CN106278290B - 基于低浓度琼脂糖、低固含量浆料的致密陶瓷凝胶注模成型方法 - Google Patents
基于低浓度琼脂糖、低固含量浆料的致密陶瓷凝胶注模成型方法 Download PDFInfo
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Abstract
本发明属于陶瓷材料技术领域,具体公开了一种基于低浓度琼脂糖、低固含量浆料的致密陶瓷凝胶注模成型方法,包括将陶瓷粉体、分散剂和琼脂糖一次性加入到水中配制成固相体积分数为20‑30%、琼脂糖浓度为1.3‑2.5wt%的混合悬浮浆料,接着调节其pH为10后依次进行球磨、除泡、注入模具加热处理,待模具自然冷却后经多步干燥得生坯,最后烧结得致密度为95‑99%的陶瓷。本发明方法一次性将各种原料配成低固相含量、低琼脂糖浓度的混合悬浮浆料,直接进行球磨和真空除泡处理,倒入模具后不需要搅拌,不会带入气泡影响陶瓷的致密性,除泡效果优异效率高,此外由于琼脂糖浓度超低用量极少,陶瓷浆料的固相含量也很低,因此烧结高致密陶瓷的成本很低。
Description
技术领域
本发明属于陶瓷材料技术领域,具体涉及一种基于低浓度琼脂糖、低固含量浆料的致密陶瓷凝胶注模成型方法。
背景技术
美国橡树岭国家实验室于上世纪90年代初发明的一种陶瓷净尺寸成型技术—凝胶注模成型,其AM-MBAM体系是被大量用于工业化生产的凝胶体系,但是AM和MBAM具有神经毒素,接触后极易被皮肤吸收影响人体健康。
近年来,利用天然多糖来凝胶注模成型开始受到关注。琼脂糖是一种天然的多糖,在水中加热到90℃以上可以溶解,当温度下降到35-40℃时形成良好的半固体状的水凝胶。琼脂糖作凝胶介质有很多优点:制备过程简单可控,环保,无毒,坯体具有一定的强度,有机物含量较少,烧结前不需要排胶等等。
现有技术中采用高固相体积分数、高固含量(大于50vol%)的陶瓷浆料制备出来的陶瓷难以达到很高的致密度,且制备过程效率不高,成本也随之增高。高固含量的陶瓷浆料真空除泡工艺在一定程度上除掉了气泡,但是注模前将溶解的高浓度琼脂糖溶液加入到真空除泡后的陶瓷浆料中往往需要搅拌均匀才能成型。然而由于高浓度的琼脂糖、高固相含量的陶瓷浆料粘度较大,搅拌过程中产生的气泡无法自己排出,致使最终陶瓷产品的致密度降低。本发明提供的低浓度琼脂糖溶液、低固含量浆料的致密陶瓷凝胶注模成型方法在一定程度上解决了上述工艺上的困难,同时还降低了成本。
发明内容
本发明的目的在于解决现有技术存在的不足,提供一种基于低浓度琼脂糖、低固含量浆料的致密陶瓷凝胶注模成型方法,该方法真空除泡效率高,不会带来气泡使陶瓷坯体产生缺陷,采用该方法可烧制出形状复杂、大小各异、显微结构均匀、致密度高达95-99%的陶瓷。本发明解决上述技术问题的技术方案如下:
一种基于低浓度琼脂糖、低固含量浆料的致密陶瓷凝胶注模成型方法,包括以下步骤:将陶瓷粉体、分散剂和琼脂糖一次性加入到水中配制成混合悬浮浆料,调节混合悬浮浆料的pH为碱性后球磨均匀,对球磨后的混合浆料进行除泡处理,将除泡后的混合浆料注入无孔模具中加热,待无孔模具自然冷却后经多步干燥得陶瓷生坯,最后烧结得致密度为95-99%的陶瓷。
上述方案中,所述混合悬浮浆料的固相体积分数为20-30%,琼脂糖含量为1.3-2.5wt%,分散剂用量占陶瓷粉体质量的0.6-1.0%。
上述方案中,所述陶瓷粉体为氧化锆、氧化铝中的一种,所述分散剂为柠檬酸铵、聚丙烯酸铵中的一种。
上述方案中,使用pH调节剂调节混合悬浮浆料的pH至10后球磨20-32h,所述pH调节剂选自PH缓冲液、氨水以及尿素中的一种。
上述方案中,除泡处理具体为在室温条件下将混合浆料真空震荡除泡30min。
上述方案中,除泡后的混合浆料直接在室温下注入到无孔模具中并且不搅拌,接着将无孔模具置于110℃环境下充分加热2-3h。
上述方案中,所述无孔模具材质为金属、聚四氟乙烯以及玻璃中的一种。
与高浓度琼脂糖、高固含量陶瓷凝胶注模成型工艺相比,本发明方法具有以下有益效果:(1)一次性将陶瓷粉体、琼脂糖和分散剂配成低固相含量、低琼脂糖浓度的混合悬浮浆料,直接将其球磨均匀并真空除泡;(2)混合浆料直接加热不需要搅拌,不会带入气泡影响陶瓷的致密性;(3)真空震荡除泡效果优异,效率高;(4)陶瓷生坯中有机物含量极少,不需要排胶,干燥成型过程不会开裂;(5)由于琼脂糖浓度超低用量极少,陶瓷浆料的固相含量很低,烧结高致密陶瓷的成本很低;(6)制备出来的陶瓷生坯具有一定的强度,可以在烧结前进行加工;(7)可以制成形状复杂、大小各异且致密度高达95-99%的陶瓷部件。
具体实施方式
为使本领域普通技术人员充分理解本发明的技术方案和有益效果,以下结合具体实施例进行进一步说明,应当说明的是下述实施例仅用于说明而不构成对本发明技术方案的限定,在不违背本发明构思的基础上进行的任何简单变换、组合、修改均应落入本发明的保护范围之内。
实施例1
量取16.8ml蒸馏水加入到球磨罐中,将共计26g的氧化锆粉体(理论密度为6.1g/cm3,粒径为1um),0.221g琼脂糖粉末和质量分数为0.6%的柠檬酸铵(约0.156g)一次性加入到球磨罐中搅拌均匀,制成固相体积分数为20.2%、琼脂糖浓度为1.3wt%的混合悬浮浆料。用氨水将所得混合浆料的pH调节至10,球磨20小时之后在室温条件下真空震荡除泡30分钟。真空除泡完成后,室温下将混合浆料注入无孔玻璃模具内,接着将模具放入110℃环境下充分加热2小时,该过程中混合浆料无需搅拌。待其冷却到室温且完全成型后,经过多步干燥获得强度较高的氧化锆生坯,最后烧结制得致密度约为99%的氧化锆陶瓷。
实施例2
量取16.8ml蒸馏水加入到球磨罐中,将共计43.9g的氧化锆粉体(理论密度为6.1g/cm3,粒径为1um),0.431g琼脂糖粉末和质量分数为1%的柠檬酸铵(约0.439g)一次性加入到球磨罐中搅拌均匀,制成固相体积分数为30%、琼脂糖浓度为2.5wt%的混合悬浮浆料。用尿素将所得混合浆料的pH调节至10,球磨32小时之后在室温条件下真空震荡除泡30分钟。真空除泡完成后,室温下将混合浆料注入无孔金属模具内,接着将模具放入110℃环境下充分加热3h,该过程中混合浆料无需搅拌。待其冷却到室温且完全成型后,经过多步干燥获得强度较高的氧化锆生坯,最后烧结制得致密度约为98%的氧化锆陶瓷。
实施例3
量取34.3ml蒸馏水加入到球磨罐中,将共计35.2g的氧化铝粉体(理论密度为3.97g/cm3),0.5g琼脂糖粉末和质量分数为1%的柠檬酸铵(约0.352g)一次性加入到球磨罐中搅拌均匀,制成固相体积分数为20.5%、琼脂糖溶度为1.4wt%的氧化铝陶瓷浆料。用尿素将所得混合浆料的pH调节至10,球磨24小时之后在室温条件下真空震荡除泡30分钟。真空除泡完成后,室温下将混合浆料注入无孔聚四氟乙烯模具内,接着将模具放入110℃环境下充分加热2h,该过程中混合浆料无需搅拌。待其冷却到室温且完全成型后,经过多步干燥获得强度较高的氧化铝生坯,最后烧结制得致密度大约为95%的氧化铝陶瓷。
实施例4
量取34.3ml蒸馏水加入到球磨罐中,将共计35.2g的氧化铝粉体(理论密度为3.97g/cm3),0.7琼脂糖粉末和质量分数为1%的柠檬酸铵(约0.352g)一次性加入到球磨罐中搅拌均匀,制成固相体积分数为20.5%、琼脂糖浓度为2wt%的混合悬浮浆料。用PH缓冲液将所得混合浆料的pH调节至10,球磨24小时之后在室温条件下真空震荡除泡30分钟。真空除泡完成后,室温下将混合浆料注入无孔玻璃模具内,接着将模具放入110℃环境下充分加热2h,该过程中混合浆料无需搅拌。待其冷却到室温且完全成型后,经过多步干燥获得强度较高的氧化铝生坯,最后烧结制得致密度大约为95%的氧化铝陶瓷。
本发明实施例1-4致密陶瓷凝胶注模成型方法工艺较为简单,制备出的陶瓷生坯有一定的强度可适当进行加工,该陶瓷生坯中有机物含量极少,不需要额外排胶,分步干燥成型过程也没有开裂现象,最终成品陶瓷的致密度高达95-99%。
Claims (4)
1.一种基于低浓度琼脂糖、低固含量浆料的致密陶瓷凝胶注模成型方法,其特征在于,包括以下步骤:
将陶瓷粉体、分散剂和琼脂糖一次性加入到水中配制成混合悬浮浆料,调节混合悬浮浆料的pH为碱性后将其球磨均匀,对球磨后的混合浆料进行除泡处理,将除泡后的混合浆料注入无孔模具中加热,待无孔模具自然冷却后经多步干燥得陶瓷生坯,最后烧结得致密度为95-99%的陶瓷;
其中,所述混合悬浮浆料的固相体积分数为20-30%,琼脂糖含量为1.3-2.5wt%,分散剂用量为陶瓷粉体质量的0.6-1.0%;采用pH调节剂调节混合悬浮浆料的pH至10后球磨20-32h,所述pH调节剂选自pH 缓冲液、氨水以及尿素中的一种;除泡后的混合浆料直接在室温下注入到无孔模具中,不用搅拌,接着将无孔模具在110℃环境下充分加热2-3h。
2.如权利要求1所述的一种基于低浓度琼脂糖、低固含量浆料的致密陶瓷凝胶注模成型方法,其特征在于:所述陶瓷粉体为氧化锆、氧化铝中的一种,所述分散剂为柠檬酸铵、聚丙烯酸铵中的一种。
3.如权利要求1所述的一种基于低浓度琼脂糖、低固含量浆料的致密陶瓷凝胶注模成型方法,其特征在于:除泡处理具体为在室温条件下将混合浆料真空震荡除泡30min。
4.如权利要求1所述的一种基于低浓度琼脂糖、低固含量浆料的致密陶瓷凝胶注模成型方法,其特征在于:所述无孔模具材质为金属、聚四氟乙烯以及玻璃中的一种。
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