JP2710388B2 - Measurement method of cured state of optical fiber coating surface - Google Patents
Measurement method of cured state of optical fiber coating surfaceInfo
- Publication number
- JP2710388B2 JP2710388B2 JP1049274A JP4927489A JP2710388B2 JP 2710388 B2 JP2710388 B2 JP 2710388B2 JP 1049274 A JP1049274 A JP 1049274A JP 4927489 A JP4927489 A JP 4927489A JP 2710388 B2 JP2710388 B2 JP 2710388B2
- Authority
- JP
- Japan
- Prior art keywords
- optical fiber
- cured state
- curable resin
- curing
- ultraviolet
- 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 - Fee Related
Links
Landscapes
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Light Guides In General And Applications Therefor (AREA)
- Optical Fibers, Optical Fiber Cores, And Optical Fiber Bundles (AREA)
- Surface Treatment Of Glass Fibres Or Filaments (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 この発明は、光ファイバ製造時において紫外線硬化樹
脂からなる被覆の表面の硬化状態を測定し、この被覆の
品質管理を迅速、容易に行えるようにしたものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention measures the cured state of the surface of a coating made of an ultraviolet curable resin at the time of manufacturing an optical fiber, and enables quick and easy quality control of the coating. It was made.
光ファイバの製造にあっては、紡糸後の光ファイバ裸
線表面にウレタンアクリレート系やエポキシアクリレー
ト系の紫外線硬化性樹脂液を塗布し、これに紫外線を照
射して硬化せしめ、保護用の紫外線硬化樹脂からなる一
次被覆などを形成することが行われている。In the production of optical fibers, a urethane acrylate or epoxy acrylate UV curable resin solution is applied to the bare optical fiber surface after spinning, and the UV curable resin solution is irradiated with UV light to cure it, and UV curing for protection is performed. Forming a primary coating made of a resin or the like has been performed.
ところで、この紫外線硬化樹脂からなる被覆の形成に
際しては、紫外線硬化樹脂が十分に硬化した状態とする
必要がある。紫外線硬化性樹脂液の硬化は紫外線の照射
量、硬化雰囲気気体の種類、流量、硬化温度、圧力など
のパラメータに依存し、これらパラメータが相互に関連
し合っている。By the way, when forming the coating made of the ultraviolet curable resin, it is necessary to make the ultraviolet curable resin sufficiently cured. Curing of the ultraviolet-curable resin liquid depends on parameters such as the amount of ultraviolet irradiation, the type of curing atmosphere gas, the flow rate, the curing temperature, and the pressure, and these parameters are mutually related.
したがって、紫外線硬化性樹脂液を十分に硬化させる
には、製造時にこれらのパラメータをそれぞれ最適化し
ていく必要があるがこの作業は各パラメータが相互に関
連しているため極めて面倒である欠点がある。特に、紫
外線硬化性樹脂は酸素存在下では、紫外線照射を行って
も硬化が阻害され、光ファイバ裸線などの表面に塗布し
た紫外線硬化性樹脂液の表面が空気等に接触すると、そ
の表面部分が十分に硬化せず、表面の硬化度が低いもの
となる。この表面が不十分な硬化の光ファイバ素線で
は、引取り時や送出し時に張力の変動が生じたり、この
上に塗布される識別用の着色インクの密着性が悪化した
りすることがある。Therefore, in order to sufficiently cure the ultraviolet-curable resin liquid, it is necessary to optimize each of these parameters at the time of manufacture, but this operation has a disadvantage that each parameter is extremely troublesome because the parameters are related to each other. . Particularly, in the presence of oxygen, the curing of an ultraviolet-curable resin is inhibited even by irradiation with ultraviolet light. Are not sufficiently cured, and the degree of curing of the surface is low. If the surface of the optical fiber is insufficiently cured, the tension may fluctuate at the time of take-off or delivery, or the adhesion of the colored ink for identification applied thereon may be deteriorated. .
このため、被覆表面の硬化状態を正確に把握する必要
がある。For this reason, it is necessary to accurately grasp the cured state of the coating surface.
この発明では、紫外線硬化樹脂からなる被覆を有する
光ファイバを試料とし、これを赤外反射法によって測定
し、赤外吸収の度合によって被覆表面の硬化状況を知
り、これによって被覆の品質管理が容易に行えるように
した。In the present invention, an optical fiber having a coating made of an ultraviolet curable resin is used as a sample, which is measured by an infrared reflection method, and the curing status of the coating surface is known by the degree of infrared absorption, thereby facilitating quality control of the coating. To be able to do it.
以下、この発明を詳しく説明する。 Hereinafter, the present invention will be described in detail.
紫外線硬化性樹脂の硬化は、通常アクリルモノマーの
付加重合によって三次元網目構造が形成されることで進
行する。したがって、硬化前の紫外線硬化性樹脂中には
炭素−炭素二重結合が数多く存在し、硬化の進行に伴っ
てこの二重結合数が減少していく。Curing of the ultraviolet curable resin usually proceeds by forming a three-dimensional network structure by addition polymerization of an acrylic monomer. Therefore, there are many carbon-carbon double bonds in the ultraviolet-curable resin before curing, and the number of these double bonds decreases as the curing progresses.
よって、この炭素−炭素二重結合に起因する赤外吸収
ピークの変化を赤外吸収スペクトル法で調べることによ
り、紫外線硬化性樹脂の硬化状況を定量的に把握するこ
とが可能となる。Therefore, by examining the change in the infrared absorption peak caused by the carbon-carbon double bond by the infrared absorption spectrum method, it is possible to quantitatively grasp the curing state of the ultraviolet curable resin.
例えば、赤外吸収スペクトルでの波数820cm-1付近の
吸収ピークは上記炭素−炭素二重結合に由来するもので
あり、この吸収ピークの吸光度がある値以下となれば、
該二重結合量が十分に減少し、硬化が完了していること
を知見することができる。For example, the absorption peak near the wave number of 820 cm -1 in the infrared absorption spectrum is derived from the carbon-carbon double bond, and if the absorbance of this absorption peak becomes a certain value or less,
It can be seen that the amount of the double bond has been sufficiently reduced and curing has been completed.
実際の光ファイバ製造ラインでの測定では、測定用試
料の調製の簡便性を考慮して赤外反射法（ATR法）によ
って行う。The measurement in the actual optical fiber production line is performed by the infrared reflection method (ATR method) in consideration of the simplicity of preparation of the measurement sample.
赤外反射法は、第１図に示すようにKRS−５などの赤
外線透過性材料からなる板状のプリズム１を用いるもの
である。このプリズム１の両端面はともに斜めに切断さ
れており、この端面の一方から測定用の赤外線を入射さ
せる。端面の角度がある角度となると入射した赤外線は
図のようにプリズム１の表面で数回全反射して進み、他
方の端面から出射する。この状態において、プリズム１
の両表面に試料2,2をホルダー3,3を用いて密着させる
と、赤外線の全反射の際、試料2,2の表面によって赤外
線の吸収が生じ、これを検知することによって試料2,2
の表面の赤外吸収スペクトルが得られるものである。The infrared reflection method uses a plate-like prism 1 made of an infrared transmitting material such as KRS-5 as shown in FIG. Both end faces of the prism 1 are cut obliquely, and infrared rays for measurement are made incident from one of the end faces. When the angle of the end face becomes a certain angle, the incident infrared ray is totally reflected several times on the surface of the prism 1 as shown in the figure, advances, and is emitted from the other end face. In this state, the prism 1
When the specimens 2, 2 are brought into close contact with both surfaces of the specimens 2 and 3 using the holders 3, 3, the surface of the specimens 2, 2 absorbs infrared rays when the infrared rays are totally reflected, and by detecting this, the specimens 2, 2 are detected.
Can be obtained an infrared absorption spectrum of the surface.
この発明では、製造ラインから適宜採取した試料とな
る光ファイバを複数本プリズム１の表面に並べて密着さ
せ、アルミニウム箔などの金属箔で被覆したゴムシート
などのパッキング材を介してホルダー3,3で圧締するこ
とにより、試料の準備が行われる。この金属箔によって
も赤外の反射量が増加して好ましい。このような試料調
製により、光ファイバ表面の紫外線硬化樹脂からなる被
覆の表面の赤外吸収スペクトルを容易に測定することが
できる。According to the present invention, a plurality of optical fibers as samples, which are appropriately collected from the production line, are arranged side by side on the surface of the prism 1 and brought into close contact therewith, and are held by the holders 3, 3 via a packing material such as a rubber sheet covered with a metal foil such as an aluminum foil. The sample is prepared by pressing. This metal foil is also preferable since the amount of infrared reflection increases. By such sample preparation, the infrared absorption spectrum of the surface of the coating made of the ultraviolet curing resin on the surface of the optical fiber can be easily measured.
そして、プリズム１の一方の端面より例えば波数820c
m-1の赤外光を入射し、その吸光度を求めることによっ
て光ファイバ表面の紫外線硬化樹脂からなる被覆表面の
硬化状態を知ることができる。Then, for example, a wave number of 820c from one end face of the prism 1
The cured state of the coating surface made of the ultraviolet curable resin on the surface of the optical fiber can be known by injecting infrared light of m -1 and determining the absorbance.
このような紫外線硬化樹脂からなる被覆表面の硬化状
態測定法によれば、赤外反射法によって求められた吸光
度によってその硬化状態を直接的にかつ一義的に求めら
れるので、その吸光度がある値以下となれば硬化完了で
あることが知られ、硬化条件のいかんにかからず被覆表
面の硬化が十分に進行した被覆を得ることができるよう
になり、製造上の品質管理が非常に容易となる。According to the method for measuring the cured state of a coating surface made of such an ultraviolet curable resin, the cured state can be directly and uniquely determined by the absorbance determined by the infrared reflection method, and the absorbance is equal to or less than a certain value. It is known that curing has been completed, and it is possible to obtain a coating with sufficiently advanced curing of the coating surface regardless of curing conditions, and it becomes very easy to control quality in production .
また、赤外反射法によるものであるので試料調製が簡
便、迅速に行え、製造ライン上で簡便に硬化状態を知る
ことができる。Further, since the method is based on the infrared reflection method, sample preparation can be performed easily and quickly, and the cured state can be easily known on a production line.
光ファイバ母材から溶融紡糸された外径125μｍの光
ファイバ裸線上にウレタンアクリレート系紫外線硬化性
樹脂液を塗布し、紫外線を照射して硬化させて一次被覆
を形成し、外径400μｍの光ファイバ素線とした。A urethane acrylate UV curable resin solution is applied to the bare optical fiber with an outer diameter of 125 μm melt-spun from the optical fiber preform, and irradiated with ultraviolet light to cure it to form a primary coating, and an optical fiber with an outer diameter of 400 μm The wire was used.
この一次被覆が施された光ファイバを採取し、長さ50
mmに切断し、これを約50本赤外反射法用のプリズムの両
面に並べて密着させて試料とし、波数820cm-1の測定光
を用いてその吸光度を求めた。The primary coated optical fiber is sampled and the length is 50
The sample was cut into mm, and about 50 prisms for the infrared reflection method were arranged side by side and adhered to each other to form a sample, and the absorbance was measured using measuring light having a wave number of 820 cm -1 .
一方、赤外吸収測定後の光ファイバを沸騰ペンタン中
に２時間浸漬し、その重量変化によって被覆のゲル化率
を求めた。On the other hand, the optical fiber after the infrared absorption measurement was immersed in boiling pentane for 2 hours, and the gelation rate of the coating was determined from the weight change.
吸光度とゲル化率との関係を第２図のグラフに示す。 The relationship between the absorbance and the gelation ratio is shown in the graph of FIG.
このグラフから、ゲル化率95〜100％の被覆では吸光
度が0.1以下となり、吸光度がこの範囲内にあればほぼ
被覆表面の硬化が完了していることがわかる。From this graph, it can be seen that the absorbance is 0.1 or less for the coating having a gelation ratio of 95 to 100%, and that the curing of the coating surface is almost completed when the absorbance is within this range.
したがって、製造時に随時、一次被覆を施した光ファ
イバを採取し、同様の手法で波数820cm-1での吸光度を
測定することで、一次被覆の表面の硬化状態を管理する
ことができる。Therefore, the cured state of the surface of the primary coating can be managed by collecting the optical fiber coated with the primary coating as needed at the time of manufacture and measuring the absorbance at a wave number of 820 cm -1 in the same manner.
以上説明したように、この発明の光ファイバ被覆表面
の硬化状態測定法は赤外反射法によってその吸光度の変
化から硬化状態を知るようにしたものであるので、被覆
表面の硬化状態を迅速、簡便に知ることができる。ま
た、得られた吸光度が所定の範囲内に収まるように硬化
条件を適宜決めればよいので、製造管理が用意となるな
どの効果を有する。As described above, the method for measuring the cured state of the coated surface of the optical fiber of the present invention is based on the fact that the cured state is known from the change in the absorbance by the infrared reflection method. You can know. In addition, since the curing conditions may be appropriately determined so that the obtained absorbance falls within a predetermined range, there is an effect that manufacturing control becomes easy.
第１図はこの発明に用いられる測定試料の例を示す概略
構成図、 第２図は実施例での被覆のゲル化率と吸光度の関係を示
すグラフである。FIG. 1 is a schematic configuration diagram showing an example of a measurement sample used in the present invention, and FIG. 2 is a graph showing the relationship between the gelation rate of the coating and the absorbance in Examples.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭63−63004（ＪＰ，Ａ) 特開 昭62−103540（ＪＰ，Ａ) 特開 昭49−16897（ＪＰ，Ａ) ────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP-A-63-63004 (JP, A) JP-A-62-103540 (JP, A) JP-A-49-16897 (JP, A)
Claims (1)
布し、紫外線を照射して紫外線硬化樹脂からなる被覆を
形成するに際し、 紫外線硬化樹脂からなる被覆を有する光ファイバを採取
し、この被覆の表面の硬化状態を赤外反射法によって測
定することを特徴とする光ファイバ被覆表面の硬化状態
測定法。1. An ultraviolet-curable resin solution is applied to the surface of an optical fiber, and when irradiating ultraviolet rays to form a coating made of an ultraviolet-curable resin, an optical fiber having a coating made of an ultraviolet-curable resin is collected. A method for measuring a cured state of a surface coated with an optical fiber, wherein the cured state of the surface is measured by an infrared reflection method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1049274A JP2710388B2 (en) | 1989-03-01 | 1989-03-01 | Measurement method of cured state of optical fiber coating surface |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1049274A JP2710388B2 (en) | 1989-03-01 | 1989-03-01 | Measurement method of cured state of optical fiber coating surface |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02228559A JPH02228559A (en) | 1990-09-11 |
| JP2710388B2 true JP2710388B2 (en) | 1998-02-10 |
Family
ID=12826270
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1049274A Expired - Fee Related JP2710388B2 (en) | 1989-03-01 | 1989-03-01 | Measurement method of cured state of optical fiber coating surface |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2710388B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4546861B2 (en) * | 2005-03-23 | 2010-09-22 | 住友ゴム工業株式会社 | Contact interface area evaluation method and contact interface area evaluation apparatus |
| DE102008041052B4 (en) * | 2008-08-06 | 2010-04-15 | Airbus Deutschland Gmbh | Device for contactless determination of the degree of drying of a lacquer layer and method |
| JP2012113228A (en) * | 2010-11-26 | 2012-06-14 | Sony Corp | Display device and method for manufacturing the same |
| JP2012247464A (en) * | 2011-05-25 | 2012-12-13 | Sumitomo Electric Ind Ltd | Method of manufacturing optical fiber with identification mark |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4916897A (en) * | 1972-06-14 | 1974-02-14 | ||
| JPS62103540A (en) * | 1985-10-30 | 1987-05-14 | Mitsubishi Heavy Ind Ltd | Method for measuring curing time of organic adhesive |
| JPS6363004A (en) * | 1986-09-04 | 1988-03-19 | Hitachi Ltd | Method and device for manufacturing optical parts |
-
1989
- 1989-03-01 JP JP1049274A patent/JP2710388B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02228559A (en) | 1990-09-11 |
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| LAPS | Cancellation because of no payment of annual fees |