JP2015504408A - スート法に従って合成石英ガラスを製造する方法 - Google Patents
スート法に従って合成石英ガラスを製造する方法 Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 101
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- XMSXQFUHVRWGNA-UHFFFAOYSA-N Decamethylcyclopentasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 XMSXQFUHVRWGNA-UHFFFAOYSA-N 0.000 claims description 4
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/01413—Reactant delivery systems
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
- C03B19/1415—Reactant delivery systems
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/30—For glass precursor of non-standard type, e.g. solid SiH3F
- C03B2207/32—Non-halide
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/80—Feeding the burner or the burner-heated deposition site
- C03B2207/85—Feeding the burner or the burner-heated deposition site with vapour generated from liquid glass precursors, e.g. directly by heating the liquid
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- General Chemical & Material Sciences (AREA)
- Glass Melting And Manufacturing (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
Abstract
Description
(A)60質量%を上回るポリアルキルシロキサンD4を有する液状のSiO2供給材料(105)を準備する工程、
(B)該液状のSiO2供給材料(105)を気化させて、ガス状のSiO2供給蒸気(107)にする工程、
(C)該SiO2供給蒸気(107)をSiO2粒子に変換する工程、
(D)該SiO2粒子を、SiO2スート体(200)を形成させながら堆積面(160)に堆積させる工程、
(E)該SiO2スート体を、合成石英ガラスを形成させながらガラス化する工程、
を含む、該合成石英ガラスの製造法に関する。
商業用途の合成石英ガラスの製造のために、ケイ素含有の出発物質からCVD法(化学気相成長)において加水分解及び/又は酸化によってSiO2粒子が作り出されて、これらが担体上に堆積させられる。この場合、外側堆積法と内側堆積法とに区別され得る。外側堆積法の場合、回転する担体の外面にSiO2粒子が施与される。例として、いわゆるOVD法(外付け気相成長)、VAD法(気相軸付け堆積)又はPECVD法(プラズマ化学気相成長)が挙げられる。内側堆積法の公知の例として、MCVD法(内付け化学気相成長)があり、この場合、外部加熱された管の内壁にSiO2粒子が堆積させられる。
公知の蒸発システムの場合、気化されるべき液体が高温表面と接触させられる。高温表面は、殊に有機材料が供給される場合、例えば分解又は重合といった予測不能な変化をもたらしかねず、そのため、蒸気の組成がどの程度なお液体の組成に相当しているのかを容易には突き止めることができない。それにより、粒子形成プロセスにおける欠損及び不均質なスート堆積につながりかねないある特定の変動性及び非再現性がプロセス操作において生じる。これは、粒子形成プロセスにおいて、互いに高い化学的類似性を有する成分の実際の組成が問題になったときに特に目立ってくる。
この課題の解決のために、特許請求項1の特徴を有する方法を提案する。従属請求項には、それぞれ有利な別の発展形態を記載している。
の通りに計算される。
の通りに計算される)場合に好ましいと判明した。2種の更なるポリアルキルシロキサンD3とD5をSiO2供給材料の主成分D4に加えることによって、粒径分布の広がりが達成されることがわかった。
・ ヘキサメチルシクロトリシロキサン(D3):0.02質量%から1質量%の間の範囲の質量分率mD3
・ ジメチルシクロペンタシロキサン(D5):0.5質量%から5質量%の間の範囲の質量分率mD5。
・ ヘキサメチルシクロトリシロキサン(D3):0.02質量%から2質量%の間の範囲の質量分率mD3
・ ジメチルシクロペンタシロキサン(D5):0.5質量%から10質量%の間の範囲の質量分率mD5。
蒸発が、以下の工程:
・ SiO2供給材料を加熱する工程、
・ 加熱された該SiO2供給材料を膨張チャンバー内に導入し、そうして該SiO2供給材料の少なくとも第一の部分を圧力降下により気化させる工程
を含むことを特徴とするプロセスがもたらされる。
蒸発が、以下の工程:
・ SiO2供給材料を加熱する工程、
・ 加熱された該SiO2供給材料を膨張チャンバー内に導入する工程、
・ 該SiO2供給材料を、加熱された希釈剤と混ぜ、そうして該SiO2供給材料の少なくとも第二の部分を、露点を下げることにより気化させる工程
を含むことを特徴とするプロセスがもたらされる。
105 SiO2供給材料
107 SiO2供給蒸気
110 貯蔵槽/貯蔵容器
115 予熱装置
116 供給部
117 排出部
120 蒸発器/蒸発器システム
122 液体ポンプ
123 流量計
124 MFC(マスフローコントローラー)
125 膨張チャンバー/蒸発チャンバー
126 管
127 フローディストリビューター
128 噴霧ノズル
130 管
140 バーナー/火炎加水分解バーナー
141 バーナーブロック
142 140の動作
143 バーナー炎
145 供給管
148 SiO2スート
150 媒体管
151 貯蔵容器
152 希釈剤
160 堆積面/担体管
161 160の縦軸
200 スート体
Claims (10)
- 以下(A)〜(E)の工程段階:
(A)60質量%を上回るポリアルキルシロキサンD4を有する液状のSiO2供給材料(105)を準備する工程、
(B)該液状のSiO2供給材料(105)を気化させてガス状のSiO2供給蒸気(107)にする工程、
(C)該SiO2供給蒸気(107)を変換してSiO2粒子にする工程、
(D)該SiO2粒子を、SiO2スート体(200)が形成するように堆積面(160)に堆積させる工程、
(E)該SiO2スート体を、合成石英ガラスが形成するようにガラス化する工程、
を含む、合成石英ガラスの製造法において、
前記液状のSiO2供給材料(105)は、質量分率mD3を有するポリアルキルシロキサンD3より成る少なくとも1種の付加的な成分と、質量分率mD5を有するポリアルキルシロキサンD5より成る少なくとも1種の付加的な成分とを、0.01から1の間の範囲の質量比mD3/mD5で有し、かつ
前記の準備した液状のSiO2供給材料(105)を、該質量比mD3/mD5を維持しながら、かつ少なくとも99質量%で、前記ガス状のSiO2供給蒸気(107)に気化させることを特徴とする製造法。 - 前記比mD3/mD5が、0.1から0.5の範囲にあることを特徴とする、請求項1記載の方法。
- 前記付加的な成分D3及び/又は前記付加的な成分D5が、前記液状のSiO2供給材料(105)の全質量の0.5質量%から30質量%の間にあり、殊に前記質量分率mD3+mD5の総計が、1質量%から15質量%の間の範囲にあり、有利には1質量%から3質量%の間の範囲にあることを特徴とする、請求項1から3までのいずれか1項記載の方法。
- 前記付加的な成分が、ポリアルキルシクロシロキサン及び該ポリアルキルシクロシロキサンのそれぞれの線状同族体を、下記の量:
・ ヘキサメチルシクロトリシロキサン(D3):0.02質量%から1質量%の間の範囲の質量分率mD3、
・ デカメチルシクロペンタシロキサン(D5):0.5質量%から5質量%の間の範囲の質量分率mD5
で含むことを特徴とする、請求項1から4までのいずれか1項記載の方法。 - 前記蒸発が、以下の工程:
・ 前記SiO2供給材料(105)を加熱する工程、
・ 加熱された該SiO2供給材料(105)を膨張チャンバー(125)内に導入し、そうして該SiO2供給材料(105)の少なくとも第一の部分を圧力降下により気化させる工程
を含むことを特徴とする、請求項1から5までのいずれか1項記載の方法。 - 前記蒸発が、以下の工程:
・ 前記SiO2供給材料(105)を加熱する工程、
・ 加熱された該SiO2供給材料(105)を膨張チャンバー(125)内に導入する工程、
・ 該SiO2供給材料(105)を、加熱された希釈剤(152)と混ぜ、そうして該SiO2供給材料(105)の少なくとも第二の部分を、露点を下げることにより気化させる工程
を含むことを特徴とする、請求項1から6までのいずれか1項記載の方法。 - 前記SiO2供給材料(105)を、圧力降下及び/又は分圧を下げることにより、少なくとも99.95質量%、有利には少なくとも99.9995質量%で、前記SiO2供給蒸気(107)に変えることを特徴とする、請求項6又は7記載の方法。
- 前記膨張チャンバー(125)内への前記加熱されたSiO2供給材料(105)の導入が、前記SiO2供給材料(105)を液状で霧化して微細な液滴にする注入段階を含み、ここで、該液滴は5μm未満、好ましくは2μm未満の平均直径を有することを特徴とする、請求項1から8までのいずれか1項記載の方法。
- 光ファイバーを製造するための、請求項1から9までのいずれか1項記載の方法に従って製造された合成石英ガラスの使用。
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DE102011119341A DE102011119341A1 (de) | 2011-11-25 | 2011-11-25 | Verfahren zur Herstellung von synthetischem Quarzglas nach der Sootmethode |
US201161569151P | 2011-12-09 | 2011-12-09 | |
US61/569,151 | 2011-12-09 | ||
PCT/EP2012/073341 WO2013076193A1 (de) | 2011-11-25 | 2012-11-22 | Verfahren zur herstellung von synthetischem quarzglas nach der sootmethode |
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US20130133377A1 (en) | 2013-05-30 |
EP2782880A1 (de) | 2014-10-01 |
KR20140098174A (ko) | 2014-08-07 |
KR101569790B1 (ko) | 2015-11-19 |
CN103946170B (zh) | 2016-05-18 |
CN103946170A (zh) | 2014-07-23 |
DE102011119341A1 (de) | 2013-05-29 |
WO2013076193A1 (de) | 2013-05-30 |
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