溶性环氧树脂体系增加5％-25％。而且由于采用了与现有技术不同的分散剂、粘结剂、助剂，它们均安全无毒，对操作人员和环境危害小，因此在使用安全性等方面具有了比现有技术更好的技术效果。
本发明和已有技术相比，其技术进步是显著的。本发明的制备方法是一种水溶性胶体成型方法，工艺简单，不需专用设备，生产过程环境友好，对操作人员和环境危害小，有机物总量低，生产成本低，容易控制，陶瓷素坯强度高，表面光滑，完好光洁，尤其适用于复杂形状陶瓷部件的成型，适用范围广，易于规模化生产，应用前景大。
附图说明
图1和图2是本发明实施例1所得坯体经过烧成后的照片，样品表面光洁无剥落。
具体实施方式
下面通过具体的实施例并结合附图对本发明作进一步阐述，但并不限于本发明。
实施例1
以去离子水为溶剂，将分散剂、粘结剂和助剂加入去离子水中，搅拌10min，制得溶液；其中，分散剂：粘结剂：助剂：去离子水的质量比为0.15:1:0.5：100，氧化铝粉体：去离子水的质量比为350：100，氧化铝陶瓷粉平均粒径20μm。用行星式球磨机混合20min，且对得到的浆料在真空条件下除气10min，制得氧化铝浆料，将所述氧化铝浆料注入特制的金属模具中，在80℃条件下固化3h，脱模，在湿度大于50％的室温条件下干燥，制得尺寸良好、表面光洁的氧化铝传感器支撑底座陶瓷坯体。
实施例2
以去离子水为溶剂，将分散剂、粘结剂和助剂加入去离子水中，搅拌10min，制得溶液；其中，分散剂：粘结剂：助剂：去离子水的质量比为0.35：0.5：0.8：100，氧化铝粉体：去离子水的质量比为450：100，氧化铝陶瓷粉平均粒径10μm。用行星式球磨机混合25min，且对得到的浆料在真空条件下除气10min，制得氧化铝浆料，将所述氧化铝浆料注入特制的金属模具中，在80℃条件下固化3.5h，脱模，在湿度大于40％的室温条件下干燥，制得尺寸完好、表面光洁的氧化铝管陶瓷坯体。
实施例3
以去离子水为溶剂，将分散剂、粘结剂和助剂加入去离子水中，搅拌5min，制得溶液；其中，分散剂：粘结剂：助剂：去离子水的质量比为1.5：2.5：0.45：100，氧化锆粉体：去离子水的质量比为650：100，氧化锆陶瓷粉平均粒径50μm。用行星式球磨机混合35min，且对得到的浆料在真空条件下除气15min，制得氧化锆悬浮浆料，将所述氧化锆浆料注入特制的橡胶模具中，在70℃条件下固化2h，然后脱模，在湿度大于70％的室温条件下干燥，可得到形状、尺寸完好的氧化锆异形陶瓷坯体。
实施例4
以去离子水为溶剂，将分散剂、粘结剂和助剂加入去离子水中，搅拌5min，制得溶液；其中，分散剂：粘结剂：助剂：去离子水的质量比为1.25：3：0.9：100，碳化硅粉体：去离子水的质量比为380：100，碳化硅陶瓷粉平均粒径10μm。用行星式球磨机混合40min，且对得到的浆料在真空条件下除气10min，制得碳化硅悬浮浆料，将所述碳化硅浆料注入特制的塑料模具中，在70℃条件下固化30min，然后脱模，将脱模后的坯体放入密闭空间，避免空气流动，放置10h以上，然后在烘箱中60℃条件下干燥2h，可得到结构完整、表面光滑的碳化硅多孔陶瓷坯体。
实施例5
以去离子水为溶剂，将分散剂、粘结剂和助剂加入去离子水中，搅拌5min，制得溶液；其中，分散剂：粘结剂：助剂：去离子水的质量比为0.15：3：0.15：100，SiC/SiO2粉体：去离子水的质量比为480：100，SiC/SiO2陶瓷粉平均粒径25μm。用超声波先后分散SiC/SiO2混合粉体20min，且对得到的浆料在真空条件下除气12min，得到均匀的悬浮液，制得混合浆料，将所述SiC/SiO2均匀混合浆料注入特制的金属模具中，在80℃条件下原位固化2h，然后脱模，在湿度大于80％的室温条件下干燥，可得到形状、尺寸完好的SiC/SiO2复合陶瓷坯体。
实施例6
以去离子水为溶剂，将分散剂、粘结剂和助剂加入去离子水中，搅拌5min，制得溶液；其中，分散剂：粘结剂：助剂：去离子水的质量比为0.80：1.5：0.75：100，抗水化处理的AlON粉体：去离子水的质量比为300：100，AlON陶瓷粉平均粒径20μm。用行星式球磨机混合40min，且对得到的浆料在真空条件下除气20min，制得AlON悬浮浆料，将所述AlON浆料注入特制的橡胶模具中，在40℃条件下固化2h，然后脱模，在湿度大于50％的室温条件下干燥，可得到形状完好、表面光洁的AlON透明陶瓷坯体。
综上所述，本发明的一种凝胶注模成型异形陶瓷坯体的制备方法，是一种水溶性胶体成型方法，工艺简单，不需专用设备，生产过程环境友好，对操作人员和环境危害小,有机物总量低，生产成本低，容易控制，陶瓷素坯强度高，表面光滑，完好光洁，尤其适用于复杂形状陶瓷部件的成型，适用范围广，易于规模化生产，应用前景大。
上述实施例的内容仅为本发明构思下的基本说明，而依据本发明的技术方案所作的任何等效变换，均应属于本发明的保护范围。
Claims (3)
1.一种凝胶注模成型异形陶瓷坯体的制备方法，其特征在于包括下列步骤：
1）以去离子水为溶剂，将粘结剂、助剂和分散剂加入去离子水中，搅拌10-30min，制得溶液，其中，分散剂、粘结剂、助剂和去离子水的质量比为（0.15-1.5）：（0.5-3)：（0.45-0.9）：100；所述分散剂为柠檬酸三铵、聚乙二醇、或者聚丙烯酸及其共聚物中的任意一种，上述物质的纯度为98.50%-99.00%；所述助剂为硅溶胶、或者稀土氧化物中的任意一种，上述物质的纯度为30.00%-50.00%；2）所述粘结剂为羧甲基纤维素-甲基丙烯酸甲酯接枝共聚物、聚维酮、或者TDE-85环氧树脂中的任意一种，上述物质的纯度为98.00%-99.00%；
2）向上述溶液中加入陶瓷粉体，球磨0.5-1.5h，对得到的浆料在真空条件下除气5~20min；其中，陶瓷粉体和去离子水的质量比为(160-650)：100；所述陶瓷粉体为氧化铝粉体、氧化锆粉体、碳化硅粉体、或者SiC/SiO2复合粉体中的任意一种；
3）将得到的陶瓷浆料注入模具中，在30-80℃条件下固化2-5h，然后脱模，干燥，制得凝胶注模成型异形构件的陶瓷坯体。
2.根据权利要求1所述凝胶注模成型异形陶瓷坯体的制备方法，其特征在于：所述的模具为由金属、玻璃、橡胶、或者塑料制成的不透水模具中的任意一种。
3.根据权利要求1所述凝胶注模成型异形陶瓷坯体的制备方法，其特征在于：所述干燥是在湿度大于40%的室温下干燥。
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