JPS5819614B2 - Manufacturing method of glass fiber for optical communication - Google Patents
Manufacturing method of glass fiber for optical communicationInfo
- Publication number
- JPS5819614B2 JPS5819614B2 JP52092793A JP9279377A JPS5819614B2 JP S5819614 B2 JPS5819614 B2 JP S5819614B2 JP 52092793 A JP52092793 A JP 52092793A JP 9279377 A JP9279377 A JP 9279377A JP S5819614 B2 JPS5819614 B2 JP S5819614B2
- Authority
- JP
- Japan
- Prior art keywords
- glass
- glass fiber
- optical communication
- deterioration
- insulating film
- 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.)
- Expired
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Description
【発明の詳細な説明】
本発明はとくに耐候性を改善した光通信用ガラスファイ
バーの製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention particularly relates to a method for producing glass fiber for optical communication with improved weather resistance.
従来の光通信用ガラスファイバーは外周囲にプラスチッ
クの保護層を設けた構造になっている。Conventional glass fiber for optical communications has a structure with a protective layer of plastic around the outside.
しかしながら、このようなガラスファイバーは高温高湿
、或いは水中に長時間曝らすと劣化して機械的強度の低
下、光散乱損失の増大を招く欠点があった。However, such glass fibers deteriorate when exposed to high temperature, high humidity, or water for a long time, resulting in a decrease in mechanical strength and an increase in light scattering loss.
特に、多成分系ガラスの場合にはその中に含まれるアル
カリイオンが溶出し、ファイバーとプラスチック保護層
との界面に一種の圧力差（浸透圧）が生じ、この圧力差
により劣化が進行すること、及びアルカリイオンの溶出
に伴ないファイバーの表面層と内部との間にアルカリイ
オン量の差が生じ、これにより表面層と内部との膨張係
数が変動してファイバーが劣化し易くなること、等によ
り劣化が顕著となる。In particular, in the case of multi-component glass, the alkali ions contained therein are eluted, creating a type of pressure difference (osmotic pressure) at the interface between the fiber and the plastic protective layer, and this pressure difference accelerates deterioration. , and due to the elution of alkali ions, there is a difference in the amount of alkali ions between the surface layer and the inside of the fiber, which causes the coefficient of expansion between the surface layer and the inside to fluctuate, making the fiber susceptible to deterioration, etc. The deterioration becomes noticeable.
このようなことから、最近、三重ルツボを用いてガラス
ファイバーの紡糸と同時に、その外側に耐候性の高いガ
ラス層を被覆する方法（特開昭・５３−７５４１号）が
提案されている。For this reason, a method has recently been proposed in which a triple crucible is used to simultaneously spin glass fibers and coat the outside with a highly weather-resistant glass layer (Japanese Patent Laid-Open No. 53-7541).
しかしながら、この方法に用いる耐候性の高いガラスは
、内側のコア、クラッドのガラスに比して高温粘性が極
めて高いため、ファイバー化が困難となったり、外側の
ガラス層に対してファイバーが偏芯し易いなどの欠点が
ある。However, the weather-resistant glass used in this method has an extremely high viscosity at high temperatures compared to the inner core and cladding glasses, making it difficult to form into fibers and making the fibers eccentric to the outer glass layer. There are disadvantages such as being easy to use.
不発明は上記欠点を解消するためになされたもので、フ
ァイバー化を阻害することなく、ガラスファイバー素材
と外界雰囲気との反応を遮断してファイバー劣化を防止
した光通信用ガラスファイ；バーの製造方法を提供しよ
うとするものである。The invention was made in order to eliminate the above-mentioned drawbacks, and it is the manufacture of a glass fiber for optical communication that prevents fiber deterioration by blocking the reaction between the glass fiber material and the external atmosphere without inhibiting fiberization. It is intended to provide a method.
以下、本発明の詳細な説明する。The present invention will be explained in detail below.
まず、ガラス、例えば多成分系ガラスを二重ルツボによ
り紡糸してコア、クラッドからなるガラスファイバー素
材を形成する。First, glass, for example multi-component glass, is spun in a double crucible to form a glass fiber material consisting of a core and a cladding.
次いで紡糸直後の、ガラスファイバー素材にＳｉ、Ａｌ
、Ｐ、Ｂ。Next, Si and Al are applied to the glass fiber material immediately after spinning.
,P,B.
Ｔｉ、Ｇｅから選ばれる金属ガスを酸素含有ガス或いは
窒素系ガス（たとえばＮ２．ＮＨ２等）の存在下でＣＶ
Ｄ法により反応させてＳｉＯ２，Ａｌ２Ｏ３゜Ｓ ｉ３
Ｎ、、’ｒｉｏ２．硅リン酸ガラス、硅ホウ酸ガ；ラス
、アルミノ硅酸ガラス、及びアルミノホウ硅酸ガラス、
ゲルマノ硅酸ガラス、から選ばれる１種または２種以上
の絶縁膜を被着せしめて光通信用多成分系ガラスを造る
。A metal gas selected from Ti and Ge is subjected to CVD in the presence of an oxygen-containing gas or a nitrogen-based gas (for example, N2, NH2, etc.).
React by method D to form SiO2, Al2O3゜S i3
N,,'rio2. Silicophosphate glass, silicoborate glass; lath, aluminosilicate glass, and aluminoborosilicate glass;
A multi-component glass for optical communication is produced by depositing one or more insulating films selected from germanosilicate glass.
本発明に使用するガラス、例えば多成分系ガラ；スはコ
ア用と１．クラッド用と異なり、コアの屈折率がクラッ
ドの屈折率より大きくなるようにコア用、クラッド用の
多成分系ガラスを選定することが必要である。Glasses used in the present invention, such as multi-component glasses, are used for the core and 1. Unlike for the cladding, it is necessary to select multicomponent glasses for the core and cladding so that the refractive index of the core is greater than the refractive index of the cladding.
本発明に使用するガラス形成用金属ガスとしては、四水
素化硅素、ハロゲン化硅素（たとえば四塩化硅素）、ハ
ロゲン化アルミニウム（たとえば三塩化アルミニウム）
、水素化ニリン、ハロゲン。Examples of the glass-forming metal gas used in the present invention include silicon tetrahydride, silicon halide (e.g. silicon tetrachloride), and aluminum halide (e.g. aluminum trichloride).
, hydrogenated niline, halogen.
化リン、ハロゲン化ホウ素、ハロゲン化チタン等を挙げ
ることができ、場合によっては５ｉｎ２゜Ａ １２０３
．Ｐ２Ｏ５，Ｂ２Ｏ３，ＴｉＯ２を加熱分解して得た金
属ガス単体を用いてもよい。Examples include phosphorus chloride, boron halide, titanium halide, etc. In some cases, 5in2゜A 1203
．． A single metal gas obtained by thermally decomposing P2O5, B2O3, and TiO2 may be used.
本発明における絶縁膜の厚さは、通常１００〜１１００
０００λ程度にすれば充分である。The thickness of the insulating film in the present invention is usually 100 to 1100
A value of about 000λ is sufficient.
またこの絶縁膜として、とくに硅素ガス（例えばＳ ｉ
Ｈ４。In addition, as this insulating film, silicon gas (for example, Si
H4.
５ｉＣＰ４）とアンモニア（Ｎ２）とをＣＶＤ法により
反応、生成されたＳ ｉ３ Ｎ４ 、及び硅素ガスとリ
ンガス（例えばＰＯＣｌ２）と酸素含有ガス（例えば。5iCP4) and ammonia (N2) by the CVD method, and silicon gas, phosphorus gas (for example, POCl2), and oxygen-containing gas (for example,
０□あるいは０２＋Ｎ２）とをＣＶＤ法により反応生成
された硅リン酸ガラスはガラスファイバーの劣化防止効
果が顕著なため有益である。Silicophosphate glass produced by reacting with 0□ or 02+N2) by the CVD method is useful because it has a remarkable effect of preventing the deterioration of glass fibers.
しかして本発明によれば、紡糸直後のガラスファイバー
素材にＣＶＤ法によりＳｉＯ２，Ａｌ２Ｏ３，！Ｓ ｉ
３Ｎ４．Ｔ１０□、硅リン酸ガラス、硅ホウ酸ガラス、
アルミノ硅酸ガラス、及びアルミノホウ硅酸ガラス、ゲ
ルマノ硅酸ガラスから選ばれる１種または２種以上の絶
縁膜を被着せしめることによって、ファイバー化の困難
性、ファイバー素材のシ偏芯化を招くことなく、ファイ
バー素材外周に均一厚の絶縁膜を設けることができ、ガ
ラスファイバー素材と外界雰囲気との反応を迅速に遮断
できるため、高温高湿、或いは水中に長時間曝しても、
絶縁膜内側のガラスファイバー素材が劣化するの；を防
止できる。However, according to the present invention, SiO2, Al2O3,! Si
3N4. T10□, silicophosphate glass, silicoborate glass,
By depositing one or more types of insulating film selected from aluminosilicate glass, aluminoborosilicate glass, and germanosilicate glass, it becomes difficult to form fibers and the fiber material becomes eccentric. It is possible to provide an insulating film of uniform thickness around the outer periphery of the fiber material, quickly blocking the reaction between the glass fiber material and the outside atmosphere, so even if exposed to high temperature, high humidity, or water for a long time,
This prevents the glass fiber material inside the insulation film from deteriorating.
特に、多成分系ガラスファイバー素材の場合では、前記
均一厚の絶縁膜によって素材中のアルカリイオンと外界
雰囲気との反応を遮断できる。In particular, in the case of a multi-component glass fiber material, the uniformly thick insulating film can block the reaction between alkali ions in the material and the external atmosphere.
したがって、ガラスファイバー素材の劣化防止により機
械的強度、光散乱損失を著しく；改善した光通信用ガラ
スファイバーを得ることができる。Therefore, by preventing deterioration of the glass fiber material, it is possible to obtain a glass fiber for optical communication with significantly improved mechanical strength and light scattering loss.
なお、本発明に採用されるＣＶＤ法の中で、とくにプラ
ズマＣＶＤ法は低温での被着が可能であり、絶縁膜の膜
質が良好となるため有益である。Note that among the CVD methods employed in the present invention, the plasma CVD method is particularly advantageous because it allows deposition at low temperatures and improves the quality of the insulating film.
次に、本発明の実施例を図面を参照して説明する。Next, embodiments of the present invention will be described with reference to the drawings.
まず、第１図に示す如く二重ルツボ１の内側ルツボ１ａ
にＳ ｉＯ２７０重量％、Ｎａ２Ｏ２１，５重量％及び
ＣａＯ３，５重量％の組成割合のコア用多成分系ガラス
２を収容し、一方外側ルツボ１ｂに５ｉＯ２７４重量係
、Ｎａ２Ｏ２３重量％及びＣａＯ３重量係重量成割合の
クラッド用多成分系ガラス３を収容し、上記二重ルツボ
１の湿度を９００°Ｃにせしめ、各多成分系ガラス２，
３を同時に紡糸してコア径６０μ、クラツド径１２５μ
のガラスファイバー素材４を形成した。First, as shown in FIG. 1, the inner crucible 1a of the double crucible 1
The core multi-component glass 2 containing 70% by weight of SiO2, 1.5% by weight of Na2O2 and 5% by weight of CaO3 is housed in the outer crucible 1b, while the multi-component glass 2 containing 70% by weight of SiO2, 1.5% by weight of Na2O2 and 5% by weight of CaO3 is housed in the outer crucible 1b. The humidity of the double crucible 1 is kept at 900°C, and each multi-component glass 2,
3 are spun simultaneously to obtain a core diameter of 60μ and a cladding diameter of 125μ.
A glass fiber material 4 was formed.
次いで、紡糸直後のガラスファイバー素材４を反応炉５
内に導入し、・該反応炉５に連結された導管６，７，８
．９からＮ２ガス（希釈ガス）０２ガス、Ｓ ＩＨ４ガ
ス及びＰＨ３ガスを夫々０２ ： Ｓ ｔＨ４： Ｐ
Ｈ３のモル比が１０：１０：１になるように供給し、か
つ反応炉５の温度を４５０℃に保持し、上記Ｓ ＩＨ４
，Ｊ Ｐ）（３を酸化せしめてガラスコアイノく一素材
４の外表面に厚さ１００００人の硅リン酸ガラスの絶縁
膜を被着せしめた。Next, the glass fiber material 4 immediately after spinning is placed in a reactor 5.
- conduits 6, 7, 8 connected to the reactor 5;
．． 9 to N2 gas (dilution gas) 02 gas, S IH4 gas and PH3 gas respectively 02: S tH4: P
H3 was supplied so that the molar ratio was 10:10:1, and the temperature of the reactor 5 was maintained at 450°C, and the above S IH4
, JP) (3) was oxidized and an insulating film of silicophosphate glass having a thickness of 10,000 wafers was applied to the outer surface of the glass core inopiece material 4.
その後、これを４００°Ｃに加熱した加熱炉１０に挿通
して硅リン酸ガラスの絶縁膜を有する光通信用多成分系
ガラスファイバー；１１を得た。Thereafter, this was inserted into a heating furnace 10 heated to 400°C to obtain a multi-component glass fiber for optical communication; 11 having an insulating film of silicophosphate glass.
得られた光通信用多成分系ガラスファイバーを切断して
長さ１０ｃｒｒＬの試料片２００本を作成し、これら試
料片を湿度６０°Ｃ１湿度９０係の環境試験器に１００
０時間、及び１． ＯＯ００時間放置し・た後取出し、
各条件毎の試験片の引張強度を測定して劣化度合を求め
た。The obtained multi-component glass fiber for optical communication was cut to create 200 sample pieces with a length of 10 crrL, and these sample pieces were placed in an environmental tester at a humidity of 60°C and a humidity of 90%.
0 hours, and 1. Leave it for OO00 hours and then take it out.
The degree of deterioration was determined by measuring the tensile strength of the test piece under each condition.
その結果を第２図の如きワイブル分布として示した。The results are shown as a Weibull distribution as shown in FIG.
なお、図中のＡ。は上記実施例１により得たガラスファ
イバーの試験片゛における劣化試験前の引張強度分布、
Ａ１は目状）駒片を環境試験器に１０００時間放置した
後の引張強度分布、Ａ２は同試験片を回状１験器に１ｏ
ｏｏ。In addition, A in the figure. is the tensile strength distribution of the glass fiber test piece obtained in Example 1 before the deterioration test,
A1 is the tensile strength distribution after leaving the piece in the environmental tester for 1000 hours, and A2 is the tensile strength distribution after leaving the same test piece in the circular tester for 1000 hours.
oo.
時間放置した後の引張強度分布、Ｂ１は硅リン酸ガラス
の絶縁膜を有さないガラスファイバーの試験片を同試験
器に１０００時間放置した後の引張１強度分布、Ｂ２は
前記Ｂ１と同様な試、駒片を同試験器に１００００時間
放置した後の引張強度分布、Ｃ１，Ｃ２は夫夫多成分系
ガラスファイバーにポリ弗化ビニリデンを直接被覆した
試料片を同試験器に１０００時間、１００００時間放置
した後の引張１度分布である。B1 is the tensile strength distribution after leaving it for 1000 hours in the same tester, and B2 is the same as B1 above. Tensile strength distribution, C1 and C2, after leaving the piece in the same tester for 10,000 hours, is the tensile strength distribution, C1, C2. This is the tensile 1 degree distribution after being left for a period of time.
第２図から明らかな如く、本発明方法により得た光通信
用多成分系ガラスファイバーは絶縁膜を有さない従来の
ガラスファイバーに比して高温高湿下に長時間曝された
場合の劣化度合が著しく低いことがわかる。As is clear from Fig. 2, the multi-component glass fiber for optical communication obtained by the method of the present invention deteriorates more easily when exposed to high temperature and high humidity for a long time than conventional glass fiber without an insulating film. It can be seen that the degree is extremely low.
実施例 ２
前述した第１図の反応炉５の導管６，７からＳ ｉＨ４
ガス、ＮＨ３ガスをＳ ｔ Ｈ４： Ｎ Ｈ３のモル比
が５：１となるように供給し、反応炉５の温度を４００
℃に保持しガラスファイバー素材の外表面に５００ＯＡ
のＳ ｉ３Ｎ４の絶縁膜を被着した以外、前記実施例１
と同様な方法により光通信用多成分系ガラスファイバー
を得た。Example 2 SiH4 from the conduits 6 and 7 of the reactor 5 in FIG.
Gas, NH3 gas was supplied so that the molar ratio of S t H4: NH3 was 5:1, and the temperature of the reactor 5 was set to 400 °C.
500OA on the outer surface of the glass fiber material kept at ℃
Example 1 except that an insulating film of Si3N4 was deposited.
A multi-component glass fiber for optical communication was obtained using the same method.
得られた光通信用多成分系ガラスファイバーを切断して
長さ１０ｃｒｒＬの試験片２００本を用意し、これら試
験片を上記実施例１と同様な環境試験器に１０００時間
、及び１００００時間放置した後取出し、各条件毎の試
験片の引張強度を測定して劣化度合を求めた。The obtained multi-component glass fiber for optical communication was cut to prepare 200 test pieces with a length of 10 crrL, and these test pieces were left in the same environmental test chamber as in Example 1 for 1000 hours and 10000 hours. After taking it out, the tensile strength of the test piece under each condition was measured to determine the degree of deterioration.
その結果を第３図の如きワイブル分布として示した。The results are shown as a Weibull distribution as shown in FIG.
なお、図中のＡ。′は上記試験片における劣化試験前の
引張強度分布、Ａ１は同試験片を環境試験器に１０００
時間放置した後の引張強度分布、Ａ２’は同試験片を同
試験器に１００００時間放置した後の引張強度分布であ
る。In addition, A in the figure. ' is the tensile strength distribution of the above test piece before the deterioration test, and A1 is the tensile strength distribution of the above test piece in the environmental tester.
Tensile strength distribution after standing for a time, A2' is the tensile strength distribution after leaving the same test piece in the same tester for 10,000 hours.
第３図から明らかな如く、Ｓｉ３Ｎ４の絶縁膜を有する
光通信用多成分系ガラスファイバーは実施例１の硅リン
酸ガラス絶縁膜を有するガラスファイバーに比して、さ
らに高温高湿下に長時間曝された場合の劣化度合が改善
されることがわかる。As is clear from FIG. 3, the multi-component glass fiber for optical communication having an Si3N4 insulating film can be exposed to higher temperatures and humidity for a longer period of time than the glass fiber having a silicophosphate glass insulating film of Example 1. It can be seen that the degree of deterioration when exposed to heat is improved.
以上詳述した如く、′本発明によればファイバー化を阻
害することなくガラスファイバー素材と外界雰囲気との
反応を遮断してファイバー劣化を防止し、特に、多成分
系ガラスファイバー素材の場合ではその中のアルガリイ
オンと外界雰囲気との反応によるファイバー劣化を防止
し、長期間安定した機械的強度、低い光伝送損失を保有
する光通信用ガラスファイバーを提供できるものである
。As detailed above, according to the present invention, it is possible to prevent fiber deterioration by blocking the reaction between the glass fiber material and the external atmosphere without inhibiting fiberization, especially in the case of multi-component glass fiber materials. It is possible to provide a glass fiber for optical communications that prevents fiber deterioration due to the reaction between the Argali ions inside and the external atmosphere, and has stable mechanical strength over a long period of time and low optical transmission loss.
第１図は本発明方法に使用される製造装置の一形態を示
す概略図、第２図は本発明の実施例１で得た光通信用多
成分系ガラスファイバーの劣化試験結果を示すワイブル
分布図、第３図は本発明の実施例２で得た光通信用多成
分系ガラスファイバーの劣化試験結果を示すワイブル分
布図である。
１・・・二重ルツボ、４・・・ガラスファイバー素材、
５・・・反応炉、１１・・・光通信用多成分系ガラスフ
ァイバー。Fig. 1 is a schematic diagram showing one form of manufacturing equipment used in the method of the present invention, and Fig. 2 is a Weibull distribution showing the results of a deterioration test of the multicomponent glass fiber for optical communication obtained in Example 1 of the present invention. 3 are Weibull distribution diagrams showing the results of a deterioration test of the multi-component glass fiber for optical communication obtained in Example 2 of the present invention. 1...Double crucible, 4...Glass fiber material,
5...Reaction furnace, 11...Multi-component glass fiber for optical communication.
Claims (1)
ｉＯ□、Ａｌ２Ｏ３，Ｓｉ３Ｎ４．ＴｉＯ２，硅リン酸
ガラス、硅ホウ酸ガラス、アルミノ硅酸ガラス、ゲルマ
ノ硅酸ガラス、及びアルミノホウ硅酸ガラスのうちの１
種または２種以上からなる絶縁膜をＣＶＤ法により金属
ガスを反応させて被着せしめることを特徴とする光通信
用ガラスファイバーの製造方法。1 S on the glass fiber material immediately after spinning the glass.
iO□, Al2O3, Si3N4. One of TiO2, silicophosphate glass, silicoborate glass, aluminosilicate glass, germanosilicate glass, and aluminoborosilicate glass
1. A method for producing glass fiber for optical communications, characterized in that an insulating film made of one or more kinds is deposited by reacting a metal gas with a CVD method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP52092793A JPS5819614B2 (en) | 1977-08-02 | 1977-08-02 | Manufacturing method of glass fiber for optical communication |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP52092793A JPS5819614B2 (en) | 1977-08-02 | 1977-08-02 | Manufacturing method of glass fiber for optical communication |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5427447A JPS5427447A (en) | 1979-03-01 |
| JPS5819614B2 true JPS5819614B2 (en) | 1983-04-19 |
Family
ID=14064291
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP52092793A Expired JPS5819614B2 (en) | 1977-08-02 | 1977-08-02 | Manufacturing method of glass fiber for optical communication |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5819614B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57209844A (en) * | 1981-06-18 | 1982-12-23 | Nippon Telegr & Teleph Corp <Ntt> | Manufacture of optical fiber |
| US4504113A (en) * | 1981-11-02 | 1985-03-12 | Schlumberger Technology Corporation | Reinforced and chemically resistant optical filament |
| JPS58110031U (en) * | 1982-10-12 | 1983-07-27 | 株式会社フジクラ | Optical fiber reinforcement device |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5164935A (en) * | 1974-11-30 | 1976-06-04 | Fujikura Ltd | Rowaboshisoo jusuru hikarifuaibano seizohoho |
| JPS51136996A (en) * | 1975-05-20 | 1976-11-26 | Matsushita Electric Works Ltd | Production of inorganic fiber strengthening material |
| JPS51147330A (en) * | 1975-06-13 | 1976-12-17 | Furukawa Electric Co Ltd:The | Production method of optical fibre |
-
1977
- 1977-08-02 JP JP52092793A patent/JPS5819614B2/en not_active Expired
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5164935A (en) * | 1974-11-30 | 1976-06-04 | Fujikura Ltd | Rowaboshisoo jusuru hikarifuaibano seizohoho |
| JPS51136996A (en) * | 1975-05-20 | 1976-11-26 | Matsushita Electric Works Ltd | Production of inorganic fiber strengthening material |
| JPS51147330A (en) * | 1975-06-13 | 1976-12-17 | Furukawa Electric Co Ltd:The | Production method of optical fibre |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5427447A (en) | 1979-03-01 |
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