TW418111B - Composition and process for removing moisture from hydrogen halides - Google Patents
Composition and process for removing moisture from hydrogen halides Download PDFInfo
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- TW418111B TW418111B TW087112304A TW87112304A TW418111B TW 418111 B TW418111 B TW 418111B TW 087112304 A TW087112304 A TW 087112304A TW 87112304 A TW87112304 A TW 87112304A TW 418111 B TW418111 B TW 418111B
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- C01B7/00—Halogens; Halogen acids
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Description
A7 B7 ;、發明説明(1 ) 發明背景 1 .發明菽圍 (請先閱讀背面之注意事項再填寫本頁〕 本發明係關於 自氫自化物移除水份之組合物與方法。 2 .以往技爇發.明 氣態及液體之氫自化物在目前是以高純度無水組合物型 式利用。無水氫南化物在半導體工業普遍用於清潔反應器 管件及盛受體,以及用作生產微電路之蚀刻劑。 在作這方面應用時,必須在其成爲符合最終作業環境 前,有效的自氫由化物如氣化氫移出水份或水蒸汽。氣化 氫通常爲氣體,偶而是以加壓下的流體型態運送。氣化氫 在壓力爲615 psig時成液態》含水氣化氫爲高腐蝕性,因此 凡與其碰觸之管件,分配管,閥等等均需時常更換。在清 潔盛受體,亦即晶圓處理支撐構造物時,氣化氫中的水份 會導致盛受體上生成新的氧化物,因此對於其原先所欲達 成的清潔功能產生反效果。而在蚀刻應用時,含水氯化氫 成爲半導體生產環境之有害水份污·染源,有可能造成在此 環境下之微電路晶片產品不良,或甚至不能爲其原目的使 用。 以往被用作移除氣化氫水份方法中所採用者是吸附水份 的分子篩。然而這種生產高純度氣化氫方法中的難處,在 於氣化氫對水在分子篩吸附位置具有競爭性。其結果爲無 法獲得到必要的低殘留水値,亦即在分子,筛接觸步驟排氣 中,體積濃度在百萬分之十範圍及更低。 氣化氫亦曾以硫酸或磷酸處理以製得脱水氣化氫。然而 -4 五、發明説明(2 ) 此種脱水方法’無法避免會產生氣化氫上增加硫或磷的缺 點,此種增加的元素在前述半導體生產應用上爲高度不利 之污染物。 另外亦有利用氧化銘撐體上氣化錢,以有效自氫自化物 移除水的方法建議。但是發現在實際上,此種純化原料在 與如液態之高壓氣化氫接觸時並不恰當,因其鋁會與氣化 風反應生之成二氣化铭顆粒’在氣化氫進行純化所經過攄 器形成阻塞。 此外,在氧化鋁上生成氣化鎂需經多重反應步驟,其中 首先將氧化鋁以例如以15重量%二丁基鎂溶於已烷溶劑中 之溶液塗佈。溶劑再於加熱時蒸發移出。該二丁基鎂加熱 到約250°C時在氧化鋁上轉化爲氫化鎂。此氫化鎂再於氧化 15上以濃縮氣化氩轉化爲氣化錢。此組合物再被用來移除 氫鹵化物水份。 溴化氫爲半導體製造界所需,在實質上完全在無水條件 之氫函化物另一例子。溴化氫在電子工業是作爲晶圓蝕刻 劑,以及盛受體清潔劑。在這種應用上,溴化氫的水份會 造成與前述氣化氫在相類似應用已發現之相同缺點。此 外’在以溪化氣作晶圓蚀刻劑時,澳化氩即使僅含極少量 水氣亦會產生起霧現象。 此技藝界亦"t試使用轉酸作乾燥劑,達到自溴化氫移除 水份的目的》此方法雖大致可用來移除水,污染物,但仍具 有在溴化氫上增加磷的缺點傾向,其與前述所指之氣化氫 情況相同,爲半導體製造過程中相當嚴重之污染物。 _____ - 5 * 4、纸乐尺度ϋ中KK家標冷((,NS ) 見格(2丨0X297公釐 第871123〇4號專利中請案 中文說明書修正頁(的年4月) A7 B7 8W4n 五、發明説明(3 經濟部中央標準局員工消費合作社印裝 η::i必要提供自氫鹵化物移除水份之組合物及方法, & S二生出ί顆粒的污染性副產物。此外,此種組合物 万/而具有咼能力自氣態或液體氩鹵化物移除水份。另 土 Α ί ^組合物的生成’應較目前生成類似组合物現有方 法為較簡化之方法。 發明摘要 ^發明提供自氫由化物流體移除水份之組合物其包括 f 一巨型多孔性碳質iX體上沉積氣化鎂或溴化鎂之鎂鹵化 勿。巨型多孔性碳質ix體表面沉積鎂函化物的第一步是 將ΪΧ fla與一丁基鎂落液混合,以在辻體表面塗佈二丁基 鎂。再於非反應性環境中,以蒸發作用移除形成溶液之溶 劑。其後,令已塗佈ix體與氫由化物接觸,將二丁基鎂轉 化為鎂自化物。此一方法免除生成氫化鎂的必要。 在應用上,經鎂函化物塗佈ix體與氫画化物流體充分密 切接觸,以自氩函化物流體極有效的將水份全部移除◊氫 鹵化物流體及鎂南化物的卣化物必須相同,以防止流體被 污染。 附圖簡述 圖1說明本發明之應用。 圖2為說明本發明组合物自氮移除水份能力之以如以 Transform Infra Red光譜。 圖3為說明本發明組合物自hci移除水份能力之Foerier Transform Infra Red光譜。 元件符號說明 10表入口; 18表濾板;及 12表谷器, 20表出口。 14 表阻流板; 16 表水份移除材料; 特定具體實例說明 -6 本紙張尺度適用中國國家標隼(CMS ) A4規格(210X297公釐〉
-----J (請先閱讀背面之注意事項再填寫本頁) '裝 訂J— 4M η ί、 • Α7 ------------Β7 五、發明説明(4 ) 本發明組合物所包含巨型多孔性碳質撐體具有之平均孔 徑大於約100埃到約1〇〇微来,而以介於約2〇八與1000 Α間較 佳’其上塗佈鎂鹵化物。適用之碳質撐體可以由例如對聚 合性樹脂裂解製成。代表性適用之撐體係以裂解磺酸化苯 乙烯/二乙埽基苯巨型多孔性離子交換樹脂製成,並於例如 美國專利字號第5,094,754號中所揭示,其爲本文列作參 考。此種碳質撐體可由位於philadelphia,pA之心—及取“ 公司提供’註册商標爲AMBERSORB®。 顆粒性巨型多孔性碳質撐體上塗佈鎂南化物的製法,是 先令撐體密切接觸二烷基鎂化合物溶液,例如二甲基,二 乙基,二丁基,或二丙基鎂。製作該溶液之代表性適用溶 劑包括己烷,庚烷等等。撐體與溶液進行接觸時間介於約 1小時與约4小時間,溫度則在約25〇c與約7〇t間。在此得 到之已塗佈撐體由溶液分離,過量溶劑則以如蒸發作用自 其移出。蒸發作用可在一惰性或非反應性大氣環境,如氡 或惰性氣體下’加熱到介於約55χ:及65乇溫度爲之。 最後步驟中,已塗佈撐體與氫鹵化物氣體以單獨形態, 或是混合在非反應性載體氣體,如氮氣,而氫_化物佔該 氣體約5到100體積%作接觸。在此最後步騍,二烷基鎂轉 化爲鎂南化物。當以經塗伟撐體乾燥氣化氫流體時,該氫 南化物採用氣化氫。當經塗佈撐體乾燥溴化氫流體時,該 氫鹵化物採用溴化氫。與氫鹵化物流體接觸,是在能夠實 貝上元王將—境•基鎂轉化爲鎂卣化物的時間與溫度下進 行。典型接觸時間介於約1 J min/m丨樹脂與5 5 min/ml樹脂之 ( C'NS ) ( 210X 297/^^ ) A7 五、發明説明(5 ) 間,較佳爲介於約16min/ml與約5.5min/ml之間。典型反應 溫度介岭約25 C與約240 C之間’較佳爲約4〇»c與约6〇«c之 間。 本發明組合物即使在壓力高的使流體爲液體情況下,仍 能自氩卣化物流移出水份’不會產生反應性產物,例如會 對氣由化物;亏染之特定反應產物。再者,本發明組合物能 耐高壓液趙流趙到50°C時的約11〇〇 pSig壓力。 鎮由化物塗佈層能使本發明組合物,自氩南化物流體移 除水份到低於約100 ppb,較佳到低於約50 ppb,同時不會 明顯的對撐體巨孔造成阻塞。本發明組合物特色之一在於 其水份吸附能力超過每公升塗佈撐體約4〇公升水,較佳爲 每公升塗佈撐趙超過約60公升水《錢鹵化物在此漠度超過 每公升碳質撐體至少約。.丨莫耳的鎂鹵化物,較佳在每公升 竣質撐體超過至少約1.2莫耳鎂_化物。 應用上’本發明组合物係與流動流體流型式之流體氫鹵 化物密切接觸’或於儲槽内靜態共存,使實質上所有的氫 鹵化物接觸到組合物。 部十欢|?-卑而·=?.!消於Atit社印黛 (請先閱讀背面之注意事項再填寫本頁) 參考圖1 ’欲乾燥氫由化物流體由入口 1〇送入容器12。流 體流過阻留板14進入本發明經塗佈碳質顆粒床18,水份經 此由流趙移出。流體再經過濾板丨8與出口 2〇流出到使用點 (圖上未示)。 以下範例説明本發明,唯不對其作任何限制:
範例I 本範例示範製造本發明之氣化鎂塗佈產物之方法。 4181Π 第87112304號專利申請案 中文說明書修正頁(89年4月) 五、發明説明(6 ) 200 1111 八11^6^〇1^@ 563碳質吸附劑以 200 111110〇/〇甲醇/水 溶液洗淨。Ambersorb® 563 由位於 Philadelphia, PA的R〇hm及 經濟部中央標準局員工消費合作社印装 yy. 4.14 年月; A7 B7 (請先閲讀背面之注意事項再填荇本頁)
Haas公司提供,表面積為550 m2/g,開孔度以氮孔隙測試為 0.23 ml/g。溶液經傾倒出後,再以甲醇沖洗珠粒三次。匕 體以空氣乾燥到自由滾動,置於一只1 〇〇〇 ml圓柱體,氮氣 由底部進入,圓柱體加熱到1 〇〇。(:約4小時,直至主要的水/ 甲醇溶液已經移除,此時再提升圓柱體溫度到24(rc 15小 時。此活化階段結束時將ix體冷卻到6〇。(:。含足量15%二丁 基鎂之庚烷溶液於此時加入,以填入碳的空出體積,再以 由圓柱體底部吹氮吹除約75%的庚烷。此步驟重覆操作,直 到庚炫•中所有二丁基鎮均加入。擾拌必須保持以達成均質 混合物且避免結焦。八11^6^〇1^@ 563碳質吸附劑上二丁基鎂 在一整天内均保持在55 °C的1 slpm氮氣流下,其後再分離 出該碳質吸附劑’送入一只儲盒,並於盒中放入適合處理 有害氣體的取樣圓柱體。此氣體取樣圓柱體及碳質吸附劑 連接到一氣體分配頭,其能容許脫水HC1與乾燥氮氣的流 動*以二倍的過量5% HC1於氮氣,壓力在15 psia,流率為 1000 seem流過碳質吸附劑,同時令純HC丨以15 psia壓力及 1000 seem流過碳質吸附劑30分鐘,再以HC丨加壓容器到60 psig到隔曰》碳質吸附劑於次晨以1〇〇〇 sccni N2驅氣,而取 樣圓柱加熱240°C 52小時。驅氣若以高壓C02會更有效。最 終產物在26°C排出低於1 ppm總碳水化合物。
範例II 此範例示範使用本發明產物自氮及HC1移除水份。 -9- 本紙張尺度適用中國國家樣準(CNS ) A4規格(210X297公釐) 41811 1 第87ll23〇4號專利申請案 中文說明書修正頁(89年4月) A7 B7 年月a if;;V . λΛ--} ;Τγ I ·:;Γ< •-.•τ' t 五、發明説明( 屬 經濟部中央橾隼局貝工消费合作社印製 此處所進行的實驗係用來判斷經塗佈碳質吸附劑是否可 以吸附氣氣流。為試驗出水含量,乂或HQ氣體以50〇 seem 由傳統氫自化物純化劑乾燥。HC1氣體再由圖1所示純化裝 置通過’或不經由純化劑而通過。未經純化劑流是作為對 照水含量的代表。所得氣體流經導入1〇米路徑長,保持在 130C之乳禮至’以作Fourier Transform Infrared 分析(FT-IR) 之用。以含45 ppm水之100 sccm N2視需求加入該氣體流(總 流量為600 seem)。 FT-IR光譜組成顯示具有自n2移出水份到低於1〇〇 ppb程度 的能力。圖2為三個FT-IR在1772 cm·1的光譜,說明本發明 組合物在N 2中保存水的能力。 經傳統純化劑乾燥並且未通過本發明組合物之N2以“乾 N2”表示。水”則代表未通過本發明組合物的澄(4 ppm) N2 氣體流,而“新純化劑+水”表示通過範例I組合物之溼N2 » ’ 由光譜明顯看出,“乾N2”與“新純化劑+水”間無差異,這 表示傳統純化劑與本發明純化劑均能在N2中保存同等程度 的水(< 100 ppb)。 參考囷3 t範例I之組合物具有自HC1移除水份到低於1 〇〇 ppb的能力。圖3為三個FT-IR在1772 cm·1的光譜,說明了範 例I組合物在HC1的保存水能力。 傳統純化劑乾燥之HC1,且其未通過範例I组合物者,以 “乾H C 1 ’’表示。“水’’代表未通過範例I組合物之溼(4 ppm) H C 1氣體流,而“新純化劑+水”代表通過範例I組合物之溼 HC1。此處明顯看出在“乾HC1”與“新純化劑+水”光譜中並無 10- 本紙張尺度適用中國國家標準(CNS > Α4规格(210Χ297公釐) )裝 - 訂. . 货 (請先閲讀背面之注意事項再填寫本頁) 4 18 111 A7 B7 五、發明説明(8 差異,説明了傳統純化劑與範例I組合物在HC1中均能留存 水在同等程度(< 100 ppb)。 -11 - 本纸張尺度试川屮SKiUH ( (·Ν5 ) Λ4規格(2iOX 297公漦) -I— 1 I - ---i I- -I - —1-----. I I. 士人· -- I - ml .1----- I.,——I ΐ~Ψ (請先聞讀背面之注意事項再填寫本頁)
Claims (1)
- 418111 -: 第871丨23〇4號專利申請案 M 中文申請專利範圍再修正本(89年4月)Μ 六、申請專利範圍經濟部中央標準局員工消費合作社印製 I. —種適合達成自氫自化物流體移除水份之組合物其 包含以鎂卣化物塗佈具有平均孔徑大於1〇〇埃而最高 達100微米之巨型多孔性碳質撑體。 2_根據申凊專利範圍第1項之組合物 氣化鎂。 3.根據申請專利範圍第1項之組合物 溴化鎂》 4_根據申請專利範圍第1項之組合物 物可吸附60升水的能力。 5. 根據申請專利範圍第2項之組合物 物可吸附60升水的能力。 6. 根據申請專利範圍第3項之組合物 物可吸附60升水的-能力。 7. —種自氫画化物流體移除水份之方法,其包括使該流 體與經鎂鹵化物塗佈具有平均孔徑大於1〇〇埃而最高 達1 0 0微米之巨型多孔性碳質ix體密切接觸,並使該 流體自該經塗佈撐體分離。 8. 根據申請專利範圍第7項之方法 化鎮。 9·根據申請專利範圍第7項之方法 化鎖:。 丨〇.根據申請專利範園第7項之方法 種氣體。 - II. 根據申請專利範圍第8項之方法,其中該氫鹵化物為一 其中該鎂由化物為 其中該鎂由化物為 其具有每升該組合 其具有每升該組合 其具有每升該組合 其中該鎂画化物為氯 其中該鎂由化物為溴 其中該氫函化物為一 I.--^------f-- (請先閲讀背面之注意事項再填寫本頁) ,tT ίι. 本紙張尺度逋用中國國家梂率(CNS > Α4規格(210X297公釐) ------種氣體。 1據中請專利範U9項之方法,其中該氫自化物為一 種氣體。 =據申SH專利圍第7項之方法,其中該氫面化物為一 種液體。 14. 根據中請專利範圍第8項之方法,其中該氩齒化物為一 種液體。 15. 根據中請專利項之方法,其中該氫由化物為一 種液體。 ---------裝— I < ,\ (請先閲讀背面之注意事項再填寫本頁) 經濟部中央標嗥局員工消費合作社印製 本紙浪尺度適用中國國家標準(CNS ) Α4規格(2丨0Χ297公釐)
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US5766565A (en) * | 1993-01-21 | 1998-06-16 | Dow Corning Corporation | Purification of hydrochloric acid |
US5827492A (en) * | 1993-01-28 | 1998-10-27 | E. I. Du Pont De Nemours And Company | Hydrogen chloride purification process |
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KR0163871B1 (ko) * | 1995-11-25 | 1998-12-01 | 김광호 | 하부에 히트 싱크가 부착된 솔더 볼 어레이 패키지 |
JPH11139805A (ja) * | 1997-07-29 | 1999-05-25 | Millipore Corp | ハロゲン化水素から水分を除去するための組成物とその方法 |
US5910292A (en) * | 1997-08-19 | 1999-06-08 | Aeronex, Inc. | Method for water removal from corrosive gas streams |
US5958356A (en) * | 1997-11-05 | 1999-09-28 | Air Products And Chemicals, Inc. | Method for removal of moisture from gaseous HCl |
US6077487A (en) * | 1997-11-05 | 2000-06-20 | Millipore Corporation | Process and apparatus of removing metal carbonyls and moisture from a gas |
US6221132B1 (en) * | 1999-10-14 | 2001-04-24 | Air Products And Chemicals, Inc. | Vacuum preparation of hydrogen halide drier |
-
1998
- 1998-07-24 JP JP10209116A patent/JPH11139805A/ja active Pending
- 1998-07-25 SG SG1998002799A patent/SG75863A1/en unknown
- 1998-07-27 DE DE69800126T patent/DE69800126T2/de not_active Expired - Lifetime
- 1998-07-27 EP EP98114019A patent/EP0894527B1/en not_active Expired - Lifetime
- 1998-07-28 KR KR1019980030358A patent/KR100572936B1/ko not_active IP Right Cessation
- 1998-07-28 TW TW087112304A patent/TW418111B/zh not_active IP Right Cessation
- 1998-07-29 CN CN98103093A patent/CN1126711C/zh not_active Expired - Lifetime
-
2002
- 2002-04-24 US US10/132,038 patent/US20020117450A1/en not_active Abandoned
-
2003
- 2003-05-01 US US10/427,736 patent/US7288201B2/en not_active Expired - Fee Related
- 2003-05-01 US US10/427,711 patent/US20040026327A1/en not_active Abandoned
- 2003-05-01 US US10/427,125 patent/US20030234222A1/en not_active Abandoned
-
2006
- 2006-09-20 US US11/524,079 patent/US20070138102A1/en not_active Abandoned
Also Published As
Publication number | Publication date |
---|---|
CN1206690A (zh) | 1999-02-03 |
JPH11139805A (ja) | 1999-05-25 |
DE69800126D1 (de) | 2000-05-31 |
US20040031758A1 (en) | 2004-02-19 |
US20020117450A1 (en) | 2002-08-29 |
EP0894527B1 (en) | 2000-04-26 |
KR19990014247A (ko) | 1999-02-25 |
EP0894527A1 (en) | 1999-02-03 |
US20040026327A1 (en) | 2004-02-12 |
CN1126711C (zh) | 2003-11-05 |
US20030234222A1 (en) | 2003-12-25 |
SG75863A1 (en) | 2000-10-24 |
KR100572936B1 (ko) | 2006-08-31 |
DE69800126T2 (de) | 2000-09-21 |
US7288201B2 (en) | 2007-10-30 |
US20070138102A1 (en) | 2007-06-21 |
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