CN111848179A - 一种可在超高温环境中使用的高强度氮化硼陶瓷的制备方法 - Google Patents
一种可在超高温环境中使用的高强度氮化硼陶瓷的制备方法 Download PDFInfo
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Abstract
本发明公开了一种可在超高温环境中使用的高强度氮化硼陶瓷的制备方法,包括如下步骤:1)将氮化硼粉料置于球磨罐中,并加入不同直径的氧化锆研磨球,然后将球磨罐抽真空或通入氮气,利用球磨设备对其进行粉磨使其粒度D50<1μm,其中球磨方式可以采用干磨或湿磨,球磨过程中控制物料温度低于40℃;2)根据产品使用性能要求,在处理后的氮化硼粉料中加入质量分数为0~25%的二硼化锆,0~15%的硼粉,进行均匀混合后得到陶瓷原料。将陶瓷原料置于热压模具中,装模,预压。3)将装完料的模具置于真空热压炉内真空度<10Pa,以3‑15℃/min的速率升温到1800‑2100℃后,开始对样品进行加压处理,压力为20‑60MPa,保温10‑120min后降温泄压,降温速率为3‑15℃/min.即得所述的高强氮化硼陶瓷材料。这种方法提高了传统氮化硼陶瓷的强度,且物相中不含影响其高温性能的氧化硼,降低高强氮化硼陶瓷材料的生产成本。该方法对原料要求简单,且危险性小,对制备的环境要求比较低,可大量制备。
Description
技术领域
本发明属于高温结构功能一体化陶瓷的技术领域,涉及一种可在超高温环境中使用的高强度氮化硼陶瓷的制备方法。
背景技术
六方氮化硼(h-BN)陶瓷便是一种有着巨大发展潜力的高温结构陶瓷材料。h-BN是一种具有类似石墨结层状结构的新材料,呈象牙白色,故俗称“白石墨”,其无明显熔点,且在高温下无软化现象,耐强酸强碱腐蚀。h-BN耐热性非常好,可以在900℃以下的氧化氛围中和2800℃以下的氮气和惰性气氛中使用。同其它陶瓷材料相比,h-BN陶瓷具有耐高温、高热导率、膨胀系数低、抗热震等一系列特性,是一种性能优异的高温结构陶瓷材料,在各个领域被广泛应用。目前六方氮化硼陶瓷也存在的一些问题:h-BN粉末具有松散、易吸潮等性质,热压烧结陶瓷致密度低,机械强度比较低,具有较明显的各向异性、且在氧气气氛中稳定性比较差,使用温度在900℃以下[1,2]。
其他专利则是通过加入第二相,来强化氮化硼基陶瓷的各项性能[3,4]。本发明研究了可在超高温环境中使用的高强度氮化硼陶瓷的制备方法,在保证氮化硼陶瓷高温性能的同时,提高了传统氮化硼陶瓷的力学性能,解决了氮化硼粉体细化与潮解氧化的矛盾,降低了高强氮化硼陶瓷材料的生产成本。
参考文献
[1]叶乃清,曾照强,胡晓清,等,BN基复合陶瓷致密化的主要障碍[J],现代技术陶瓷,1998,19(1):7-10;
[2]陈广乐,彭珍珍,范仕刚,等,热压烧结高纯h-BN陶瓷材料及其致密性研究[J],硅酸盐通报,2010,29(2):436-439;
[3]严密,徐崟,一种高强度高抗氧化性BN陶瓷及其制备方法[P],浙江:CN103420677A,2013-12-04;
[4]贾德昌,梁斌,杨治华,王胜金,何培刚,段小明,周玉,一种片层状BN(C)晶粒增韧的Si#B#C#N陶瓷的制备方法[P],黑龙江:CN106518075A,2017-03-22。
发明内容
本发明研究了可在超高温环境中使用的高强度氮化硼陶瓷的制备方法,在保证氮化硼陶瓷高温性能的同时,提高了传统氮化硼陶瓷的力学性能,解决了氮化硼粉体细化与潮解氧化的矛盾,降低了高强氮化硼陶瓷材料的生产成本。本发明是采取球磨介质级配、球磨环境控制和参数优化将氮化硼粉体球磨到纳米级别,然后根据材料的性能要求在氮化硼中添加二硼化锆粉或硼粉,再将原料放入模具中进行热压烧结并对热压烧结的升温和降温速率进行控制。该方法对原料要求简单,制备过程中无污染物排放,对制备的环境和设备要求比较低,利于工业大规模制备。
为此本发明的技术方案如下:
一种超高温环境中使用的高强度氮化硼陶瓷的制备方法,包括如下步骤:
(1)将氮化硼粉料置于球磨罐中,并加入不同直径的氧化锆研磨球,然后将球磨罐抽真空或通入氮气,利用球磨设备对其进行粉磨使其粒度D50<1μm,其中球磨方式可以采用干磨或湿磨,球磨过程中控制物料温度低于40℃;
(2)根据产品使用性能要求,在处理后的氮化硼粉料中加入体积分数为0~20%的硼粉,进行均匀混合后得到陶瓷原料。将陶瓷原料置于热压模具中,装模,预压;
(3)将装完料的模具置于真空热压炉内,炉内真空度<10Pa,以3-15℃/min的速率升温到1800-2100℃后,开始对样品进行加压处理,压力为20-60MPa,保温10-120min后降温泄压,降温速率为3-15℃/min.即得所述的高强氮化硼陶瓷材料。
优选,步骤(1)所述氮化硼原料是六方氮化硼,氮化硼(BN)含量≥99.0%,粒度D50<3μm;
优选,步骤(1)原料在球磨过程中加入不同直径的氧化锆球,并按照一定的比例混合使用;
优选,步骤(1)原料的球磨方式分为干磨和湿磨两种方式,其中湿磨的球磨介质为有机溶剂;
优选,步骤(1)所述的球磨时间为1-5h;
优选,步骤(3)的升温过程分为三步,第一步以10~15℃/min的速率由室温升温到1200~1400℃,第二步以6~10℃/min的速率升温到1500~1700℃,第三步以5~8℃/min的速率升温到1800~2100℃;
优选,步骤(3)的加压方式为1000-1300℃进行预压约10 MPa,1800~2100℃加压到20~60 MPa。加压方式为缓慢加压。
本发明采取球磨介质级配、球磨环境控制和参数优化将氮化硼粉体球磨到纳米级别。根据产品使用性能要求在处理好的氮化硼粉末中添加二硼化锆或硼粉。利用热压烧结的工艺,控制好升温速率、保温时间、热压温度以及降温速率,控制氮化硼晶粒生长从而获得高于现有氮化硼材料强度和电学性能的新型高强氮化硼材料,且物相中不含影响其高温性能的氧化硼。该项发明提供了一种新的技术,可提高氮化硼物理性能,同时制备成本较低,利于工业化生产制备。
附图说明
图1为氮化硼粉体干磨与湿磨粒度对比。测试结果如图所示:在相同的时间内,干磨的效果比湿磨的更加明显。
图2为球磨后氮化硼粉与氮化硼陶瓷的XRD图谱。
图3 原料细化SEM图片(a:原料;b:干法球磨210min)。
图4为氮化硼陶瓷断口形貌SEM图片。
图5为氮化硼-硼粉复合陶瓷断面SEM照片(a:热压烧结陶瓷;b:2000℃流动氩气热暴露2h后陶瓷)。
图6为氮化硼基陶瓷的物理性质。
具体实施例
具体实施例一:
(1)将氮化硼(BN)含量为99.8%,粒度D50为2μm低温相氮化硼置于球磨罐中加入直径为20mm,8mm,12mm的氧化锆球,其比例为:2:5:3,然后将球磨罐抽真空再通入氮气至0.8个大气压,球磨过程中控制物料温度低于40℃。采用干法球磨5h后,获得粒度D50为0.4μm的氮化硼粉。
(2)将陶瓷原料置于热压模具中,装模,预压。
(3)将装完料的模具置于真空热压炉内,炉内真空度<10Pa,分三步进行升温:第一步以10℃/min的速率由室温升温到1400℃,第二步以8℃/min的速率升温到1700℃,第三步以5℃/min的速率升温到1900℃。与此同时,在1400℃进行预压约10 MPa,1900℃加压到30MPa。加压方式为缓慢加压。在1900℃保温60min后降温泄压,降温速率为3℃/min。冷却后脱模即得所述的高强氮化硼陶瓷材料。
材料的密度为:1.99g/cm3,抗弯强度为:88MPa,在流动氩气的氛围下,2000℃,保温12小时质量损失为:0.99%。
具体实施例二:
(1)将氮化硼(BN)含量为99.2%,粒度D50为3μm低温相氮化硼置于球磨罐中加入直径为20mm,8mm,12mm的氧化锆球,其比例为:2:5:3,然后在球磨罐抽中倒入正己烷,球磨过程中控制物料温度低于40℃。采用湿法球磨3h后,获得粒度D50为0.8μm的氮化硼粉。
(2)根据产品使用性能要求,在处理后的氮化硼粉料中加入质量分数为5%的硼粉,进行均匀混合后得到陶瓷原料。将陶瓷原料置于热压模具中,装模,预压。
(3)将装完料的模具置于真空热压炉内,炉内真空度<10Pa,分三步进行升温:第一步以10℃/min的速率由室温升温到1300℃,第二步以8℃/min的速率升温到1600℃,第三步以5℃/min的速率升温到2000℃。与此同时,在1400℃进行预压约10 MPa,2000℃加压到20MPa。加压方式为缓慢加压。在2000℃保温90min后降温泄压,降温速率为5℃/min。冷却后脱模即得所述的高强氮化硼陶瓷材料。
材料的密度为:1.83g/cm3,抗弯强度为:113MPa,在流动氩气的氛围下,2000℃,保温2小时质量损失为:0.56%。
Claims (7)
1.一种可在超高温环境中使用的高强度氮化硼陶瓷的制备方法,其特征在于包括如下步骤:
(1)将氮化硼粉料置于球磨罐中,并加入不同直径的氧化锆研磨球,然后将球磨罐抽真空或通入氮气,利用球磨设备对其进行粉磨使其粒度D50<1μm,其中球磨方式可以采用干磨或湿磨,球磨过程中控制物料温度低于40℃;
(2)根据产品使用性能要求,在球磨后的氮化硼粉料中加入体积分数为0~20%的硼粉,进行均匀混合后得到陶瓷原料;将陶瓷原料置于热压模具中,装模,预压;
(3)将装完料的模具置于真空热压炉内,炉内真空度<10Pa,以3-15℃/min的速率升温到1800-2100℃后,开始对样品进行加压处理,压力为20-60MPa,保温10-120min后降温泄压,降温速率为3-15℃/min.即得所述的高强氮化硼陶瓷材料。
2.如权利要求1所述的制备方法,其特征在于:所述氮化硼原料是六方氮化硼,氮化硼(BN)含量≥99.0%,粒度D50<3μm。
3.如权利要求1所述的制备方法,其特征在于:步骤1)原料球磨过程中加入不同直径的氧化锆球,并按照一定的比例混合使用。
4.如权利要求1所述的制备方法,其特征在于:步骤1)原料的球磨方式分为干磨和湿磨两种方式,其中湿磨的球磨介质为有机溶剂。
5.如权利要求1所述的制备方法,其特征在于:步骤1)所述的球磨时间为1-5h。
6.如权利要求1所述的制备方法,其特征在于:步骤3)的升温过程分为三步,第一步以10~15℃/min的速率由室温升温到1200~1400℃,第二步以6~10℃/min的速率升温到1500~1700℃,第三步以5~8℃/min的速率升温到1800~2100℃。
7.如权利要求1所述的制备方法其特征在于:步骤3)的加压方式为1000-1300℃进行预压约10 MPa,1800~2100℃加压到20~60 Mpa;加压方式为缓慢加压。
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