CN110511021A - 一种新型的氧化锆陶瓷成型方法 - Google Patents
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Abstract
本发明公开了一种新型的氧化锆陶瓷成型方法以及干燥工艺,属于功能陶瓷领域。凝胶注模成型方法制备氧化锆相比传统的注浆成型氧化锆强度更高、成型密度更大,为制备大尺寸及复杂形状的陶瓷制品提供了有效的技术途径。具有很大的发展空间。氧化锆粉体采用超细氧化锆粉体,粒度为d50=0.5μm。其特征在于,采用不同的干燥方式达到快速干燥湿坯,从而缩短工艺流程时间。
Description
技术领域
本发明属于无机非金属材料与功能陶瓷领域,涉及到一种氧化锆陶瓷的成型方法以及干燥工艺。
背景技术
目前,陶瓷的成型方法可以分为两大类,干法成型与湿法成型。干法成型所得到的氧化锆坯体致密性较差,一般只能用来制作一些形状简单的陶瓷产品。湿法成型较干法成型提升了成型后氧化锆陶瓷的致密性,并且大大提高了氧化锆陶瓷生坯以及烧结后强度。
20世纪90年代由美国Janeey和Omatete教授研究出一种全新的胶态快速成型技术,简称凝胶注模成型。凝胶注模成型是一种综合利用了高分子化学、胶体化学、高分子物理与传统陶瓷成型工艺等多种学科的理论的新型成型技术。该技术在制备性能优良且形状复杂的陶瓷零件时十分具有优势,因为其浆料的流动性较好,可以很好的填充满模具,并且陶瓷浆料内粉料分散的均匀,烧结后可形成强度较高的产品。
氧化锆陶瓷在凝胶注模成型中面临问题如下:
目前,1.凝胶注模所用氧化锆粉体多为亚微米或纳米级别陶瓷粉体,由于陶瓷粉体较细,比表面积大,陶瓷粉体容易团聚。凝胶注模成型氧化锆陶瓷的关键在于制备高固相含量、低粘度的浆料,选择合适的分散剂可降低浆料的粘度来提高浆料的固含量,从而可提高氧化锆陶瓷的致密性和强度。2.为了防止湿坯在干燥过程中发生变形,湿坯通常需要至于空气中干燥2~4天,然后再置于电鼓风干燥箱中干燥5~7天,整个工艺流程时间相对较长。
发明内容
发明目的;提供一种陶瓷的成型方法,为了克服传统陶瓷成型方法的不足,制备坯体强度高、相对密度大、复杂形状的近净尺寸精密陶瓷部件,同时选择不同的干燥方式来缩短工艺时间。
技术方案:为解决以上问题,采用以下技术方案实现:
A、以去离子水为溶剂,加入单体、交联剂与防起泡剂,装入球磨罐中球磨5分钟或使用搅拌机强力搅拌15分钟配置成预混液,调节pH为10.5.
B、配置好的预混液中加入氧化锆粉体(体积含量44%~50%),球磨4.5小时配置浆料,加入消泡剂、引发剂与催化剂搅拌后注模,置于真空干燥箱70℃固化。
C、①将固化后的湿坯置于空气中干燥3天,然后再置于电鼓风干燥箱中干燥逐渐升温干燥6天。②将固化后的湿坯置于PEG10000溶液中8h,然后置于电鼓风干燥箱中干燥逐渐升温干燥6天。③将固化后的湿坯置于恒温恒湿箱中干燥12h,湿度逐渐降低,最后至于电鼓风干燥箱中干燥至恒重。
D、将干燥后的氧化锆生坯根据干凝胶的DTA曲线进行烧结至1520℃并保温2小时。
如上述的方法,优选的,单体为甲基丙烯酰胺(MAM)。
如上述的方法,优选的,交联剂为N,N-亚甲基双丙烯酰胺(MBAM)。
如上述的方法,优选的,催化剂为四甲基乙二胺。
如上述的方法,优选的,引发剂为过硫酸铵(APS)。
如上述的方法,优选的,分散剂为2-膦酸丁烷-1,2,4-三羧酸。
如上述的方法,优选的,氧化锆粉体含量为50%。
有益效果:
1.凝胶注模成型氧化锆陶瓷相对与传统的陶瓷成型方法相比,生坯与烧结品强度得到了提高,氧化锆陶瓷成型密度高,内部颗粒致密。
2.使用湿法干燥或使用恒温恒湿干燥箱干燥可大大减少干燥湿坯时间。
附图说明
图1为氧化锆生坯SEM图,图2为氧化锆陶瓷烧结SEM图。
具体实施方式
该发明具体实施步骤如下:
实施例1:
取20ml去离子水加入3g甲基丙烯酰胺,0.56g聚乙烯比咯烷酮,0.2g亚甲基双丙烯酰胺,在球磨机中球磨5min配置预混液,使用氨水调节预混液pH为10.5,加入体积含量为50%的部分钇稳定氧化锆粉体与2wt%(氧化锆分体质量百分比)的2-磷酸丁烷-1,2,4三羧酸,并球磨5h制备浆料。
将制备好的浆料倒入烧杯中并抽真空5min,依次加入正辛醇(浆料质量的0.1%)、过硫酸铵(单体质量的2.5%)与四甲基乙二胺(一滴)搅拌均匀后注入50×10×10模具中,放入70℃真空干燥箱(不抽真空)中固化30min左右。固化完成后脱模,首先将湿坯在空气中干燥3天,然后将湿坯放入电鼓风干燥箱中按照设定的曲线逐渐升温干燥,最终温度设定为100℃,最终将生坯根据TG-DTA曲线设定烧至1520℃保温2h。
经干燥后氧化锆陶瓷生坯抗弯强度达到18.7MPa,生坯密度3.08g/cm3,生坯的干燥收缩率为2.5%,烧结后氧化锆陶瓷抗弯强度达到502.3MPa,体积密度为5.87g/cm3。
实施例2:
取20ml去离子水加入3g甲基丙烯酰胺,0.56g聚乙烯比咯烷酮,0.2g亚甲基双丙烯酰胺,在球磨机中球磨5min配置预混液,使用氨水调节预混液pH为10.5,加入体积含量为50%的部分钇稳定氧化锆粉体与2wt%(氧化锆分体质量百分比)的2-磷酸丁烷-1,2,4三羧酸,并球磨5h制备浆料。
将制备好的浆料倒入烧杯中并抽真空5min,依次加入正辛醇(浆料质量的0.1%)、过硫酸铵(单体质量的2.5%)与四甲基乙二胺(一滴)搅拌均匀后注入50×10×10模具中,放入70℃真空干燥箱(不抽真空)中固化30min左右。固化完成后脱模,将湿坯放入配置好浓度为20%的PEG10000溶液中8h,然后将湿坯按照例1干燥方式进行干燥,最终温度设定为100℃,最后将生坯根据TG-DTA曲线设定烧制1520℃保温2h。
经干燥后氧化锆陶瓷生坯抗弯强度达到12.3MPa,生坯密度2.97g/cm3,生坯的干燥收缩率为2%,烧结后氧化锆陶瓷抗弯强度达到263.4MPa,体积密度为5.73g/cm3。
实施例3:
取20ml去离子水加入3g甲基丙烯酰胺,0.56g聚乙烯比咯烷酮,0.2g亚甲基双丙烯酰胺,在球磨机中球磨5min配置预混液,使用氨水调节预混液pH为10.5,加入体积含量为50%的部分钇稳定氧化锆粉体与2wt%(氧化锆分体质量百分比)的2-磷酸丁烷-1,2,4三羧酸,并球磨5h制备浆料。
将制备好的浆料倒入烧杯中并抽真空5min,依次加入正辛醇(浆料质量的0.1%)、过硫酸铵(单体质量的2.5%)与四甲基乙二胺(一滴)搅拌均匀后注入50×10×10模具中,放入70℃真空干燥箱(不抽真空)中固化30min左右。固化完成后脱模,将湿坯放入恒温恒湿箱中,首先在40℃、98%RH的环境中干燥2h,随后升高温度到80℃干燥2h,然后把湿度降低到40%RH并且把温度升高到100℃干燥3h,最后将坯体放入80℃的烘箱中干燥到恒重。最后将生坯根据TG-DTA曲线设定烧制1520℃保温2h。
经干燥后氧化锆陶瓷生坯抗弯强度达到15.7MPa,生坯密度为2.92g/cm3,生坯干燥收缩率为3%,烧结后氧化锆陶瓷抗弯强度达到274.6MPa,体积密度为5.86g/cm3。
对实施例1所制备的氧化锆生坯及氧化锆陶瓷进行SEM分析,如图1、图2所示,从图1氧化锆生坯观测,氧化锆颗粒之间接触较为紧密,有少数气孔存在,整体来说,氧化锆生坯内部分布较为均匀。
Claims (10)
1.一种凝胶注模成型高强度氧化锆陶瓷的方法,其工艺原理:以去离子水为溶剂,加入单体与交联剂,在催化剂与引发剂的作用下,形成三维网状结构包裹氧化锆粉体,从而能够达到原位固化成型,能够得到高致密度的氧化锆陶瓷坯体。
2.根据权利1所述的成型方法,其特征在于,所采用的氧化锆粉体为部分钇稳定超细粉体,粒径在0.5μm,氧化钇含量为5.25wt%。
3.据权利1所述的成型方法,其特征在于:诉述氧化锆粉体加入量为44%~50%。
4.根据权利1所述的成型方法,其特征在于:所述单体为甲基丙烯酰胺(MAM)。
5.根据权利1所述的成型方法,其特征在于:所述交联剂为N,N-亚甲基双丙烯酰胺(MBAM)。
6.根据权利1所述的成型方法,其特征在于:所述引发剂为过硫酸铵(APS)。
7.根据权利1所述的成型方法,其特征在于:所述催化剂为四甲基乙二胺(TEMED)。
8.根据权利1所述的成型方法,其特征在于:所述分散剂为2-膦酸丁烷-1,2,4-三羧酸或六偏磷酸钠或柠檬酸铵或四甲基乙氢氧化铵。
9.根据权利1所述的成型方法,其特征在于,所属氧化锆凝胶注模成型方法如下步骤:
①配置预混液:将去离子水、交联剂、消泡剂、单体配置成预混液并调节pH,加入氧化锆粉体球磨制备浆料;
②湿坯干燥:将制备好的浆料加入引发剂和催化剂,然后注模,固化,干燥,烧结,得到氧化锆生坯与烧结品;采用三种干燥方式:1.首先在空气中干燥,然后将湿坯置于电鼓风干燥箱中;2.首先将湿坯置于PEG溶液中,然后再将湿坯置于电鼓风干燥箱中;3.使用恒温恒湿箱干燥湿坯;
③烧结:对干凝胶做TG-DTA分析,根据TG-DTA曲线分析设置烧结曲线,最终烧结温度为1520℃,并保温2小时。
10.根据权利9所述,其特征在于:根据步骤②所制氧化锆生坯抗弯强度为10~20MPa,生坯成型密度为2.7~3.1g/cm3;根据步骤③烧成后氧化锆陶瓷抗弯强度为200~500MPa,烧成后氧化锆成型密度为5.6~6g/cm3。
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CN111848157A (zh) * | 2020-06-11 | 2020-10-30 | 深圳美鸣科技有限公司 | 一种凝胶注膜工艺制备的氧化锆瓷块及其制备方法 |
CN113800906A (zh) * | 2021-09-30 | 2021-12-17 | 河南工业大学 | 一种湿法改性纳米氧化锆粉体方法 |
CN116375467A (zh) * | 2023-02-13 | 2023-07-04 | 三祥新材股份有限公司 | 可穿戴设备氧化锆陶瓷背板的制备方法 |
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Cited By (3)
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CN111848157A (zh) * | 2020-06-11 | 2020-10-30 | 深圳美鸣科技有限公司 | 一种凝胶注膜工艺制备的氧化锆瓷块及其制备方法 |
CN113800906A (zh) * | 2021-09-30 | 2021-12-17 | 河南工业大学 | 一种湿法改性纳米氧化锆粉体方法 |
CN116375467A (zh) * | 2023-02-13 | 2023-07-04 | 三祥新材股份有限公司 | 可穿戴设备氧化锆陶瓷背板的制备方法 |
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