CN107663090B - 一种合成高纯度Ti3B2N的方法 - Google Patents
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- 239000000843 powder Substances 0.000 claims abstract description 69
- 229910000048 titanium hydride Inorganic materials 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000005303 weighing Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 230000001681 protective effect Effects 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 4
- 238000007731 hot pressing Methods 0.000 abstract description 2
- 239000010936 titanium Substances 0.000 description 30
- 229910052582 BN Inorganic materials 0.000 description 21
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 10
- 239000013078 crystal Substances 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 229910052786 argon Inorganic materials 0.000 description 4
- 235000015895 biscuits Nutrition 0.000 description 4
- 238000002003 electron diffraction Methods 0.000 description 4
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 229910033181 TiB2 Inorganic materials 0.000 description 2
- 229910026551 ZrC Inorganic materials 0.000 description 2
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 229910011208 Ti—N Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- -1 titanium hydride Chemical compound 0.000 description 1
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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
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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