JP2023521697A - 勾配ガラス状セラミック構造体及びそのボトムアップ製造方法 - Google Patents
勾配ガラス状セラミック構造体及びそのボトムアップ製造方法 Download PDFInfo
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- QYBKVVRRGQSGDC-UHFFFAOYSA-N triethyl methyl silicate Chemical compound CCO[Si](OC)(OCC)OCC QYBKVVRRGQSGDC-UHFFFAOYSA-N 0.000 description 1
- XYJRNCYWTVGEEG-UHFFFAOYSA-N trimethoxy(2-methylpropyl)silane Chemical compound CO[Si](OC)(OC)CC(C)C XYJRNCYWTVGEEG-UHFFFAOYSA-N 0.000 description 1
- JCGDCINCKDQXDX-UHFFFAOYSA-N trimethoxy(2-trimethoxysilylethyl)silane Chemical compound CO[Si](OC)(OC)CC[Si](OC)(OC)OC JCGDCINCKDQXDX-UHFFFAOYSA-N 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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Abstract
Description
本出願は、その開示が参照により本明細書に組み込まれる、2020年4月6日出願の、同時係属中の米国仮特許出願第63,005,506号に対する優先権を主張する。
有機置換基のβ位で置換する好ましい可溶性で液体のホモポリマー及びコポリマーシルセスキオキサンとしては、ハロゲン、例えば2-クロロエチルシルセスキオキサン及び2-ブロモエチルシルセスキオキサン、エーテル、例えば2-メトキシエチルシルセスキオキサン並びにカルボキシレート、例えば2-アセトキシエチルシルセキオキサンが挙げられる。これらの材料は、連続構造と考えることができるベースポリマーと見なすことができ、連続構造は、セラミック変換時に1種又は複数の共反応成分を変化させて勾配を形成することによって変性される。
本明細書に記載のSiO2リッチ構造体を形成するための適切な有機官能性シラン類は、好ましくは有機官能性アルコキシシラン類である。SiO2リッチ構造体を調製する際に、1種、2種、又はそれ以上のこれらのシラン類を含めることは、本開示の範囲内である。適切なアルコキシシラン類は、概してトリアルコキシシランであるが、アルコキシ基がメトキシ基又はエトキシ基(低質量の揮発性副生成物をもたらす)であるジアルコキシシランも使用することができ、例えば、アルキル置換基(ジアルキルジアルコキシシラン、アルキルトリアルコキシシラン)を含有するものが挙げられる。好ましいアルコキシ基としては、メトキシ基及びエトキシ基が挙げられる。プロポキシ基及びイソプロポキシ基等の高級アルコキシ基を有するシラン類を利用することは、本開示の範囲内であるが、得られる膜はより割れを生じやすい。適切なアルキル基としては、1個の炭素原子(メチル)から20個超の炭素原子を有するものが挙げられる。メトキシ(ポリエチレンオキシ)基等で置換されたアルキル基についても、本開示の範囲内である。また、それらに限定されないが、フェニルトリメトキシシラン等の芳香族置換基を含有するシラン類を利用することは、本開示の範囲内である。好ましいアルコキシシラン類としては、以下に示すイソブチルトリエトキシシラン及びメトキシ(ポリエチレンオキシ)プロピルトリメトキシシランが挙げられる。
アルコキシシランを、1種又は複数の金属アルコキシド類に置き換えることも本開示の範囲内であり、金属アルコキシド類としては、それらに限定されないが、例えば酸化ゲルマニウム勾配を生成するためのゲルマニウムイソプロポキシド、酸化タンタル勾配を生成するためのタンタルエトキシド、酸化チタン勾配を生成するためのチタンn-ブトキシド、酸化ジルコニウム勾配を生成するためのジルコニウムn-プロポキシド、及び酸化ハフニウム勾配を生成するためのハフニウムn-ブトキシドが挙げられる。これらの金属酸化物の使用により、そのような元素を組み込んだSiO2リッチ構造体が得られ、他の特性の中でも、光学デバイス、例えばレンズ、導波路、及び光ファイバーに用途を有する屈折率の勾配が生成される。例示的な反応スキームを、以下のスキーム3に示す。
本開示において、SiO2リッチという用語は、複数のケイ素原子がそれぞれ4つの酸素原子に結合し、ケイ素原子の約50%以下が炭素原子に結合している材料を記載するために使用される。
<実施例1>
<実施例3(予言的)>
<実施例4(予言的)>
Claims (27)
- 勾配特性を有するSiO2リッチ構造体であって、電気陰性β置換基を有するシルセスキオキサン、及び少なくとも1種の有機官能性シランから形成される、SiO2リッチ構造体。
- 勾配疎水性/親水性特性を有する、請求項1に記載のSiO2リッチ構造体。
- シルセスキオキサンがβ位にハロゲン、エーテル、又はカルボキシレート官能基を有する、請求項1に記載のSiO2リッチ構造体。
- シルセスキオキサンが、2-アセトキシエチルシルセスキオキサンである、請求項3に記載のSiO2リッチ構造体。
- 少なくとも1種の有機官能性シランが、ジアルキルジアルコキシシラン又はアルキルトリアルコキシシランである、請求項1に記載のSiO2リッチ構造体。
- 少なくとも1種の有機官能性シランが、ジアルキルジメトキシシラン又はジアルキルジエトキシシランである、請求項5に記載のSiO2リッチ構造体。
- 少なくとも1種の有機官能性シランが、アルキルトリメトキシシラン又はアルキルトリエトキシシランである、請求項5に記載のSiO2リッチ構造体。
- 少なくとも1種の有機官能性シランが、メトキシ(ポリエチレンオキシ)プロピルトリメトキシシラン又はイソブチルトリエトキシシランである、請求項5に記載のSiO2リッチ構造体。
- 2-アセトキシエチルシルセスキオキサン、メトキシ(ポリエチレンオキシ)プロピルトリメトキシシラン、及びイソブチルトリエトキシシランから形成される、請求項1に記載のSiO2リッチ構造体。
- ゲルマニウム、タンタル、チタン、ジルコニウム及びハフニウムの酸化物からなる群から選択される少なくとも1種の金属酸化物の勾配濃度を有するSiO2リッチ構造体であって、対応する金属アルコキシド、及び電気陰性β置換基を有するシルセスキオキサンから形成される、SiO2リッチ構造体。
- 勾配屈折率を有する、請求項10に記載のSiO2リッチ構造体。
- 複数のケイ素原子が、それぞれ4個の酸素原子に結合しており、ケイ素原子の約50%以下が、炭素原子に結合している、請求項1に記載のSiO2リッチ構造体。
- セラミック膜である、請求項1に記載のSiO2リッチ構造体。
- セラミック膜が、約15~約500nmの厚さを有する、請求項13に記載のSiO2リッチ構造体。
- 勾配特性を有するSiO2リッチ構造体を形成する方法であって、電気陰性β置換基を有するシルセスキオキサンと、少なくとも1種の有機官能性シランと、場合により溶媒とを含むコーティング組成物を調製する工程と、基板に混合物をコーティングする工程と、コーティングされた基板に加熱及び/又はUV照射する工程とを含む、方法。
- コーティング組成物が、揮発性極性溶媒を含む、請求項15に記載の方法。
- コーティングが、スピンオン堆積、3Dプリンティング、マイクロコンタクトプリンティング、又は直接書き込みを含む、請求項15に記載の方法。
- 加熱及び/又はUV照射が、少なくとも約0.5%の相対湿度を含有する雰囲気中で実施される、請求項15に記載の方法。
- 加熱が、約150℃~約700℃で実施される、請求項15に記載の方法。
- コーティングする工程が、少なくとも1種の有機官能性シランの相対流量を調整する工程を含む、請求項15に記載の方法。
- コーティング組成物が、種々の量の少なくとも1種の有機官能性シランを含む、請求項15に記載の方法。
- 勾配特性を有するSiO2リッチ構造体を形成する方法であって、電気陰性β置換基を有するシルセスキオキサンと、少なくとも1種の金属アルコキシドと、場合により溶媒とを含むコーティング組成物を調製する工程と、基板に混合物をコーティングする工程と、コーティングされた基板に加熱及び/又はUV照射する工程とを含む、方法。
- 金属アルコキシドが、ゲルマニウムイソプロポキシド、タンタルエトキシド、チタンn-ブトキシド、ジルコニウムn-プロポキシド、及びハフニウムn-ブトキシドからなる群から選択される、請求項22に記載の方法。
- SiO2リッチ構造体が、勾配屈折率を有する、請求項22に記載の方法。
- SiO2リッチ構造体が、勾配金属酸化物濃度を有する、請求項22に記載の方法。
- コーティングする工程が、少なくとも1種の金属アルコキシドの相対流量を調整する工程を含む、請求項22に記載の方法。
- コーティング組成物が、種々の量の少なくとも1種の金属アルコキシドを含む、請求項22に記載の方法。
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PCT/US2021/025370 WO2021206999A2 (en) | 2020-04-06 | 2021-04-01 | Gradient glass-like ceramic structures and bottom-up fabrication method thereof |
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US4973526A (en) * | 1990-02-15 | 1990-11-27 | Dow Corning Corporation | Method of forming ceramic coatings and resulting articles |
US5283056A (en) | 1993-07-01 | 1994-02-01 | International Flavors & Fragrances Inc. | Transparent oil-in-water microemulsion flavor or fragrance concentrate, process for preparing same, mouthwash or perfume composition containing said transparent microemulsion concentrate, and process for preparing same |
US5320868A (en) * | 1993-09-13 | 1994-06-14 | Dow Corning Corporation | Method of forming SI-O containing coatings |
WO1997010282A1 (en) * | 1995-09-12 | 1997-03-20 | Gelest, Inc. | Beta-substituted organosilsesquioxanes and use thereof |
US6770726B1 (en) * | 1995-09-12 | 2004-08-03 | Gelest, Inc. | β-substituted organosilsesquioxane polymers |
US6927270B2 (en) * | 2001-06-27 | 2005-08-09 | Hybrid Plastics Llp | Process for the functionalization of polyhedral oligomeric silsesquioxanes |
KR100464198B1 (ko) * | 2002-04-18 | 2005-01-03 | (주)아이컴포넌트 | 디스플레이용 적층막 |
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US20090274974A1 (en) * | 2008-04-30 | 2009-11-05 | David Abdallah | Spin-on graded k silicon antireflective coating |
US8389663B2 (en) * | 2009-10-08 | 2013-03-05 | International Business Machines Corporation | Photo-patternable dielectric materials curable to porous dielectric materials, formulations, precursors and methods of use thereof |
US20130241390A1 (en) * | 2012-03-14 | 2013-09-19 | Peter Guschl | Metal-containing encapsulant compositions and methods |
US10494295B2 (en) * | 2015-02-04 | 2019-12-03 | Agency For Science, Technolofy And Research | Anti-reflection coating |
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KR20220163404A (ko) | 2022-12-09 |
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