CN107010964A - 一种增强超轻泡沫陶瓷坯体强度的方法 - Google Patents
一种增强超轻泡沫陶瓷坯体强度的方法 Download PDFInfo
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Abstract
本发明开发了一种利用聚乙烯醇冷冻解冻增强超轻泡沫陶瓷坯体强度的方法,该方法包括如下步骤:将陶瓷浆料进行球磨分散,加入表面疏水化修饰剂和聚乙烯醇,将浆料的pH值调节至合适的范围,然后对浆料进行机械搅拌发泡得到颗粒稳定泡沫浆料,将所得泡沫浆料进行冷冻解冻得到泡沫凝胶。待泡沫凝胶干燥后直接进行烧结。本方法可以获得气孔率在92~98%之间的超轻干燥陶瓷泡沫坯体(以下简称泡沫坯体)。经过聚乙烯醇冷冻解冻增强后,所获得的超轻泡沫坯体强度得到明显提高,保证其在运输过程中不会被破坏。进一步的,本发明制备的泡沫坯体具有很好的可加工性,可先对其进行切割、雕刻等机械加工后再烧结,降低了泡沫陶瓷的加工成本。
Description
技术领域
本发明属于泡沫陶瓷制备技术领域,具体涉及一种增强超轻泡沫陶瓷坯体强度的方法。
背景技术
泡沫陶瓷具有陶瓷材料和多孔材料的双重优点,因而具有轻质、保温、绝热、耐高温、耐化学腐蚀等许多特点,因此广泛应用于流体过滤,催化剂载体,热、电、声音等绝缘材料以及人工骨骼等领域。
浆料直接发泡法相比于其它方法,更易于制备高气孔率泡沫陶瓷,而且其制备工艺相对简单。直接发泡法的关键在于陶瓷泡沫的稳定性,因为泡沫巨大的表面能以及气体密度低于液体而产生的逸出趋势使得泡沫是一个热力学不稳定体系。传统发泡工艺通过加入表面活性剂、蛋白质等物质可以提高陶瓷泡沫体系的稳定性。近十年发展起来了一种利用陶瓷颗粒本身稳定泡沫浆料的方法——即颗粒稳定泡沫法。该方法是采用具有两亲性的分子修饰氧化物颗粒表面,使其具有部分疏水性从而不可逆的吸附在气/液界面,以抵制泡沫的破裂、排液、歧化、奥斯瓦尔德熟化等不稳定因素。该方法无需附加凝胶等辅助其固化,更加经济、简单。进一步的,该方法可以制备具有高气孔率的泡沫陶瓷,其气孔率一般介于80~95%之间。
干燥后的陶瓷泡沫坯体仅靠陶瓷粉体之间的范德华引力保持坯体完整,其强度很低,在移动过程中外力作用易使其破碎。特别是对颗粒稳定泡沫法制备的泡沫坯体而言,因其具有超高气孔率,从而强度非常低。因此要想实现超轻泡沫陶瓷特别是大尺寸泡沫陶瓷的大批量工业化生产,就必须要克服干燥陶瓷泡沫坯体强度不足的瓶颈。有报道利用硅溶胶或者利用水泥的水化反应增强陶瓷泡沫坯体。但是这些方法都不可避免地引入杂质相,弱化了泡沫陶瓷的强度和使用稳定性。
发明内容
本发明的目的是提供一种增强超轻泡沫陶瓷坯体强度的方法,其特征在于,以常用陶瓷或蓝晶石为粉体原料,利用聚乙烯醇冷冻解冻形成微结晶对陶瓷泡沫坯体进行增强工艺得到高强、超轻泡沫陶瓷坯体,并通过烧结最终制备了微观结构均匀完整的泡沫陶瓷;本方法的前提是制备稳定的陶瓷泡沫浆料,核心是利用聚乙烯醇冷冻解冻形成微结晶对陶瓷泡沫坯体进行增强。聚乙烯醇可以在烧结过程中排除,因此不会引入杂质相,不会弱化泡沫陶瓷的性能。本发明可以制备气孔率在92~98%之间的超轻陶瓷泡沫坯体。所制备的超轻陶瓷泡沫坯体相比不采用增强手段制备的坯体而言,其强度得到明显提高,完全能够满足生产需求,保证其在运输过程中不会被破坏。进一步的,本发明制备的泡沫坯体具有很好的可加工性,可以对泡沫坯体进行切割、雕刻等机械加工。对加工后的泡沫坯体进行烧结,这样可以有效减少烧结后坯体的机械加工量,降低了成本,因此本发明也为泡沫陶瓷的机械加工提供了一条新思路。
具体步骤如下:
(1)以常用陶瓷或蓝晶石中的一种粉体制成陶瓷浆料;
(2)将质量分数为15~60%的陶瓷浆料进行球磨分散;
(3)在球磨后的浆料中加入陶瓷粉体疏水化修饰剂和聚乙烯醇,并将浆料的pH值调节至合适的范围;
(4)通过机械搅拌对浆料进行发泡得到颗粒稳定泡沫;
(5)将发泡后所得泡沫浆料,立刻在-10℃下冷冻12~24h,然后在0~10℃范围内解冻3~12h,重复该冷冻解冻过程1~5次,得到干燥泡沫坯体;干燥泡沫坯体气孔率介于92~98%;
(6)待陶瓷泡沫坯体干燥后在1400~1900℃的烧结温度下进行烧结,冷却后得到微观结构均匀完整的泡沫陶瓷;所制备的泡沫陶瓷孔径均匀,各向同性,孔径分布在30~200μm,陶瓷晶粒之间结合良好。
所述陶瓷粉体的粒径为50nm~4μm。
所述步骤1中陶瓷浆料为氧化铝、氧化锆、蓝晶石、氮化硅或者碳化硅中的一种粉体制成。
所述粉体为氧化铝、氧化锆、蓝晶石时,陶瓷粉体疏水化修饰剂为十二烷基硫酸钠、十六烷基硫酸钠、十八烷基硫酸,疏水化修饰剂添加量为陶瓷浆料质量的0.01~0.5wt%;聚乙烯醇添加量为陶瓷浆料质量的0.5~1.5wt%;陶瓷浆料pH调节为4.0~6.5;上述疏水化修饰剂对相应的陶瓷粉体进行原位修饰,提高疏水性,从而制备稳定的泡沫。
所述陶瓷粉体为氮化硅或碳化硅时,陶瓷粉体疏水化修饰剂为十二烷基氯化铵或者十六烷基氯化铵,添加量为陶瓷浆料质量的0.02~0.3wt%;聚乙烯醇添加量为陶瓷浆料质量的0.3~1.2wt%;陶瓷浆料的pH调节至9.0~11.5之间;上述疏水化修饰剂对相应的陶瓷粉体进行原位修饰,提高疏水性,从而制备稳定的泡沫。
所述氧化铝体系,聚乙烯醇的加入量为0.5~1.5wt%,其烧结温度为1400~1600℃;所述氧化锆体系或蓝晶石体系,聚乙烯醇的加入量为0.5~1.5wt%,其烧结温度为1300~1500℃;所述氮化硅或碳化硅体系,聚乙烯醇的加入量为0.3~1.2wt%,需要在氮气气氛保护下烧结,其烧结温度为1700~1900℃。
本发明的有益效果是:(1)所制备的陶瓷泡沫浆料均匀稳定,无需采用凝胶等方式辅助固化。(2)表面活性剂和坯体增强剂聚乙烯醇添加量较少,烧结时无需排胶工序,工艺简单,生产成本低廉。(3)本发明采用的增强陶瓷泡沫坯体的方法不会引入杂质相,因此不会弱化泡沫陶瓷的性能。(5)所制备的超轻陶瓷泡沫坯体相比不采用增强手段制备的泡沫坯体而言,其强度得到明显提高,能够满足生产需求,为大尺寸泡沫陶瓷的规模化生产提供了一个方案。(6)本发明制备的泡沫坯体具有很好的可加工性,可以对泡沫坯体进行切割、雕刻等机械加工,因此可对泡沫坯体进行先加工再烧结,降低了泡沫陶瓷的加工成本。
附图说明
图1是氧化铝泡沫坯体的宏观照片。
图2是氧化铝泡沫坯体的微观照片。
具体实施方式
本发明提供一种增强超轻泡沫陶瓷坯体强度的方法,是以常用陶瓷或蓝晶石中的一种粉体为原料,利用聚乙烯醇冷冻解冻形成微结晶对陶瓷泡沫坯体进行增强工艺得到高强、超轻泡沫陶瓷坯体,并通过烧结最终制备了微观结构均匀完整的泡沫陶瓷;下面结合附图和实施例予以说明。
实施例1
(1)配制质量分数为20%的氧化铝浆料,利用滚筒球磨机球磨2h。所述氧化铝陶瓷粉体平均粒径为0.41μm。
(2)在球磨后的浆料中加入相对浆料质量0.05wt%的十二烷基硫酸钠和1.0wt%聚乙烯醇,将浆料的pH值调节至4.5。
(3)然后将浆料在1800rmp的转速下机械搅拌10min进行发泡得到颗粒稳定泡沫。
(4)将发泡后所得泡沫浆料立刻在-10℃下冷冻20h,然后在10℃解冻6h。重复所述冷冻解冻过程2次。
(5)将干燥的陶瓷泡沫坯体以3℃/min的升温速率加热至1550℃,然后保温2h。
所制备的氧化铝泡沫坯体如图1氧化铝泡沫坯体的宏观照片所示,气孔率为97.1%,泡沫坯体微观形貌如图2所示。烧结后制备的氧化铝泡沫陶瓷气孔率为95.3%。从图1照片可以看出本发明制备的泡沫坯体具有很好的可加工性,可以对泡沫坯体进行切割、雕刻等机械加工;从图2照片可以看出泡沫坯体气孔分布均匀,各向同性,孔洞完整,陶瓷粉体间结合紧密。
实施例2
(1)配制质量分数为30%的氧化锆浆料,利用滚筒球磨机球磨4h。所述氧化锆陶瓷粉体平均粒径为0.76μm。
(2)在球磨后的浆料中加入相对浆料质量0.06wt%的十六烷基硫酸钠和1.2wt%聚乙烯醇,将浆料的pH值调节至5.1。
(3)然后将浆料在1600rmp的转速下机械搅拌15min进行发泡得到颗粒稳定泡沫。
(4)将发泡后所得泡沫浆料立刻在-10℃下冷冻24h,然后在10℃解冻4h。重复所述冷冻解冻过程3次。
(5)将干燥的陶瓷泡沫坯体以3℃/min的升温速率加热至1400℃,然后保温2h。
所制备的氧化锆泡沫坯体气孔率为95.9%,烧结后制备的氧化锆泡沫陶瓷气孔率为93.4%.
实施例3
(1)配制质量分数为30%的蓝晶石浆料,利用滚筒球磨机球磨5h,蓝晶石粉体平均粒径为0.98μm。
(2)在球磨后的浆料中加入相对浆料质量0.05wt%的十二烷基硫酸钠和0.8wt%聚乙烯醇,将浆料的pH值调节至6.0。
(3)然后将浆料在1800rmp的转速下机械搅拌10min进行发泡得到颗粒稳定泡沫。
(4)将发泡后所得泡沫浆料立刻在-10℃下冷冻24h,然后在10℃解冻3h。重复所述冷冻解冻过程3次。
(5)将干燥的陶瓷泡沫坯体以3℃/min的升温速率加热至1450℃,然后保温2h。
所制备蓝晶石泡沫坯体气孔率为94.8%,烧结后制备的泡沫陶瓷气孔率为92.2%。
实施例4
(1)配制质量分数为30%的氮化硅浆料,利用滚筒球磨机球磨4h。氮化硅粉体平均粒径为0.33μm。
(2)在球磨后的浆料中加入相对浆料质量0.13wt%的十六烷基氯化铵和0.7wt%聚乙烯醇,将浆料的pH值调节至11.2。
(3)将浆料在1400rmp的转速下机械搅拌10min进行发泡得到氮化硅颗粒稳定泡沫。
(4)将发泡后所得泡沫浆料立刻在-10℃下冷冻24h,然后在10℃解冻4h。重复所述冷冻解冻过程3次。
(5)将干燥的陶瓷泡沫坯体在氮气炉内以3℃/min的升温速率加热至1750℃,然后保温3h。
所制备的氮化硅泡沫坯体气孔率为93.9%,烧结后制备的氮化硅泡沫陶瓷气孔率为86.9%。
Claims (7)
1.一种增强超轻泡沫陶瓷坯体强度的方法,其特征在于,以常用陶瓷或蓝晶石为粉体原料,利用聚乙烯醇冷冻解冻形成微结晶对泡沫陶瓷坯体进行增强工艺得到高强、超轻泡沫陶瓷坯体,并通过烧结最终制备了微观结构均匀完整的泡沫陶瓷;具体步骤如下:
(1)以常用陶瓷或蓝晶石中的一种粉体制成陶瓷浆料;
(2)将质量分数为15~60%的陶瓷浆料进行球磨分散;
(3)在球磨后的浆料中加入陶瓷粉体疏水化修饰剂和聚乙烯醇,并将浆料的pH值调节至合适的范围;
(4)通过机械搅拌对浆料进行发泡得到颗粒稳定泡沫;
(5)将发泡后所得泡沫浆料,立刻在-10℃下冷冻12~24h,然后在0~10℃范围内解冻3~12h,重复该冷冻解冻过程1~5次;得到泡沫陶瓷坯体;干燥泡沫坯体气孔率介于92~98%;
(6)待陶瓷泡沫坯体干燥后在烧结温度为1400~1900℃下进行烧结,冷却后得到微观结构均匀完整的泡沫陶瓷。
2.根据权利要求1所述一种增强超轻泡沫陶瓷坯体强度的方法,其特征在于,所述陶瓷粉体的粒径为50nm~4μm。
3.根据权利要求1所述一种增强超轻泡沫陶瓷坯体强度的方法,其特征在于,所述步骤1中陶瓷浆料为氧化铝、氧化锆、蓝晶石、氮化硅或者碳化硅中的一种粉体制成。
4.根据权利要求1所述一种增强超轻泡沫陶瓷坯体强度的方法,其特征在于,所述陶瓷粉体为氧化铝、氧化锆、蓝晶石时,粉体疏水化修饰剂为十二烷基硫酸钠、十六烷基硫酸钠、十八烷基硫酸,疏水化修饰剂添加量为陶瓷浆料质量的0.01~0.5wt%;聚乙烯醇添加量为陶瓷浆料质量的0.5~1.5wt%;陶瓷浆料pH调节为4.0~6.5;上述疏水化修饰剂对相应的陶瓷粉体进行原位修饰,提高疏水性,从而制备稳定的泡沫陶瓷。
5.根据权利要求3所述一种增强超轻泡沫陶瓷坯体强度的方法,其特征在于,所述陶瓷粉体为氮化硅或者碳化硅时,陶瓷粉体疏水化修饰剂为十二烷基氯化铵或者十六烷基氯化铵,添加量为陶瓷浆料质量的0.02~0.3wt%;聚乙烯醇添加量为陶瓷浆料质量的0.3~1.2wt%;陶瓷浆料的pH调节至9.0~11.5之间;上述疏水化修饰剂对相应的陶瓷粉体进行原位修饰,提高疏水性,从而制备稳定的泡沫陶瓷。
6.根据权利要求4所述一种增强超轻泡沫陶瓷坯体强度的方法,其特征在于,所述陶瓷粉体为氧化铝时,其烧结温度为1400~1600℃;所述陶瓷粉体为氧化锆或蓝晶石时,烧结温度为1300~1500℃;所述陶瓷粉体为氮化硅或碳化硅时,在氮气气氛保护下,1700~1900℃烧结;由于聚乙烯醇的加入量非常少,因此无需排胶,直接进行烧结。
7.根据权利要求1所述一种增强超轻泡沫陶瓷坯体强度的方法,其特征在于,所述制备稳定的泡沫陶瓷的孔径均匀,各向同性,孔径分布在30~200μm,陶瓷晶粒之间结合良好。
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