CN1538944A - 一种生产含金属的单一相组合物的方法 - Google Patents
一种生产含金属的单一相组合物的方法 Download PDFInfo
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- 239000000203 mixture Substances 0.000 title claims abstract description 26
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 13
- 239000002184 metal Substances 0.000 title claims abstract description 13
- 239000010936 titanium Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 21
- 150000001875 compounds Chemical class 0.000 claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 9
- 229910052729 chemical element Inorganic materials 0.000 claims abstract description 8
- 239000011651 chromium Substances 0.000 claims abstract description 8
- 239000010955 niobium Substances 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052755 nonmetal Inorganic materials 0.000 claims abstract description 7
- 239000010703 silicon Substances 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 4
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 4
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 4
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 4
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 239000004411 aluminium Substances 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000000843 powder Substances 0.000 abstract description 3
- 229910009817 Ti3SiC2 Inorganic materials 0.000 abstract 1
- 238000010494 dissociation reaction Methods 0.000 abstract 1
- 230000005593 dissociations Effects 0.000 abstract 1
- 150000002739 metals Chemical class 0.000 abstract 1
- 150000002843 nonmetals Chemical class 0.000 abstract 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 21
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 238000001816 cooling Methods 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- 238000007669 thermal treatment Methods 0.000 description 4
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 description 3
- 238000010894 electron beam technology Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 206010024769 Local reaction Diseases 0.000 description 1
- 229910008484 TiSi Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
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- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910021344 molybdenum silicide Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001902 propagating effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
一种生产单一相组合物Mn+1AzXn的方法，其中n的范围为0.8～3.2，z的范围为0.8～1.2，M是选自金属Ti(钛)、Sc(钪)、V(钒)、Cr(铬)、Zr(锆)、Nb(铌)和Ta(钽)的至少一种金属，X是非金属C(碳)和N(氮)其中至少之一，且A是化学元素Si(硅)、Al(铝)和Sn(锡)的至少一种或者是所述元素的化合物，使得最后期望的化合物将包含组分Mn+1AzXn，其中该方法还包括形成所述金属、非金属和化学元素或所述元素的化合物的粉末混合物，并将这种粉末混合物在惰性气氛下引燃以防止离解升级，该组分通过这种方式反应。该方法的特征在于保持反应温度等于或高于引起组分反应的温度，但低于单一相组合物离解的温度。本发明主要涉及单一相材料Ti3SiC2的生产。
Description
本发明涉及一种生产含金属的单一相组合物的方法。本发明主要涉及钛硅碳化物和属于同一族的复合物的生产。
无氧燃烧合成，也称为SHS(自蔓延高温合成)，通常用于生产金属间化合物产品和陶瓷组合物。
在SHS技术中，通过强热源介质局部引燃两种或更多种材料的混合物。例如，这种强热源可以由一个加热线圈或其他加热元件如激光束或电子束组成。这种强放热反应的结果是局部燃烧导致局部反应。这引起过剩能量的释放，并引燃临近部分的材料并最终使全部材料引燃。这种链式反应非常迅速，而且当反应加以控制时，提供了一种大量生产金属间化合物和陶瓷的高效率方法。该系统能达到的最高温度是绝热温度。
自20世纪80年代中期以来，已有多种生产Ti3SiC2的尝试。Pampuch等人(R.Pampuch等，“Ti3SiC2的固体燃烧合成”，J.EUR.CERAM.SOC.，5，283-87(1999))和其他人在惰性气氛下引燃Ti、Si和C的粉末混合物，得到了Ti3SiC2和约10-30％的其他相，如TiC、TiSi2和SiC。
Goesmann等人(F.Goesmann等，“Ti3SiC2的电子束引燃固态反应制备”，J.Amer.Ceram.Soc.81，11，3025-28(1998))认为由于金属硅在2000℃以上的极高反应温度引起的排气作用，SHS将不能产生主要由Ti3SiC2组成的单一相。Goesmann从Ti和SiC的混合物开始，该混合物的化学组成为Ti3SiC2+12.5％(重量)的过量硅。他利用电子束引燃该混合物。该混合物的处理分为三个阶段，即800℃热处理，900℃引燃，接着在1600℃热处理实现过量硅的排气。这种方法使得样品中的第二相少于8％。
在我们1999年12月的美国专利申请09/469,893中，我们说明了由于形成了与高温引起的硅蒸发有根本差别的气态SiO，气氛中的氧在生产过程以及随后的烧结过程中对Ti3SiC2热稳定性有影响。
因此，以前所述的方法难以制备不含其他反应产物的钛硅碳化物。
上面已经提到本发明也涉及同族中的组合物。该族可由作为单一相的组合物M3SiZ2来指定，其中M是至少一种金属，Z是化学元素C(碳)和N(氮)中的至少一种。
本发明涉及有关钛硅碳化物生产中的高成本问题。
本发明因此涉及生产单一相组合物Mn+1AzXn的方法，其中n的范围为0.8～3.2，z的范围为0.8～1.2，M是选自金属Ti(钛)、Sc(钪)、V(钒)、Cr(铬)、Zr(锆)、Nb(铌)和Ta(钽)的至少一种金属，X是非金属C(碳)和N(氮)的至少一种，且A是化学元素Si(硅)、Al(铝)和Sn(锡)的至少一种或是所述几种元素的化合物，以便获得最后期望的化合物组分Mn+1AzXn，其中该方法还包含由所述金属、非金属和最后提到的化学元素或所述元素的化合物形成粉末混合物，并将所述粉末混合物在惰性气氛下引燃以免离解升级，所述加入的组分通过这种方式反应，并且其中该方法的特征在于使反应物的温度保持在等于或高于引起组分反应的温度，但低于单一相组合物离解的温度。
下面将部分地参照三个实施例更详细地描述本发明。
本方法涉及单一相(或单相)组合物Mn+1AzXn的生产，其中n的范围为0.8～3.2，z的范围为0.8～1.2，M是选自金属Ti(钛)、Sc(钪)、V(钒)、Cr(铬)、Zr(锆)、Nb(铌)和Ta(钽)的至少一种金属，X是非金属C(碳)和N(氮)的至少一种，且A是化学元素Si(硅)、Al(铝)和Sn(锡)的至少一种或是所述元素的化合物，使得最后期望的化合物将包含组分Mn+1AzXn。该方法包括形成所述金属、非金属和最后提到的化学元素或化合物的粉末混合物，并将这种粉末混合物引燃以使其在惰性气氛下反应。该惰性气氛包括一种气氛，该气氛具有足够低氧气分压以防止离解升级。
按照本发明，反应温度应保持在等于或高于引起组分反应的水平，但低于单一相组合物发生离解的温度。
因此，本发明的一个必要特征在于实现反应期间温度的保持，但仍然高于一个特定的水平。
这是生产单一相组合物Ti3SiC2的优选方法。
按照一个高度优选的实施方案，通过加入预先反应的Ti3SiC2来控制温度，该材料起到热潭(heat sink)的作用。
优选含量最高到约25％(重量)的Ti3SiC2用作热潭。
选择性地，可以通过其他方法控制反应过程中的温度，例如通过材料的受控冷却。
下面是一些实施例。
实施例1
将Ti、SiC和石墨粉末混合以制成Ti3SiC2的化学计量混合物。将该混合物与12％(重量)预先反应的Ti3SiC2混合。
将该混合物置于反应容器内，其中通有流速为0.5l/min的氩气。粉末料层厚度约20cm。
通过置于反应容器底部的硅化钼元件引燃料层，使料层组分反应。
冷却后，将粉末从反应容器中移出。料层可容易的碾碎。
用X射线衍射的方法对从料层中取出的样品进行分析。
料层经过确定含有约2-4％(重量)的TiC。
实施例2
将25％(重量)预先反应的Ti3SiC2加入混合物，除此之外与实施例1相同。
引燃并冷却后，发现料层中含有15-20％(重量)的TiC。
实施例2表明，除其他因素之外，预先反应材料的过度稀释作用导致不完全反应，为获得单一相材料，料层需要在1400℃热处理8小时。
实施例3
采用与实施2相同的方法，将Ti、Si和石墨粉与25％(重量)的预先反应Ti3SiC2混合并加入到混合物中。
引燃并冷却后，发现料层含有25-30％(重量)的TiC。
将料层在1400℃热处理8小时之后，发现其中含有少于2％(重量)的TiC。
该实施例表明Si可用来代替SiC。
虽然以上通过其多个实施方案描述了本发明，在本发明的范围内，当然还可以通过不同于上述的方法将温度控制在所述范围内。
因此不应认为本发明仅局限于上述作为范例的实施方案，因为在所附权利要求的范围内可做出变化。
Claims (6)
1.一种生产单一相组合物Mn+1AzXn的方法，其中n的范围为0.8～3.2，z的范围为0.8～1.2，M是选自金属Ti(钛)、Sc(钪)、V(钒)、Cr(铬)、Zr(锆)、Nb(铌)和Ta(钽)的至少一种金属，X是非金属C(碳)和N(氮)的至少一种，且A是化学元素Si(硅)、Al(铝)和Sn(锡)的至少一种或者是所述元素的化合物，使得最后期望的化合物将包含组分Mn+1AzXn，其中该方法还包括由所述金属、非金属和所述化学元素或所述元素的化合物形成粉末混合物，并将所述粉末混合物在惰性气氛下引燃以防止离解升级，该组分通过这种方式反应，且该方法的特征在于保持反应温度等于或高于引起组分反应的温度但又低于单一相组合物离解的温度。
2.按照权利要求1的方法，其特征在于n＝1，2或3。
3.按照权利要求1的方法，其特征在于该单一相材料为Ti3SiC2。
4.按照权利要求1，2或3的方法，其特征在于加入预先反应状态的期望化合物Mn+1AzXn，所述材料起热潭的作用。
5.按照权利要求1，2、3或4的方法，其特征在于使用约25％(重量)预先反应的材料作为热潭。
6按照权利要求1，2、3、4或5的方法，其特征在于单一相材料是Ti2AlC或Ti2SnC。
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| CN110041075A (zh) * | 2019-05-21 | 2019-07-23 | 哈尔滨师范大学 | 一种高纯Nb2SnC陶瓷粉体的快速制备方法 |
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| DE10262174B4 (de) * | 2001-07-23 | 2007-03-15 | Kabushiki Kaisha Kobe Seiko Sho (Kobe Steel, Ltd.), Kobe | Harte verschleissfeste Schicht, Verfahren zum Bilden derselben und Verwendung |
| SE521794C2 (sv) * | 2002-04-05 | 2003-12-09 | Sandvik Ab | Tillverkningsförfarande för ett värmeelement av molybdensilicidtyp, jämte ett värmeelement |
| EP1492740B1 (en) * | 2002-04-05 | 2007-09-05 | Sandvik Intellectual Property AB | Method of making a heating element of molybdenum silicide type |
| SE521796C2 (sv) * | 2002-04-05 | 2003-12-09 | Sandvik Ab | Förfarande för tillverkning av ett värmeelement av molybdensilicidtyp jämte ett värmeelement |
| SE527199C2 (sv) * | 2003-02-07 | 2006-01-17 | Sandvik Intellectual Property | Användning av ett material i oxiderande miljö vid hög temperatur |
| US7553564B2 (en) * | 2004-05-26 | 2009-06-30 | Honeywell International Inc. | Ternary carbide and nitride materials having tribological applications and methods of making same |
| SE0402904L (sv) * | 2004-11-26 | 2006-05-27 | Sandvik Intellectual Property | Belagd produkt och produktionsmetod för denna |
| CN100429326C (zh) * | 2005-09-29 | 2008-10-29 | 中国科学院上海硅酸盐研究所 | 一种铝碳二铬块体材料的制备方法 |
| CN1331759C (zh) * | 2006-03-21 | 2007-08-15 | 北京交通大学 | 一种低温合成碳化锡钛的方法 |
| JP4836263B2 (ja) * | 2007-01-04 | 2011-12-14 | 独立行政法人産業技術総合研究所 | 高強度チタンシリコンカーバイド基複合材料及びその製造方法 |
| JP5220353B2 (ja) * | 2007-04-12 | 2013-06-26 | 独立行政法人科学技術振興機構 | 自己伝播高温合成方法 |
| KR100882923B1 (ko) | 2007-12-07 | 2009-02-10 | 한국과학기술연구원 | 기계가공성을 갖는 Ｃｒ₂ＡｌＣ 소결체의 저가 제조방법 |
| MX2012009067A (es) * | 2010-02-04 | 2013-01-28 | Third Millennium Metals Llc | Composiciones de metal-carbon. |
| KR101542607B1 (ko) | 2013-06-28 | 2015-08-06 | (주) 빛과환경 | 자전연소반응을 이용한 티타늄 합금의 제조방법 |
| US10913129B2 (en) * | 2014-01-24 | 2021-02-09 | Raytheon Technologies Corporation | Additive manufacturing an object from material with a selective diffusion barrier |
| CN104557045B (zh) * | 2015-02-05 | 2016-06-15 | 安徽工程大学 | 一种碳化锡钛材料常压低温制备方法 |
| CN106119593A (zh) * | 2016-08-05 | 2016-11-16 | 东南大学 | 一种Ti2SnC增强Ag基电触头材料的制备方法 |
| CN113044842B (zh) * | 2021-01-12 | 2022-05-17 | 辽宁中色新材科技有限公司 | 一种高纯碳化铝钛的生产工艺 |
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| US4961529A (en) * | 1987-12-24 | 1990-10-09 | Kernforschungsanlage Julich Gmbh | Method and components for bonding a silicon carbide molded part to another such part or to a metallic part |
| US4946643A (en) * | 1988-10-21 | 1990-08-07 | The United States Of America As Represented By The United States Department Of Energy | Dense, finely, grained composite materials |
| US4909842A (en) * | 1988-10-21 | 1990-03-20 | The United States Of America As Represented By The United States Department Of Energy | Grained composite materials prepared by combustion synthesis under mechanical pressure |
| US5330701A (en) * | 1992-02-28 | 1994-07-19 | Xform, Inc. | Process for making finely divided intermetallic |
| US6171709B1 (en) * | 1995-09-27 | 2001-01-09 | The Ishizuka Research Institute, Ltd. | Super-abrasive grain-containing composite material and method of making |
| KR20010021722A (ko) * | 1997-07-11 | 2001-03-15 | 존슨매테이일렉트로닉스, 인코퍼레이티드 | 내부 금속성인 알루미늄 화합물 및 규소 화합물 스퍼터링타겟과 그의 생성방법 |
| US6231969B1 (en) * | 1997-08-11 | 2001-05-15 | Drexel University | Corrosion, oxidation and/or wear-resistant coatings |
| CN1120816C (zh) * | 1998-08-19 | 2003-09-10 | 中国科学院金属研究所 | 一种钛碳化硅粉末的制备方法 |
| CN1120817C (zh) | 1998-10-07 | 2003-09-10 | 中国科学院金属研究所 | 一种原位热压固－液相反应制备钛碳化硅体材料的方法 |
| US6461989B1 (en) * | 1999-12-22 | 2002-10-08 | Drexel University | Process for forming 312 phase materials and process for sintering the same |
| SE0004819L (sv) | 2000-12-21 | 2002-02-05 | Sandvik Ab | Motståndselement för extrema temperaturer |
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| CN110041075A (zh) * | 2019-05-21 | 2019-07-23 | 哈尔滨师范大学 | 一种高纯Nb2SnC陶瓷粉体的快速制备方法 |
| CN110041075B (zh) * | 2019-05-21 | 2021-05-28 | 哈尔滨师范大学 | 一种高纯Nb2SnC陶瓷粉体的快速制备方法 |
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| KR20040030683A (ko) | 2004-04-09 |
| TW567168B (en) | 2003-12-21 |
| SE0102214L (sv) | 2002-12-22 |
| JP2004532788A (ja) | 2004-10-28 |
| US20040156772A1 (en) | 2004-08-12 |
| EP1397325A1 (en) | 2004-03-17 |
| EP1397325B1 (en) | 2009-10-28 |
| DE60234177D1 (de) | 2009-12-10 |
| SE521882C2 (sv) | 2003-12-16 |
| SE0102214D0 (sv) | 2001-06-21 |
| JP4045239B2 (ja) | 2008-02-13 |
| KR100831244B1 (ko) | 2008-05-22 |
| CN1295190C (zh) | 2007-01-17 |
| ATE446944T1 (de) | 2009-11-15 |
| WO2003000618A1 (en) | 2003-01-03 |
| US6986873B2 (en) | 2006-01-17 |
| ES2335088T3 (es) | 2010-03-22 |
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