CN111875382B - 一种耐磨特种陶瓷的制备方法及其产品 - Google Patents
一种耐磨特种陶瓷的制备方法及其产品 Download PDFInfo
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Abstract
本发明公开了一种耐磨特种陶瓷的制备方法及其产品。该陶瓷是通过按照原料配比进行混合,球磨,干燥,压制成型,烧结得到W和Nb共掺杂Ti3SiC2陶瓷材料,通过W和Nb的掺杂能够显著提高Ti3SiC2的硬度和抗弯强度,降低磨损率,使其具有硬度Hv为13.2~14.3GPa,抗弯强度为430~450MPa,磨损率为8.1×10‑5~8.5×10‑5,本发明的制备方法简单,性能优异,是用于制备汽车刹车盘的理想材料。
Description
技术领域
本发明属于陶瓷制备领域,具体涉及一种耐磨特种陶瓷的制备方法及其产品。
背景技术
陶瓷材料具有耐高温、耐腐蚀、耐磨损、重量轻等很多优点,在能源、冶金、航天航空、石油化工等领域有着广泛的应用前景。但是,陶瓷材料本身脆性大,对缺陷十分敏感,导致使用可靠性和可重复性差,限制了其应用。
刹车盘作为汽车制动系统中主要磨损部件,需求量也非常大。刹车盘作为汽车盘刹的一个制动元件,其性能的优劣(耐磨性、导热性等等)决定了汽车刹车效果的好坏。
而Ti3SiC2是一种兼有金属和陶瓷优良性能的三元层状化合物,首先拥有陶瓷材料的高屈服强度、高熔点、高弹性模量、高热稳定性和良好的抗氧化性能;其次,和金属一样在常温下,有良好的导电导热性能、较低的vichers硬度,可以像金属和石墨一样直接进行机械加工,能在没有润滑和冷却的条件下使用高速钢刀具加工。因而,Ti3SiC2的开发受到了材料人员的广泛关注。
但是在实际的应用中,由于Ti3SiC2的摩擦系数较高,而且由于晶粒的断裂和拔出,使得其具有较高的磨损率,而且其硬度和抗弯强度也并不满足实际的需求。通常来说,在材料基体中添加润滑相或硬质相可以改善材料的摩擦磨损性能和力学性能。文怀兴等研究了Mo掺杂对Ti3SiC2陶瓷性能的影响,研究发现在适宜的Mo掺杂量下能够显著提高其硬度和抗弯强度,且能够显著降低其磨损率。但是上述研究对Ti3SiC2陶瓷性能的提升并不是很理想,如何更好的提高Ti3SiC2陶瓷硬度的同时提高其抗弯强度,降低磨损率,仍是目前急需解决的问题。
发明内容
本发明所要解决的技术问题在于针对上述现有技术中的不足,提供一种耐磨特种陶瓷的制备方法及其产品,其致密性好,具有较高的硬度和抗弯强度,较低的磨损率,即具体的硬度Hv为13.2~14.3GPa,抗弯强度为430~450MPa,磨损率为8.1×10-5~8.5×10-5。
本发明采用以下技术方案:
一种耐磨特种陶瓷的制备方法,包括以下步骤:
(1)将纯度大于99.5%的TiC粉、W粉、Nb粉、Ti粉和Si粉按照摩尔比为2:x:y:1-x-y:1.2称取,其中x=0.15~0.35;y=0.15~0.35,然后将称取的原料放入球磨罐中进行球磨,其中,球磨介质为无水乙醇;
(2)球磨结束后,将得到的混合物料进行干燥,然后加入质量分数为5%的聚乙烯醇(PVA)水溶液造粒,将造粒的粉体通过压片机预成型后再经20MPa~30MPa下压制成胚体,将所得的胚体在马弗炉中在500~700℃下排胶2~4h,然后于1500~1600℃下烧结2~6h,随炉冷却至室温得到陶瓷。
优选的,在步骤(1)中,所述球磨时间为3~5h,转速为180~240r/min。
优选的,在步骤(2)中,所述干燥是在80~100℃下干燥4~6h。
优选的,在步骤(2)中,所述排胶过程的升温速率为2~3℃/min,于1500~1600℃下烧结2~6h的升温速率为8~12℃/min。
本发明的另一个技术方案是,基于上述制备方法制备的一种耐磨特种陶瓷。
所述陶瓷材料致密性好,且该耐磨特种陶瓷的硬度Hv为13.2~14.3GPa,抗弯强度为430~450MPa,磨损率为8.1×10-5~8.5×10-5,是用于制备精密机械工具的理想材料。
与现有技术相比,本发明至少具有以下有益效果:
1)一种耐磨特种陶瓷的制备方法及其产品。通过按照TiC粉、W粉、Nb粉、Ti粉和Si粉按照摩尔比为2:x:y:1-x-y:1.2称取,其中x=0.15~0.35;y=0.15~0.35,进行混合,球磨,干燥,压制成型,烧结得到W和Nb共掺杂Ti3SiC2陶瓷材料,通过W和Nb的掺杂能够显著提高Ti3SiC2的硬度和抗弯强度,降低磨损率,使其具有硬度Hv为13.2~14.3GPa,抗弯强度为430~450MPa,磨损率为8.1×10-5~8.5×10-5,本发明的制备方法简单,性能优异,是用于制备汽车刹车盘的理想材料。
2)W和Nb两种元素掺杂进入Ti3SiC2晶格内,且两种元素之间的协同作用促进了Ti3SiC2陶瓷材料的硬度和抗弯强度得到显著的提高,而且具有较低的磨损率。
3)通过采用添加聚乙烯醇压制成型,并排胶处理,使其具有良好的烧结特性,陶瓷材料的孔隙率得到显著降低,致密性得到提高,硬度和抗弯强度也得到进一步的提高。
综上所述,本发明制备的一种耐磨特种陶瓷,由于致密性好,具有较高的硬度和抗弯强度,较低的磨损率,是一种用于制备汽车刹车盘的理想材料。
下面通过实施例,对本发明的技术方案做进一步的详细描述。
具体实施方式
本发明提供的一种耐磨特种陶瓷的制备方法,包括以下步骤:
(1)将纯度大于99.5%的TiC粉、W粉、Nb粉、Ti粉和Si粉按照摩尔比为2:x:y:1-x-y:1.2称取,其中x=0.15~0.35;y=0.15~0.35,然后将称取的原料放入球磨罐中进行球磨,球磨时间为3~5h,转速为180~240r/min,其中,球磨介质为无水乙醇;
(2)球磨结束后,将得到的混合物料进行在80~100℃下干燥4~6h,然后加入质量分数为5%的聚乙烯醇(PVA)水溶液造粒,将造粒的粉体通过压片机预成型后再经20MPa~30MPa下压制成胚体,将所得的胚体在马弗炉中在500~700℃下排胶2~4h,升温速率为2~3℃/min,然后于1500~1600℃下烧结2~6h,升温速率为8~12℃/min,随炉冷却至室温得到陶瓷。
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。通常在所示的本发明实施例的组件可以通过各种不同的配置来布置和设计。因此,以下对本发明的实施例的详细描述并非旨在限制要求保护的本发明的范围,而是仅仅表示本发明的选定实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
一种耐磨特种陶瓷的制备方法,包括以下步骤:
(1)将纯度大于99.5%的TiC粉、W粉、Nb粉、Ti粉和Si粉按照摩尔比为2:0.25:0.25:0.5:1.2称取,然后将称取的原料放入球磨罐中进行球磨,球磨时间为4h,转速为200r/min,其中,球磨介质为无水乙醇;
(2)球磨结束后,将得到的混合物料进行在90℃下干燥5h,然后加入质量分数为5%的聚乙烯醇(PVA)水溶液造粒,将造粒的粉体通过压片机预成型后再经25MPa下压制成胚体,将所得的胚体在马弗炉中在600℃下排胶3h,升温速率为3℃/min,然后于1550℃下烧结2~6h,升温速率为10℃/min,随炉冷却至室温得到陶瓷。
实施例2
一种耐磨特种陶瓷的制备方法,包括以下步骤:
(1)将纯度大于99.5%的TiC粉、W粉、Nb粉、Ti粉和Si粉按照摩尔比为2:0.15:0.35:0.5:1.2称取,然后将称取的原料放入球磨罐中进行球磨,球磨时间为5h,转速为180r/min,其中,球磨介质为无水乙醇;
(2)球磨结束后,将得到的混合物料进行在80℃下干燥6h,然后加入质量分数为5%的聚乙烯醇(PVA)水溶液造粒,将造粒的粉体通过压片机预成型后再经30MPa下压制成胚体,将所得的胚体在马弗炉中在500℃下排胶4h,升温速率为2℃/min,然后于1500℃下烧结6h,升温速率为8℃/min,随炉冷却至室温得到陶瓷。
实施例3
一种耐磨特种陶瓷的制备方法,包括以下步骤:
(1)将纯度大于99.5%的TiC粉、W粉、Nb粉、Ti粉和Si粉按照摩尔比为2:0.15:0.15:0.7:1.2称取,然后将称取的原料放入球磨罐中进行球磨,球磨时间为5h,转速为240r/min,其中,球磨介质为无水乙醇;
(2)球磨结束后,将得到的混合物料进行在100℃下干燥4h,然后加入质量分数为5%的聚乙烯醇(PVA)水溶液造粒,将造粒的粉体通过压片机预成型后再经30MPa下压制成胚体,将所得的胚体在马弗炉中在700℃下排胶2h,升温速率为2℃/min,然后于1600℃下烧结3h,升温速率为12℃/min,随炉冷却至室温得到陶瓷。
实施例4
一种耐磨特种陶瓷的制备方法,包括以下步骤:
(1)将纯度大于99.5%的TiC粉、W粉、Nb粉、Ti粉和Si粉按照摩尔比为2:0.3:0.2:0.5:1.2称取,然后将称取的原料放入球磨罐中进行球磨,球磨时间为4h,转速为200r/min,其中,球磨介质为无水乙醇;
(2)球磨结束后,将得到的混合物料进行在90℃下干燥5h,然后加入质量分数为5%的聚乙烯醇(PVA)水溶液造粒,将造粒的粉体通过压片机预成型后再经25MPa下压制成胚体,将所得的胚体在马弗炉中在600℃下排胶3h,升温速率为3℃/min,然后于1550℃下烧结2~6h,升温速率为10℃/min,随炉冷却至室温得到陶瓷。
实施例5
一种耐磨特种陶瓷的制备方法,包括以下步骤:
(1)将纯度大于99.5%的TiC粉、W粉、Nb粉、Ti粉和Si粉按照摩尔比为2:0.2:0.3:0.5:1.2称取,然后将称取的原料放入球磨罐中进行球磨,球磨时间为4h,转速为200r/min,其中,球磨介质为无水乙醇;
(2)球磨结束后,将得到的混合物料进行在90℃下干燥5h,然后加入质量分数为5%的聚乙烯醇(PVA)水溶液造粒,将造粒的粉体通过压片机预成型后再经25MPa下压制成胚体,将所得的胚体在马弗炉中在600℃下排胶3h,升温速率为3℃/min,然后于1550℃下烧结2~6h,升温速率为10℃/min,随炉冷却至室温得到陶瓷。
对比例1
一种陶瓷材料的制备方法,包括以下步骤:
(1)将纯度大于99.5%的TiC粉、W粉、Ti粉和Si粉按照摩尔比为2:05:0.5:1.2称取,然后将称取的原料放入球磨罐中进行球磨,球磨时间为4h,转速为200r/min,其中,球磨介质为无水乙醇;
(2)球磨结束后,将得到的混合物料进行在90℃下干燥5h,然后加入质量分数为5%的聚乙烯醇(PVA)水溶液造粒,将造粒的粉体通过压片机预成型后再经25MPa下压制成胚体,将所得的胚体在马弗炉中在600℃下排胶3h,升温速率为3℃/min,然后于1550℃下烧结2~6h,升温速率为10℃/min,随炉冷却至室温得到W掺杂Ti3SiC2陶瓷。
对比例2
一种陶瓷材料的制备方法,包括以下步骤:
(1)将纯度大于99.5%的TiC粉、W粉、Nb粉、Ti粉和Si粉按照摩尔比为2:0.5:0.5:1.2称取,然后将称取的原料放入球磨罐中进行球磨,球磨时间为4h,转速为200r/min,其中,球磨介质为无水乙醇;
(2)球磨结束后,将得到的混合物料进行在90℃下干燥5h,然后加入质量分数为5%的聚乙烯醇(PVA)水溶液造粒,将造粒的粉体通过压片机预成型后再经25MPa下压制成胚体,将所得的胚体在马弗炉中在600℃下排胶3h,升温速率为3℃/min,然后于1550℃下烧结2~6h,升温速率为10℃/min,随炉冷却至室温得到Nb掺杂Ti3SiC2陶瓷。
对比例3
一种陶瓷材料的制备方法,包括以下步骤:
(1)将纯度大于99.5%的TiC粉、Ti粉和Si粉按照摩尔比为2:1:1.2称取,然后将称取的原料放入球磨罐中进行球磨,球磨时间为4h,转速为200r/min,其中,球磨介质为无水乙醇;
(2)球磨结束后,将得到的混合物料进行在90℃下干燥5h,然后加入质量分数为5%的聚乙烯醇(PVA)水溶液造粒,将造粒的粉体通过压片机预成型后再经25MPa下压制成胚体,将所得的胚体在马弗炉中在600℃下排胶3h,升温速率为3℃/min,然后于1550℃下烧结2~6h,升温速率为10℃/min,随炉冷却至室温得到Ti3SiC2陶瓷。
将实施例1-5和对比例1-3进行力学性能及摩擦学性能的测试。
采用显微维氏硬度计测量材料的维氏硬度,载荷为10N,加载时间为5S,硬度值是测量五次的平均值;采用PT-1036PC型万能材料实验机测试样品的弯曲强度,试样尺寸为3mm×4mm×20mm,跨距为16mm,压头加载速度为0.5mm/min,弯曲强度取三次测量结果的平均值,采用球盘式摩擦机(HT-1000,兰州中科凯华科技开发有限公司)测试样品的摩擦学性能。具体测试结果见表1:
表1实施例1-5和对比例1-3的力学性能和摩擦学性能
综上所述,本发明制备的一种耐磨特种陶瓷,制备方法简单,而且通过实施例1和对比例1-3的对比例可以发现,由于W和Nb两者之间的协同作用,能够显著提高Ti3SiC2的硬度和抗弯强度,降低磨损率,使其具有硬度Hv和抗弯强度最高分别可达14.3GPa和450MPa,磨损率为最低8.5×10-5。
以上内容仅为说明本发明的技术思想,不能以此限定本发明的保护范围,凡是按照本发明提出的技术思想,在技术方案基础上所做的任何改动,均落入本发明权利要求书的保护范围之内。
Claims (7)
1.一种耐磨特种陶瓷的制备方法,其特征在于,包括以下步骤:
(1)将纯度大于99.5%的TiC粉、W粉、Nb粉、Ti粉和Si粉按照摩尔比为2:x:y:1-x-y:1.2称取,其中x=0.15~0.35;y=0.15~0.35,然后将称取的原料放入球磨罐中进行球磨,其中,球磨介质为无水乙醇;
(2)球磨结束后,将得到的混合物料进行干燥,然后加入质量分数为5%的聚乙烯醇(PVA)水溶液造粒,将造粒的粉体通过压片机预成型后再经20MPa~30MPa下压制成胚体,将所得的胚体在马弗炉中在500~700℃下排胶2~4h,然后于1500~1600℃下烧结2~6h,随炉冷却至室温得到陶瓷。
2.根据权利要求1所述的制备方法,其特征在于:在步骤(1)中,所述球磨时间为3~5h,转速为180~240r/min。
3.根据权利要求1所述的制备方法,其特征在于:在步骤(2)中,所述干燥是在80~100℃下干燥4~6h。
4.根据权利要求1所述的制备方法,其特征在于:在步骤(2)中,所述排胶过程的升温速率为2~3℃/min,于1500~1600℃下烧结2~6h的升温速率为8~12℃/min。
5.根据权利要求1-4任一项所述的制备方法制备的一种耐磨特种陶瓷。
6.根据权利要求5所述的一种耐磨特种陶瓷,其特征在于:所述耐磨特种陶瓷的硬度Hv为13.2~14.3GPa,抗弯强度为430~450MPa,磨损率为8.1×10-5~8.5×10-5。
7.根据权利要求6所述的耐磨特种陶瓷的用途,其特征在于,将所述陶瓷在汽车刹车盘中的应用。
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