CN105753455B - 一种氧化铝陶瓷柱塞的制备方法 - Google Patents
一种氧化铝陶瓷柱塞的制备方法 Download PDFInfo
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Abstract
一种氧化铝陶瓷柱塞的制备方法,首先制备乙醇、十二烷基磺酸钠、脂肪醇聚氧乙烯醚和去离子水的混合溶液;然后量取氧化铝粉末,并将氧化铝粉末倒入混合溶液中进行洗涤沉淀干燥;再然后将干燥后的沉淀物、氧化镁粉末、氧化钇粉末、氧化锆粉末、PVA溶液、甘油和聚丙烯混合均匀,混合均匀后造粒,将造粒好的物料成型制备成呈柱塞状的陶瓷湿坯。接着将陶瓷湿坯进行干燥制备陶瓷生坯;干燥完全后,对陶瓷生坯做脱胶处理。再接着将脱胶后的陶瓷生坯分两步进行烧制。通过氧化铝陶瓷柱塞的制备方法制备的氧化铝陶瓷柱塞,硬度、强度和韧性高,耐磨性好,使用寿命长。
Description
技术领域
本发明涉及一种陶瓷的制备方法,具体涉及一种能够制备出强度高耐磨性好的陶瓷的制备方法。利用该技术生产的陶瓷主要应用于陶瓷金属化粘接、焊接、镶嵌、耐磨材料、套接组装技术等方面。
背景技术
氧化铝陶瓷柱塞因具有较高的强度和耐磨性,原料来源丰富等特征,在工业中得到了广泛的应用。目前,现有制备方法中,大多采用甲基纤维素作为粘结剂,对于氧化铝陶瓷柱塞而言,添加剂与粘结剂的形貌和残留物形态对氧化铝陶瓷柱塞的密度高低和均匀一致性密切相关,如常用纤维素等所造孔为细扁长形孔,对气孔形态均匀性存在一定范围内的降低;若分散工艺不合理,也将导致内部应力集中区。从生产工艺来看,如传统技术中采用压制成型制备氧化铝陶瓷柱塞,其径向强度只能达到40Mpa~50Mpa,满足不了高压柱塞泵对氧化铝陶瓷柱塞的高强度要求。
发明内容
为了解决现有技术中氧化铝陶瓷柱塞因分散工艺易造成内部应力集中区和制备的氧化铝陶瓷柱塞强度和韧性低的问题,本发明提供一种氧化铝陶瓷柱塞的制备方法。
一种氧化铝陶瓷柱塞的制备方法,具体步骤如下:
第一步,制备乙醇、十二烷基磺酸钠、脂肪醇聚氧乙烯醚和去离子水的混合溶液。混合溶液中乙醇的重量比为1wt%~3wt%,十二烷基磺酸钠的重量比为0.1wt%~0.5wt,脂肪醇聚氧乙烯醚溶液的重量比为0.1wt%~10wt%。
第二步,称取粒径在0.2μm~1μm之间的氧化铝粉末,以及称取氧化镁粉末、氧化钇粉末、氧化锆粉末、PVA溶液、甘油和聚丙烯。其中,氧化铝粉末重量份为75~95,氧化镁粉末重量份为1~2,氧化钇粉末重量份为1~2,氧化锆粉末重量份为5~20,PVA溶液重量份为0.5~1,甘油重量份为0.5~1,聚丙烯重量份为1。将氧化铝粉末投入第一步获取的混合溶液中进行洗涤。
将洗涤完成后的混合溶液进行过滤,得到沉淀物,将沉淀物置入干燥炉内进行干燥得到中间物A。
将中间物A、去离子水、氧化镁粉末、氧化钇粉末、氧化锆粉末、PVA溶液、甘油和聚丙烯混合均匀,混合均匀后造粒,再接着将造粒好的物料通过挤出机或者等静压机制备呈柱塞状的陶瓷湿坯。
第三步,将陶瓷湿坯进行干燥制备陶瓷生坯;干燥完全后,陶瓷生坯做脱胶处理。
第四步,将脱胶后的陶瓷生坯送入感应加热炉中以10℃/小时升温速度加热至300℃,然后保温3~6小时。接着以15~20℃/小时升温速度缓慢加热至650℃。再然后以80~100℃/小时升温至1100℃。再接着以100℃/小时迅速冷却至1050℃,最后将烧制的陶瓷坯体随炉冷却至室温。
第五步,陶瓷坯体出炉后,进行切割整理,然后在感应加热炉中以80~100℃/小时升温到1410℃,然后保温3~6小时。接着以100℃/小时冷却至1050℃~1100℃,最后陶瓷坯体随炉冷却至室温。
优选的,在第二步中,首先将中间物A分成两批次使用,将第一批次使用的中间物A、氧化镁粉末、氧化钇粉末、氧化锆粉末依次加入到混合机内初步混合均匀,再将第二批次使用的中间物A加入到混合机内进一步混合均匀。然后将去离子水、PVA溶液、甘油和聚丙烯混合后加入混合机内继续混合均匀。接着将混合均匀后的物料送入高粘捏混和机内捏混混匀,随后造粒。
优选的,第三步中,所述脱胶处理在真空气氛脱胶炉中进行。首先将陶瓷生坯置入真空气氛脱胶炉内,真空气氛脱胶炉真空度大于99%。然后以5℃/小时加热速度加热至350度,再然后以5~10L/min的速度往真空气氛脱胶炉中送入工业氮气,最后陶瓷生坯随炉冷却至室温。
优选的,第二步中,氧化铝粉末的重量份为90,氧化镁粉末的重量份为1,氧化钇粉末的重量份为2,氧化锆粉末的重量份为5。
本发明提供的一种氧化铝陶瓷柱塞的制备方法与现有技术相比,具有以下有益效果:
上述一种氧化铝陶瓷柱塞的制备方法,在洗涤后,氧化铝粉末粘附有混合溶液中的有机物;洗涤沉淀干燥后分步混合,混合更均匀,且在混合过程中,添加了PVA溶液、甘油和聚丙烯。脱胶处理后,通过两步烧制,在第四步即第一次烧制后进行切割整理,切割难度较低。烧制过程为:首先通过第四步烧制,然后通过第五步的感应加热的方式进一步烧制,通过两步烧制,烧制的氧化铝陶瓷柱塞韧性更好,密度更稳定。
通过本发明提供的一种氧化铝陶瓷柱塞的制备方法制备的陶瓷柱塞,耐磨性高,在10N压力,以碳化硅颗粒为耐磨料,陶瓷柱塞单位面积的磨损量小于2.5mg/h;制备的陶瓷柱塞强度高,抗拉强度大于400Mpa;制备的陶瓷柱塞韧性高,断裂韧度大于7Mpa·m1/2;制备的陶瓷柱塞密度高,密度在3.76g/cm3~3.9g/cm3之间。具有耐酸碱型强,光洁度好,粗糙度在0.03μm以下;制备的陶瓷柱塞使用寿命长,使用寿命超过16000小时。
具体实施方式
一种氧化铝陶瓷柱塞的制备方法,实施例的具体步骤如下:
第一步,制备乙醇、十二烷基磺酸钠、脂肪醇聚氧乙烯醚和去离子水的混合溶液。混合溶液中乙醇的重量比为1wt%~3wt%,十二烷基磺酸钠的重量比为0.1wt%~0.5wt,脂肪醇聚氧乙烯醚溶液的重量比为0.1wt%~10wt%。
第二步,称取粒径在0.2μm~1μm之间的氧化铝粉末,以及称取氧化镁粉末、氧化钇粉末、氧化锆粉末、PVA溶液、甘油和聚丙烯。其中,氧化铝粉末重量份为75~95,氧化镁粉末重量份为1~2,氧化钇粉末重量份为1~2,氧化锆粉末重量份为5~20,PVA溶液重量份为0.5~1,甘油重量份为0.5~1,聚丙烯重量份为1。将氧化铝粉末投入第一步获取的混合溶液中进行洗涤。将洗涤完成后的混合溶液进行过滤,得到沉淀物,将沉淀物置入干燥炉内进行干燥得到中间物A。
接着将中间物A分成两批次使用,将第一批次使用的中间物A、氧化镁粉末、氧化钇粉末、氧化锆粉末依次加入到混合机内初步混合均匀,再将第二批次使用的中间物A加入到混合机内进一步混合均匀。然后将去离子水、PVA溶液、甘油和聚丙烯混合后加入混合机内继续混合均匀。再然后将混合均匀后的物料送入高粘捏混和机内捏混混匀,随后造粒;再接着将造粒好的物料通过挤出机或者等静压机制备呈柱塞状的陶瓷湿坯。
第三步,将陶瓷湿坯进行干燥制备陶瓷生坯;干燥完全后,陶瓷生坯做脱胶处理。所述脱胶处理在真空气氛脱胶炉中进行。首先将陶瓷生坯置入真空气氛脱胶炉内,真空气氛脱胶炉真空度大于99%。然后以5℃/小时加热速度至350度,再然后以5~10L/min的速度往真空气氛脱胶炉中送入工业氮气,最后陶瓷生坯随炉冷却至室温。
第四步,将脱胶后的陶瓷生坯送入感应加热炉中以10℃/小时升温速度加热至300℃,然后保温3~6小时。接着以15~20℃/小时升温速度缓慢加热至650℃。再然后以80~100℃/小时升温至1100℃。再接着以100℃/小时迅速冷却至1050℃,最后将烧制的陶瓷坯体随炉冷却至室温。
第五步,陶瓷坯体出炉后,进行切割整理,然后在感应加热炉中以80~100℃/小时升温到1410℃,再然后保温3~6小时。接着以100℃/小时冷却至1050℃~1100℃,最后陶瓷坯体随炉冷却至室温。
实施例1
本实施例中第二步量取的氧化铝粉末为9kg,氧化镁粉末为0.1kg,氧化钇粉末为0.2kg,氧化锆粉末为0.5kg;PVA溶液0.1kg,甘油0.1kg,聚丙烯0.1kg;第二步得到的沉淀物通过干燥炉进行干燥,干燥炉内温度为150℃;造粒后制备的陶瓷湿坯呈柱塞状。
上述实施例1制备的氧化铝陶瓷柱塞,耐磨性高,在10N压力,以碳化硅颗粒为耐磨料,陶瓷柱塞单位面积的磨损量为1.93mg/h;制备的陶瓷柱塞强度高,抗拉强度为491Mpa;制备的陶瓷柱塞韧性高,断裂韧度为8.91Mpa·m1/2;制备的陶瓷柱塞密度高,密度为3.83g/cm3。具有耐酸碱型强,光洁度好,粗糙度为0.024μm;制备的陶瓷柱塞使用寿命长,使用寿命为1932小时。
实施例2
本实施例中第二步量取的氧化铝粉末为7.5kg,氧化镁粉末为0.1kg,氧化钇粉末为0.2kg,氧化锆粉末为0.2kg;PVA溶液0.1kg,甘油0.1kg,聚丙烯0.1kg;第二步得到的沉淀物通过干燥炉进行干燥,干燥炉内温度为150℃;造粒后制备的陶瓷湿坯呈柱塞状。
上述实施例2制备的氧化铝陶瓷柱塞,耐磨性高,在10N压力,以碳化硅颗粒为耐磨料,陶瓷柱塞单位面积的磨损量为2.27mg/h;制备的陶瓷柱塞强度高,抗拉强度为507Mpa;制备的陶瓷柱塞韧性高,断裂韧度为9.15Mpa·m1/2;制备的陶瓷柱塞密度高,密度为3.89g/cm3。具有耐酸碱型强,光洁度好,粗糙度为0.027μm;制备的陶瓷柱塞使用寿命长,使用寿命为1653小时。
实施例3
本实施例中第二步量取的氧化铝粉末为9kg,氧化镁粉末为0.2kg,氧化钇粉末为0.1kg,氧化锆粉末为0.6kg;PVA溶液0.05kg,甘油0.05kg,聚丙烯0.1kg;第二步得到的沉淀物通过干燥炉进行干燥,干燥炉内温度为150℃;造粒后制备的陶瓷湿坯呈柱塞状。
上述实施例3制备的氧化铝陶瓷柱塞,耐磨性高,在10N压力,以碳化硅颗粒为耐磨料,陶瓷柱塞单位面积的磨损量为2.23mg/h;制备的陶瓷柱塞强度高,抗拉强度为476Mpa;制备的陶瓷柱塞韧性高,断裂韧度为8.53Mpa·m1/2;制备的陶瓷柱塞密度高,密度为3.75g/cm3。具有耐酸碱型强,光洁度好,粗糙度为0.025μm;制备的陶瓷柱塞使用寿命长,使用寿命为1674小时。
实施例4
本实施例中第二步量取的氧化铝粉末为8.5kg,氧化镁粉末为0.1kg,氧化钇粉末为0.2kg,氧化锆粉末为1kg;PVA溶液0.1kg,甘油0.1kg,聚丙烯0.1kg;第二步得到的沉淀物通过干燥炉进行干燥,干燥炉内温度为150℃;造粒后制备的陶瓷湿坯呈柱塞状。
上述实施例4制备的氧化铝陶瓷柱塞,耐磨性高,在10N压力,以碳化硅颗粒为耐磨料,陶瓷柱塞单位面积的磨损量为2.15mg/h;制备的陶瓷柱塞强度高,抗拉强度为485Mpa;制备的陶瓷柱塞韧性高,断裂韧度为8.73Mpa·m1/2;制备的陶瓷柱塞密度高,密度为3.85g/cm3。具有耐酸碱型强,光洁度好,粗糙度为0.029μm;制备的陶瓷柱塞使用寿命长,使用寿命为1695小时。
实施例5
本实施例中第二步量取的氧化铝粉末为9kg;氧化镁粉末为0.1kg,氧化钇粉末为0.2kg,氧化锆粉末为0.7kg;PVA溶液0.1kg,甘油0.1kg,聚丙烯0.1kg;第二步得到的沉淀物通过干燥炉进行干燥,干燥炉内温度为150℃;造粒后制备的陶瓷湿坯呈柱塞状。
上述实施例5制备的氧化铝陶瓷柱塞,耐磨性高,在10N压力,以碳化硅颗粒为耐磨料,陶瓷柱塞单位面积的磨损量为2.43mg/h;制备的陶瓷柱塞强度高,抗拉强度为497Mpa;制备的陶瓷柱塞韧性高,断裂韧度为8.95Mpa·m1/2;制备的陶瓷柱塞密度高,密度为3.87g/cm3。具有耐酸碱型强,光洁度好,粗糙度为0.025μm;制备的陶瓷柱塞使用寿命长,使用寿命为1672小时。
当然,上述说明并非是对本发明的限制,本发明也并不仅限于上述举例,本技术领域的技术人员在本发明的实质范围内所做出的变化、改型、添加或替换,也应属于本发明的保护范围。
Claims (4)
1.一种氧化铝陶瓷柱塞的制备方法,其特征在于,具体步骤如下:
第一步,制备乙醇、十二烷基磺酸钠、脂肪醇聚氧乙烯醚和去离子水的混合溶液;混合溶液中乙醇的重量比为1wt%~3wt%,十二烷基磺酸钠的重量比为0.1wt%~0.5wt,脂肪醇聚氧乙烯醚溶液的重量比为0.1wt%~10wt%;
第二步,称取粒径在0.2μm~1μm之间的氧化铝粉末,以及称取氧化镁粉末、氧化钇粉末、氧化锆粉末、PVA溶液、甘油和聚丙烯;其中,氧化铝粉末重量份为75~95,氧化镁粉末重量份为1~2,氧化钇粉末重量份为1~2,氧化锆粉末重量份为5~20,PVA溶液重量份为0.5~1,甘油重量份为0.5~1,聚丙烯重量份为1;将氧化铝粉末投入第一步获取的混合溶液中进行洗涤;
将洗涤完成后的混合溶液进行过滤,得到沉淀物,将沉淀物置入干燥炉内进行干燥得到中间物A;
将中间物A、去离子水、氧化镁粉末、氧化钇粉末、氧化锆粉末、PVA溶液、甘油和聚丙烯混合均匀,混合均匀后造粒;再接着将造粒好的物料通过挤出机或者等静压机制备呈柱塞状的陶瓷湿坯;
第三步,将陶瓷湿坯进行干燥制备陶瓷生坯;干燥完全后,陶瓷生坯做脱胶处理;
第四步,将脱胶后的陶瓷生坯送入感应加热炉中以10℃/小时升温速度加热至300℃,然后保温3~6小时;接着以15~20℃/小时升温速度缓慢加热至650℃;再然后以80~100℃/小时升温至1100℃;再接着以100℃/小时迅速冷却至1050℃,最后将烧制的陶瓷坯体随炉冷却至室温;
第五步,陶瓷坯体出炉后,进行切割整理,然后在感应加热炉中以80~100℃/小时升温到1410℃,然后保温3~6小时;接着以100℃/小时冷却至1050℃~1100℃,最后陶瓷坯体随炉冷却至室温。
2.如权利要求1所述的一种氧化铝陶瓷柱塞的制备方法,其特征在于,在第二步中,首先将中间物A分成两批次使用,将第一批次使用的中间物A、氧化镁粉末、氧化钇粉末、氧化锆粉末依次加入到混合机内初步混合均匀,再将第二批次使用的中间物A加入到混合机内进一步混合均匀;然后将去离子水、PVA溶液、甘油和聚丙烯混合后加入混合机内继续混合均匀;接着将混合均匀后的物料送入高粘捏混和机内捏混混匀,随后造粒。
3.如权利要求1所述的一种氧化铝陶瓷柱塞的制备方法,其特征在于,第三步中,所述脱胶处理在真空气氛脱胶炉中进行;首先将陶瓷生坯置入真空气氛脱胶炉内,真空气氛脱胶炉真空度大于99%;然后以5℃/小时加热速度加热至350度,再然后以5~10L/min的速度向真空气氛脱胶炉中送入工业氮气,最后陶瓷生坯随炉冷却至室温。
4.如权利要求1所述的一种氧化铝陶瓷柱塞的制备方法,其特征在于,第二步中,氧化铝粉末的重量份为90,氧化镁粉末的重量份为1,氧化钇粉末的重量份为2,氧化锆粉末的重量份为5。
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