CN110590374A - 一种Flashing法制备MoSi2-SiC复合材料的方法 - Google Patents

一种Flashing法制备MoSi2-SiC复合材料的方法 Download PDF

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CN110590374A
CN110590374A CN201911033183.6A CN201911033183A CN110590374A CN 110590374 A CN110590374 A CN 110590374A CN 201911033183 A CN201911033183 A CN 201911033183A CN 110590374 A CN110590374 A CN 110590374A
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张小立
曹文艳
段佳玮
王进才
李启泉
刘�英
裴海燕
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Zhongyuan University of Technology
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Abstract

本发明提供了一种Flashing法制备MoSi2‑SiC复合材料的方法，以Mo和/或MoSi2、C、Si和/或SiO2、酚醛树脂为原料，在500‑1200℃范围内，对以上混合物压片，通过Flashing的方法进行低温短时烧结，获得了MoSi2‑SiC复合材料。与传统烧结工艺相比，FS与陶瓷化所需的时间和温度的大幅降低有关，这意味着明显的节能、更便宜的设备，以及更广泛的环境效益。本发明和方法还可以应用于碳化物陶瓷、氮化物陶瓷、氧化物陶瓷及其复合材料体系的制备，其中控制非氧化性气氛是该复合材料体系FS的关键因素之一。

Description

一种Flashing法制备MoSi2-SiC复合材料的方法
技术领域
本发明涉及MoSi2-SiC复合材料制备领域，具体涉及一种Flashing法制备MoSi2-SiC复合材料的方法。
背景技术
Flashing，简称FS，是由美国科罗拉多大学博尔德分校的科隆纳等人于2010年在RRaij教授指导的实验室中发现的。FS通常在电场炉温的特定起始组合下，材料在极短的时间内致密化，通常从几秒到几分钟不等。
FS的基本特征在于在闪蒸事件(FE)中发生的非常迅速的致密化(大约小于一分钟或更少)。因此，可以定义flash烧结作为电场辅助烧结技术的特点是：快速致密化；电导率突然下降和强劲明亮的光发射。
与传统烧结工艺相比，FS具有许多优点。最明显的一个原因显然与陶瓷化所需的时间和温度的大幅降低有关，这意味着明显的节能、更便宜的设备，以及更广泛的环境效益。固结时间一般从1个数里级减少到3个数里级，从传统工艺的几个小时缩短到闪蒸烧结的几秒钟；固结温度也明显降低(有时降低约1000℃)。FS的另一个优点是它是一个不平衡的过程，它与极高的加热速率和极短的加工时间有关。因此，烧结亚稳态材料或避免不必要的相变是可能的。
发明内容
本发明提出了一种Flashing法制备MoSi2-SiC复合材料的方法，使用Mo、MoSi2、Si、C、SiO2、酚醛树脂、导电胶等为原料，在500-1200℃范围内，对以上混合物压片，通过FS的方法进行低温短时烧结，获得了MoSi2-SiC复合材料，控制非氧化性气氛是该复合材料闪速烧结的关键因素之一。
实现本发明的技术方案是：
一种Flashing法制备MoSi2-SiC复合材料的方法，以Mo和/或MoSi2、C、Si和/或SiO2、酚醛树脂为原料，搅拌均匀、压片固化，通过导电胶给试样施加电流电压进行Flashing法低温短时烧结，得到MoSi2-SiC复合材料。
所述原料中各物质的重量份数分别为：Mo和/或MoSi2 24-45份、Si和/或SiO2 1.5-11.2份、C 2-4.8份、酚醛树脂10-12份。
所述的Flashing法制备MoSi2-SiC复合材料的方法，具体步骤如下：
（1）将Mo和/或MoSi2、Si和/或SiO2、C和酚醛树脂混合均匀，压制成片；
（2）在步骤（1）压片表面或边侧刷上导电胶，并粘结导线，于110℃固化；
（3）在非氧化性气氛中，升温至500-1200℃，并给导线施加电场；
（4）压片发生闪烧，获得MoSi2-SiC复合材料。
所述步骤（3）中电场电流为0.1-60A，步骤（4）闪烧的时间为0.1-10min。
所述导电胶以碳化硅、酚醛树脂和石墨导电胶为原料，按照质量比为（0.5-1）：（0.5-0.7）：（0.3-1），混合均匀研磨成膏状制得。
本发明的有益效果是：本发明能够获得任意相组成的MoSi2-SiC复合材料，且实现了低温短时烧结，环保节能；该FS方法还可以用于氮化物陶瓷，碳化物陶瓷及其氧化物陶瓷复合材料等的烧结。该方法陶瓷化所需的时间和温度的大幅降低，具有明显的节能、更便宜的设备，以及更广泛的环境效益。
具体实施方式
下面将结合本发明实施例，对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有付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
Flashing法制备MoSi2-SiC复合材料的方法，步骤如下：
将32 g MoSi2粉末，2.4 g C粉末，5.0g Si粉末，余量为0.6g SiO2粉末，均匀混合，后加入12g酚醛树脂，搅拌均匀后，压成直径12mm的圆片，并于110℃固化。
导电胶以碳化硅、酚醛树脂和石墨导电胶为原料，按照质量比为0.5：0.5：0.3，混合均匀研磨成膏状制得。
将以上圆片边缘刷上自制导电胶，将铂丝固定在边缘。然后将该样品放入炉温为790℃的管式炉中，通入氩气保护。对样品施加50A的电流，2分钟后，样品烧结完成。
实施例2
Flashing法制备MoSi2-SiC复合材料的方法，步骤如下：
将24 g MoSi2粉末，4.8 g C粉末11.2g Si粉末，均匀混合，后加入10g酚醛树脂，搅拌均匀后，压成直径50*4*1mm的长条片，并于110℃固化。
导电胶以碳化硅、酚醛树脂和石墨导电胶为原料，按照质量比为1：0.7：1，混合均匀研磨成膏状制得。
将以上压条边缘刷上碳导电胶，将铂丝固定在边缘。然后将该样品放入炉温为798℃的管式炉中，通入氩气保护。对样品施加0.1A的电流，10分钟后，样品烧结完成。
实施例3
Flashing法制备MoSi2-SiC复合材料的方法，步骤如下：
将45.0g MoSi2粉末，2g C粉末，1.5g Si粉末均匀混合，后加入10g酚醛树脂，搅拌均匀后，压成直径50*4*1mm的长条片，并于110℃固化。
导电胶以碳化硅、酚醛树脂和石墨导电胶为原料，按照质量比为0.8：0.6：0.6，混合均匀研磨成膏状制得。
将以上压条边缘刷上碳化硅和酚醛树脂的混合物，将铂丝固定在边缘。然后将该样品放入炉温为780℃的管式炉中，通入氩气保护。对样品施加60A的电流，0.1分钟后，样品烧结完成。
实施例4
Flashing法制备MoSi2-SiC复合材料的方法，步骤如下：
制备方法同实施例1，不同的是烧结温度为500℃。
实施例5
Flashing法制备MoSi2-SiC复合材料的方法，步骤如下：
制备方法同实施例1，不同的是烧结温度为1200℃。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (5)

1.一种Flashing法制备MoSi2-SiC复合材料的方法，其特征在于：以Mo和/或MoSi2、C、Si和/或SiO2、酚醛树脂为原料，搅拌均匀、压片固化，通过导电胶给试样施加电流电压进行Flashing法低温短时烧结，得到MoSi2-SiC复合材料。
2.根据权利要求1所述的Flashing法制备MoSi2-SiC复合材料的方法，其特征在于：所述原料中各物质的重量份数分别为：Mo和/或MoSi2 24-45份、Si和/或SiO2 1.5-11.2份、C 2-4.8份、酚醛树脂10-12份。
3.根据权利要求1-2任一项所述的Flashing法制备MoSi2-SiC复合材料的方法，其特征在于具体步骤如下：
（1）将Mo和/或MoSi2、Si和/或SiO2、C和酚醛树脂混合均匀，压制成片；
（2）在步骤（1）压片表面或边侧刷上导电胶，并粘结导线，于110℃固化；
（3）在非氧化性气氛中，升温至500-1200℃，并给导线施加电场；
（4）压片发生闪烧，获得MoSi2-SiC复合材料。
4.根据权利要求3所述的Flashing法制备MoSi2-SiC复合材料的方法，其特征在于：所述步骤（3）中电场电流为0.1-60A，步骤（4）闪烧的时间为0.1-10min。
5.根据权利要求3所述的Flashing法制备MoSi2-SiC复合材料的方法，其特征在于：所述导电胶以碳化硅、酚醛树脂和石墨导电胶为原料，按照质量比为（0.5-1）：（0.5-0.7）：（0.3-1），混合均匀研磨成膏状制得。
CN201911033183.6A 2019-10-28 2019-10-28 一种Flashing法制备MoSi2-SiC复合材料的方法 Pending CN110590374A (zh)

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Cited By (1)

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CN116547253A (zh) * 2020-10-20 2023-08-04 赛峰集团陶瓷 一种由短纤维增强的金属基体或陶瓷基体复合材料制成的空心部件的制造方法

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Application publication date: 20191220