CN106587946A - 一种精密异形陶瓷管件的制备方法 - Google Patents
一种精密异形陶瓷管件的制备方法 Download PDFInfo
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Abstract
本发明公开了一种精密异形陶瓷管件的制备方法,包括如下步骤:制备复合粉料、制备陶瓷浆料、压注成型、排烧、烧结,其中,复合粉料由陶瓷粉料和辅料按重量比10~40:1混合而成,陶瓷浆料由复合粉料与有机添加剂按重量比为8~15:1的比例混合后经去泡得到,异形管件坯体由陶瓷浆料通过热压注成型机注入模具中成型后脱模制得,异形管件坯体经排烧、烧结后得到精密异形陶瓷管件。该制备方法适用于精密异形陶瓷管件的制备,并且,制备出来的管件的尺寸精度高、强度高、最高使用温度可达1300℃以上。
Description
技术领域
本发明属于无机非金属材料技术领域,特别提供了一种精密异形陶瓷管件的制备方法。
背景技术
近年来随着材料科技和制备加工方法的发展,陶瓷材料不仅在尺寸精度、强度、韧性和塑性上大幅提高,还具有防污、防湿、耐刮、耐磨、防火、隔热等功能,大大增进了精密陶瓷的应用范围及效能,使得陶瓷材料渗透到世界的每一个角落,从洗手间的马桶到太空船驾驶舱的隔热板都可见到其踪迹。
从20世纪80年代以来,世界先进国家一直不断研究各种材质和尺寸的管状精密陶瓷异型材料的制备,在相关的领域已取得了良好效果。例如:美国格鲁曼公司、杜邦公司、日本东陶机器株式会社等知名企业开发制备的管状陶瓷件被广泛的应用于排气、卫浴等相关领域。
我国在对精密陶瓷异形件的研究起步较晚,1990年以后,广东工学院、哈尔滨工业大学等相关单位,才陆续进行管状精密陶瓷异形件的基础研究。与发达国家相比,还有很大的差距,一些高性能高精度精密陶瓷异形件的研制还停留在实验室阶段,科技与生产力的转化率较低,虽然现在有一些厂家的产品已经投产,但是主要集中在广东、深圳等地,并且产品的性能普遍较国外产品低,存在生产效率低,质量不稳定等问题。无法满足市场的需求。
随着研究的不断深入,精密异形陶瓷管件的制备技术也不断丰富、完善。制备技术直接决定了陶瓷管件的结构和使用性能,常见的制备方法有等静压法、注射法、挤出法等等,其中,等静压成型法制备的精密异形陶瓷管件,密度大、强度高、尺寸精准,但是主体非圆形的管件无法一次性等静压成型,后期的加工量大;注射成型法自动化程度加高,可以大批量制备精密异形陶瓷管件,但是有机添加剂的含量较高,管件的密度较小,尺寸精准无法保证;挤出成型法自动化程度也很高,且可以制备很长的管件,但是管件的横截面需要完全相同,无法制备形状复杂的异形件,另外对浆料和烧结的要求高,管件的密度、强度极易不均,尺寸精准无法保证。
因此,研究一套适合制备精密异形陶瓷管件的制备方法,成为人们亟待解决的问题。
发明内容
鉴于此,本发明的目的在于提供一种精密异形陶瓷管件的制备方法,以至少解决现有制备方法制备出来的管件尺寸精度低、强度低、使用温度低等问题。
本发明提供的技术方案为:一种精密异形陶瓷管件的制备方法,包括以下步骤:
1)制备复合粉料:
11)将陶瓷粉体主料进行球磨混合,得到陶瓷粉料,其中,所述陶瓷粉料的粒度在0.2~200微米之间;
12)在所述陶瓷粉料中添加辅料,并在常温、常压下进行搅拌混合,得到复合粉料,其中,所述陶瓷粉体主料与所述辅料的重量比为10~40:1;
2)制备陶瓷浆料:
21)在温度为50~100℃条件下,将所述复合粉料与有机添加剂按重量比为8~15:1的比例混合,并搅拌2~12h,得到混合均匀的浆料;
22)在真空条件下,去除所述混合均匀的浆料中的气泡,得到陶瓷浆料;
3)压注成型:
31)将所述陶瓷浆料通过热压注成型机注入模具中成型,得到成型坯体,其中,所述模具的温度为30~80℃,成型压力为0.3~0.8Pa,成型时间为3~60s;
32)在室温下,将成型坯体脱模,得到异形管件坯体;
4)排烧:将所述异形管件坯体放置于排烧炉中加热,得到陶瓷坯体,其中,加热温度为400~1200℃,加热时间为8~48h;
5)烧结:将所述陶瓷坯体放入高温马弗炉内,以1~5℃/min的升温速度升温至1350~1700℃,保温2~8h,然后随炉冷却,得到精密异形陶瓷管件。
优选,在将所述陶瓷浆料通过热压注成型机注入模具中成型的步骤中,所述模具的温度为60℃,成型压力为0.6Pa,成型时间为20s。
进一步优选,在所述烧结步骤中,将所述陶瓷坯体放入高温马弗炉内,以3℃/min的升温速度升温至1600℃,保温3h,然后随炉冷却,得到精密异形陶瓷管件。
进一步优选,所述陶瓷粉体主料为氧化铝或氧化锆。
进一步优选,所述辅料为氧化镁、氧化钙、氧化铈、氧化钇、氧化硅、膨润土、高岭土、黏土中的一种或多种。
进一步优选,所述有机添加剂为石蜡、变性蜡、PE、PVC、PBMA中的一种或多种。
本发明提供的精密异形陶瓷管件的制备方法的有益效果如下:
1、使用热压注工艺更便于形状复杂、尺寸精密的异形陶瓷管件的成型;
2、复合粉体的粒度级配和成分的合理选择,使得烧结时各成分可以互相促进反应的进行,降低了陶瓷坯体的烧结温度,烧结后的产品密度和强度均可控,具有优异的性能;
3、本发明制备的异形陶瓷管件的尺寸精度高、强度高、使用温度高。
具体实施方式
以往陶瓷管件的制备方法不适用于制备精密异形陶瓷管件,为了解决采用以往制备方法制备出来的陶瓷管件尺寸精度低、强度低、不适于在高温下使用的问题,本实施方案提供了一种精密异形陶瓷管件的制备方法,具体包括以下步骤:
1)制备复合粉料:
11)将陶瓷粉体主料进行球磨混合,得到陶瓷粉料,其中,所述陶瓷粉料的粒度在0.2~200微米之间;
12)在所述陶瓷粉料中添加辅料,并在常温、常压下进行搅拌混合,得到复合粉料,其中,所述陶瓷粉体主料与所述辅料的重量比为10~40:1;
2)制备陶瓷浆料:
21)在温度为50~100℃条件下,将所述复合粉料与有机添加剂按重量比为8~15:1的比例混合,并搅拌2~12h,得到混合均匀的浆料;
22)在真空条件下,去除所述混合均匀的浆料中的气泡,得到陶瓷浆料;
3)压注成型:
31)将所述陶瓷浆料通过热压注成型机注入模具中成型,得到成型坯体,其中,所述模具的温度为30~80℃,成型压力为0.3~0.8Pa,成型时间为3~60s;
32)在室温下,将成型坯体脱模,得到异形管件坯体;
4)排烧:将所述异形管件坯体放置于排烧炉中加热,得到陶瓷坯体,其中,加热温度为400~1200℃,加热时间为8~48h;
5)烧结:将所述陶瓷坯体放入高温马弗炉内,以1~5℃/min的升温速度升温至1350~1700℃,保温2~8h,然后随炉冷却,得到精密异形陶瓷管件。
其中,本实施方案通过陶瓷粉料与辅料的合理配比,可以得到高性能的复合粉料,高性能的复合粉料与有机添加剂的合理配比,能够得到具有良好的流动性、适合各种形状的模具的陶瓷浆料,上述陶瓷浆料更适合高精密异形陶瓷管件的制备,陶瓷浆料搭配合理的成型条件、排烧条件和烧结条件,使得制备出来的异形陶瓷管件尺寸精度更高、强度更高,最高使用温度可达1300℃以上。
在将所述陶瓷浆料通过热压注成型机注入模具中成型的步骤中,所述模具的温度优选为60℃,成型压力优选为0.6Pa,成型时间优选为20s。
在所述烧结步骤中,将所述陶瓷坯体放入高温马弗炉内,优选以3℃/min的升温速度升温至1600℃,保温3h,然后随炉冷却,得到精密异形陶瓷管件。
所述陶瓷粉体主料为氧化铝或氧化锆。
所述辅料为氧化镁、氧化钙、氧化铈、氧化钇、氧化硅、膨润土、高岭土、黏土中的一种或多种。
所述有机添加剂为石蜡、变性蜡、PE、PVC、PBMA中的一种或多种。
下面以具体的实施例对本发明进行进一步解释,但并不用于限制本发明的保护范围。
实施例1
1)制备复合粉料:
11)将20重量份粒度为0.2微米的氧化铝粉料和20重量份粒度为20微米的氧化铝粉料进行干粉球磨混合2h,得到陶瓷粉料;
12)在所述陶瓷粉料中添加4重量份粒度为400微米的专用95瓷辅料,并在常温、常压下进行搅拌混合,得到复合粉料;
2)制备陶瓷浆料:
21)在温度为50℃条件下,将所述复合粉料与石蜡按重量比为8:1的比例混合,并不停的机械搅拌2h,得到混合均匀的浆料;
22)在真空条件下,去除所述混合均匀的浆料中的气泡,得到陶瓷浆料;
3)压注成型:
31)将所述陶瓷浆料通过热压注成型机注入模具中成型,得到成型坯体,其中,所述模具的温度为80℃,成型压力为0.3Pa,成型时间为60s;
32)在室温下,将所述成型坯体脱模,得到异形管件坯体;
4)排烧:将所述异形管件坯体放置于排烧炉中加热,得到陶瓷坯体,其中,加热温度为1200℃,加热时间为8h;
5)烧结:将所述陶瓷坯体放入高温马弗炉内,以1℃/min的升温速度升温至1350℃,保温2h,然后随炉冷却,得到精密异形陶瓷管件。
实施例2
1)制备复合粉料:
11)将10重量份粒度为5微米的氧化铝粉料和30重量份粒度为200微米的氧化铝粉料进行干粉球磨混合1h,得到陶瓷粉料;
12)在所述陶瓷粉料中添加1重量份的氧化钇和氧化铈混合粉料,并在常温、常压下进行搅拌混合,得到复合粉料;
2)制备陶瓷浆料:
21)在温度为100℃条件下,将所述复合粉料与有机添加剂按重量比为15:1的比例混合,并不停的机械搅拌2h,得到混合均匀的浆料,其中,所述有机添加剂按重量比包括1份石蜡和2份变性蜡;
22)在真空条件下,去除所述混合均匀的浆料中的气泡,得到陶瓷浆料;
3)压注成型:
31)将所述陶瓷浆料通过热压注成型机注入模具中成型,得到成型坯体,其中,所述模具的温度为30℃,成型压力为0.8Pa,成型时间为3s;
32)在室温下,将所述成型坯体脱模,得到异形管件坯体;
4)排烧:将所述异形管件坯体放置于排烧炉中加热,得到陶瓷坯体,其中,加热温度为400℃,加热时间为48h;
5)烧结:将所述陶瓷坯体放入高温马弗炉内,以5℃/min的升温速度升温至1700℃,保温8h,然后随炉冷却,得到精密异形陶瓷管件。
实施例3
1)制备复合粉料:
11)将30重量份粒度为20微米的氧化锆粉料和30重量份粒度为100微米的氧化锆粉料进行干粉球磨混合1h,得到陶瓷粉料;
12)在所述陶瓷粉料中添加2重量份的氧化钇和氧化铈混合粉料,并在常温、常压下进行搅拌混合,得到复合粉料;
2)制备陶瓷浆料:
21)在温度为80℃条件下,将所述复合粉料与有机添加剂按重量比为12:1的比例混合,并不停的机械搅拌2h,得到混合均匀的浆料,其中,所述有机添加剂按重量比包括1份石蜡和2份变性蜡;
22)在真空条件下,去除所述混合均匀的浆料中的气泡,得到陶瓷浆料;
3)压注成型:
31)将所述陶瓷浆料通过热压注成型机注入模具中成型,得到成型坯体,其中,所述模具的温度为50℃,成型压力为0.5Pa,成型时间为30s;
32)在室温下,将所述成型坯体脱模,得到异形管件坯体;
4)排烧:将所述异形管件坯体放置于排烧炉中加热,得到陶瓷坯体,其中,加热温度为600℃,加热时间为20h;
5)烧结:将所述陶瓷坯体放入高温马弗炉内,以1℃/min的升温速度升温至1700℃,保温2h,然后随炉冷却,得到精密异形陶瓷管件。
实施例4
与实施例3的区别如下:
5)烧结:将所述陶瓷坯体放入高温马弗炉内,以3℃/min的升温速度升温至1600℃,保温3h,然后随炉冷却,得到精密异形陶瓷管件。
实施例5
1)制备复合粉料:
11)将30重量份粒度为20微米的氧化锆粉料和30重量份粒度为100微米的氧化锆粉料进行干粉球磨混合1h,得到陶瓷粉料;
12)在所述陶瓷粉料中添加2重量份的氧化钇和氧化铈混合粉料,并在常温、常压下进行搅拌混合,得到复合粉料;
2)制备陶瓷浆料:
21)在温度为80℃条件下,将所述复合粉料与有机添加剂按重量比为12:1的比例混合,并不停的机械搅拌2h,得到混合均匀的浆料,其中,所述有机添加剂按重量比包括1份石蜡和2份变性蜡;
22)在真空条件下,去除所述混合均匀的浆料中的气泡,得到陶瓷浆料;
3)压注成型:
31)将所述陶瓷浆料通过热压注成型机注入模具中成型,得到成型坯体,其中,所述模具的温度为60℃,成型压力为0.6Pa,成型时间为20s;
32)在室温下,将所述成型坯体脱模,得到异形管件坯体;
4)排烧:将所述异形管件坯体放置于排烧炉中加热,得到陶瓷坯体,其中,加热温度为600℃,加热时间为20h;
5)烧结:将所述陶瓷坯体放入高温马弗炉内,以1℃/min的升温速度升温至1700℃,保温2h,然后随炉冷却,得到精密异形陶瓷管件。
实施例6
与实施例5的区别如下:
5)烧结:将所述陶瓷坯体放入高温马弗炉内,以3℃/min的升温速度升温至1600℃,保温3h,然后随炉冷却,得到精密异形陶瓷管件。
实施例7
从实施例1、实施例2、实施例3、实施例4、实施例5、实施例6中制备的精密异形陶瓷管件中随机各取1000个样品件,对应记为A组、B组、C组、D组、E组、F组,再获取用现有方法制备的异形陶瓷管件1000件,记为G组,对上述七组精密异形陶瓷管件的尺寸精度和强度进行测试,测试结果见表1。
表1:测试结果对比表
Claims (6)
1.一种精密异形陶瓷管件的制备方法,其特征在于,包括以下步骤:
1)制备复合粉料:
11)将陶瓷粉体主料进行球磨混合,得到陶瓷粉料,其中,所述陶瓷粉料的粒度在0.2~200微米之间;
12)在所述陶瓷粉料中添加辅料,并在常温、常压下进行搅拌混合,得到复合粉料,其中,所述陶瓷粉体主料与所述辅料的重量比为10~40:1;
2)制备陶瓷浆料:
21)在温度为50~100℃条件下,将所述复合粉料与有机添加剂按重量比为8~15:1的比例混合,并搅拌2~12h,得到混合均匀的浆料;
22)在真空条件下,去除所述混合均匀的浆料中的气泡,得到陶瓷浆料;
3)压注成型:
31)将所述陶瓷浆料通过热压注成型机注入模具中成型,得到成型坯体,其中,所述模具的温度为30~80℃,成型压力为0.3~0.8Pa,成型时间为3~60s;
32)在室温下,将成型坯体脱模,得到异形管件坯体;
4)排烧:将所述异形管件坯体放置于排烧炉中加热,得到陶瓷坯体,其中,加热温度为400~1200℃,加热时间为8~48h;
5)烧结:将所述陶瓷坯体放入高温马弗炉内,以1~5℃/min的升温速度升温至1350~1700℃,保温2~8h,然后随炉冷却,得到精密异形陶瓷管件。
2.按照权利要求1所述的精密异形陶瓷管件的制备方法,其特征在于:在将所述陶瓷浆料通过热压注成型机注入模具中成型的步骤中,所述模具的温度为60℃,成型压力为0.6Pa,成型时间为20s。
3.按照权利要求1所述的精密异形陶瓷管件的制备方法,其特征在于:在所述烧结步骤中,将所述陶瓷坯体放入高温马弗炉内,以3℃/min的升温速度升温至1600℃,保温3h,然后随炉冷却,得到精密异形陶瓷管件。
4.按照权利要求1所述的精密异形陶瓷管件的制备方法,其特征在于:所述陶瓷粉体主料为氧化铝或氧化锆。
5.按照权利要求1所述的精密异形陶瓷管件的制备方法,其特征在于:所述辅料为氧化镁、氧化钙、氧化铈、氧化钇、氧化硅、膨润土、高岭土、黏土中的一种或多种。
6.按照权利要求1至5中任一项所述的精密异形陶瓷管件的制备方法,其特征在于:所述有机添加剂为石蜡、变性蜡、PE、PVC、PBMA中的一种或多种。
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