CN110550957B - 一种原位合成氮化硅/硼化锆复相陶瓷及其制备方法和应用 - Google Patents

一种原位合成氮化硅/硼化锆复相陶瓷及其制备方法和应用 Download PDF

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CN110550957B
CN110550957B CN201910774763.4A CN201910774763A CN110550957B CN 110550957 B CN110550957 B CN 110550957B CN 201910774763 A CN201910774763 A CN 201910774763A CN 110550957 B CN110550957 B CN 110550957B
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詹创添
吴利翔
牛文彬
朱林林
郭伟明
林华泰
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Guangdong University of Technology
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Abstract

本发明属于于陶瓷材料技术领域，公开了一种原位合成氮化硅/硼化锆复相陶瓷及其制备方法和应用，所述氮化硅/硼化锆复相陶瓷是将预氧化的ZrB2、Si粉和烧结助剂MgO‑Y2O3经混料，干燥后得到Si‑ZrB2‑MgO‑Y2O3混合粉体；将混合粉体进行造粒和成型，再采用冷等静压制得Si‑ZrB2‑MgO‑Y2O3坯体；将坯体在氮气气氛下，升温至1300～1450℃烧结，然后升温至1500～1600℃烧结并保温制得。本发明方法所制备的Si3N4‑ZrB2复相陶瓷的相对密度为95～99％，硬度为18～25GPa，断裂韧性为10～15MPa·m1/2，抗弯强度为800～1200MPa。

Description

一种原位合成氮化硅/硼化锆复相陶瓷及其制备方法和应用
技术领域
本发明属于陶瓷材料技术领域，更具体地，涉及一种原位合成氮化硅/硼化锆(Si3N4-ZrB2)复相陶瓷及其制备方法和应用。
背景技术
Si3N4陶瓷作为一种结构陶瓷，具有高强、高硬、高韧、耐磨、耐高温、以及高导热等优异性能，在工业界具有广泛的应用。通常Si3N4陶瓷以高纯Si3N4粉体为原料，添加烧结助剂促进致密化，但是这种方法制备成本较高。
近年来，虽然出现了以Si粉为原料，通过反应气压烧结制备Si3N4陶瓷，降低成本。但是由于Si粉氮化的速度比较缓慢，并且氮化后形成的Si3N4致密化较困难，很难获得高致密、高性能的Si3N4陶瓷。即Si粉反应烧结制备Si3N4陶瓷主要存在Si粉氮化时间较长的问题，如此长周期并且苛刻的制备工艺部分抵消了以Si粉为原料带来的低成本优势。基于以上Si粉氮化困难，目前主要通过往Si粉中添加ZrO2、TiO2、稀土氧化物等作为催化剂促进氮化，但是，在现有的技术中都只是通过Si粉反应烧结制备Si3N4陶瓷，然而，考虑到有些需要更高硬度以及导电的场合，现有技术却无法满足。
发明内容
为了解决上述现有技术存在的不足和缺点，本发明的首要目的在于提供一种氮化硅/硼化锆陶瓷。
本发明另一目的在于提供上述氮化硅/硼化锆陶瓷的制备方法。
本发明再一目的在于提供上述氮化硅/硼化锆陶瓷的应用。
本发明的目的通过下述技术方案来实现：
一种原位合成氮化硅/硼化锆复相陶瓷，所述氮化硅/硼化锆复相陶瓷是将预氧化的ZrB2、Si粉和烧结助剂MgO-Y2O3经球磨混料干燥后，得到Si-ZrB2-MgO-Y2O3混合粉体；将混合粉体进行造粒和成型，再采用冷等静压在100～300MPa保压制得Si-ZrB2-MgO-Y2O3坯体；将坯体在氮气气氛下，升温至1300～1450℃烧结，然后升温至1500～1600℃烧结制得。
优选地，所述氮化硅/硼化锆复相陶瓷的相对密度为95～99％，硬度为18～25GPa，断裂韧性为10～15MPa·m1/2，抗弯强度为800～1200MPa。
优选地，所述Si粉、预氧化的ZrB2、MgO-Y2O3的质量比为(50～98)：(1～40)：(1～10)。
优选地，所述的Si粉的纯度为95～99％，Si粉的粒径为0.1～10μm；ZrB2的纯度为95～99％，ZrB2的粒径为0.1～10μm；MgO粉的纯度98～100％，Y2O3的纯度98～100％。
优选地，所述的预氧化的ZrB2预氧化是将ZrB2在500～1000℃保温1～10h处理制得。
优选地，所述MgO-Y2O3中的MgO：Y2O3的质量比为(3～5)：(5～7)。
优选地，所述升温至1300～1450℃烧结的时间为0.5～4h；升温至1500～1600℃烧结的时间为0.5～2h。
优选地，所述升温至1300～1450℃的速率为10～20℃/min；所述升温至1500～1600℃的速率为5～10℃/min。
所述的原位合成氮化硅/硼化锆复相陶瓷的制备方法，包括如下具体步骤：
S1.将预氧化的ZrB2，Si粉和MgO-Y2O3烧结助剂，经球磨混料，干燥后得到Si-ZrB2-MgO-Y2O3混合粉体；
S2.将Si-ZrB2-MgO-Y2O3混合粉体进行造粒，然后将造粒粉体进行成型，通过冷等静压在100～300MPa保压1～10min，制得Si-ZrB2-MgO-Y2O3坯体；
S3.将Si-ZrB2-MgO-Y2O3坯体在1～20atm的氮气气氛下，升温至1300～1450℃烧结，然后升温至1500～1600℃烧结，制得氮化硅/硼化锆复相陶瓷。
所述原位合成氮化硅/硼化锆复相陶瓷在陶瓷轴承球、陶瓷刀具或导电陶瓷领域中的应用。
与现有技术相比，本发明具有以下有益效果：
1.本发明的预氧化后的ZrO2在促进Si粉氮化的同时，引入了ZrB2硬质相；往Si3N4中添加硬质相ZrB2，可以显著提高其硬度，将ZrB2进行预氧化可使得ZrB2表面的ZrO2充当氮化助剂，在促进Si粉氮化的同时引入ZrB2硬质相。
2.本发明通过Si粉氮化的同时引入ZrB2硬质导电相，不仅提高了Si3N4陶瓷的力学性能，而且随着ZrB2的加入可以对其导电性进行调节，ZrB2作为导电陶瓷，Si3N4作为绝缘陶瓷，随着ZrB2含量的增加，导电性增强。
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Si粉(粒径1μm)为原料，以10％ZrB2(粒径为0.1μm)为第二相，将在1000℃保温10h的预处理ZrB2，5％MgO粉(纯度为99.9％)和5％Y2O3粉(纯度为99.9％)为添加剂进行配料，以乙醇为溶剂，以Si3N4球为球磨介质，在球磨机上混合8h，经球磨混料干燥后，得到均匀的Si-ZrB2-MgO-Y2O3混合粉体。
2.将Si-ZrB2-MgO-Y2O3混合粉体放入模具进行成型获得坯体，然后通过冷等静压，在压力200MPa下保压时间为5min，获得Si-ZrB2-MgO-Y2O3坯体。
3.将Si-ZrB2-MgO-Y2O3坯体放入石墨坩埚，以20℃/min的速率升温至1400℃保温2h，气氛为1atm的氮气，再以10℃/min的速率升温至1500℃保温4h，气氛为10atm的氮气，通过气压烧结，获得Si3N4-ZrB2陶瓷。
本实施例制备得到的Si3N4-ZrB2陶瓷的相对密度为99％，硬度为23GPa，断裂韧性为15MPa·m1/2，弯曲强度为1200MPa。
实施例2
与实施例1不同的在于：将在500℃保温1h的预处理ZrB2、Si粉、MgO、Yb2O3粉的质量比为40：55：2.5：2.5进行配料，其中，首先升温至1300℃保温4h，然后升温至1500℃保温2h，制得Si3N4-ZrB2陶瓷。
制备所得Si3N4-ZrB2陶瓷的相对密度为99％，材料的硬度为25GPa，断裂韧性为10MPa·m1/2，弯曲强度为1200MPa。
实施例3
与实施例1不同的在于：将在800℃保温5h的预处理ZrB2、Si粉、MgO、Yb2O3粉质量比为20：75：2.5：2.5进行配料，其中，首先升温至1450℃保温0.5h，然后升温至1600℃保温1h，制得Si3N4-ZrB2陶瓷。
制备所得Si3N4-ZrB2陶瓷的相对密度为99％，材料的硬度为20GPa，断裂韧性为12MPa·m1/2，弯曲强度为1000MPa。
实施例4
与实施例1不同的在于：将在1000℃保温10h的预处理ZrB2、Si粉、MgO、Yb2O3粉质量比为5：85：5：5进行配料，其中，首先升温至1400℃保温4h，然后升温至1500℃保温1h，制得Si3N4-ZrB2陶瓷。
制备所得Si3N4-ZrB2陶瓷的相对密度为99％，材料的硬度为20GPa，断裂韧性为15MPa·m1/2，弯曲强度为1200MPa。
实施例5
与实施例1不同的在于：将在600℃保温5h的预处理ZrB2、Si粉、MgO、Yb2O3粉质量比为20：75：2.5：2.5进行配料，其中首先升温至1450℃保温4h，然后升温至1600℃保温4h，制得Si3N4-ZrB2陶瓷。
制备所得Si3N4-ZrB2陶瓷的相对密度为99％，材料的硬度为20GPa，断裂韧性为10MPa·m1/2，弯曲强度为1000MPa。
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 (6)

1.一种原位合成氮化硅/硼化锆复相陶瓷，其特征在于，所述氮化硅/硼化锆复相陶瓷是将预氧化的ZrB2、Si粉和烧结助剂MgO-Y2O3经球磨混料，干燥后得到Si-ZrB2-MgO-Y2O3混合粉体；将混合粉体进行造粒和成型，再采用冷等静压在100~300MPa下制得Si-ZrB2-MgO-Y2O3坯体；将坯体在氮气气氛下，升温至1300~1450℃烧结，然后升温至1500~1600℃烧结制得；所述Si粉、预氧化的ZrB2、MgO-Y2O3的质量比为（50~98）：（1~40）：（1~10）；所述的预氧化的ZrB2预氧化是将ZrB2在500~1000℃保温1~10h处理制得；所述的Si粉的纯度为95~99%，Si粉的粒径为0.1~10μm；ZrB2的纯度为95~99%，ZrB2的粒径为0.1~10μm；MgO粉的纯度98~100%，Y2O3的纯度98~100%；所述MgO-Y2O3中的MgO：Y2O3的质量比为（3~5）：（5~7）。
2.根据权利要求1所述的原位合成氮化硅/硼化锆复相陶瓷，其特征在于，所述氮化硅/硼化锆复相陶瓷的相对密度为95~99%，硬度为18~25GPa，断裂韧性为10~15MPa×m1/2，抗弯强度为800~1200MPa。
3.根据权利要求1所述的原位合成氮化硅/硼化锆复相陶瓷，其特征在于，所述升温至1300~1450℃烧结的时间为0.5~4h；升温至1500~1600℃烧结的时间为0.5~2h。
4.根据权利要求1所述的原位合成氮化硅/硼化锆复相陶瓷，其特征在于，所述升温至1300~1450℃的速率为10~20℃/min；所述升温至1500~1600℃的速率为5~10℃/min。
5.根据权利要求1-4任一项所述的原位合成氮化硅/硼化锆复相陶瓷的制备方法，其特征在于，包括如下具体步骤：
S1. 将预氧化的ZrB2，Si粉和MgO-Y2O3烧结助剂，经球磨混料，干燥后得到Si-ZrB2-MgO-Y2O3混合粉体；
S2. 将Si-ZrB2-MgO-Y2O3混合粉体进行造粒，然后将造粒粉体进行成型，通过冷等静压在100~300MPa保压1~10min，制得Si-ZrB2-MgO-Y2O3坯体；
S3. 将Si-ZrB2-MgO-Y2O3坯体在1~20atm的氮气气氛下，升温至1300~1450℃烧结，然后升温至1500~1600℃烧结，制得氮化硅/硼化锆复相陶瓷。
6.权利要求1~4任一项所述原位合成氮化硅/硼化锆复相陶瓷在陶瓷轴承球或导电陶瓷领域中的应用。
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