CN110054496B - 一种钛铝硅锡碳三相层间固溶体粉料及其制备方法 - Google Patents
一种钛铝硅锡碳三相层间固溶体粉料及其制备方法 Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 74
- 239000006104 solid solution Substances 0.000 title claims abstract description 34
- -1 Titanium-aluminum-silicon-tin-carbon Chemical compound 0.000 title claims abstract description 28
- 239000011229 interlayer Substances 0.000 title claims description 11
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000010936 titanium Substances 0.000 claims abstract description 27
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000498 ball milling Methods 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 238000003825 pressing Methods 0.000 claims abstract description 12
- 229910052786 argon Inorganic materials 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 229910021035 SixSny Inorganic materials 0.000 claims abstract description 7
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims abstract description 6
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 6
- 229910009819 Ti3C2 Inorganic materials 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims abstract description 3
- 239000013078 crystal Substances 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 229910002804 graphite Inorganic materials 0.000 claims description 18
- 239000010439 graphite Substances 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 12
- 239000011863 silicon-based powder Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 6
- 239000010410 layer Substances 0.000 claims description 5
- 229910009817 Ti3SiC2 Inorganic materials 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 239000011135 tin Substances 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract description 3
- 238000005507 spraying Methods 0.000 abstract description 3
- 229910052710 silicon Inorganic materials 0.000 abstract description 2
- 229910052718 tin Inorganic materials 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 229910006686 Si—Sn—C Inorganic materials 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 description 1
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种钛铝硅锡碳层间固溶体粉料及其制备方法。该粉料中，Ti3Al1.2‑x‑ ySixSnyC2的体积含量>95％，表达式中：0.1≤x≤1，0.1≤y≤1，0.2≤x+y<1.2；Ti3Al1.2‑x‑ ySixSnyC2具有与Ti3AlC2相同的层状晶体结构，固溶的Si、Sn原子和Al原子共存于两层Ti3C2层之间。其制备方法：原料粉按摩尔比Ti：Al：Si：Sn：TiC＝1.0：(0.1～1.2)：(0.1～1)：(0.1～1)：(1.8～2.0)的比例配料；球磨混料后，将干燥的混合原料压制成块，置于高温炉中，氩气保护，在1350～1500℃下煅烧，保温5～15min，冷却后得到蓬松的块状反应产物，将其粉碎、球磨即得到本发明的钛铝硅锡碳层间固溶体粉料。该粉料可用于制备各种用途的复合材料或冷(热)喷涂层材料领域或具有摩擦调节作用的钛铝硅锡碳块体材料。
Description
技术领域
本发明涉及一种钛铝硅锡碳三相层间固溶体粉料及其制备方法，属于新型陶瓷材料领域。
背景技术
MAX相陶瓷材料是一种新型的三元层状化合物，其具有陶瓷材料所特有的抗热震性、耐化学腐蚀等性能，又具有高导电性、导热性、可加工性等特点，同时由于其层状结构也具有像石墨一样的自润滑性；这类新型材料在防腐蚀材料、耐磨材料、高温结构部件、电极电刷材料等方面有广阔的应用前景。
固溶强化是工业上常用的一种重要强化方法，适当控制溶质含量，可明显提高材料的强度、硬度，同时还能保持一定的塑性和韧性。艾明星等人发现，制备Ti3AlC2时，原料中添加一定量的Sn进行固溶可以抑制TiC,TixAly等中间产物的生成，有效提高了Ti3AlC2合成产物的纯度(参考文献Ai Mingxing,et al,J.Am.Ceram.Soc.,2006,89[3]:1114)；黄振莺等人采用二次热压的方法，制备了Ti3Al(Sn)C2固溶体，当分别添加0.2Sn和0.4Sn时，材料的弯曲强度增至560MPa和620MPa，比Ti3AlC2的弯曲强度值提高了51％和67％。并且Sn的加入使得该材料表现出良好的摩擦学特性，当与低碳钢盘干滑动摩擦时，Sn含量的变化时摩擦系数具有可调控性，而磨损率始终保持在较低范围内(参考文献Z-Y Huang,et al,CreamInt.,2015,41[3]:3701)。由此可知A位固溶元素的添加使得MAX材料的力学性能、氧化性能、摩擦性能等特性得到改善和优化。但是迄今为止，还没有对2种以上的A位元素固溶体的制备进行相关报道。这主要是由于2种以上A元素之间的相容性、分子固溶度等的相关机理及对应的制备方法与2种A位元素固溶有很大的差别，技术难度远远提高。
本发明采用3种A位原子(Al、Si和Sn)加入，制备一种钛铝硅锡碳三相层间固溶体粉体材料，这类粉体材料可应用于冷(热)喷涂层材料领域，也可作为增强相应用于复合材料领域，还可作为二次热压方法制备钛铝硅锡碳块体的原料粉。3种及以上A位原子的添加，使化合物层间的化学关系发生改变，因而固溶体的某些特性，如抗高温氧化性，摩擦学特性可比钛硅碳化物和钛铝碳化物或者其含有2种元素固溶的固溶体(如钛铝锡碳、钛硅铝碳)得到显著增强，从而可以扩大这种材料的应用领域。
发明内容
本发明的目的在于提供一种钛铝硅锡碳三相层间固溶体粉料及其制备方法。
本发明的钛铝硅锡碳三相层间固溶体粉料，其成分和显微结构如下：
(1)Ti3Al1.2-x-ySixSnyC2的体积含量>95％，表达式中：0.1≤x≤1，0.1≤y≤1，0.2≤x+y<1.2；
(2)杂质相的体积含量<5％；
(3)Ti3Al1.2-x-ySixSnyC2具有与Ti3SiC2或Ti3AlC2相同的层状晶体结构，Al原子、Si原子和Sn原子共存于两层Ti3C2层之间。
本发明的一种钛铝硅锡碳三相层间固溶体粉料的制备方法，包括以下各步骤：
(1)配料：将Ti粉、Al粉、Si粉、Sn粉和TiC粉按摩尔比Ti：Al：Si：Sn：TiC＝1.0：(0.1～1.2)：(0.1～1)：(0.1～1)：(1.8～2.0)的比例配料；
(2)混料：每100克上述配料中加入200～250克的玛瑙球，球磨5～10小时；
(3)过筛：用10～20目的筛子将上述的玛瑙球筛出，得到混合均匀的原料；
(4)预压：将上述筛出后的原料压制成任何形状的坯体；
(5)装模：将上述保持完整的坯体放置入石墨模具中；
(6)煅烧：将上述放入石墨模具中的坯体置于高温烧结炉中，在氩气保护下，按10～40℃/min的升温速率，将炉温升至1350～1500℃，保温5～15min后冷却，得到蓬松的块状反应产物；
(7)将反应产物粉碎、球磨，即得到如权利要求1所述的钛铝硅锡碳三相层间固溶体粉料。
用本发明的方法制备钛铝硅锡碳三相层间固溶体粉料，方法简单、可靠，易于工业化生产；所制备的钛铝硅锡碳三相层间固溶体粉料，不含或只含少量的TiC等杂相，可用其为原料制备各种用途的复合材料领域，也可作用于冷(热)喷涂层材料领域，还可作为二次热压方法制备单相的钛铝硅锡碳三相层间固溶体块体原料。
附图说明
图1是Ti3Al1.2-x-ySixSnyC2的x值为0.4、0.2，y值为0.1和0.2时的钛铝硅锡碳固溶体粉料的X-射线衍射谱；图2是钛铝硅锡碳固溶体粉料的SEM微观结构形貌，图2(a)(b)为x为0.4、y为0.1时的钛铝硅锡碳固溶体粉料的微观结构形貌，图2(c)(d)为x为0.2、y为0.2时的钛铝硅锡碳固溶体粉料的微观结构形貌。
具体实施方式
实施例1
称取Ti粉4.77克、Al粉1.88克、Si粉1.12克、Sn粉1.18克、TiC粉11.04克，混合后加入40克玛瑙球，球磨混料5小时，过10目筛后压制成块状坯体，放入石墨模具后移入高温炉中，在氩气保护下，以10℃/min的速率升温至1450℃，保温5min后冷却，将反应生成的疏松块状产物取出，粉碎、球磨，即得到主相为Ti3Al0.7Si0.4Sn0.1C2的钛铝硅锡碳固溶体粉料。
实施例2
称取Ti粉4.57克、Al粉2.06克、Si粉0.53克、Sn粉2.27克、TiC粉10.56克，混合后加入50克玛瑙球，球磨混料10小时，过10目筛后压制成块状坯体，放入石墨模具后移入高温炉中，在氩气保护下，以40℃/min的速率升温至1450℃，保温10min后冷却，将反应生成的疏松块状产物取出，粉碎、球磨，即得到主相为Ti3Al0.8Si0.2Sn0.2C2的钛铝硅锡碳固溶体粉料。
实施例3
称取Ti粉4.56克、Al粉1.54克、Si粉1.07克、Sn粉2.26克、TiC粉10.55克，混合后加入40克玛瑙球，球磨混料8小时，过10目筛后压制成块状坯体，放入石墨模具后移入高温炉中，在氩气保护下，以30℃/min的速率升温至1450℃，保温15min后冷却，将反应生成的疏松块状产物取出，粉碎、球磨，即得到主相为Ti3Al0.6Si0.4Sn0.2C2的钛铝硅锡碳固溶体粉料。
实施例4
称取Ti粉4.20克、Al粉0.95克、Si粉0.98克、Sn粉4.16克、TiC粉9.71克，混合后加入40克玛瑙球，球磨混料5小时，过20目筛后压制成块状坯体，放入石墨模具后移入高温炉中，在氩气保护下，以20℃/min的速率升温至1400℃，保温15min后冷却，将反应生成的疏松块状产物取出，粉碎、球磨，即得到主相为Ti3Al0.4Si0.4Sn0.4C2的钛铝硅锡碳固溶体粉料。
实施例5
称取Ti粉3.88克、Al粉0.44克、Si粉0.91克、Sn粉5.78克、TiC粉8.99克，混合后加入40克玛瑙球，球磨混料5小时，过10目筛后压制成块状坯体，放入石墨模具后移入高温炉中，在氩气保护下，以20℃/min的速率升温至1350℃，保温15min后冷却，将反应生成的疏松块状产物取出，粉碎、球磨，即得到主相为Ti3Al0.2Si0.4Sn0.6C2的钛铝硅锡碳固溶体粉料。
实施例6
称取Ti粉3.62克、Al粉0.41克、Si粉0.42克、Sn粉7.18克、TiC粉8.37克，混合后加入40克玛瑙球，球磨混料10小时，过10目筛后压制成块状坯体，放入石墨模具后移入高温炉中，在氩气保护下，以20℃/min的速率升温至1350℃，保温10min后冷却，将反应生成的疏松块状产物取出，粉碎、球磨，即得到主相为Ti3Al0.2Si0.2Sn0.8C2的钛铝硅锡碳固溶体粉料。
实施例7
称取Ti粉4.19克、Al粉0.47克、Si粉1.48克、Sn粉4.16克、TiC粉9.7克，混合后加入40克玛瑙球，球磨混料5小时，过10目筛后压制成块状坯体，放入石墨模具后移入高温炉中，在氩气保护下，以10℃/min的速率升温至1450℃，保温15min后冷却，将反应生成的疏松块状产物取出，粉碎、球磨，即得到主相为Ti3Al0.2Si0.6Sn0.4C2的钛铝硅锡碳固溶体粉料。
实施例8
称取Ti粉4.55克、Al粉0.51克、Si粉2.14克、Sn粉2.26克、TiC粉10.54克，混合后加入40克玛瑙球，球磨混料5小时，过10目筛后压制成块状坯体，放入石墨模具后移入高温炉中，在氩气保护下，以10℃/min的速率升温至1500℃，保温5min后冷却，将反应生成的疏松块状产物取出，粉碎、球磨，即得到主相为Ti3Al0.2Si0.8Sn0.2C2的钛铝硅锡碳固溶体粉料。
Claims (2)
1.一种钛铝硅锡碳三相层间固溶体粉料，其特征在于：其成分和显微结构如下：
(1)Ti3Al1.2-x-ySixSnyC2的体积含量>95％，表达式中：0.1≤x≤1，0.1≤y≤1，0.2≤x+y<1.2；
(2)杂质相的体积含量<5％；
(3)Ti3Al1.2-x-ySixSnyC2具有与Ti3SiC2或Ti3AlC2相同的层状晶体结构，Al原子、Si原子和Sn原子共存于两层Ti3C2层之间。
2.一种如权利要求1所述的钛铝硅锡碳三相层间固溶体粉料的制备方法，其特征在于：该方法包括以下各步骤：
(1)配料：将Ti粉、Al粉、Si粉、Sn粉和TiC粉按摩尔比Ti：Al：Si：Sn：TiC＝1.0：
(0.1～1.2)：(0.1～1)：(0.1～1)：(1.8～2.0)的比例配料；
(2)混料：每100克上述配料中加入200～250克的玛瑙球，球磨5～10小时；
(3)过筛：用10～20目的筛子将上述的玛瑙球筛出，得到混合均匀的原料；
(4)预压：将上述筛出后的原料压制成任何形状的坯体；
(5)装模：将上述保持完整的坯体放置入石墨模具中；
(6)煅烧：将上述放入石墨模具中的坯体置于高温烧结炉中，在氩气保护下，按10～40℃/min的升温速率，将炉温升至1350～1500℃，保温5～15min后冷却，得到蓬松的块状反应产物；
(7)将反应产物粉碎、球磨，即得到如权利要求1所述的钛铝硅锡碳三相层间固溶体粉料。
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| CN101050116A (zh) * | 2007-03-20 | 2007-10-10 | 北京交通大学 | 一种钛硅铝碳层间固溶体粉料及其制备方法 |
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