JP4497482B2 - デバイスへの酸素および水分の浸透を防ぐ方法 - Google Patents
デバイスへの酸素および水分の浸透を防ぐ方法 Download PDFInfo
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims description 28
- 239000001301 oxygen Substances 0.000 title claims description 28
- 229910052760 oxygen Inorganic materials 0.000 title claims description 28
- 230000000149 penetrating effect Effects 0.000 title claims description 4
- QUBMWJKTLKIJNN-UHFFFAOYSA-B tin(4+);tetraphosphate Chemical compound [Sn+4].[Sn+4].[Sn+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QUBMWJKTLKIJNN-UHFFFAOYSA-B 0.000 claims description 126
- 238000010438 heat treatment Methods 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 32
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 22
- 229910052721 tungsten Inorganic materials 0.000 claims description 22
- 239000010937 tungsten Substances 0.000 claims description 22
- GEZAUFNYMZVOFV-UHFFFAOYSA-J 2-[(2-oxo-1,3,2$l^{5},4$l^{2}-dioxaphosphastannetan-2-yl)oxy]-1,3,2$l^{5},4$l^{2}-dioxaphosphastannetane 2-oxide Chemical compound [Sn+2].[Sn+2].[O-]P([O-])(=O)OP([O-])([O-])=O GEZAUFNYMZVOFV-UHFFFAOYSA-J 0.000 claims description 21
- 230000008021 deposition Effects 0.000 claims description 17
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- 239000000203 mixture Substances 0.000 claims description 12
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 8
- 229910001887 tin oxide Inorganic materials 0.000 claims description 8
- 230000005693 optoelectronics Effects 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 5
- XBZLJCFBSXPJBL-UHFFFAOYSA-J dihydrogen phosphate;tin(4+) Chemical compound [Sn+4].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O XBZLJCFBSXPJBL-UHFFFAOYSA-J 0.000 claims description 3
- LRGKLCMGBJZMTB-UHFFFAOYSA-J hydrogen phosphate;tin(4+) Chemical compound [Sn+4].OP([O-])([O-])=O.OP([O-])([O-])=O LRGKLCMGBJZMTB-UHFFFAOYSA-J 0.000 claims description 3
- 150000002822 niobium compounds Chemical class 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 description 87
- 239000010410 layer Substances 0.000 description 54
- 239000007858 starting material Substances 0.000 description 50
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- 238000012360 testing method Methods 0.000 description 16
- 239000011575 calcium Substances 0.000 description 14
- 229910052791 calcium Inorganic materials 0.000 description 14
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 13
- 229910052718 tin Inorganic materials 0.000 description 10
- 230000009477 glass transition Effects 0.000 description 9
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 8
- 239000011521 glass Substances 0.000 description 7
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
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- 229910052758 niobium Inorganic materials 0.000 description 3
- 239000010955 niobium Substances 0.000 description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 3
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
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- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
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- 229910052731 fluorine Inorganic materials 0.000 description 2
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- -1 for example Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
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- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- RYNDRPIGKFQDLD-UHFFFAOYSA-N 2-(methylamino)-1h-imidazole-4,5-dione Chemical compound CNC1=NC(=O)C(=O)N1 RYNDRPIGKFQDLD-UHFFFAOYSA-N 0.000 description 1
- RICKKZXCGCSLIU-UHFFFAOYSA-N 2-[2-[carboxymethyl-[[3-hydroxy-5-(hydroxymethyl)-2-methylpyridin-4-yl]methyl]amino]ethyl-[[3-hydroxy-5-(hydroxymethyl)-2-methylpyridin-4-yl]methyl]amino]acetic acid Chemical compound CC1=NC=C(CO)C(CN(CCN(CC(O)=O)CC=2C(=C(C)N=CC=2CO)O)CC(O)=O)=C1O RICKKZXCGCSLIU-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
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- 239000011248 coating agent Substances 0.000 description 1
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- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
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- 239000010408 film Substances 0.000 description 1
- 238000005247 gettering Methods 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
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- 239000011368 organic material Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000006187 pill Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
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Description
本発明のデバイスは、デバイスの少なくとも一部分が酸素および/または水分に対して敏感である任意のデバイス、例えば、有機発光ダイオード(「OLED」)、ポリマー発光ダイオード(「PLED」)、または薄膜トランジスタなどの有機電子素子;薄膜センサ;光スイッチまたはエバネッセント導波路センサなどの光電子素子;光起電力素子;食品容器;または医薬品容器であって差し支えない。
本発明において、低液相線温度無機材料の、低ガラス転移温度などの物理的性質により、気密シールの形成が促進される。本発明のある態様において、リン酸スズ低液相線温度無機出発材料、またはLLT出発材料は、デバイスの少なくとも一部分の上に堆積させることができ、堆積された材料は、そのデバイスの内部層を熱で損傷せずに、細孔のないまたは実質的に細孔のないバリア層を得るために比較的低温で熱処理される。堆積され熱処理された低液相線温度無機材料は、様々なデバイス上のバリア層として使用できることを認識すべきである。
本発明において、リン酸スズLLT出発材料は、熱蒸発などの蒸発プロセスによって、デバイスの少なくとも一部分の上に堆積させることができる。本発明の蒸発および堆積工程は、任意の特定の設備または幾何学的配置に制限されるものではない。その蒸発および堆積工程は、別々の工程または組合せ工程と称しても差し支えないことに留意すべきである。一旦、リン酸スズLLT出発材料が気化されたら、蒸発した材料は一般に、抵抗加熱素子に近接して位置する表面に堆積される。一般に用いられる蒸発システムは、例えば、約10-8から約10-5トルの圧力の真空下で動作し、抵抗加熱素子に電流を提供するためのリードが備え付けられている。蒸発は、実質的に酸素と水分が含まれない条件が、蒸発、堆積、および封止プロセス中ずっと維持されていることを確実にするために、不活性雰囲気中で行って差し支えない。被覆すべきデバイスの性質により要求されない限り、堆積および/または熱処理環境は、酸素と水分が完全に含まれない必要はないが、その環境は実質的に酸素と水分を含まないまたは実質的に含まなくて差し支えない。ボート、リボン、または坩堝を含む、様々な抵抗加熱素子を用いて差し支えない。一般的な蒸発プロセスにおいて、リン酸スズLLT出発材料を抵抗加熱素子と接触して配置することができる。その後、一般に、80から180ワットの範囲の電流を抵抗加熱素子に通して、リン酸スズLLT出発材料を気化させる。特定の材料を蒸発させるのに要するパワーは、材料自体、圧力、および加熱素子の抵抗に応じて、様々であろう。特定の堆積の速度と時間は、材料、堆積条件、および堆積される層の所望の厚さに応じて、様々であろう。蒸発システムは、例えば、米国ペンシルバニア州、クレアトン所在のカート・ジェイ・レスカー(Kurt J. Lesker)社から市販されている。当業者には、リン酸スズLLT材料を堆積させるのに必要な動作条件および蒸発システムを容易に選択できよう。
堆積されたリン酸スズLLT材料は必要に応じてさらに酸化スズを含んで差し支えない。ある態様において、堆積されたリン酸スズLLT材料は、約60から約85モルパーセントの酸化スズを含んで差し支えない。上述したように、堆積されたリン酸スズLLT材料の特定の化学構造および化学量論は、リン酸スズLLT出発材料のものとは異なっていて差し支えない。堆積されたリン酸スズLLT材料中の酸化スズの存在は、酸化スズ材料のリン酸スズLLT出発材料への随意的な添加から、または堆積プロセス中に生じるまたはデバイス表面上で生じる化学的および/または化学量論的な変化から生じ得る。
熱処理またはアニール工程によって、リン酸スズLLT材料の堆積層中の欠陥および細孔を最小にして、気密シールすなわちリン酸スズLLTバリア層を形成することができる。ある態様において、熱処理されたリン酸スズLLTバリア層は、細孔を含まないまたは実質的に細孔を含まない。熱処理されたリン酸スズLLTバリア層中に残っている細孔の数および/またはサイズは、酸素と水分の浸透を防ぐのに十分に低いべきである。ある態様において、熱処理は真空下で行われる。別の態様において、熱処理工程は、不活性雰囲気中で行われる。熱処理工程は、堆積工程の直後に同じ系内で行っても、デバイス中への酸素と水分の侵入を防ぐために環境条件が維持されるという条件で、別の時間と場所で行っても差し支えない。
リン酸スズLLTバリア層の気密性は、リン酸スズLLTバリア層の酸素および/または水分に対する気密性を試験する様々な方法を用いて評価できる。ある態様において、リン酸スズLLTバリア層は、カルシウムパッチテストを用いて評価することができ、ここで、カルシウム薄膜を基板に堆積させる。次いで、リン酸スズLLTバリア層を形成し、リン酸スズLLTバリア層と基板との間でカルシウム薄膜を封止する。次いで、得られたデバイスに、選択された温度と湿度、例えば、85℃と85%の相対湿度での環境老化を施す。酸素および/または水分がリン酸スズLLTバリア層に浸透した場合、高反応性のカルシウム薄膜が反応して、容易に特定できる不透明白色の外皮が生成する。一般に、ディスプレイ産業において、85℃、85%の相対湿度の環境中に約1,000時間に亘りカルシウムパッチに耐えたことは、気密層が、少なくとも約5年に亘り酸素と水分の浸透を防げることを意味すると認識されている。
第1の具体例において、シリコンウェハー上にピロリン酸スズLLT材料を熱蒸発によって堆積させた。ピロリン酸スズのペレット(米国マサチューセッツ州、ワードヒル所在のアルファ・アイサー社)を、自家製のピル・プレス機で調製し、100℃のオーブン内に貯蔵した。ピロリン酸スズのペレットを3インチ×0.75インチ(約7.5cm×約1.9cm)のタングステン製ボート(米国カリフォルニア州、ロングビーチ所在のアール・ディー・マティス(R.D. Mathis)社から得られるS7−.010W)内に入れ、蒸発システムの2本の銅線の間に取り付けた。この蒸発システムの真空チャンバを10-6と10-5トルの間の到達圧力まで排気し、シリコンウェハーを蒸発噴出路から外して配置した。出力を約20ワットに調節し、約30分間保持して、ピロリン酸スズおよびタングステンボートを反応させた。電流を印加したときに、15Å毎秒ほど高い安定な堆積速度が達成された。
第2の具体例において、ピロリン酸スズLLT材料をカルシウムパッチテストデバイス上に堆積させた。ピロリン酸スズのペレットは、具体例1におけるように調製し、蒸発させた。出力は20ワットに調節し、30分間保持して、ピロリン酸スズおよびタングステンボートを反応させた。次いで、出力を増加させて、タングステンボートに80から125ワットを供給した。蒸発中、残留ガス分析器により真空チャンバの環境をモニタした。図3に示されているように、蒸発中に比較的低濃度のバックグラウンドガスが存在した。初期期間後、出力を調節して、10と15Å毎秒の間の安定な堆積速度を達成し、このとき、テストデバイスは、LLT材料を堆積するために、蒸発噴出路内に位置していた。
第3の具体例において、具体例2におけるようなカルシウムパッチテストデバイスを調製し、LLT材料で封止した。この具体例において、蒸発前に、ピロリン酸スズ出発材料に1モルパーセントの五酸化ニオブを加えた。具体例2の堆積速度と同様の堆積速度が達成された。次いで、テストデバイスに、具体例6に記載するような加速老化試験を施した。その結果が表1に詳述されている。
さらに別の具体例において、カルシウムパッチテストデバイスを調製した。そのテストデバイスは、コーニング1737ガラス基板(約1ミリメートル厚および2.5インチ(約6.25cm)の正方形)からなり、その上に、100ナノメートル厚のカルシウム薄膜(約1インチ×約0.5インチ(約2.5cm×約1.25cm))を堆積し、その上に、200ナノメートル厚のアルミニウム層(約1インチ×約0.5インチ(約2.5cm×約1.25cm))を堆積した。このテストデバイスを真空堆積チャンバ内の可動台に固定した。
20 光電子層
30 リン酸スズLLTバリア層
40 基板
Claims (7)
- デバイスへの酸素および水分の浸透を防ぐ方法であって、
a. リン酸スズ低液相線温度無機材料を、タングステンを含む抵抗加熱素子を用いて蒸発させて前記デバイスの少なくとも封止すべき部分の上に堆積させて、堆積低液相線温度無機材料を形成する工程、および
b. 前記堆積低液相線温度無機材料を、酸素と水分を含まない環境中で熱処理して、前記デバイスの前記少なくとも封止すべき部分に気密シールを形成する工程、
を有してなることを特徴とする方法。 - 前記リン酸スズ低液相線温度無機材料が、メタリン酸スズ、オルトリン酸水素スズ、オルトリン酸二水素スズ、ピロリン酸スズ、またはそれらの混合物を含むことを特徴とする請求項1記載の方法。
- 前記リン酸スズ低液相線温度無機材料が酸化スズをさらに含むことを特徴とする請求項1記載の方法。
- 前記リン酸スズ低液相線温度無機材料が60モルパーセントから85モルパーセントのSnOを含むことを特徴とする請求項1記載の方法。
- 前記リン酸スズ低液相線温度無機材料がフッ素を含まないかあるいは含んでいても1質量%未満であることを特徴とする請求項1記載の方法。
- 前記リン酸スズ低液相線温度無機材料がニオブ化合物をさらに含むことを特徴とする請求項1記載の方法。
- 前記デバイスが、
有機電子素子、
薄膜センサ、
光電子素子、
光起電力素子、
食品容器、または
医薬品容器、
の内の少なくとも1つを含むことを特徴とする請求項1から6いずれか1項記載の方法。
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- 2007-08-04 EP EP07015335.8A patent/EP1892775B1/en not_active Not-in-force
- 2007-08-16 JP JP2007212096A patent/JP4497482B2/ja not_active Expired - Fee Related
- 2007-08-22 KR KR1020070084492A patent/KR100903245B1/ko active IP Right Grant
- 2007-08-22 TW TW096131180A patent/TWI359518B/zh not_active IP Right Cessation
- 2007-08-24 CN CN2007101418005A patent/CN101130861B/zh not_active Expired - Fee Related
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Also Published As
Publication number | Publication date |
---|---|
TW200830597A (en) | 2008-07-16 |
EP1892775A3 (en) | 2009-11-25 |
CN101130861A (zh) | 2008-02-27 |
CN101130861B (zh) | 2010-11-03 |
US20090324830A1 (en) | 2009-12-31 |
US20080048178A1 (en) | 2008-02-28 |
EP2955767B1 (en) | 2019-03-06 |
TWI359518B (en) | 2012-03-01 |
KR100903245B1 (ko) | 2009-06-17 |
EP1892775A2 (en) | 2008-02-27 |
US7749811B2 (en) | 2010-07-06 |
JP2008053715A (ja) | 2008-03-06 |
KR20080018817A (ko) | 2008-02-28 |
EP2955767A1 (en) | 2015-12-16 |
EP1892775B1 (en) | 2015-10-07 |
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