CN107663090B - 一种合成高纯度Ti3B2N的方法 - Google Patents

一种合成高纯度Ti3B2N的方法 Download PDF

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CN107663090B
CN107663090B CN201610603619.0A CN201610603619A CN107663090B CN 107663090 B CN107663090 B CN 107663090B CN 201610603619 A CN201610603619 A CN 201610603619A CN 107663090 B CN107663090 B CN 107663090B
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胡前库
陈进峰
吴庆华
周爱国
王李波
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Henan University of Technology
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Abstract

本发明属于结构材料领域，尤其公开一种合成高纯度Ti3B2N的方法。按TiH2粉、无定型B粉、六方BN粉三种原料的摩尔比TiH2：B：BN=3：(0.9~1.1)：(0.9~1.1)，称取TiH2粉、无定型B粉和六方BN粉；将称取的TiH2粉、无定型B粉、六方BN粉混匀，压片，然后在惰性保护气氛下以5~10℃/min的速率升温至1200~1300℃，保温3~6h；烧结完成后，在惰性保护气氛下，自然冷却至室温，得高纯Ti3B2N。本发明具有以下优点：1、工艺简单，无需热压；2、工艺设备简单、维护保养方便；3、本发明制备的Ti3B2N材料的纯度高达75%。

Description

一种合成高纯度Ti3B2N的方法
技术领域
本发明属于结构材料领域，尤其涉及一种合成高纯度Ti3B2N的方法。
背景技术
Ti3B2N是一种新型的三元层状化合物，它具有高模量（杨氏模量430.22 GPa，剪切模量181.06 GPa），高强度等。同时，Ti3B2N具有很低的密度（理论密度4.80 g/cm3）。作为一种最新发现的晶体具有较好的硬度和导电性，但其制备方法并不完善，申请人在早前申请的专利（申请号2016100610872）中，以Ti粉作为Ti源合成Ti3B2N的方法，产品纯度并不高，杂质TiN、TiB2含量较高。因此，制备高纯度Ti3B2N在研究高硬度、导电陶瓷材料领域具有很好的现实意义。
发明内容
为解决新型材料Ti3B2N合成纯度低的问题，本发明的目的在于提供一种合成高纯度Ti3B2N的方法，该方法工艺简单，适合工业规模化生产。
为实现上述目的，本发明采取的技术方案如下：
一种合成高纯度Ti3B2N的方法：按TiH2（氢化钛）粉、无定型B（硼）粉、六方BN（氮化硼）粉三种原料的摩尔比TiH2：B：BN=3：(0.9~1.1)：(0.9~1.1)，称取TiH2粉、无定型B粉和六方BN粉；将称取的TiH2粉、无定型B粉、六方BN粉混匀，压片，然后在惰性保护气氛下以5~10℃/min的速率升温至1200~1300℃，保温3~6h；烧结完成后，在惰性保护气氛下，自然冷却至室温，得高纯（75%以上）Ti3B2N。
为使物料混合更加均匀，在TiH2粉、无定型B粉、六方BN粉的混匀过程中优选添加无水乙醇作为分散剂，该混匀过程具体为：将称取的TiH2粉、无定型B粉、六方BN粉加入无水乙醇混合5~30h后，自然晾干。
较好地，无水乙醇的加入量保证其液面没过物料，优选没过物料1~5mm。
本发明的TiH2粉、无定型B粉和六方BN粉纯度为99.9%以上。
本发明具有以下优点：1、工艺简单，无需热压；2、工艺设备简单、维护保养方便；3、本发明制备的Ti3B2N材料的纯度高达75%。
附图说明
图1：实施例1制备的Ti3B2N的XRD图谱。
图2：实施例1制备的Ti3B2N的透射电镜照片。
图3：实施例1制备的Ti3B2N的电子衍射斑点。
图4：对照例1制备的Ti3B2N的XRD图谱。
图5：对照例1制备的Ti3B2N的透射电镜照片。
图6：对照例1制备的Ti3B2N的电子衍射斑点。
图7：Ti3B2N晶体结构模型。
图8：Ti3B2N的理论XRD图谱。
具体实施方式
下面结合实施例对本发明的技术方案作进一步详细说明，但本发明的保护范围不限于下述的实施例。
以下实施例中Ti粉、TiH2粉、无定型B粉和六方BN粉均为市售产品，纯度为99.9%以上。
实施例1
一种合成高纯度Ti3B2N的方法：按TiH2粉、无定型B粉、六方BN粉三种原料的摩尔比TiH2：B：BN=3：1.0：1.0，称取TiH2粉、无定型B粉和六方BN粉；将称取的TiH2粉、无定型B粉、六方BN粉加入无水乙醇，使无水乙醇的液面没过物料3 mm，混合18h后，自然晾干；用压片机5MPa压力下，冷压成素坯块体；将素坯块体置于管式炉，氩气保护气氛中进行烧结；烧结步骤为：以10℃/min的升温速率升至1300℃，保温6h；烧结完成后，在氩气保护气氛下，自然冷却至室温，得产品Ti3B2N。
本实施例1制备的产品的XRD图谱、透射电镜照片、电子衍射斑点分别见图1、2、3。
对照例1
按Ti粉和六方BN粉两种原料的摩尔比Ti：BN=2：1，称取Ti粉和六方BN粉；将称取的Ti粉和六方BN粉加入无水乙醇，使无水乙醇的液面没过物料3 mm，混合18h后，自然晾干；用压片机5 MPa压力下，冷压成素坯块体；将素坯块体置于管式炉，氩气保护气氛中进行烧结；烧结步骤为：以10℃/min的升温速率升至1100℃，保温6h；烧结完成后，在氩气保护气氛下，自然冷却至室温，得产品Ti3B2N。
本对照例1制备的产品的XRD图谱、透射电镜照片、电子衍射斑点分别见图4、5、6。
实施例2
本实施例与实施例1的不同之处在于：以5℃/min升温速率升至1300℃，保温3h；其他同实施例1。
实施例3
本实施例与实施例1的不同之处在于：TiH2粉、无定型B粉、六方BN粉三种原料的摩尔比为TiH2：B：BN=3：0.9：0.9；加入无水乙醇，使无水乙醇的液面没过物料1 mm，混合15h；以5℃/min升温速率升至1200℃，保温3h；其他同实施例1。
实施例4
本实施例与实施例1的不同之处在于：TiH2粉、无定型B粉、六方BN粉三种原料的摩尔比为TiH2：B：BN=3：1.1：1.1；加入无水乙醇，使无水乙醇的液面没过物料5 mm，加入无水乙醇混合20h；以10℃/min升温速率升至1200℃，保温6h；其他同实施例1。
实施例1、对照例1两种不同合成方法结果对照分析：
1、产品为同一物质
采用晶体结构预测软件USPEX和VASP，可得Ti3B2N最稳定晶体结构，其模型见图7。采用晶体XRD谱图模拟软件poudrix，可得Ti3B2N的理论XRD图谱，见图8。
实施例1以及对照例1相对应的X-射线衍射分析，可确定两种合成方法制备的产品的晶体结构参数均为：正交晶系，空间点群为Cmmm，晶格常数为a = 3.032 (4) Å，b =3.189 (3) Å，c = 12.897 (4) Å，α = β = γ = 90°；Ti-N键长分别为2.198 (3) Å、1.999(3) Å，Ti-B键长为2.317 (3) Å，B-B键长为1.805 (3) Å。
图1与图8对比、图4与图8对比，可知：与图8（103）、（014）、（111）晶面对应图1/图4中的36.3°、39.8°、41.7°位置的三强峰以及其他强度较弱衍射峰从位置上一致，可以证明实施例1以及对照例1制备出的产品的主相均为Ti3B2N；图2、图3(或图5、图6)反映的结果与XRD对应的结构一致，进一步证实了此结论；并且经过分析，图3为Ti3NB2 [010]方向的衍射斑点。
2、产品纯度不同
图1与图8对比、图4与图8对比，可知：虽然与图8（103）、（014）、（111）晶面对应图1/图4中的36.3°、39.8°、41.7°位置的三强峰以及其他强度较弱衍射峰从位置上一致，但是各峰强度明显存在差异，根据图1与图8、图4与图8中Ti3B2N特征峰的强度比值，可以计算出实施例1产品的Ti3B2N纯度约为75%，而对照例产品的Ti3B2N纯度约为30%；并且实施例1相比对照例1以Ti粉做为原料的烧结产品，杂质TiB2、TiN的含量明显减少，衍射峰尖锐，说明晶体发育良好。
最后，根据Xingqiu Chen等人提出的硬度计算模型(文献：Intermetallics,2011, 19, P1275-1281.)，本发明所述Ti3B2N晶体的维氏硬度约28GPa。Ti3B2N硬度与碳化钛（TiC）、碳化锆（ZrC）相当，比氮化钛（TiN）更硬，可应用于钛合金、钢、硬质合金和铝结构的涂层以改善表面性质，例如工具模表面镀层的应用，可以提高工具模的加工效率和使用时间。Ti3B2N也可应用于制造金属陶瓷和硬质合金。

Claims (4)

1.一种合成高纯度Ti3B2N的方法，其特征在于：按TiH2粉、无定型B粉、六方BN粉三种原料的摩尔比TiH2：B：BN=3：(0.9~1.1)：(0.9~1.1)，称取TiH2粉、无定型B粉和六方BN粉；将称取的TiH2粉、无定型B粉、六方BN粉混匀，压片，然后在惰性保护气氛下以5~10℃/min的速率升温至1200~1300℃，保温3~6h；烧结完成后，在惰性保护气氛下，自然冷却至室温，得高纯Ti3B2N；其中，TiH2粉、无定型B粉和六方BN粉纯度为99.9%以上。
2.如权利要求1所述的合成高纯度Ti3B2N的方法，其特征在于，所述混匀过程为：将称取的TiH2粉、无定型B粉、六方BN粉加入无水乙醇混合5~30h后，自然晾干。
3.如权利要求2所述的合成高纯度Ti3B2N的方法，其特征在于：无水乙醇的加入量保证其液面没过物料。
4.如权利要求3所述的合成高纯度Ti3B2N的方法，其特征在于：无水乙醇的加入量保证其液面没过物料1~5mm。
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CN108862301B (zh) * 2018-08-23 2020-04-10 河南理工大学 高纯度Ti3B2N材料的制备方法
CN109160520B (zh) * 2018-09-01 2021-04-27 河南理工大学 一种球磨处理原料合成高纯度Ti3B2N材料的方法
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