JPH0283236A - Production of chalcogenide glass - Google Patents
Production of chalcogenide glassInfo
- Publication number
- JPH0283236A JPH0283236A JP23560388A JP23560388A JPH0283236A JP H0283236 A JPH0283236 A JP H0283236A JP 23560388 A JP23560388 A JP 23560388A JP 23560388 A JP23560388 A JP 23560388A JP H0283236 A JPH0283236 A JP H0283236A
- Authority
- JP
- Japan
- Prior art keywords
- alkyl
- chalcogenide glass
- hydrogen sulfide
- dry gel
- thiosilicate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000005387 chalcogenide glass Substances 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims abstract description 10
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 6
- -1 alkyl mercaptan Chemical compound 0.000 claims abstract description 6
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000005049 silicon tetrachloride Substances 0.000 claims abstract description 5
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 4
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 2
- 239000013307 optical fiber Substances 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 229910020343 SiS2 Inorganic materials 0.000 abstract description 2
- 239000004065 semiconductor Substances 0.000 abstract description 2
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 6
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000004770 chalcogenides Chemical class 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- KHDSWONFYIAAPE-UHFFFAOYSA-N silicon sulfide Chemical compound S=[Si]=S KHDSWONFYIAAPE-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/32—Non-oxide glass compositions, e.g. binary or ternary halides, sulfides or nitrides of germanium, selenium or tellurium
- C03C3/321—Chalcogenide glasses, e.g. containing S, Se, Te
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/006—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route
Abstract
Description
【発明の詳細な説明】
【産業上の利用分野】
本、発明はゾル−ゲル法によるカルコゲナイドガラスを
作製する製造方法に関する。
［従来の技術］
従来のカルコゲナイドガラスはＡｓｋ？Ｐ系のＡｓｓ
Ｓａ 、Ｐ２Ｓ５ 、やＡｓｔＳｅ３、Ｐｉ Ｓｅｚ
、Ａｓｓ Ｔｅａ 、Ｐｇ Ｔｅａであり、Ｓｉ系のも
のはなかった。また、通常に、カルコゲナイドガラスは
、ＣＶＤやＭＯＣＶＤプロセスによって製造しているた
め薄膜がほとんどである。
［発明が解決しようとする課題１
しかし、前述の従来技術では、薄膜の形成が主であるた
め、赤外線光ファイバーや各種の素子を形成するために
はバルク状のカルコゲナイドガラスが必要である。
そこで本発明はこのような問題点を解決するもので、そ
の目的とするところは、バルク状のカルコゲナイドガラ
スの製造方法を提供するところにある。
［課題を解決するための手段］
本発明のカルコゲナイドガラスの製造方法は、ＳｉＳ−
で示される硫化物を以下の工程で作製することを特徴と
する。
ａ）四塩化ケイ素とアルキルメルカプタンの反応により
下式で示されるアルキルチオシリケートとする工程。
Ｓｉ（ＳＲ）４ （ただし、Ｒはアルキル基を示す）
ｂ）アルキルチオシリケートをアルキルメルカプタンの
溜液にし硫化水素と反応させる工程。
Ｃ）重縮合反応を経て、アルギルメルカプタンと硫化水
素を留去しドライゲルとする工程。
ｄ）ドライプルを熱処理することでＳｉＳ２のカルコゲ
ナイドガラスとする工程。
［実 施 例１
市販の四塩化ケイ素１モルを二硫化炭素溶液にし、エチ
ルメルカプタン５モルを加＾よく撹拌した０反応終了後
、過剰のエチルメルカプタンと二硫化炭素を留去し、エ
チルチオシリケートとした０反応式は下式である。
Ｓ ｉ Ｃｒ２＜ ＋４Ｃｚ Ｈａ ５Ｈ−Ｉｓ ｉ
（ＳＣｚＨ５）４
次に、得られたエチルチオシリケートをエチルメルカプ
タンの溶液にし、硫化水素ガスを通じた。よく撹拌し反
応させ、ゾルとした。
このゾルはすぐにゲル化し、室温で、ドラフト中に置い
ておくとドライゲルが得られた。
ドライゲルをＮ２雰囲気中で５００℃まで加熱すると余
分な硫化水素ガスが抜け、最終的にはＳｉＳ、のカルコ
ゲナイドガラスになった。
［発明の効果］
以上述べたように、本発明によれば、アルキルチオシリ
ケートと硫化水素との反応によりゾルとし、ゲル死後ド
ライゲルとし、熱処理により硫化シリコンとすることに
より、以前では作製できなかったカルコゲナイドガラス
をバルク状等の任意の形状に作製できるという効果を有
する。
このようにして得られたカルコゲナイドガラスは、赤外
線透過光ファイバーや、超低損失光ファイバー、半導体
素子等へ応用でき、大きく貢献することになるであろう
。
以上
出願人 セイコーエプソン株式会社DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for producing chalcogenide glass by a sol-gel method. [Conventional technology] Is the conventional chalcogenide glass Ask? P-type Ass
Sa, P2S5, AstSe3, Pi Sez
, Ass Tea, and Pg Tea, and there were no Si-based ones. Further, chalcogenide glass is usually manufactured by a CVD or MOCVD process, so that most of it is a thin film. [Problem to be Solved by the Invention 1] However, since the above-mentioned prior art mainly involves the formation of thin films, bulk chalcogenide glass is required to form infrared optical fibers and various elements. SUMMARY OF THE INVENTION The present invention aims to solve these problems, and its purpose is to provide a method for producing bulk chalcogenide glass. [Means for Solving the Problems] The method for producing chalcogenide glass of the present invention includes SiS-
The sulfide represented by is produced by the following steps. a) A step of producing an alkylthiosilicate represented by the following formula by reacting silicon tetrachloride with an alkylmercaptan. Si(SR)4 (R represents an alkyl group) b) A step of converting alkylthiosilicate into a reservoir of alkylmercaptan and reacting it with hydrogen sulfide. C) A step of distilling off argyl mercaptan and hydrogen sulfide to form a dry gel through a polycondensation reaction. d) A step of heat-treating the dry pull to form SiS2 chalcogenide glass. [Example 1] 1 mol of commercially available silicon tetrachloride was made into a carbon disulfide solution, 5 mol of ethyl mercaptan was added and stirred well. After the reaction was completed, excess ethyl mercaptan and carbon disulfide were distilled off to form ethyl thiosilicate. The zero reaction formula is the following formula. S i Cr2< +4Cz Ha 5H-Is i
(SCzH5)4 Next, the obtained ethyl thiosilicate was made into a solution of ethyl mercaptan, and hydrogen sulfide gas was passed through the solution. The mixture was stirred thoroughly and reacted to form a sol. This sol immediately gelled and a dry gel was obtained when left in a fume hood at room temperature. When the dry gel was heated to 500° C. in an N2 atmosphere, excess hydrogen sulfide gas was released, and it finally became a chalcogenide glass of SiS. [Effects of the Invention] As described above, according to the present invention, chalcogenide, which could not be produced previously, can be produced by making a sol by reacting an alkylthiosilicate with hydrogen sulfide, making a dry gel after gel death, and making silicon sulfide by heat treatment. This has the effect that glass can be made into any shape, such as a bulk shape. The chalcogenide glass thus obtained can be applied to infrared-transmitting optical fibers, ultra-low loss optical fibers, semiconductor devices, etc., and will make a significant contribution. Applicant: Seiko Epson Corporation
Claims (1)
とを特徴とするカルコゲナイドガラスの製造方法。 ａ）四塩化ケイ素とアルキルメルカプタンの反応により
下式で示されるアルキルチオシリケートとする工程。 Ｓｉ（ＳＲ）＿４（ただし、Ｒはアルキル基を示す） ｂ）アルキルチオシリケートをアルキルメルカプタンの
溶液にし硫化水素と反応させる工程。 ｃ）重縮合反応を経て、アルキルメルカプタンと硫化水
素を留去しドライゲルとする工程。 ｄ）ドライゲルを熱処理することでＳｉＳ＿２のカルコ
ゲナイドガラスとする工程。[Claims] A method for producing chalcogenide glass, characterized in that a sulfide represented by SiS_2 is produced in the following steps. a) A step of producing an alkylthiosilicate represented by the following formula by reacting silicon tetrachloride with an alkylmercaptan. Si(SR)_4 (R represents an alkyl group) b) A step in which alkylthiosilicate is made into a solution of alkylmercaptan and reacted with hydrogen sulfide. c) A step of distilling off alkyl mercaptan and hydrogen sulfide to form a dry gel through a polycondensation reaction. d) A step of heat-treating the dry gel to form SiS_2 chalcogenide glass.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23560388A JPH0283236A (en) | 1988-09-20 | 1988-09-20 | Production of chalcogenide glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23560388A JPH0283236A (en) | 1988-09-20 | 1988-09-20 | Production of chalcogenide glass |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0283236A true JPH0283236A (en) | 1990-03-23 |
Family
ID=16988455
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23560388A Pending JPH0283236A (en) | 1988-09-20 | 1988-09-20 | Production of chalcogenide glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0283236A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6145342A (en) * | 1998-01-30 | 2000-11-14 | The United States Of America As Represented By The Secretary Of The Navy | Catalyzed preparation of amorphous chalcogenides |
-
1988
- 1988-09-20 JP JP23560388A patent/JPH0283236A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6145342A (en) * | 1998-01-30 | 2000-11-14 | The United States Of America As Represented By The Secretary Of The Navy | Catalyzed preparation of amorphous chalcogenides |
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