CN109251033A - 一种微波合成Ti2AlC块体材料的方法 - Google Patents

一种微波合成Ti2AlC块体材料的方法 Download PDF

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CN109251033A
CN109251033A CN201811265345.4A CN201811265345A CN109251033A CN 109251033 A CN109251033 A CN 109251033A CN 201811265345 A CN201811265345 A CN 201811265345A CN 109251033 A CN109251033 A CN 109251033A
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王顺
王晖
王仁杰
关春龙
刘玉明
张莹莹
牛放
赵志伟
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Henan University of Technology
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Abstract

本发明涉及一种微波合成Ti2AlC块体材料的方法，其特征在于制备步骤如下：（1）按照2~x：1：1~x：x(0≤x≤1)的摩尔比称取钛粉、铝粉、石墨粉和碳化钛粉，进行球磨混合；（2）将混合均匀的原料置于钢制磨具中在一定压力下进行压制，形成圆柱坯体；（3）将压制后的坯体置于微波热压烧结装置中，对坯体施加一定的轴向压力，在氩气气氛保护下进行加热，经冷却后即可获得Ti2AlC块体材料。本发明合成过程简单、温度低、用时短、能耗少，并能够合成致密度好、纯度高、晶粒细小的Ti2AlC块体材料。

Description

一种微波合成Ti2AlC块体材料的方法
技术领域
本发明涉及一种三元MAX陶瓷材料的制备技术领域，具体涉及一种Ti2AlC块体材料的微波合成方法。
背景技术
Ti2AlC是一种三元层状过渡族金属碳化物，属于MAX陶瓷中的典型代表，它兼具陶瓷和金属两者的性能特点，具有低密度、低膨胀系数、高弹性模量、高强度、可加工、良好导电导热性能和优异抗热震抗氧化性能，因此，Ti2AlC可作为结构材料，广泛应用于航空航天、核工业、电子信息等领域。
目前Ti2AlC块体材料的合成方法主要有热压烧结、热等静压烧结、放电等离子烧结、高温自蔓延烧结以及燃烧合成。1997年，Barsoum等人[J. Mater. Syn. Process.,1997, 5:197~216]采用热压烧结方法，在1600℃、40MPa的条件下保温4h首次制备得到Ti2AlC块体材料。文献[Metall. Mater. Trans. A, 2000, 31A, 1857~1865]采用热等静压烧结方法，在1300℃、40MPa的条件下保温30h得到Ti2AlC块体材料。文献[J. Chin.Ceram. Soc., 2003, 31:991~993]采用放电等离子烧结方法，在1100℃、30MPa条件下保温8min得到高致密Ti2AlC块体材料。文献[J. Euro. Ceram. Soc., 2009, 29:187~194；Chem. Eng. J.,2016, 288:532~538]采用高温自蔓延烧结和燃烧合成的方法制备得到Ti2AlC块体材料，然而产物存在较多Ti3AlC2、TiC、AlTi等杂质相。综上所述，目前Ti2AlC块体材料的合成仍然存在温度高、合成时间长、纯度低、工艺复杂的问题，因此需要寻求一种低能耗、高效率的新工艺来制备高纯度Ti2AlC块体材料。本发明采用的微波烧结方法可以在低温度条件下短时间内合成高纯度的Ti2AlC块体材料。
发明内容
本发明基于目前Ti2AlC块体材料合成中存在的温度高、合成时间长、纯度低、工艺复杂的问题，提供了一种低温下短时间内合成高纯度的Ti2AlC块体材料的方法。
本发明可通过以下技术方案来实现高纯度Ti2AlC块体材料的合成：
微波热压烧结合成Ti2AlC块体材料的具体步骤包括：
步骤(1)：按照2~x：1：1~x：x (0≤x≤1)的摩尔比称取钛粉、铝粉、石墨粉和碳化钛粉，以无水乙醇为溶剂，采用行星式球磨机进行湿法球磨混合15~30h，随后在真空、50℃条件下干燥5h，得到混合均匀的原料；
步骤(2)：将混合均匀的原料置于钢制磨具中在10~30MPa压力下压制30~60s，形成圆柱坯体；
步骤(3)：将压制后的坯体置于微波热压烧结装置中，对坯体施加1500KN~3000KN的轴向压力，在氩气气氛保护下，加热至800~950℃，保温3~20min，经冷却后即可获得Ti2AlC块体材料。
与现有Ti2AlC块体材料的合成方法相比，本发明的有益效果如下：
（1）合成温度低，时间短，能耗少。本发明充分利用了微波烧结的加热特点，升温速率可达200℃/min，同时合成温度也大幅度下降。在850~950℃的条件下，仅需保温3~20min即可制备出Ti2AlC，大大较少能源消耗，提高生产效率。
（2）纯度高。本发明采用微波烧结加热的方式，由于Ti2AlC合成时间短，可有效的抑制铝粉的挥发，原料时可直接采用Ti2AlC的原子配比，合成Ti2AlC的纯度大于95%。
（3）混合均匀的原料在合成过程中属于整体加热且时间短，避免了微观组织不均匀问题，合成Ti2AlC块体材料的晶粒细小。
附图说明
图1为实施例1合成Ti2AlC的物相分析图。
具体实施方式
实施例1：按照1.5：1：0.5：0.5的摩尔比分别称取钛粉、铝粉、石墨粉和碳化钛粉作为原料，采用行星式球磨机，球磨介质为无水乙醇，球料比为2：1，将原料进行湿法球磨混15~30h，随后在50℃条件下真空干燥5h，得到混合均匀的原料。将混合均匀的原料置于钢制磨具中在10~30MPa压力下压制30~60s，形成圆柱坯体.将压制后的坯体置于微波热压烧结装置中，对坯体施加1500KN~3000KN的轴向压力，在氩气气氛保护下，加热至850℃，保温10min，即可获得Ti2AlC块体材料。
实施例2：按照1.8：1：0.8：0.2的摩尔比分别称取钛粉、铝粉、石墨粉和碳化钛粉作为原料，采用行星式球磨机，球磨介质为无水乙醇，球料比为2：1，将原料进行湿法球磨混15~30h，随后在50℃条件下真空干燥5h，得到混合均匀的原料。将混合均匀的原料置于钢制磨具中在10~30MPa压力下压制30~60s，形成圆柱坯体.将压制后的坯体置于微波热压烧结装置中，对坯体施加1500KN~3000KN的轴向压力，在氩气气氛保护下，加热至900℃，保温5min，即可获得Ti2AlC块体材料。
实施例3：按照1.1：1：0.1：0.9的摩尔比分别称取钛粉、铝粉、石墨粉和碳化钛粉作为原料，采用行星式球磨机，球磨介质为无水乙醇，球料比为2：1，将原料进行湿法球磨混15~30h，随后在50℃条件下真空干燥5h，得到混合均匀的原料。将混合均匀的原料置于钢制磨具中在10~30MPa压力下压制30~60s，形成圆柱坯体.将压制后的坯体置于微波热压烧结装置中，对坯体施加1500KN~3000KN的轴向压力，在氩气气氛保护下，加热至800℃，保温15min，即可获得Ti2AlC块体材料。

Claims (6)

1.一种微波合成Ti2AlC块体材料的方法，其特征是一种利用微波热压烧结工艺合成Ti2AlC块体材料的方法，具体步骤包括：
（1）按照2~x：1：1~x：x (0≤x≤1)的摩尔比称取钛粉、铝粉、石墨粉和碳化钛粉，进行球磨混合；
（2）将混合均匀的原料置于钢制磨具中在一定压力下进行压制，形成圆柱坯体；
（3）将压制后的坯体置于微波热压烧结装置中，对坯体施加1500KN~3000KN的轴向压力，在氩气气氛保护下，进行加热，经冷却后即可获得Ti2AlC块体材料。
2.根据权利要求1所述的一种微波合成Ti2AlC块体材料的方法，其特征在于：步骤（1）中钛粉、铝粉、石墨粉和碳化钛粉的摩尔比为2~x：1：1~x：x，其中x的取值范围为0≤x≤1。
3.根据权利要求1所述的一种微波合成Ti2AlC块体材料的方法，其特征在于：步骤（1）中球磨混合为为采用行星式球磨机进行湿法混合15~30h，溶剂为无水乙醇。
4.根据权利要求1所述的一种微波合成Ti2AlC块体材料的方法，其特征在于：步骤（2）中混合原料在钢制磨具中压制的压力为10~30MPa，压力保持30~60s。
5.根据权利要求1所述的一种微波合成Ti2AlC块体材料的方法，其特征在于：步骤（3）中对坯体施加的轴向压力为1500KN~3000KN。
6.根据权利要求1所述的一种微波合成Ti2AlC块体材料的方法，其特征在于：步骤（3）中微波加热温度为800~950℃，保温3~20min。
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CN110817875A (zh) * 2019-12-20 2020-02-21 武汉科技大学 一种Ti3AlC2粉体及其制备方法
CN110893466A (zh) * 2019-12-05 2020-03-20 沈阳工业大学 石墨烯-钛铝碳复合耐磨材料
CN111747749A (zh) * 2020-07-06 2020-10-09 南京理工大学 一种原位激光选区成形结合反应烧结制备Ti2AlC复杂件的方法
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110893466A (zh) * 2019-12-05 2020-03-20 沈阳工业大学 石墨烯-钛铝碳复合耐磨材料
CN110817875A (zh) * 2019-12-20 2020-02-21 武汉科技大学 一种Ti3AlC2粉体及其制备方法
CN111747749A (zh) * 2020-07-06 2020-10-09 南京理工大学 一种原位激光选区成形结合反应烧结制备Ti2AlC复杂件的方法
CN112719272A (zh) * 2020-12-18 2021-04-30 苏州科技大学 一种增材制造高熵合金齿轮的方法
CN115582547A (zh) * 2022-10-18 2023-01-10 郑州航空工业管理学院 一种Cu/C/SiC复合材料及其制备方法
CN115582547B (zh) * 2022-10-18 2024-02-23 郑州航空工业管理学院 一种Cu/C/SiC复合材料及其制备方法

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