CN107021759A - 一种新型陶瓷晶体Ti3B2N及其制备方法 - Google Patents
一种新型陶瓷晶体Ti3B2N及其制备方法 Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 36
- 239000000919 ceramic Substances 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000010936 titanium Substances 0.000 claims abstract description 46
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 9
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 8
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical group Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 claims abstract description 4
- 230000001681 protective effect Effects 0.000 claims abstract description 3
- 238000010792 warming Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 6
- 229910011208 Ti—N Inorganic materials 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 6
- 238000005245 sintering Methods 0.000 abstract description 2
- 238000001228 spectrum Methods 0.000 description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 5
- 229910052593 corundum Inorganic materials 0.000 description 5
- 239000010431 corundum Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 229910033181 TiB2 Inorganic materials 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 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
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002003 electron diffraction Methods 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- -1 transition metal nitride Chemical class 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [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
- 102100021164 Vasodilator-stimulated phosphoprotein Human genes 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000011195 cermet Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002737 metalloid compounds Chemical class 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 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 1
- 108010054220 vasodilator-stimulated phosphoprotein Proteins 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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Abstract
本发明属于陶瓷领域，尤其公开一种新型陶瓷晶体Ti3B2N及其制备方法。该晶体的分子式为Ti3B2N，晶体结构为正交晶系，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°。将钛粉和六方氮化硼粉末以1.5‑2.5:1的摩尔比在空气中混合、研磨、压片，然后在惰性保护气氛下以5‑10℃/min的速率升温至1100‑1200℃，保温3‑12h，自然冷却至室温，即制得目标产品。本发明通过高温烧结，成功制备出一种新的晶体结构Ti3B2N，提供了一种新型高硬度材料。
Description
技术领域
本发明属于陶瓷领域，尤其涉及一种新型陶瓷晶体Ti3B2N及其制备方法。
背景技术
氮化钛（TiN）与二硼化钛（TiB2）组成的多元复合材料广泛应用于各种耐高温部件及功能部件，如高温坩埚、引擎部件等，也是制作装甲防护材料的最好材料之一。TiB2是硼和钛最稳定的化合物，属六方晶系的准金属化合物，具有导电性和金属光泽，并具有高硬度和脆性特点。TiN晶体结构属面心立方点阵，具有典型的NaCl型结构，TiN抗热冲击性好，TiN熔点比大多数过度金属氮化物的熔点高，而密度却比大多数金属氮化物低，因此是一种很有特色的耐热材料。
Ti-B-N三元晶体，目前只有Ti4N3B2一种晶体化合物存在，其晶体结构与TiN相同，属立方晶系。Ti-B-N具有和TiN与TiB2类似的材料成份和价键结构，因此具有相近的物理化学性能。扩展并探索不同晶系的Ti-B-N三元晶体结构，在研究高硬度陶瓷材料领域具有很好的现实意义。
发明内容
针对现有技术存在的问题，本发明的目的在于提供一种新型陶瓷晶体Ti3B2N及其制备方法。
为实现上述目的，本发明采取的技术方案如下：
一种新型陶瓷晶体，该晶体的分子式为Ti3B2N，晶体结构为正交晶系，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°。
所述晶体结构中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。
制备方法：将钛粉和六方氮化硼粉末以1.5-2.5:1的摩尔比在空气中混合、研磨、压片，然后在惰性保护气氛下以5-10℃/min的速率升温至1100-1200℃，保温3-12h，自然冷却至室温，即制得目标产品。
本发明通过高温烧结，成功制备出一种新的晶体结构Ti3B2N，提供了一种新型高硬度材料。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。
附图说明
图1：Ti3B2N的理论XRD图谱。
图2：本发明实施例1制备的Ti3B2N的XRD图谱。
图3：本发明实施例1制备的Ti3B2N的透射电镜照片。
图4：本分明实施例1制备的Ti3B2N的电子衍射斑点。
图5：本发明实施例2制备的Ti3B2N的XRD图谱。
图6：本发明实施例3制备的Ti3B2N的XRD图谱。
图7：本发明实施例4制备的Ti3B2N的XRD图谱。
图8：本发明实施例5制备的Ti3B2N的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。
实施例1
将纯度大于99.9%的钛（Ti）粉和六方氮化硼（BN）粉末按摩尔比2:1在空气中混合研磨，粉压成型后，将样品用刚玉坩埚盛放，然后放入高温管式炉中氩气保护，以每分钟10℃的升温速率，将管式炉温度升至1100℃，保温6小时，停止加热后样品自然冷却至室温，即得产品。
采用晶体结构预测软件USPEX和VASP，可得Ti3B2N最稳定晶体结构。采用晶体XRD谱图模拟软件poudrix，可得Ti3B2N的理论XRD图谱，见图1。
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2、3、4；经X-射线衍射分析，确定的晶体结构参数为：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2对比可知：与（103）、（014）、（111）晶面对应的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和强度都一致，可以证明本实施例1制备出的产品即为Ti3B2N晶体；图3、图4反映的结果与XRD对应的结构一致，进一步证实了此结论。
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。
实施例2
将纯度大于99.9%的钛（Ti）粉和六方氮化硼（BN）粉末按摩尔比2:1混合，粉压成型后，将样品用刚玉坩埚盛放，然后放入高温管式炉中氩气保护，以每分钟10℃的升温速率，将管式炉温度升至1100℃，保温12小时，停止加热后样品自然冷却至室温，即得产品，其XRD图谱见图5，与Ti3B2N的理论XRD图谱比对，证实该产品即为Ti3B2N晶体。
实施例3
将纯度大于99.9%的钛（Ti）粉和六方氮化硼（BN）粉末按摩尔比2:1混合，粉压成型后，将样品用刚玉坩埚盛放，然后放入高温管式炉中氩气保护，以每分钟5℃的升温速率，将管式炉温度升至1200℃，保温3小时，停止加热后样品自然冷却至室温，即得产品，其XRD图谱见图6，与Ti3B2N的理论XRD图谱比对，证实该产品即为Ti3B2N晶体。
实施例4
将纯度大于99.9%的钛（Ti）粉和六方氮化硼（BN）粉末按摩尔比2:1混合，粉压成型后，将样品用刚玉坩埚盛放，然后放入高温管式炉中氩气保护，以每分钟10℃的升温速率，将管式炉温度升至1200℃，保温6小时，停止加热后样品自然冷却至室温，即得产品，其XRD图谱见图7，与Ti3B2N的理论XRD图谱比对，证实该产品即为Ti3B2N晶体。
实施例5
将纯度大于99.9%的钛（Ti）粉和六方氮化硼（BN）粉末按摩尔比2:1混合，粉压成型后，将样品用刚玉坩埚盛放，然后放入高温管式炉中氩气保护，以每分钟10℃的升温速率，将管式炉温度升至1200℃，保温12小时，停止加热后样品自然冷却至室温，即得产品，其XRD图谱见图8，与Ti3B2N的理论XRD图谱比对，证实该产品即为Ti3B2N晶体。
Claims (3)
1.一种新型陶瓷晶体，其特征在于：该晶体的分子式为Ti3B2N，晶体结构为正交晶系，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°。
2.如权利要求1所述的新型陶瓷晶体，其特征在于：所述晶体结构中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。
3.一种制备如权利要求1所述的新型陶瓷晶体的方法，其特征在于：将钛粉和六方氮化硼粉末以1.5-2.5:1的摩尔比在空气中混合、研磨、压片，然后在惰性保护气氛下以5-10℃/min的速率升温至1100-1200℃，保温3-12h，自然冷却至室温，即制得目标产品。
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Cited By (4)
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| CN107665274A (zh) * | 2017-09-08 | 2018-02-06 | 东南大学 | 一种设计低弹性模量钛合金的方法 |
| CN108862301A (zh) * | 2018-08-23 | 2018-11-23 | 河南理工大学 | 高纯度Ti3B2N材料的新型制备方法 |
| CN109160520A (zh) * | 2018-09-01 | 2019-01-08 | 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 |
| CN109607559A (zh) * | 2018-02-08 | 2019-04-12 | 河南理工大学 | 一种采用金属粉助熔剂合成三元层状化合物的方法 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107665274A (zh) * | 2017-09-08 | 2018-02-06 | 东南大学 | 一种设计低弹性模量钛合金的方法 |
| CN109607559A (zh) * | 2018-02-08 | 2019-04-12 | 河南理工大学 | 一种采用金属粉助熔剂合成三元层状化合物的方法 |
| CN109607559B (zh) * | 2018-02-08 | 2020-01-21 | 河南理工大学 | 一种采用金属粉助熔剂合成三元层状化合物的方法 |
| CN108862301A (zh) * | 2018-08-23 | 2018-11-23 | 河南理工大学 | 高纯度Ti3B2N材料的新型制备方法 |
| 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 |
| CN109160520A (zh) * | 2018-09-01 | 2019-01-08 | 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 |
| 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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