JP4917607B2 - ケイ素の結晶化用の坩堝およびその製造方法 - Google Patents
ケイ素の結晶化用の坩堝およびその製造方法 Download PDFInfo
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Description
a)内部体積を規定する底部表面および側壁を含む基体を用意する工程、
b)80質量%〜95質量%の窒化ケイ素および5質量%〜20質量%の低温無機物結合剤を含み、内部体積に面する側壁の表面において総酸素含量が5質量%よりも高い保護被覆を適用する工程、を含む方法である。
−窒化ケイ素粉末と、好ましくはシロキサン、テトラエチルオルトシリケート、テトラエトキシシラン、ポリジメチルシラン、またはそれらの組み合わせ(有機金属化合物は市場で知られており、また入手できる)からなる群から選ばれたケイ素化合物系有機金属化合物を混合する工程、
−塩化アンモニウム、アンモニア、窒素を含む溶液または本方法に適切ないずれかの他の反応性液体、の群からの反応性液体によって坩堝上に被覆を噴霧する工程、
−被覆の安定化のために500℃より低い温度で被覆した坩堝を加熱する工程、を含んでいる。
−窒化ケイ素粉末を、好ましくはシリコーンオイル、シロキサン、クロロシランまたはそれらの組み合わせからなる群から選ばれるシリカ系結合剤と混合する工程、
−アミノ−有機金属化合物に関する塩基加水分解の中和として、酸(塩酸、硝酸、ケイ酸、四塩化ケイ素、またはこの方法に適切な他のいずれかの酸)の群からの反応性液体による被覆を噴霧する工程、
−反応液体を取り除くために500℃未満の温度で被覆された坩堝を加熱する工程、を含んでいる。他の実施態様では、噴霧工程は、酸加水分解系へのアンモニア蒸気または溶液を基にした反応を用いて実施される。
− 窒化ケイ素粉末を、懸濁液、好ましくはコロイド状シリカを形成するのに適合したシリカの1ミクロン以下の(<10−6)および/またはナノ粒子と混合する工程、
− 熱反応、蒸気反応、または適当な中和化学物質を用いた、酸塩基の、アルコールの、もしくはpH反応を形成する均等な化学直接反応を通した、調製された混合物の、坩堝表面への沈殿、
− 500℃未満の温度で被覆された坩堝を、好ましくは使用の前に、加熱する工程、を含んでいる。
TEOSはテトラエチルオルトシリケートを意味している。
好ましい例はコロイド状シリカ系組成物であり、それはそれらが取扱いが容易で、安全であるからである。組成物は、目的とする酸素含量および機械的耐磨耗性を得るために、用いられる方法の機能で選択される。
RBSNは、「反応で結合された窒化ケイ素」を意味し、また坩堝の知られた型式である。
6および7は比較例であり、また米国特許第6165425号明細書の実施例1および2に相当する。C1は、酸素含量が1.3%で、また低温無機物結合剤を含まない窒化ケイ素粉末を含んでいる。C2は、酸素含量が6%で、また低温無機物結合剤を含まない窒化ケイ素粉末を含んでいる。
例6に関しては、ケイ素金属を坩堝に充てんした時に被覆の損傷が認められた。例7に関しては、米国特許第6165425号明細書で説明されているように、物質の相当の損失が認められた。
Claims (11)
- a)内部体積を規定する底部表面(21)および側壁(22)を含む基体(2)、
b)内部体積に面する窒化ケイ素系保護被覆(3)を含むケイ素の結晶化のための坩堝(1)であって、保護被覆(3)が80質量%〜95質量%の窒化ケイ素および5質量%〜20質量%の低温無機物結合剤を含み、低温無機物結合剤が、以下の、
シロキサン、テトラエチルオルトシリケート、テトラエトキシシラン、ポリジメチルシラン、またはそれらの組み合わせからなる群から選ばれるケイ素化合物系有機金属化合物を含む結合剤、
シリコーンオイル、シロキサン、クロロシランまたはそれらの組み合わせを含むシリカ系結合剤、および、
懸濁液を形成するためにシリカの1ミクロン以下の粒子を含む結合剤、からなる群から選ばれ、総酸素含量が5質量%〜15質量%の範囲にあることを特徴とする坩堝。 - 総酸素含量が8質量%〜12質量%の範囲であることを特徴とする請求項1記載の坩堝。
- 窒化ケイ素保護被覆(3)が50μm〜500μmの範囲の厚さを有することを特徴とする請求項1または2記載の坩堝。
- 窒化ケイ素保護被覆が、1μm以下の粒子を含むことを特徴とする請求項1〜3のいずれか1項記載の坩堝。
- 窒化ケイ素保護被覆が、1μmよりもより粗い粒子を更に含むことを特徴とする請求項4記載の坩堝。
- より粗い粒子が2μm〜50μmの範囲を含むことを特徴とする請求項5記載の坩堝。
- より粗い粒子の量が20質量%〜50質量%であることを特徴とする請求項5または6記載の坩堝。
- ケイ素の結晶化のための坩堝(1)を調製する方法であって、
a)内部体積を規定する底部表面(21)および側壁(22)を含む基体(2)を用意する工程、
b)80質量%〜95質量%の窒化ケイ素および5質量%〜20質量%の低温無機物結合剤を含み、低温無機物結合剤が、以下の、
シロキサン、テトラエチルオルトシリケート、テトラエトキシシラン、ポリジメチルシラン、またはそれらの組み合わせからなる群から選ばれるケイ素化合物系有機金属化合物を含む結合剤、
シリコーンオイル、シロキサン、クロロシランまたはそれらの組み合わせを含むシリカ系結合剤、および、
懸濁液を形成するためにシリカの1ミクロン以下の粒子を含む結合剤、からなる群から選ばれ、
内部体積に面する側壁(22)の表面において総酸素含量が5質量%よりも高い保護被覆(3)を適用する工程、を含む方法。 - c)被覆した坩堝を、窒化ケイ素の酸化の温度よりも低い温度で加熱する工程、を更に含むことを特徴とする請求項8記載の方法。
- 工程b)が噴霧によって行われることを特徴とする請求項8または9記載の方法。
- 請求項9記載の方法によって得られるケイ素の結晶化のための坩堝。
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Application Number | Priority Date | Filing Date | Title |
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EP05447224 | 2005-10-06 | ||
EP05447224.6 | 2005-10-06 | ||
PCT/EP2006/009671 WO2007039310A1 (en) | 2005-10-06 | 2006-10-06 | Crucible for the crystallization of silicon and process for making the same |
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JP2009510387A JP2009510387A (ja) | 2009-03-12 |
JP2009510387A5 JP2009510387A5 (ja) | 2009-08-20 |
JP4917607B2 true JP4917607B2 (ja) | 2012-04-18 |
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US (1) | US8298333B2 (ja) |
EP (1) | EP1954856B1 (ja) |
JP (1) | JP4917607B2 (ja) |
KR (1) | KR101212924B1 (ja) |
CN (1) | CN101278078B (ja) |
AT (1) | ATE439461T1 (ja) |
AU (1) | AU2006298957B2 (ja) |
BR (1) | BRPI0616485A2 (ja) |
CA (1) | CA2624887C (ja) |
DE (1) | DE602006008498D1 (ja) |
ES (1) | ES2327570T3 (ja) |
NO (1) | NO20082102L (ja) |
PL (1) | PL1954856T3 (ja) |
RU (1) | RU2401889C2 (ja) |
TW (1) | TWI400369B (ja) |
UA (1) | UA89284C2 (ja) |
WO (1) | WO2007039310A1 (ja) |
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KR101212924B1 (ko) | 2012-12-14 |
RU2008117093A (ru) | 2009-11-20 |
AU2006298957B2 (en) | 2010-06-03 |
ES2327570T3 (es) | 2009-10-30 |
NO20082102L (no) | 2008-05-05 |
US20080260608A1 (en) | 2008-10-23 |
AU2006298957A1 (en) | 2007-04-12 |
KR20080051144A (ko) | 2008-06-10 |
CN101278078A (zh) | 2008-10-01 |
ZA200803754B (en) | 2009-09-30 |
JP2009510387A (ja) | 2009-03-12 |
BRPI0616485A2 (pt) | 2012-12-25 |
US8298333B2 (en) | 2012-10-30 |
EP1954856A1 (en) | 2008-08-13 |
RU2401889C2 (ru) | 2010-10-20 |
TW200720496A (en) | 2007-06-01 |
EP1954856B1 (en) | 2009-08-12 |
DE602006008498D1 (de) | 2009-09-24 |
TWI400369B (zh) | 2013-07-01 |
CN101278078B (zh) | 2011-01-19 |
CA2624887C (en) | 2013-07-09 |
WO2007039310A1 (en) | 2007-04-12 |
CA2624887A1 (en) | 2007-04-12 |
UA89284C2 (ru) | 2010-01-11 |
ATE439461T1 (de) | 2009-08-15 |
PL1954856T3 (pl) | 2010-01-29 |
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