TW567168B - A method of producing a metal-containing single-phase composition - Google Patents
A method of producing a metal-containing single-phase composition Download PDFInfo
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- TW567168B TW567168B TW091111293A TW91111293A TW567168B TW 567168 B TW567168 B TW 567168B TW 091111293 A TW091111293 A TW 091111293A TW 91111293 A TW91111293 A TW 91111293A TW 567168 B TW567168 B TW 567168B
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- 239000000203 mixture Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 14
- 239000002184 metal Substances 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 150000001875 compounds Chemical class 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000010936 titanium Substances 0.000 claims abstract description 11
- 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
- 239000010955 niobium Substances 0.000 claims abstract description 8
- 229910052755 nonmetal Inorganic materials 0.000 claims abstract description 8
- 239000010703 silicon Substances 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910009817 Ti3SiC2 Inorganic materials 0.000 claims abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 150000002739 metals Chemical class 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
- 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
- 150000002843 nonmetals Chemical class 0.000 claims abstract description 3
- 239000011651 chromium Substances 0.000 claims abstract 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract 2
- 229910052804 chromium Inorganic materials 0.000 claims abstract 2
- 230000017525 heat dissipation Effects 0.000 claims description 4
- 238000000354 decomposition reaction Methods 0.000 claims description 3
- 229910010013 Ti2SnC Inorganic materials 0.000 claims 1
- -1 Zr (hammer) Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract 1
- 239000004411 aluminium Substances 0.000 abstract 1
- 238000010494 dissociation reaction Methods 0.000 abstract 1
- 230000005593 dissociations Effects 0.000 abstract 1
- 229910052706 scandium Inorganic materials 0.000 abstract 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 abstract 1
- 229910052726 zirconium Inorganic materials 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 238000010894 electron beam technology Methods 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 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
- 239000000919 ceramic Substances 0.000 description 2
- 238000005049 combustion synthesis Methods 0.000 description 2
- 229910003465 moissanite 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
- 229910008479 TiSi2 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 description 1
- BROYGXJPKIABKM-UHFFFAOYSA-N [Ta].[Au] Chemical compound [Ta].[Au] BROYGXJPKIABKM-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 description 1
- DFJQEGUNXWZVAH-UHFFFAOYSA-N bis($l^{2}-silanylidene)titanium Chemical compound [Si]=[Ti]=[Si] DFJQEGUNXWZVAH-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000002131 composite material Chemical class 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 229910021344 molybdenum silicide Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000376 reactant Substances 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
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical class C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
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Description
567168 A7 B7 五、發明説明（彳 本發明係關於一種製造含金屬單相組合物之方法。本發明主 要關於碳化石夕鈦及屬於同一家族之複合化合物之製造。 無氧燃燒合成，亦稱為SHS(自我散佈高溫合成）一般用 於製造半金屬產物及陶瓷組合物。 在SHS技術中，二或更多材料之混合物透過強熱源之媒 介局部點燃。此熱源可由例如加熱絲或一些其他加熱元 件、雷射束或電子束組成。局部點燃造成局部反應，因強 烈放熱反應之結果。這造成過剩能量之釋放，這點燃材料 之鄰近部分而最後為整個材料。此鏈反應非常迅速且當反 應受控制時提供高效率方法大量生產之半金屬及陶瓷。系 統可達到之最高溫度為絕熱溫度。 自從1980年代中期已做了許多生產Ti3SiC2之嘗試。潘 邦奇（Pampuch)等人（R.潘邦奇等人，” Ti3SiC2之固體 燃燒合成 ”J. EUR. CERAM. SOC·， 5,2 8 3 -8 7 ( 1 989))”及其他人已在惰性氣氛中點燃Ti、Si及C之粉末 混合物。這產生T i 3 S i C 2 +約1 0 - 3 0 %之其他相，如τ i C、 TiSi2 及 SiC。 葛斯曼（Goesmann)等人（F.葛斯曼等人，”由電子束點 燃固態反應”，J. Amer，Ceram Soc. 81，11，3〇25-28 ( 1 998))”咸信SHS將不產生由Ti3SiC2之預定單相，由於 反應極高溫（高於2000 °C)之結果產生金屬矽之除氧。葛 斯曼以化學組成為ThSiC2 + 12.5重量％過剩矽之丁丨及 S i C混合物開始。他使用電子束點燃混合物。此混合物以 三階段處理，即在8 0 0 t熱處理，在9 0 0 °C點燃，隨後在 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐）
裝 訂
線 567168 A7 B7 五、發明説明（2 1 6 0 0 °C熱處理完成過剩矽之除氣。此法產生樣品中小於 8 %之第二相。 在我們自己之1999年12月之美國專利申請案第 09/469,893號中’我們已顯示大氣中之氧影響在製造過 程中且亦在隨後燒結過程中Ti3 Si C2之熱安定性，其藉形 成基本上與由於高溫之矽氣化不同之氣體si〇。 如此，已發現在前述方法中不得到其他反應產物製造碳 化矽鈦很困難。 上面已提及本發明亦關於相同家族之組合物。此家族指 名為單相組合物M3SiZ2，此處Μ為至少一種金屬，z為化 學元素C(碳）及Ν(氮）之至少一種。 本發明係關於製造碳化矽鈦之高成本問題。 如此本發明關於一種製造單相組合物]Vi η + ! A ζ X η之方 法，此處11在0.8-3.2之範圍内，ζ在0.8-1.2之範圍内，Μ 為至少一種取自金屬Ti(鈦）、Sc(銃）、V(釩）、Cr(鋁）， Zr(鍅），Nb(鈮）及Ta(钽）之金屬，而X為非金屬c(碳）及 N(氮）中之至少一種且A為化學元素Si(矽），A1(鋁）及 S η (錫）或使得到最終要求化合物組分μ n +〖A z X n之該等元 素的化合物之一，其中此法亦包括由該金屬、非金屬及最 後提及之化學元素或該元素之化合物形成粉末混合物，及 在惰性氣氛中點燃該粉末混合物以不助長分解（其藉此該 新進組分反應），其中此法之特徵為使反應物溫度保持在 該組分引起反應之溫度或之上，但在單相組合物分解之溫 度之下。 -6 - 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐）
裝 訂
線 567168 A7 ____ B7 五、發明説明（ ） 3 ’ 本發明現在將更詳細部分參照三個實例敘述。 本方法係關於製造單相（或一相）組合物Mn + 1 AzXn，其 中η在〇·8-3·2之範圍内，2在〇.8-1.2之範圍内，Μ為至少 一種取自金屬Ti(鈦）、Sc(銃）、ν(釩）、Cr(鋁）， Zr(結）’ Nb(鈮）及Ta(钽）之金屬，而X為非金屬c(碳）及 N(氮）中之至少一種且A為化學元素Si(矽）、μ(鋁）及 Sn(锡）或使最終，要求化合物將包括組分Μη+ιΑζΧη之該 等兀素的化合物之一。此法包括形成該金屬、非金屬及最 後k及化干元素或化合物之粉末混合物，及在惰性氣氛中 點燃粉末混合物使其反應。惰性氣氛包括具足夠低分壓氧 之空氣以防止促進分解。 根據本發明，引起之反應溫度維持在組分引起反應之水 準或更高，但在單相組合物分解之溫度之下。 如此，將了解本發明之基本特徵為在反應時溫度受壓 制，但仍在特定水準之上。 這是一種製造單相組合物Ti3SiC2之較佳方法。 根據極佳之具體貫施例，溫度藉添加預反應之T i 3 s i c 2 壓制’此材料作為散熱用。 最高約25重量-% TisSiC2作為散熱用較佳。 另一種選擇為溫度在以其他方式之反應中可受壓制，例 如藉控制地冷却材料。 下面為一些實例。 實例1
Ti、SiC及石墨粉末一起混合產生Ti3Sic2之計量混合 本紙張尺度適用中國國家標準(CNS) A4規格(210X297公釐） 567168 A7 B7 五、發明説明（4 物。此混合物以12重量％預反應之Ti3SiCyl合。 混合物置於反應容器中並通流速為〇 . 5升/分鐘之氬。粉 末床之厚度為約2 〇公分。 粉末床以置於反應容器底部之矽化鉬元素點燃。粉末床 組分起反應。 粉末冷却後由容器中移出。粉末床將迅速破碎。
取自粉末床之樣品以X線繞射分析。 已確定粉末床含約2-4重量-% Tic。 實例2 如實例1之相同樣品但除了 2 5重量-%預反應之丁 i 3 S i C 2 加入混合物之外。 訂
線 粉末床發現含1 5 - 2 0重量-%之T i C，隨後點燃及冷却。 實例2顯示，在其他物品中，過量稀釋之預反應材料造 成不完全之反應，因此粉末床要求在丨4 〇 〇 °C 8小時之熱處 理以得到單相材料。 實例3 如實例2之相同樣品，τ i、s i及石墨粉末一起與2 5重量-%預反應Ti3SiCy\l合並加到混合物中。 粉末床發現在點燃及冷却後含2 5 - 3 0重量-%之T i C。 隨後在1 4 0 〇 °C熱處理粉末床8小時，粉末床發現含小於 2重量％之T i C。 此實例顯示S i可用於取代S i C。 雖然本發明已參照一些其具體實施例敘述，應了解溫度 可由上面敘述之外的方法保持在敘述之範圍内，其在本發 本紙張尺度適用中國國家標準(CNS) a4規格(21〇x297公釐) 567168 A7 B7 五、發明説明（5 明之範圍内。 本發明因此未視為限制在前述例示之具體實施例中，因 為可作改變而仍在附帶”申請專利範圍”内之範圍内。 -9- 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐)
Claims (1)
- 1. 一種製造單相組合物Mn+1AzXn之方法，此處。在0.8-3.2 之範圍内，2在〇.8-1.2之範圍内，Μ為至少一種取自金屬 Ti(鈦）、Sc(钪）、V(釩）、Cr(鉻）、Zr(錘）、Nb(鈮）及 Ta(鈕）之金屬，而X為非金屬C(碳）及N(氮）之至少一種且 A為化學元素Si(矽）、A1(鋁）及Sn(錫）或使最終、要求化 合物將包括組分Mn+1AzXn之該等元素化合物之一，其中 此法亦包括由該金屬、非金屬及該化學元素或該等元素之 化合物形成粉末混合物，及在惰性氣氛下點燃該粉末混合 物以防止助長分解，因此該組分反應，而此處此方法之特 徵為保持反應溫度在組分引起反應之溫度或在之上，但在 單相組合物分解之溫度之下。 2. 如申請專利範圍第1項之方法，其特徵為η == 1，2或3。 3. 如申請專利範圍第1項之方法，其特徵為該單相材料為 Ti3SiC2。 4. 如申請專利範圍第1、2或3項之方法，其特徵為在預反應 I 狀態下添加要求化合物Mn+1AzXn，之後該材料作為散熱 用。 5. 如申請專利範圍第3項之方法，其特徵為使用25重量-%預 反應材料作為散熱用。 6. 如申請專利範圍第3項之方法，其特徵為該單相材料為 Ti2AlC 或Ti2SnC 0 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐)
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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 |
| SE521796C2 (sv) * | 2002-04-05 | 2003-12-09 | Sandvik Ab | Förfarande för tillverkning av ett värmeelement av molybdensilicidtyp jämte ett värmeelement |
| KR100639138B1 (ko) * | 2002-04-05 | 2006-10-30 | 산드빅 인터렉츄얼 프로퍼티 에이비 | 규화몰리브덴 타입의 발열 소자 제조 방법 |
| 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 |
| EP2531629A1 (en) * | 2010-02-04 | 2012-12-12 | Third Millennium Metals, Llc | Metal-carbon compositions |
| 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 |
| 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 |
| 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 |
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| US6461989B1 (en) * | 1999-12-22 | 2002-10-08 | Drexel University | Process for forming 312 phase materials and process for sintering the same |
| SE516644C2 (sv) | 2000-12-21 | 2002-02-05 | Sandvik Ab | Motståndselement för extrema temperaturer |
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| JP2004532788A (ja) | 2004-10-28 |
| KR20040030683A (ko) | 2004-04-09 |
| ATE446944T1 (de) | 2009-11-15 |
| US20040156772A1 (en) | 2004-08-12 |
| EP1397325B1 (en) | 2009-10-28 |
| KR100831244B1 (ko) | 2008-05-22 |
| CN1538944A (zh) | 2004-10-20 |
| SE0102214L (sv) | 2002-12-22 |
| SE0102214D0 (sv) | 2001-06-21 |
| ES2335088T3 (es) | 2010-03-22 |
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| DE60234177D1 (de) | 2009-12-10 |
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| SE521882C2 (sv) | 2003-12-16 |
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