TWI400369B - 用於矽結晶的坩堝及其製造方法 - Google Patents
用於矽結晶的坩堝及其製造方法 Download PDFInfo
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Description
本發明係關於矽結晶之坩堝及關於坩堝之脫模塗層之製備和應用,該坩堝係用於處理在坩堝中予以固化,然後移出成為錠之熔融材料,更特別係關於多晶矽的固化時所使用之坩堝之脫模塗層。
典型,在多晶矽的固化方面使用各種坩堝(例如,由熔凝矽石、碳化矽、石英、氮化矽、反應黏合之氮化矽、或石墨所造成)。主要地,為了高純度和可用性而選擇矽石。然而,於使用矽石作為經由此方法製造矽之坩堝時有許多問題。
呈其熔融狀態之矽能與它接觸之矽石坩堝起反應。熔融矽與矽石起反應而形成一氧化矽和氧。氧能污染矽。一氧化矽是揮發性且能與爐內部之石墨成分起反應。一氧化矽與石墨起反應而形成碳化矽和一氧化碳。然後,一氧化碳與熔融矽起反應形成另外之揮發性一氧化矽、金屬微量或添加劑和碳的碳化物和氧化物。碳會污染矽。矽亦可與經包含在坩堝中之各種雜質(鐵、硼、鋁…)及/或經包含在氮化物塗層中者起反應。
矽石與矽間之反應促進矽對坩堝的黏著。此項黏著,與兩材料間之熱膨脹係數之差相結合,在矽錠中製造應力,而於冷卻時,致使它破裂。該項技藝中熟知將保護塗層施加至坩堝的內部,在與錠接觸之區域上,可防止矽與矽石間之反應,此反應導致錠污染和破裂。為了有效,該塗層必須充分厚來防止矽與矽石坩堝起反應,且單獨或來自其內部之污染物必須不能不利地污染矽。
其試圖解決與熔融材料接觸之坩堝起反應與黏著問題的各種材料和技術記述於文獻中。
已知氮化矽塗層能防止熔融矽與來自坩堝之矽石間之化學反應。美國專利第4,741,925號中記述經由在1250℃時之化學蒸氣沉漬施加於坩堝的氮化矽塗層,同時WO-A1-2004/053207揭示一種藉噴灑漿體而施加之氮化矽塗層。美國專利第4,218,418號中記述經由在熔體處理期間,快速加熱來防止矽的破裂,形成一玻璃層在矽石坩堝內部之技術。
較早技藝包括明確提到在矽的定向固化時用於施加至坩堝之粉狀脫模劑。另外,述及使用化學蒸氣沉漬、溶劑蒸發、高溫火焰處理、和其他昂貴且複雜方法用來施加坩堝塗層。提到特定黏結劑和溶劑。提到粉狀塗層的漿體之混合、噴霧或刷塗。
熟知氮化矽塗層能防止熔融矽與來自坩堝之矽石間之化學反應。
然而,氮化矽塗層本身可能導致各種問題。必須防止矽與矽石坩堝起反應,氮化矽塗層的厚度是十分重要(約300μm),因此使塗覆操作昂貴且耗時。此外,此氮化矽塗層之機械性弱且在使用期間或甚至使用之前,可剝離或剝落。因此,建議在使用前之最後一刻才施加此塗層,即,在使用者設施上,因此,留下施加此厚塗層的負擔至使用者。
提供穩定氮化矽塗層至陶瓷坩堝上之所熟知技術包括(1)在受控制之燒盡循環下,在範圍自700℃至1450℃之高溫下,氧化氮化物塗層及(2)添加燒結/黏著(或黏附)助劑至氮化物組成物。添加劑可為金屬或氧化物添加劑例如Al2
O3
、SiO2
、AlN、Al、Si、熱解或細矽石及其他。包括熱解矽石之氮化矽塗層記述於同在申請程序中之歐洲申請案04447105中。將氮化矽氧化成為氧化矽增加塗層中之氧的數量而導致上述之問題。另外,氧化的程度及所產生之氧的數量不容易控制。
需要維持坩堝塗層中之低氧含量係由敘述在光生伏特和半導體應用期間化學和物理相互作用之矽製造商的大多數出版物中予以強調。推薦使用低氧之氮化矽塗層用於高品質晶圓製造。使用具有低氧含量之高純度氮化矽粉末顯著記述於美國專利第6,165,425號中。此文獻中記述之氮化矽塗層具有範圍自0.3重量%至至多5重量%之極低氧含量。該塗層可包含黏著促進劑例如聚乙烯醇並在較佳範圍自500℃至700℃之溫度下,於空氣中被乾燥。在此等低乾燥之溫度下,氮化矽的氧化不會發生,沒有形成SiO2
在顆粒邊界上,而保持氮化矽的完全有效性。然而,一些問題繼續存在。因為沒有塗層之氧化,塗層仍然呈粉末,且當將液體矽裝填入坩堝中時,容易被損壞。
因此,需要提供不呈現出上述問題之坩堝,其包括較強之塗層(避免剝離和剝落),具有改良之機械耐磨性,製造快速且價廉,同時防止熔融矽與坩堝間之化學反應並維持以氧含量計之另外必要條件。
現已發現此等問題可使用用於矽結晶之坩堝予以解決;此坩堝包括:a)基體,其包括界定內部容積之底面和側壁;b)面對內部容積之側壁表面上的以氮化矽為主之保護塗層,該塗層包括80至95重量%之氮化矽及5至20重量%之低溫礦物黏結劑,總氧含量範圍自5至15重量%。依據本發明,該低溫礦物黏結劑係選自由下列所構成之群組,- 包含矽化學為主之有機金屬化合物,諸如矽氧烷、原矽酸四乙酯、四乙氧基矽烷、聚二甲基矽烷或其組合之黏結劑;- 包含聚矽氧油、矽氧烷、氯矽烷或其組合之矽石系之黏結劑;包含亞微米粒子及/或適於形成懸浮液之矽石奈米粒子,諸如矽石膠體之黏結劑。該低溫黏結劑較佳為以矽石為主之黏結劑。亦可使用氧氮化矽粉末而較佳為氮化矽與氧氮化矽粉末的組合。該氧氮化矽粉末可為循環之氧氮化物或水活化之氧氮化物。本發明的一個不可忽視之優點即:氮化矽粉末中的含量再也不重要且可考慮使用包含定量的氧之粉末作為例如循環之粉末。氮化矽粉末的結晶相可為α或β。
按低溫度黏結劑意指在低於氮化矽之氧化所需要之溫度的溫度時,創造鍵之黏結劑。較佳,該鍵係在低於800℃
之溫度時被創造,更佳係低於500℃。
按礦物黏結劑意指包含礦物基之黏結劑,其殘基經常產生連同碳或不連同碳之礦物。相對地,有機黏結劑例如(如羧甲基纖維素)(CMC)、膠、界面活性劑產生僅是碳之殘渣。黏結劑的高反應性係由礦物基予以部分地顯示出。
氮化矽或氧氮化矽粉末的粒度測定通常是亞微米,粒子大小1μm。然而,亦可使用包含不同粒子大小之氮化物粉末的摻合物,且顯著地包括包含2至50μm間之較粗粒子或粒,較佳為2至5μm之間。選擇摻合物以便改良一或數種特性。該摻合物可改進懸浮液的穩定性及/或進一步增加塗層的黏著至坩堝上。根據本發明,如果另外之塗層存在於氮化物塗層的下面及/或頂上,摻合物亦可促進不同塗層間之黏著。其他塗層例如可為含矽石之塗層如專利申請案WO2005/106084及同在申請中之申請案PCT/EP2006/006347等中所述。通常相對於亞微米粒子,較粗粒子的數量構成在20至50重量%之間。較粗之氮化矽粉末價廉,引入此粉末亦降低塗層的成本。
基於應用,保護塗層可具有50μm至500μm的厚度,較佳為200至500μm。為了避免任何污染,保護塗層應具有極高純度且附有超低碳含量甚為重要。
此種新穎技術係基於使用有限且受控制數量的氧在塗層中。將氧連同低溫礦物黏結劑(溶膠凝膠、有機金屬、奈米粒子、微絮凝劑、不互溶溶液、微乳液、氧化物)而引入。創造一極低溫度黏結相遍及塗層,增加保護塗層的機械
耐磨性,同時保持氮化矽的所需要之性質。大為減少塗層剝離和剝落之虞。
選擇添加劑和數量以便獲得範圍自5至15重量%之全部氧含量,最佳為8至12重量%。低於5%之全部氧含量不能產生充分之黏結相而導致塗層的低機械耐磨性。當氧的含量太高時,存在看上文所解釋之污染的問題。
創造鍵之加熱溫度係低於使氮化矽氧化時所需要之溫度。該加熱之溫度係低於800℃,較佳低於500℃。此種方式,氧的數量經由加成經測定數量的低溫礦物黏結劑予以完全控制。沒有進一步之氧化反應可變更氧含量。
鍵分散體中之氧對經由氮化矽氧化所產生之氧正造成差別。黏結系統與氮化物粉末間之低內聚力容許保持氮化物的充分有效性作為非潤濕劑。環繞著顆粒創造化學鍵且在其周圍上氮化矽的顆粒未被氧化成為SiO2
。此效應經由化學設定所創造之鍵所需要之低溫稠化予以加強,代替氧化的典型熱反應。本發明的塗層容許經由充分控制黏結系統的目的來增加塗層之機械抗性,同時保持氮化矽顆粒的充分有效性。
因為根據本發明,沒有關於塗層之剝離或剝落的問題,所以在到達使用者設施之前,可將它製備。
本發明的另外目的是用來塗覆用於矽結晶之坩堝之組成物,其反應80至95重量%的氮化矽及5至20重量%的低溫礦物黏結劑,全部氧含量係高於5重量%。該組成物可經由不同方法來施加。一種較佳方法中,係將該組成物
與液相混合而形成懸浮液以便施加至坩堝上。
本發明的另外目的是用於製造包含根據本發明之保護塗層之坩堝的方法;該方法包括下列步驟:a)提供包括界定內部容積之底面和側壁之基體b)施加保護塗層,其包括80至95重量%的氮化矽和5至20重量%的低溫礦物黏結劑,在面對內部容積之側壁的表面上;總氧含量係高於5重量%。依據本發明,該低溫礦物黏結劑係選自由下列所構成之群組,- 包含矽化學為主之有機金屬化合物,諸如矽氧烷、原矽酸四乙酯、四乙氧基矽烷、聚二甲基矽烷或其組合之黏結劑;- 包含聚矽氧油、矽氧烷、氯矽烷或其組合之矽石系之黏結劑;包含亞微米粒子及/或適於形成懸浮液之矽石奈米粒子,諸如矽石膠體之黏結劑。
通常,將表面層經由噴霧或刷塗在水中或在溶劑中來施加,較佳係由在包含適當數量的水之水溶性系統中之噴霧來施加以容許形成整個組成物的懸浮液。
在根據本發明方法的較佳實施例中,施加塗層的步驟後,接著在一種溫度下之加熱步驟(c)並歷一段持續時間以便適當煅燒存在於塗層中之大體上所有有機化合物及創造鍵。較佳實施例中,加熱之溫度保持在氮化矽的氧化之溫度下。此種方式,將塗層中之氧含量保持在控制下。氮化矽的氧化之溫度可基於塗層組成變更,但是通常是約800℃
。加熱已塗覆之坩堝亦可在客戶場所實行。亦可能在運送至客戶之前,實行預熱及在客戶場所,最後或進一步加熱。
本發明現在參照所包括之圖予以敘述,其僅用來舉例說明本發明並無意欲限制本發明之範圍。第1圖顯示根據本發明之坩堝的剖面。
該圖上,坩堝以參考數字1指示。此坩堝包括一個基體2,其包含界定用於矽結晶之內部容積之底面21和側壁22。該坩堝包含一保護層3,其由80至95重量%之氮化矽和5至20重量%之本發明的低溫礦物黏結劑構成,在面對內部容積之側壁22的表面上,總氧含量係高於5重量%。
本發明現在將經由根據本發明之實例和比較實例予以舉例說明。施加塗層在基體上之程序可以不同方式予以實現。組成係基於所選擇之方法。
第一較佳方法(反應層)包括下列步驟:- 將氮化矽粉末與基於矽化學之有機金屬化合物混合,其較佳係選自下列所構成之族群:矽氧烷、原矽酸四乙酯、四乙氧基矽烷、聚二甲基矽烷或其組合(有機金屬化合物其本身係熟知且市場上可供應);- 經由來自該族的氯化銨、氨、硝酸溶液之反應液體或適合於此程序之任何其他反應液體,噴灑塗層至坩堝上;- 在低於500℃之溫度時加熱已塗覆之坩堝以便穩定
化該塗層。
第二較佳方法(黏結劑溶液)包括下列步驟:- 將氮化矽粉末與以矽石為主之黏結劑混合,此黏結劑較佳係選自下列所構成之族群:聚矽氧油、矽氧烷、氯矽烷或其組合;- 經由來自該族的酸(氫氯酸、硝酸、矽酸、四氯化矽或適合此程序之任何其他適當酸)之反應液體來噴灑該塗層作為中和(作用)以便關於胺基-有機金屬化合物之鹼水解;- 在低於500℃之溫度時加熱已塗覆之坩堝來移除反應液體。
另外實施例中,該噴灑步驟使用基於氨蒸氣之反應或酸解系統之溶液予以實施。
第三較佳方法(飽和溶液和沉澱)包括下列步驟:
- 將氮化矽粉末與適應於形成懸浮液之矽石的亞微米粒子(<10-6
)及/或奈米粒子混合,較佳為膠體矽石;
- 透過熱反應、蒸氣反應、或使用適當中和化學品來形成酸鹼、醇或pH反應、甚至化學直接反應來沉澱所製備之混合物在坩堝表面上。
- 在低於500℃之溫度時,加熱已塗覆之坩堝,較佳在使用之前。
三種方法的塗層組成物的實例顯示於表1中。
較佳之實例是以膠態矽石為基礎之組成物,因為彼等容易處理且安全。組成物係以所使用之方法的功能,獲得標的之氧含量及機械耐磨性予以選擇。
下表中,各種塗層之黏著至坩堝上係依照ASTM(美國材料試驗學會)D4541使用POSITEST PULL-OFF黏著試驗器(來自DEFELSKO公司)予以測定。此試驗器經由測定在分離之前,塗層可承受之最大抗拉拉離力來評估塗層的黏著,即,使用液壓將特定試驗直徑的塗層拉動遠離其基體所需要之力。該力以壓力(KPa)予以表記。
坩堝的實例及相關性能示於表2中。
關於實例6,當將矽金屬注入坩堝中時,看到塗層的損壞。關於實例7,看到材料的相當大的損失,如美國專利第6,165,425號中所解釋。
1‧‧‧坩堝
2‧‧‧基體
3‧‧‧底面
21‧‧‧側壁
22‧‧‧保護層
第1圖顯示根據本發明之坩堝的剖面。
1...坩堝
2...基體
3...底面
21...側壁
22...保護層
Claims (16)
- 一種用於矽的結晶之坩堝(1),包括a)包括界定內部容積之底面(21)和側壁(22)之基體(2);b)面對內部容積之氮化矽為主之保護塗層(3);其特徵為:該保護塗層(3)包括80至95重量%之氮化矽,5至20重量%之低溫礦物黏結劑,該低溫礦物黏結劑係選自由下列所構成之群組,包含矽化學為主之有機金屬化合物之黏結劑;包含聚矽氧油、矽氧烷、氯矽烷或其組合之矽石系之黏結劑;包含亞微米粒子及/或適於形成懸浮液之矽石奈米粒子之黏結劑;總氧含量範圍自5至15重量%。
- 如申請專利範圍第1項之坩堝,其中包含矽化學為主之有機金屬化合物之黏結劑係矽氧烷、原矽酸四乙酯、四乙氧基矽烷、聚二甲基矽烷或其組合。
- 如申請專利範圍第1項之坩堝,其中包含亞微米粒子及/或適於形成懸浮液之矽石奈米粒子之黏結劑係矽石膠體。
- 如申請專利範圍第1項之坩堝,其中總氧含量之範圍係自8至12重量%。
- 如申請專利範圍第1項之坩堝,其中氮化矽保護塗層(3) 之厚度為50μm至500μm之間。
- 如申請專利範圍第1或4項之坩堝,其中氮化矽保護塗層(3)之厚度為200至500μm之間。
- 如申請專利範圍第5項之坩堝,其中該氮化矽保護塗層包括粒子1μm。
- 如申請專利範圍第7項之坩堝,其中該氮化矽保護塗層亦包括較粗之粒子。
- 如申請專利範圍第8項之坩堝,其中該較粗之粒子為2至50μm之間。
- 如申請專利範圍第8項之坩堝,其中該較粗之粒子為2至5μm之間。
- 如申請專利範圍第9或10項之坩堝,其中該較粗之粒子的數量為20至50重量%。
- 一種用於製備矽結晶的坩堝(1)之方法,包括下列步驟:a)提供包括界定內部容積之底面(21)和側壁(22)之基體(2);及b)施加保護塗層(3),其包括80至95重量%的氮化矽和5至20重量%的低溫礦物黏結劑,該低溫礦物黏結劑係選自由下列所構成之群組,包含矽化學為主之有機金屬化合物之黏結劑;包含聚矽氧油、矽氧烷、氯矽烷或其組合之矽石系之黏結劑;包含亞微米粒子及/或適於形成懸浮液之矽石奈米粒子之黏結劑, 在面對內部容積之側壁(22)的表面上,總氧含量係高於5重量%。
- 如申請專利範圍第12項之方法,其中另外包括步驟c):在低於氮化矽的氧化溫度之溫度下,加熱經塗覆之坩堝。
- 如申請專利範圍第12項之方法,其中步驟b)係經由噴霧來進行。
- 如申請專利範圍第12項之方法,其中包含矽化學為主之有機金屬化合物之黏結劑係矽氧烷、原矽酸四乙酯、四乙氧基矽烷、聚二甲基矽烷或其組合。
- 如申請專利範圍第12項之方法,其中包含亞微米粒子及/或適於形成懸浮液之矽石奈米粒子之黏結劑係矽石膠體。
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UA89284C2 (ru) | 2010-01-11 |
JP2009510387A (ja) | 2009-03-12 |
CA2624887A1 (en) | 2007-04-12 |
DE602006008498D1 (de) | 2009-09-24 |
NO20082102L (no) | 2008-05-05 |
TW200720496A (en) | 2007-06-01 |
ZA200803754B (en) | 2009-09-30 |
RU2401889C2 (ru) | 2010-10-20 |
KR20080051144A (ko) | 2008-06-10 |
KR101212924B1 (ko) | 2012-12-14 |
US20080260608A1 (en) | 2008-10-23 |
PL1954856T3 (pl) | 2010-01-29 |
AU2006298957A1 (en) | 2007-04-12 |
JP4917607B2 (ja) | 2012-04-18 |
AU2006298957B2 (en) | 2010-06-03 |
ATE439461T1 (de) | 2009-08-15 |
WO2007039310A1 (en) | 2007-04-12 |
ES2327570T3 (es) | 2009-10-30 |
CA2624887C (en) | 2013-07-09 |
CN101278078A (zh) | 2008-10-01 |
EP1954856B1 (en) | 2009-08-12 |
US8298333B2 (en) | 2012-10-30 |
CN101278078B (zh) | 2011-01-19 |
BRPI0616485A2 (pt) | 2012-12-25 |
RU2008117093A (ru) | 2009-11-20 |
EP1954856A1 (en) | 2008-08-13 |
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