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CN113307627B - 一种Nb2SB陶瓷块体的制备方法 - Google Patents

一种Nb2SB陶瓷块体的制备方法 Download PDF

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CN113307627B
CN113307627B CN202110616062.5A CN202110616062A CN113307627B CN 113307627 B CN113307627 B CN 113307627B CN 202110616062 A CN202110616062 A CN 202110616062A CN 113307627 B CN113307627 B CN 113307627B
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胡春峰
覃燕如
萨尔瓦托·格拉索
冯庆国
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Abstract

本发明公开了一种Nb2SB陶瓷块体的制备方法，具体为：将Nb粉、S粉和B粉按照2:1～1.3:1的比例混合均匀；将混合粉末置于放电等离子烧结炉中，从室温升温到700℃，烧结环境为真空；从700℃升温1250～1650℃，并保温5～20min；待保温程序结束后，将温降温至900℃，然后随炉冷却至室温；去除表面渗碳层，得到高纯的块体Nb2SB。本发明制备工艺简单、耗时少、纯度高、成本低，环保节能，易于工业化推广。

Description

一种Nb2SB陶瓷块体的制备方法
技术领域
本发明属于新型陶瓷块体制备技术领域，尤其涉及一种Nb2SB陶瓷块体的制备方法。
背景技术
Nb2SB陶瓷是纳米层状结构的三元过渡金属硼化物，该硼化物是由过渡金属硼化物八面体层Nb-B与S元素层的交替堆叠所形成。2019年，有人通过微波反应炉合成了MAX相硼化物Nb2SB粉末，但合成Nb2SB陶瓷所需时间长，合成一次需要超过140小时的时间，且工艺复杂，不利于批量生产。目前还未合成出块状的Nb2SB陶瓷，未对其一些物理性能、力学性能等进行研究；此外，放电等离子烧结具有升温速度快、烧结时间短、节能环保等鲜明特点。
发明内容
针对上述问题，本发明提供一种Nb2SB陶瓷块体的制备方法。
本发明的一种Nb2SB陶瓷块体的制备方法，包括以下步骤：
步骤1：将Nb粉、S粉和B粉按照2:1～1.3:1的比例混合均匀。
步骤2：将步骤1得到的混合粉末置于放电等离子烧结炉中，从室温升温到700℃，升温速率为40～60℃/min，压力为20～40MPa，烧结环境为真空。
步骤3：从700℃升温到1250～1650℃，升温速率为5～20℃/min，压力为20～40MPa，并在1250～1650℃处保温5～20min。
步骤4：待保温程序结束后，将温度按50℃/min的降温速率降温至900℃，压力为20～ 40MPa，然后随炉冷却至室温。
步骤5：去除表面渗碳层，得到高纯的块体Nb2SB。
进一步的，步骤1中Nb粉、S粉和B粉的粒径大小分别为200～400目、4～6μm和4～6μm，经人工称量混合，在滚筒式混料机上混合均匀，混料5～20小时。
优选的，步骤1中Nb粉、S粉和B粉的粒径大小分别为300目、5μm和5μm，经人工称量混合，在滚筒式混料机上混合均匀，混料12小时。
进一步的，步骤1中使用NbS和NbB的混合粉末，或者使用NbS2和NbB的混合粉末，但需保持三种元素比例不变。
采用上述的制备方法制备而成的Nb2SB陶瓷块体，由过渡金属硼化物八面体层Nb-B与 S元素层的交替堆叠所形成。Nb2SB陶瓷块体由于具有特殊的三元层状结构，使得它具有较好的导电导热性能，以及具有较好的高温稳定性、高硬度等性能。
本发明的有益技术效果为：
(1)本发明采用Nb、S、B粉的混合粉末，通过高温反应后，可以得到高纯度的Nb2SB陶瓷块体，制备工艺简单、成本低，且节能环保。
(2)本发明制备高纯Nb2SB陶瓷块体，性能优异，高温稳定性好，强度硬度高，热导率较高，潜在应用为陶瓷增强相、热控制材料等方面。
附图说明
图1为制备的Nb2SB陶瓷块体的X射线衍射图谱。
图2为Nb2SB陶瓷块体腐蚀表面的SEM图。
图3为Nb2SB陶瓷的晶体结构图。
具体实施方式
下面结合附图和具体实施例对本发明做进一步详细说明。
实施例1
(1)将Nb粉、S粉和B粉按照摩尔配比为2:1:1混合，在滚筒式球磨机中混粉12小时。
(2)将步骤(1)得到的混合粉末置于放电等离子烧结炉中，从室温升温到700℃，升温速率为50℃/min，压力为20MPa，烧结环境为真空。
(3)从700℃升温到1350℃，升温速率为10℃/min，压力为30MPa，并在1350℃处保温10min。
(4)待保温程序结束后，将温度按50℃/min的降温速率降温至900℃，压力为30MPa，然后随炉冷却至室温。
(5)去除表面渗碳层，得到高纯的块体Nb2SB。测试得到Nb2SB陶瓷在24-1100℃范围内的热膨胀系数为7.1×10-6K-1。随着温度的升高，Nb2SB陶瓷的热扩散系数从25℃时的5.58mm2/s增加到800℃时的7.07mm2/s。
实施例2
(1)将Nb粉、S粉和B粉按照摩尔配比为2:1.1:1混合，在滚筒式球磨机中混粉12 小时。
(2)将步骤(1)得到的混合粉末置于放电等离子烧结炉中，从室温升温到700℃，升温速率为50℃/min，压力为20MPa，烧结环境为真空。
(3)从700℃升温到1350℃，升温速率为10℃/min，压力为30MPa，并在1350℃处保温10min。
(4)待保温程序结束后，将温度按50℃/min的降温速率降温至900℃，压力为30MPa，然后随炉冷却至室温。
(5)去除表面渗碳层，得到高纯的块体Nb2SB。Nb2SB陶瓷的弯曲强度和断裂韧性分别为249±17MPa和4.76±0.36MPa·m1/2；Nb2SB的压缩强度为1157±73MPa，硬度为11.89±0.37GPa。
实施例3
(1)将Nb粉、S粉和B粉按照摩尔配比为2:1.2:1混合，在滚筒式球磨机中混粉12 小时。
(2)将步骤(1)得到的混合粉末置于放电等离子烧结炉中，从室温升温到700℃，升温速率为50℃/min，压力为20MPa，烧结环境为真空。
(3)从700℃升温到1350℃，升温速率为10℃/min，压力为30MPa，并在1350℃处保温10min。
(4)待保温程序结束后，将温度按50℃/min的降温速率降温至900℃，压力为30MPa，然后随炉冷却至室温。
(5)去除表面渗碳层，得到高纯的块体Nb2SB。测试得到25℃时的热容和导热系数分别为0.36J·g-1·K-1和13.79W·m-1·K-1，在25℃时电导率为1.17×106Ω-1·m-1。
图1为所制备高纯度Nb2SB陶瓷的X射线衍射图，可以看出仅有少量的NbB杂质相存在。图2为Nb2SB陶瓷的显微结构图，可以明显观察到纳米层状结构。图3为Nb2SB陶瓷块体的晶体结构图。Nb2SB陶瓷是纳米层状结构的三元过渡金属硼化物，该硼化物是由过渡金属硼化物八面体层Nb-B与S元素层交替堆叠形成。
本发明将Nb粉、S粉和B粉按照不同的摩尔配比进行混合，在高温条件下反应处理后得到Nb2SB陶瓷块体，纯度可达到96％以上，潜在应用于陶瓷增强相、热控制材料等方面。

Claims (5)

1.一种Nb2SB陶瓷块体的制备方法，其特征在于，包括以下步骤：
步骤1：将Nb粉、S粉和B粉按照2:1～1.3:1的比例混合均匀；
步骤2：将步骤1得到的混合粉末置于放电等离子烧结炉中，从室温升温到700℃，升温速率为40～60℃/min，压力为20～40MPa，烧结环境为真空；
步骤3：从700℃升温到1250～1650℃，升温速率为5～20℃/min，压力为20～40MPa，并在1250～1650℃处保温5～20min；
步骤4：待保温程序结束后，将温度按50℃/min的降温速率降温至900℃，压力为20～40MPa，然后随炉冷却至室温；
步骤5：去除表面渗碳层，得到高纯的块体Nb2SB。
2.根据权利要求1所述的一种Nb2SB陶瓷块体的制备方法，其特征在于，所述步骤1中Nb粉、S粉和B粉的粒径大小分别为200～400目、4～6μm和4～6μm，经人工称量混合，在滚筒式混料机上混合均匀，混料5～20小时。
3.根据权利要求2所述的一种Nb2SB陶瓷块体的制备方法，其特征在于，所述步骤1中Nb粉、S粉和B粉的粒径大小分别为300目、5μm和5μm，经人工称量混合，在滚筒式混料机上混合均匀，混料12小时。
4.根据权利要求1所述的一种Nb2SB陶瓷块体的制备方法，其特征在于，所述步骤1中使用NbS和NbB的混合粉末，或者使用NbS2和NbB的混合粉末，但需保持三种元素比例不变。
5.一种Nb2SB陶瓷块体，采用如权利要求1-4任一所述的制备方法制备而成，其特征在于，由过渡金属硼化物八面体层Nb-B与S元素层的交替堆叠所形成。
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JPH06228712A (ja) * 1993-02-03 1994-08-16 Hitachi Metals Ltd 高温強度および被削性の優れたオーステナイト系耐熱鋳鋼およびそれからなる排気系部品
CN110105069A (zh) * 2019-04-25 2019-08-09 西南交通大学 一种新的max相层状化合物及其制备方法

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