CN110627507A - 一种低温碳化硅陶瓷及其制备方法和应用 - Google Patents

一种低温碳化硅陶瓷及其制备方法和应用 Download PDF

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CN110627507A
CN110627507A CN201910882493.9A CN201910882493A CN110627507A CN 110627507 A CN110627507 A CN 110627507A CN 201910882493 A CN201910882493 A CN 201910882493A CN 110627507 A CN110627507 A CN 110627507A
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silicon carbide
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郭伟明
吴利翔
袁进豪
牛文彬
詹创添
朱林林
林华泰
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Guangdong University of Technology
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Abstract

本发明属于陶瓷技术领域，公开了一种低温碳化硅陶瓷及其制备方法和应用，所述低温碳化硅陶瓷是将Al粉、Si粉和C粉均匀混合后，先将Al‑Si‑C混合粉体在1500～1800℃下加热反应，然后将反应后所得粉体A在空气或氧气下继续在600～1000℃加热处理，再将热处理后所得粉体B在真空或氩气下1500～1800℃烧结制得。本发明制得的碳化硅陶瓷的致密度为95～100％，粒径为10nm～10μm，硬度为25～40GPa，断裂韧性为8～12MPa·m1/2，抗弯强度800～1500MPa。本发明的碳化硅陶瓷可应用于防弹装甲、航空航天或核能领域中。

Description

一种低温碳化硅陶瓷及其制备方法和应用
技术领域
本发明属于非氧化物陶瓷材料技术领域，更具体地，涉及一种低温碳化硅陶瓷及其制备方法和应用。
背景技术
碳化硅(SiC)陶瓷是一种共价键化合物，类似于金刚石结构，具有非常优异的力学性能和物理、化学性能，因为其高弹性模量、良好的光学性能、低中子吸收截面、优异的抗辐照性能以及抗高温等性能，使其在防弹装甲、航空航天和核能领域具有非常好的应用。
传统的碳化硅制备主要是在高温(＞1800℃)高压下(＞30MPa)制备得到，而且，因为碳化硅烧结性能低，在烧结过程中SiC的扩散系数极低，因此，通常需要在碳化硅粉体中引入添加剂促进碳化硅陶瓷的烧结，然而，烧结助剂的引入往往存在一定程度的团聚，尤其是纳米颗粒的引入，因此，在研究低温制备碳化硅时，虽然引入的是高烧结活性的原料粉体以及烧结助剂，但是因为在机械混合时已经发生了团聚，这使得碳化硅的烧结性能受到限制。为了迎合碳化硅在工业和军事领域的应用，急需寻求一种低温低压下实现致密碳化硅陶瓷的制备。
发明内容
为了解决上述现有技术存在的不足和缺点，本发明首要的目的在于提供一种低温碳化硅陶瓷。
本发明的另一目的在于提供上述低温碳化硅陶瓷的制备方法。
本发明的再一目的在于提供上述低温碳化硅陶瓷的应用。
本发明的目的通过下述技术方案来实现：
一种低温碳化硅陶瓷，所述低温碳化硅陶瓷是将Al粉、Si粉和C粉均匀混合后，先将Al-Si-C混合粉体在1500～1800℃下加热反应，然后将反应后所得粉体A在空气或氧气下继续在600～1000℃加热处理，再将热处理后所得粉体B在真空或氩气下1500～1800℃烧结制得。
优选地，所述的低温碳化硅陶瓷的致密度为95～100％，其粒径为10nm～10μm，硬度为25～40GPa，断裂韧性为8～12MPa·m1/2，抗弯强度800～1500MPa。
优选地，所述的Al粉的纯度为95～99％，Si粉的纯度为95～99％，C粉的纯度为98～100％；所述的Al粉、Si粉和C粉的粒径均为0.01～10μm。
优选地，所述的Al粉、Si粉、C粉的摩尔比为(4～6)：(1～1.5)：(3.5～4)。
优选地，所述在1500～1800℃下加热反应的时间为0.5～2h，在600～1000℃加热处理的时间为1～10h，所述1500～1800℃烧结的时间为10～120min。
优选地，所述在1500～1800℃加热和在600～1000℃加热的升温速率均为3～20℃/min。
优选地，所述1500～1800℃烧结的温速率为5～200℃/min。
优选地，所述烧结的方式为无压烧、气压烧结、放电等离子烧结、热压烧结或热等静压烧结。
所述的低温碳化硅陶瓷的制备方法，包括如下具体步骤：
S1.将Al粉、Si粉和C粉在磁力搅拌下进行均匀混合，得到Al-Si-C的混合粉体；
S2.将Al-Si-C混合粉体在真空或氩气下1500～1800℃加热反应，制得粉体A；
S3.将粉体A在空气或氧气下继续在600～1000℃加热处理，制得粉体B；
S4.将粉体B在真空或氩气下1500～1800℃烧结，制得碳化硅陶瓷。
所述的低温碳化硅陶瓷在防弹装甲、航空航天或核能领域中的应用。
与现有技术相比，本发明具有以下有益效果：
1.本发明通过原位合成反应实现掺杂Al4SiC4的碳化硅粉体的合成，作为烧结助剂的Al4SiC4均匀分布在碳化硅粉体中，并且Al4SiC4和碳化硅粉体粒径可控。
2.本发明首次将Al-Si-C混合粉体在反应气氛为真空或氩气下通过三步加热，可实现碳化硅的低温致密化。
3.本发明通过对原料粉体的粒径以及后续烧结工艺的选择可对制备碳化硅的晶粒以及性能进行调控。
附图说明
图1为实施例1中经第一步加热反应后所得粉体A的XRD图；
图2为实施例1中经第一步加热反应后所得粉体A的形貌图；
图3为实施例1中经第二步加热热处理后所得粉体B的XRD图；
图4为实施例1中经第二步加热热处理后所得粉体B的形貌图。
具体实施方式
下面结合具体实施例进一步说明本发明的内容，但不应理解为对本发明的限制。若未特别指明，实施例中所用的技术手段为本领域技术人员所熟知的常规手段。除非特别说明，本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
实施例1
1.以Al粉(粒径5μm)、Si粉(粒径为1μm)和C粉(粒径为5μm)为原料，Al-Si-C按质量比为4:1:4的在磁力搅拌下进行混合，混合粉体经混料、干燥后，得到均匀的Al-Si-C混合粉体。
2.将Al-Si-C混合粉体在无压炉中以10℃/min升温到1700℃保温1h，此时为Ar气气氛，得到粉体A；
3.将粉体A在马弗炉空气气氛中进行800℃保温1h热处理后，得到粉体B；
4.将热处理后的粉体B在1700℃无压炉Ar气氛下保温1h烧结，制得致密的SiC陶瓷。
图1为本实施例中第一步加热制得的粉体A的XRD图；从图1中可知，粉体A中主要成分为β-SiC、Al4SiC4相以及碳，说明粉体A含有碳杂质；图2为本实施例中经第一步加热反应后所得粉体A的形貌图。图2中片状晶粒为石墨相，进一步证明经第一步加热后存在片状形的碳，图3为本实施例中经第二步热处理后粉体B的XRD图，图3中只有β-SiC和Al4SiC4相，说明经第二步热处理在去除碳杂质的同时并没有引入其他杂质相，图4为本实施例中经第二步热处理后粉体B的形貌图，图4中并没有观察到片状碳的存在，进一步证明碳杂质相的彻底清除。
本实施例制备得到的碳化硅陶瓷的致密度为99％，粒径为5μm，硬度为30GPa，断裂韧性为12MPa·m1/2，弯曲强度为1200MPa。
实施例2
与实施例1不同在于：Al粉的粒径为0.01μm，Si粉的粒径为0.01μm，C粉的粒径为0.01μm，Al-Si-C的质量为4.5:1:3.5，第一步加热温度为1750℃保温1h，第二步热处理为600℃保温5h，第三步加热为在放电等离子烧结设备中进行1500℃保温10min，加压30MPa，Ar气氛，烧结制得致密碳化硅陶瓷。
本实施例制备得到的碳化硅陶瓷的致密度为99％，粒径为10nm，硬度为38GPa，断裂韧性为10MPa·m1/2，弯曲强度为1500MPa。
实施例3
与实施例1不同在于：Al粉的粒径为0.1μm，Si粉的粒径为0.1μm，C粉的粒径为0.1μm，第二步加热为在800℃保温5h，第三步加热为在无压烧结炉中Ar气氛下加热到1600℃保温1h，通过无压、低温烧结制得碳化硅陶瓷。
本实施例制备得到的碳化硅陶瓷的致密度为99％，粒径为0.1μm，硬度为35GPa，断裂韧性为10MPa·m1/2，弯曲强度为1000MPa。
实施例4
与实施例1不同在于：Al粉的粒径为10μm，Si粉的粒径为10μm，C粉的粒径为10μm，第二步加热为1200℃保温1h，第三步加热为无压烧结炉中真空气氛加热到1800℃保温1h，烧结制备制得碳化硅陶瓷。
本实施例制备得到的碳化硅陶瓷的致密度为99％，粒径为10μm，硬度为25GPa，断裂韧性为12MPa·m1/2，弯曲强度为1000MPa。
实施例5
与实施例1不同在于：Al粉的粒径为1μm，Si粉的粒径为1μm，C粉的粒径为1μm，第一步加热为1500℃保温1h，第二步加热为1000℃保温1h，第三步加热为在热等静压中进行1600℃保温1h，烧结制备制得碳化硅陶瓷。
本实施例制备得到的碳化硅陶瓷的致密度为99％，粒径为5μm，硬度为30GPa，断裂韧性为10MPa·m1/2，弯曲强度为1200MPa。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合和简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (10)

1.一种低温碳化硅陶瓷，其特征在于，所述低温碳化硅陶瓷是将Al粉、Si粉和C粉均匀混合后，先将Al-Si-C混合粉体在1500～1800℃下加热反应，然后将反应后所得粉体A在空气或氧气下继续在600～1000℃加热处理，再将热处理后所得粉体B在真空或氩气下1500～1800℃烧结制得。
2.根据权利要求1所述的低温碳化硅陶瓷，其特征在于，所述的低温碳化硅陶瓷的致密度为95～100％，其粒径为10nm～10μm，硬度为25～40GPa，断裂韧性为8～12MPa·m1/2，抗弯强度800～1500MPa。
3.根据权利要求1所述的低温碳化硅陶瓷，其特征在于，所述的Al粉的纯度为95～99％，Si粉的纯度为95～99％，C粉的纯度为98～100％；所述的Al粉、Si粉和C粉的粒径均为0.01～10μm。
4.根据权利要求1所述的低温碳化硅陶瓷，其特征在于，所述的Al粉、Si粉、C粉的摩尔比为(4～6)：(1～1.5)：(3.5～4)。
5.根据权利要求1所述的低温碳化硅陶瓷，其特征在于，所述在1500～1800℃下加热反应的时间为0.5～2h，在600～1000℃加热处理的时间为1～10h，所述1500～1800℃烧结的时间为10～120min。
6.根据权利要求1所述的低温碳化硅陶瓷，其特征在于，所述在1500～1800℃加热和在600～1000℃加热的升温速率均为3～20℃/min。
7.根据权利要求1所述的低温碳化硅陶瓷，其特征在于，所述1500～1800℃烧结的温速率为5～200℃/min。
8.根据权利要求1所述的低温碳化硅陶瓷，其特征在于，所述烧结的方式为无压烧、气压烧结、放电等离子烧结、热压烧结或热等静压烧结。
9.根据权利要求1-8任一项所述的低温碳化硅陶瓷的制备方法，其特征在于，包括如下具体步骤：
S1.将Al粉、Si粉和C粉在磁力搅拌下进行均匀混合，得到Al-Si-C的混合粉体；
S2.将Al-Si-C混合粉体在真空或氩气下1500～1800℃加热反应，制得粉体A；
S3.将粉体A在空气或氧气下继续在600～1000℃加热处理，制得粉体B；
S4.将粉体B在真空或氩气下1500～1800℃烧结，制得碳化硅陶瓷。
10.权利要求1-8任一项所述的低温碳化硅陶瓷在防弹装甲、航空航天或核能领域中的应用。
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