CN113307635A - 一种通过轨道的凝胶注模直接滴定成型陶瓷微球的方法 - Google Patents
一种通过轨道的凝胶注模直接滴定成型陶瓷微球的方法 Download PDFInfo
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Abstract
一种通过轨道的凝胶注模直接滴定成型陶瓷微球的方法,先加工具有多条半圆形轨道的轨道盘,在轨道盘与半圆形轨道相背一侧的表面粘贴加热带,并在半圆形轨道的表面喷涂疏水涂料,通过加热带将疏水涂料烘干;然后制备陶瓷浆料;最后进行滴定成型,将轨道盘倾斜放置,使轨道盘与水平方向之间具有10‑15°的夹角且半圆形轨道朝上,将滴定盘放置在轨道盘的顶端,使滴定盘的多个滴定针筒分别与多条半圆形轨道的顶端对齐,然后使加热带以120‑150℃对轨道盘进行加热,再将陶瓷浆料注入滴定盘,使陶瓷浆料液滴在半圆形轨道上向下滚动并被加热固化成陶瓷微球球坯。本发明具有工艺成本低、工序少、容易实现自动化生产的优点,制成的陶瓷微球的球形度高,内部结构均匀。
Description
技术领域
本发明涉及陶瓷微球成型领域,尤其涉及一种通过轨道的凝胶注模直接滴定成型陶瓷微球的方法。
背景技术
陶瓷微球指直径在1mm以下,通常为0.1mm~1mm的球体结构或功能材料,常用的陶瓷微球种类包括,研磨介质类如ZrO2陶瓷微球,用于砂磨机研磨粉料;功能类如Gd2O2S、锂陶瓷、ZrN等陶瓷微球,分别用于G-M超低温制冷机中新型蓄冷材料以及核工业领域中的产氚包层功能材料和惰性基质材料。现有的陶瓷微球成型技术中,主要包括滚制法和常规滴定法。其中滚制法需要制核、加入粘结剂喷湿、滚制、自磨修正等多道工序,且受工艺影响,锅体不能继续增大,若提高产量就需要大量锅体和操作工人,而且一般情况下一个操作工只能操作一台滚锅,造成人工成本增加,同时滚制法制备的陶瓷微球球坯圆度不高,坯体均匀性较差,容易导致烧结后成品球磨耗增加、使用寿命降低。而常规滴定法是一种将陶瓷粉浆滴入固化液池中成型的方法,相对于滚制法,其在直径0.2mm规格以下产品中的优势明显,但由于在固化液中保持球状并在短时间内发生固化反应,当陶瓷液滴进入固化液瞬时,液滴容易形成拖尾,导致球形度不十分理想,容易出现椭球形产品,并且该方法固化后的微球表皮容易脱落,固化池占地面积较大,固化液内的杂质容易造成陶瓷微球污染,且不易实现自动化控制或自动化控制成本偏高,工序繁多且成本高。
发明内容
为解决现有的陶瓷微球成型技术中陶瓷微球均匀性不高、圆度不足、制作过程繁琐、生产效率低的问题,本发明提供了一种通过轨道的凝胶注模直接滴定成型陶瓷微球的方法。
本发明为解决上述技术问题所采用的技术方案是:一种通过轨道的凝胶注模直接滴定成型陶瓷微球的方法,包括以下步骤:
步骤一、加工轨道盘
选取一块长方形金属板,在金属板一侧的表面加工多条截面为半圆形的凹槽,半圆形轨道的长度方向与金属板的长边平行,多条半圆形轨道沿金属板的宽度方向均匀间隔排列,金属板的长度为15-20m,半圆形轨道的直径为4-5mm,相邻两条半圆形轨道的间距为5-6mm,得到具有多条半圆形轨道的轨道盘,对轨道盘的表面进行喷砂处理,在轨道盘与半圆形轨道相背一侧的表面粘贴加热带,并在半圆形轨道的表面喷涂疏水涂料,通过加热带将疏水涂料烘干;
步骤二、制备原料
称取平均粒径为0.08-0.12μm的ZrO2粉粒,并按照质量百分比,称取占ZrO2粉粒总质量比例为2-2.5%的丙烯酰胺、0.2-0.3%的N-N’亚甲基双丙烯酰胺、1-1.5%的聚羧酸铵、0.4-0.5%的过硫酸铵和0.15-0.2%的四甲基乙二胺;
将丙烯酰胺、N-N’亚甲基双丙烯酰胺、N-N’亚甲基双丙烯酰胺加入水中搅拌,得到固含量为70-80%的预混液;将ZrO2粉粒和预混液加入球磨罐内进行球磨,球磨介质为ZrO2球体,球磨时间6-10h,得到球磨浆料;将过硫酸铵和四甲基乙二胺加入球磨浆料并搅拌,得到陶瓷浆料,将陶瓷浆料存放至储浆罐内,并进行抽真空除泡,备用;
步骤三、滴定成型
将轨道盘倾斜放置,使轨道盘与水平方向之间具有10-15°的夹角且半圆形轨道朝上,将收集装置放置在轨道盘的底端,并将滴定盘放置在轨道盘的顶端,使滴定盘的多个滴定针筒分别与多条半圆形轨道的顶端对齐,然后使加热带以120-150℃对轨道盘进行加热,再将步骤二制备的陶瓷浆料注入滴定盘,对滴定盘的气动压力进行控制,使陶瓷浆料从滴定盘的多个滴定针筒以相同的液滴形成速率同步滴落至多条半圆形轨道内,从而使陶瓷浆料液滴在半圆形轨道上向下滚动并被加热固化成陶瓷微球球坯,然后将落入收集装置内的陶瓷微球球坯加工成陶瓷微球,即完成陶瓷微球的滴定成型。
优选的,轨道盘的材料为铝合金或不锈钢,轨道盘的厚度为9-12mm,喷砂处理后保证轨道盘的表面粗糙度Ra≤1.6μm。
优选的,步骤一中,使加热带以80-100℃对轨道盘加热3-5h,从而烘干疏水涂料。
优选的,所述的球磨罐为聚氨酯制成的行星球磨罐,球磨介质为直径3mm的ZrO2球体,原料与球体的质量比为2:1,球磨转速为200r/min。
优选的,所述球磨浆料在室温、转速20s-1条件下的粘度值为90-95mPa·s。
优选的,步骤三中,采用30#滴定针筒,控制陶瓷浆料液滴的直径为0.1-0.12mm。
优选的,步骤三中,使陶瓷微球球坯在200℃干燥3h,然后在600℃进行脱脂处理15h,最后在1500℃保温2h,得到陶瓷微球。
根据上述技术方案,本发明的有益效果是:
本发明具有工艺成本低、工序少、容易实现自动化生产的优点,轨道盘经过简单加工和表面处理即可制成,制作工艺简单、成本低,轨道盘上半圆形轨道的数量可以大量增加,可同时提高生产效率和规模,且工艺设定好之后可自动完成滴定,不需要大量人力进行操作,由于将半圆形轨道加工成半圆弧形,所以倾斜后浆料液滴小球滚动顺畅,不易堵塞或停滞,整个生产过程可控性强、可靠性高。
本发明所成型的陶瓷微球的球形度高,内部结构均匀,由于陶瓷浆料液滴始终在疏水涂料表面滚动,同时浆料的固含量较高,水分含量较低,所以在蒸发固化过程中,球坯的收缩变形量极小,滚动过程本身也有利于球形化,因此整个滴定过程可始终保持较高的球形度,能保证陶瓷微球的球形度高于现有的滚制法以及常规滴定法所制备的陶瓷微球;由于陶瓷液滴在固化过程中处于运动状态,且固化时间较短,故其内部浆料不易发生沉降,可保持球坯内部颗粒的均匀分布,在蒸发干燥过程中,因毛细管力使球坯进一步收缩,进一步提高了球坯密度,有利于提高陶瓷微球成品的强度,烧成后直径为0.1mm的陶瓷微球成品,其相对密度超过99.2%,压溃强度较常规滴定成型法提高5~10%;而且由于本发明的成型方法不接触固化液,可避免固化液中的杂质对陶瓷微球造成污染,保证陶瓷微球具有很高的纯度;通过控制加热带的温度,本发明可使陶瓷浆料液滴快速固化成球,大幅提高成球效率,并且由于疏水涂料的作用,能够防止球坯在较高温度下发生变形和开裂,保证陶瓷微球的高效高质量生产。
附图说明
图1为轨道盘的示意图。
具体实施方式
本发明提供了一种通过轨道的凝胶注模直接滴定成型陶瓷微球的方法,包括以下步骤:
步骤一、加工轨道盘
选取一块长方形金属板,在金属板一侧的表面加工多条截面为半圆形的凹槽,半圆形轨道的长度方向与金属板的长边平行,多条半圆形轨道沿金属板的宽度方向均匀间隔排列,轨道盘的材料为铝合金或不锈钢,金属板的厚度为9-12mm,金属板的长度为15-20m,半圆形轨道的直径为4-5mm,相邻两条半圆形轨道的间距为5-6mm,得到具有多条半圆形轨道的轨道盘,对轨道盘的表面进行喷砂处理,喷砂处理后保证轨道盘的表面粗糙度Ra≤1.6μm,在轨道盘与半圆形轨道相背一侧的表面粘贴加热带,并在半圆形轨道的表面喷涂疏水涂料,使加热带以80-100℃对轨道盘加热3-5h,从而烘干疏水涂料。
步骤二、制备原料
称取平均粒径为0.08-0.12μm的ZrO2粉粒,并按照质量百分比,称取占ZrO2粉粒总质量比例为2-2.5%的丙烯酰胺、0.2-0.3%的N-N’亚甲基双丙烯酰胺、1-1.5%的聚羧酸铵、0.4-0.5%的过硫酸铵和0.15-0.2%的四甲基乙二胺;
将丙烯酰胺、N-N’亚甲基双丙烯酰胺、N-N’亚甲基双丙烯酰胺加入水中搅拌,得到固含量为70-80%的预混液;将ZrO2粉粒和预混液加入球磨罐内进行球磨,球磨罐为聚氨酯制成的行星球磨罐,球磨介质为直径3mm的ZrO2球体,原料与球体的质量比为2:1,球磨转速为200r/min,球磨介质为ZrO2球体,球磨时间6-10h,得到球磨浆料,球磨浆料在室温、转速20s-1条件下的粘度值为90-95mPa·s;将过硫酸铵和四甲基乙二胺加入球磨浆料并搅拌,得到陶瓷浆料,将陶瓷浆料存放至储浆罐内,并进行抽真空除泡,备用。
步骤三、滴定成型
将轨道盘倾斜放置,使轨道盘与水平方向之间具有10-15°的夹角且半圆形轨道朝上,将收集装置放置在轨道盘的底端,并将滴定盘放置在轨道盘的顶端,使滴定盘的多个滴定针筒分别与多条半圆形轨道的顶端对齐,然后使加热带以120-150℃对轨道盘进行加热,再将步骤二制备的陶瓷浆料注入滴定盘,对滴定盘的气动压力进行控制,使陶瓷浆料从滴定盘的多个滴定针筒以相同的液滴形成速率同步滴落至多条半圆形轨道内,采用30#滴定针筒,控制陶瓷浆料液滴的直径为0.1-0.12mm,从而使陶瓷浆料液滴在半圆形轨道上向下滚动并被加热固化成陶瓷微球球坯,然后将落入收集装置内的陶瓷微球球坯在200℃干燥3h,然后在600℃进行脱脂处理15h,最后在1500℃保温2h,得到陶瓷微球,即完成陶瓷微球的滴定成型。
实施例:首先加工轨道盘,轨道盘采用不锈钢,长度20m,厚度10mm,共开设有9条半圆形轨道,半圆形轨道的直径为5mm,相邻两条半圆形轨道的间距为5 mm,对轨道盘的表面进行喷砂处理,喷砂处理后轨道盘的表面粗糙度小于1.6μm,然后在轨道盘的表面粘贴加热带并喷涂疏水涂料,使加热带以80℃对轨道盘加热3h,烘干疏水涂料。
然后制备原料,称取平均粒径为0.1μm的ZrO2粉粒800g,并按照质量百分比,称取占ZrO2粉粒总质量比例为2.3%的丙烯酰胺、0.25%的N-N’亚甲基双丙烯酰胺、1.2%的聚羧酸铵、0.45%的过硫酸铵和0.17%的四甲基乙二胺;将丙烯酰胺、N-N’亚甲基双丙烯酰胺、N-N’亚甲基双丙烯酰胺加入水中搅拌,得到固含量为80%的预混液;将ZrO2粉粒和预混液加入球磨罐内进行球磨,球磨罐为聚氨酯制成的行星球磨罐,球磨介质为直径3mm的ZrO2球体,原料与球体的质量比为2:1,球磨转速为200r/min,球磨介质为ZrO2球体,球磨时间8h,得到球磨浆料,球磨浆料在室温、转速20s-1条件下的粘度值为93mPa·s;将过硫酸铵和四甲基乙二胺加入球磨浆料,用机械棒搅拌3min,得到陶瓷浆料,将陶瓷浆料存放至带有自动搅拌装置的储浆罐内,并进行抽真空除泡。
最后进行滴定成型,将轨道用支腿固定于地面,轨道平面与地面保持10°夹角,通过加热带将不锈钢轨道面板加热至120℃,通过气动装置将陶瓷浆料推送至滴定盘上的30#滴定针筒中,通过调整压缩空气的气压,可使陶瓷浆料液滴直径可保持为约0.12mm,调整合适的滴定工艺,将陶瓷浆料液滴由轨道上端滴下并滚落至最低位置的收集槽中,得到固化后的陶瓷浆料球坯。若按照3滴/s的滴定速率进行生产,含9个半圆形轨道的设备按8h一天可生产多达约80万粒陶瓷微球。成型后的ZrO2球坯经200℃继续干燥3h、600℃脱脂15h、最后于1500℃条件下保温2h后,制得直径约0.1mm的成品陶瓷微球。经测试,其相对密度约为99.50%,压溃强度较常规滴定成型法平均提高约6%。
Claims (7)
1.一种通过轨道的凝胶注模直接滴定成型陶瓷微球的方法,其特征在于,包括以下步骤:
步骤一、加工轨道盘
选取一块长方形金属板,在金属板一侧的表面加工多条截面为半圆形的凹槽,半圆形轨道的长度方向与金属板的长边平行,多条半圆形轨道沿金属板的宽度方向均匀间隔排列,金属板的长度为15-20m,半圆形轨道的直径为4-5mm,相邻两条半圆形轨道的间距为5-6mm,得到具有多条半圆形轨道的轨道盘,对轨道盘的表面进行喷砂处理,在轨道盘与半圆形轨道相背一侧的表面粘贴加热带,并在半圆形轨道的表面喷涂疏水涂料,通过加热带将疏水涂料烘干;
步骤二、制备原料
称取平均粒径为0.08-0.12μm的ZrO2粉粒,并按照质量百分比,称取占ZrO2粉粒总质量比例为2-2.5%的丙烯酰胺、0.2-0.3%的N-N’亚甲基双丙烯酰胺、1-1.5%的聚羧酸铵、0.4-0.5%的过硫酸铵和0.15-0.2%的四甲基乙二胺;
将丙烯酰胺、N-N’亚甲基双丙烯酰胺、N-N’亚甲基双丙烯酰胺加入水中搅拌,得到固含量为70-80%的预混液;将ZrO2粉粒和预混液加入球磨罐内进行球磨,球磨介质为ZrO2球体,球磨时间6-10h,得到球磨浆料;将过硫酸铵和四甲基乙二胺加入球磨浆料并搅拌,得到陶瓷浆料,将陶瓷浆料存放至储浆罐内,并进行抽真空除泡,备用;
步骤三、滴定成型
将轨道盘倾斜放置,使轨道盘与水平方向之间具有10-15°的夹角且半圆形轨道朝上,将收集装置放置在轨道盘的底端,并将滴定盘放置在轨道盘的顶端,使滴定盘的多个滴定针筒分别与多条半圆形轨道的顶端对齐,然后使加热带以120-150℃对轨道盘进行加热,再将步骤二制备的陶瓷浆料注入滴定盘,对滴定盘的气动压力进行控制,使陶瓷浆料从滴定盘的多个滴定针筒以相同的液滴形成速率同步滴落至多条半圆形轨道内,从而使陶瓷浆料液滴在半圆形轨道上向下滚动并被加热固化成陶瓷微球球坯,然后将落入收集装置内的陶瓷微球球坯加工成陶瓷微球,即完成陶瓷微球的滴定成型。
2.根据权利要求1所述的一种通过轨道的凝胶注模直接滴定成型陶瓷微球的方法,其特征在于:轨道盘的材料为铝合金或不锈钢,轨道盘的厚度为9-12mm,喷砂处理后保证轨道盘的表面粗糙度Ra≤1.6μm。
3.根据权利要求1所述的一种通过轨道的凝胶注模直接滴定成型陶瓷微球的方法,其特征在于:步骤一中,使加热带以80-100℃对轨道盘加热3-5h,从而烘干疏水涂料。
4.根据权利要求1所述的一种通过轨道的凝胶注模直接滴定成型陶瓷微球的方法,其特征在于:所述的球磨罐为聚氨酯制成的行星球磨罐,球磨介质为直径3mm的ZrO2球体,原料与球体的质量比为2:1,球磨转速为200r/min。
5.根据权利要求1所述的一种通过轨道的凝胶注模直接滴定成型陶瓷微球的方法,其特征在于:所述球磨浆料在室温、转速20s-1条件下的粘度值为90-95mPa·s。
6.根据权利要求1所述的一种通过轨道的凝胶注模直接滴定成型陶瓷微球的方法,其特征在于:步骤三中,采用30#滴定针筒,控制陶瓷浆料液滴的直径为0.1-0.12mm。
7.根据权利要求1所述的一种通过轨道的凝胶注模直接滴定成型陶瓷微球的方法,其特征在于:步骤三中,使陶瓷微球球坯在200℃干燥3h,然后在600℃进行脱脂处理15h,最后在1500℃保温2h,得到陶瓷微球。
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