JP2742450B2 - Method for measuring the degree of cure of UV-curable resin - Google Patents
Method for measuring the degree of cure of UV-curable resinInfo
- Publication number
- JP2742450B2 JP2742450B2 JP1188327A JP18832789A JP2742450B2 JP 2742450 B2 JP2742450 B2 JP 2742450B2 JP 1188327 A JP1188327 A JP 1188327A JP 18832789 A JP18832789 A JP 18832789A JP 2742450 B2 JP2742450 B2 JP 2742450B2
- Authority
- JP
- Japan
- Prior art keywords
- curable resin
- degree
- cure
- measuring
- sample
- 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 Analyzing Materials By The Use Of Electric Means (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」 本発明は、光ファイバの被覆材に用いられている紫外
線硬化型樹脂（以下、UV硬化型樹脂と略称する。）の硬
化度を、正確に測定することができるUV硬化型樹脂の硬
化度測定方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention accurately measures the degree of curing of an ultraviolet curable resin (hereinafter abbreviated as UV curable resin) used for a coating material of an optical fiber. The present invention relates to a method for measuring the degree of curing of a UV-curable resin, which can be measured at a time.
「従来の技術」 従来より、光ファイバの被覆材として、UV硬化型樹脂
が用いられている。このUV硬化型樹脂は、その硬化度に
より、樹脂の物性（ヤング率、引張強度等）が変化し、
この物性の変化は、上記UV硬化型樹脂に被覆される光フ
ァイバの伝送特性等の諸特性に大きな影響を与える。従
って、光ファイバの伝送特性等の諸特性を安定させるた
めには、このUV硬化型樹脂の硬化度を、一定に保つこと
が必要であり、このためには、UV硬化型樹脂の硬化の状
態を、定量的に把握することが重要である。[Prior art] Conventionally, UV curable resins have been used as coating materials for optical fibers. This UV-curable resin changes its physical properties (Young's modulus, tensile strength, etc.) depending on the degree of curing.
This change in physical properties greatly affects various characteristics such as the transmission characteristics of the optical fiber coated with the UV-curable resin. Therefore, in order to stabilize various characteristics such as the transmission characteristics of the optical fiber, it is necessary to keep the degree of curing of the UV-curable resin constant. It is important to grasp quantitatively.
このUV硬化型樹脂を定量的に把握する方法の一つとし
てUV硬化型樹脂のガラス転移点（以下、Tgとする。）の
値を用いる方法がある。One method of quantitatively grasping the UV-curable resin is to use the value of the glass transition point (hereinafter, referred to as Tg) of the UV-curable resin.
「発明が解決しようとする課題」 ところが、このTgの値は、通常、動的な粘弾性を測定
することにより与えられるが、この動的粘弾性の測定方
法には、 温度依存性のみを考慮し、周波数依存性を考慮してい
ないため精度が悪い。"Problems to be Solved by the Invention" However, the value of Tg is usually given by measuring dynamic viscoelasticity, but in this method of measuring dynamic viscoelasticity, only temperature dependency is considered. However, accuracy is poor because frequency dependence is not taken into account.
動的な測定であるので、高温時の体積膨張による誤差
が生じる。Since the measurement is a dynamic measurement, an error occurs due to volume expansion at a high temperature.
サンプルの形状が制限される。The shape of the sample is limited.
測定のバラツキのため、明確にTgが決定できない といった問題点がある。There is a problem that Tg cannot be clearly determined due to measurement variations.
従って、UV硬化型樹脂の硬化度を把握する場合、Tgの
値が、上記問題点などにより正確に求められないため、
UV硬化型樹脂の硬化度の把握が正確にできないという問
題がある。また、動的粘弾性によりTgを測定する場合
は、UV硬化型樹脂の試料が光ファイバに付着した状態で
は測定できないため、サンプル採取に時間がかかるなど
の不都合がある。Therefore, when grasping the degree of cure of the UV curable resin, the value of Tg is not accurately obtained due to the above-mentioned problems, etc.
There is a problem that the degree of curing of the UV curable resin cannot be accurately grasped. Further, when Tg is measured by dynamic viscoelasticity, measurement cannot be performed in a state where a sample of a UV-curable resin is attached to an optical fiber.
本発明は上記事情に鑑みてなされたもので、UV硬化型
樹脂の硬化度の把握が正確にできる測定方法で、かつ、
サンプルの採取が容易なUV硬化型樹脂の硬化度測定方法
の提供を目的とするものである。The present invention has been made in view of the above circumstances, a measurement method that can accurately grasp the degree of cure of the UV curable resin, and,
It is an object of the present invention to provide a method for measuring the degree of cure of a UV-curable resin, which makes it easy to collect a sample.
「課題を解決するための手段」 本発明においては、UV硬化型樹脂の誘電緩和スペクト
ルからTgを測定し、このTgから光ファイバを被覆してい
るUV硬化型樹脂の硬化度を知ることにより上記問題を解
決するようにした。`` Means for solving the problem '' In the present invention, the Tg is measured from the dielectric relaxation spectrum of the UV-curable resin, and the degree of curing of the UV-curable resin coating the optical fiber is determined from the Tg to determine the degree of cure. Try to solve the problem.
以下、本発明のUV硬化型樹脂の硬化度測定方法につい
て詳しく説明する。Hereinafter, the method for measuring the degree of cure of the UV-curable resin of the present invention will be described in detail.
前述したように、本発明のUV硬化型樹脂の硬化度測定
方法の特徴は、UV硬化型樹脂の誘電緩和スペクトルを測
定し、この誘電緩和スペクトルからこの樹脂のTgを求
め、このTgの値からUV硬化型樹脂の硬化度を知るところ
にある。As described above, the characteristic of the method for measuring the degree of cure of the UV-curable resin of the present invention is that the dielectric relaxation spectrum of the UV-curable resin is measured, the Tg of the resin is determined from the dielectric relaxation spectrum, and the value of the Tg is determined from the value of the Tg. Know the degree of cure of UV curable resin.
この光ファイバを被覆するUV硬化型樹脂の誘電緩和ス
ペクトルの測定は、市販の誘電緩和スペクトル測定装置
を用いて行なわれる。また、この測定に用いられるUV硬
化型樹脂の試料としては、光ファイバを被覆した状態の
試料、光ファイバから剥離した状態の試料、もしくは別
に調製した試料などが用いられる。The measurement of the dielectric relaxation spectrum of the UV-curable resin coating the optical fiber is performed using a commercially available dielectric relaxation spectrum measuring device. Further, as a sample of the UV-curable resin used for this measurement, a sample coated with an optical fiber, a sample separated from the optical fiber, or a separately prepared sample is used.
上記誘電緩和スペクトルの具体的な測定法としては、
まず、試料温度を20〜150℃の範囲で適当な温度を数点
選択し、この選択された各温度において、交番電場の周
波数を1Hz〜1GHzの範囲で変化させつつ、その周波数に
おける誘電損失を測定する。この測定により得られる周
波数と誘電損失とのグラフにおいて、誘電損失は、ある
周波数においてピーク値を示す。この誘電損失がピーク
値を示す周波数（以下、最大緩和周波数とする。）を、
各測定温度においてそれぞれ測定する。このようにして
得られた各測定温度と、最大緩和周波数との関係から、
誘電緩和スペクトルが得られる。As a specific measuring method of the dielectric relaxation spectrum,
First, the sample temperature is selected from several suitable temperatures in the range of 20 to 150 ° C. At each of the selected temperatures, the frequency of the alternating electric field is changed in the range of 1 Hz to 1 GHz, and the dielectric loss at that frequency is reduced. Measure. In the graph of the frequency and the dielectric loss obtained by this measurement, the dielectric loss shows a peak value at a certain frequency. The frequency at which this dielectric loss shows a peak value (hereinafter referred to as the maximum relaxation frequency) is
The measurement is performed at each measurement temperature. From the relationship between each measured temperature thus obtained and the maximum relaxation frequency,
A dielectric relaxation spectrum is obtained.
第１図は、この誘電緩和スペクトルの一例を示すもの
である。図中符号Ｔ（゜K）は、測定温度を示し、ｆ（H
z）は、最大緩和周波数を示す。ここで、この最大緩和
周波数（ｆ）と、誘電緩和時間（τ）との関係は、 ｆ＝1/2πτ （１） で表される。誘電緩和時間（τ）が１秒となる最大緩和
周波数（f1）を（１）式から求め、第１図より、このlo
g f1に対応する測定温度の逆数（T-1）を読み取りこの
ＴをUV硬化型樹脂のTgとする。FIG. 1 shows an example of this dielectric relaxation spectrum. The symbol T (゜ K) in the figure indicates the measured temperature, and f (H
z) indicates the maximum relaxation frequency. Here, the relationship between the maximum relaxation frequency (f) and the dielectric relaxation time (τ) is represented by f = 1 / 2πτ (1) The maximum relaxation frequency (f 1 ) at which the dielectric relaxation time (τ) is 1 second is obtained from equation (1), and from FIG.
The reciprocal (T -1 ) of the measured temperature corresponding to gf 1 is read, and T is defined as Tg of the UV-curable resin.
このように、誘電緩和スペクトルからTgを測定する方
法は、 周波数依存性を考慮しているので精度が高い。As described above, the method of measuring Tg from the dielectric relaxation spectrum has high accuracy because the frequency dependence is considered.
静的な測定法であるので、系外の影響を受けにくい。Since it is a static measurement method, it is hardly affected by outside the system.
一義的に決定できる方法である。This is a method that can be uniquely determined.
といった特徴を有するものである。It has such a feature.
次に、このようにして得られたTgを用いて、UV硬化型
樹脂の硬化度を測定する方法の一例を示す。Next, an example of a method for measuring the degree of cure of the UV-curable resin using the Tg thus obtained will be described.
通常、UV硬化型樹脂は、その硬化度が進むに連れて、
内部の分子が高分子となることなどにより、Tgが上昇す
る。つまり、UV硬化型樹脂の硬化度と、そのときのTgと
は一定の関係を有する。従って、予めその樹脂の硬化度
とTgとの関係を求めておき、そのデータと、測定した試
料のTgとを比較することにより、その試料の硬化度が測
定できる。Normally, as the degree of curing of UV-curable resin increases,
Tg increases due to the internal molecules becoming macromolecules. That is, the degree of cure of the UV-curable resin and the Tg at that time have a certain relationship. Therefore, the relationship between the degree of cure of the resin and Tg is determined in advance, and the degree of cure of the sample can be measured by comparing the data with the measured Tg of the sample.
「実施例」 ウレタンアクリレート系のUV硬化型樹脂からなる試料
を数個用意し、それぞれの試料に異なる量のUV照射を行
い、それぞれの試料のTgを上記誘電緩和スペクトルによ
り求めた。また、それぞれの試料の硬化度を示すものと
して、ゲル分率を測定した。第２図に測定結果、すなわ
ち、UV照射量と、そのときの樹脂のゲル分率およびTgと
の関係を示す。ここで、図中符号Ａは照射量とTgとの関
係を示し、Ｂは照射量とゲル分率との関係を示す。"Examples" Several samples made of urethane acrylate-based UV-curable resin were prepared, each sample was irradiated with a different amount of UV, and the Tg of each sample was determined from the above-mentioned dielectric relaxation spectrum. The gel fraction was measured to indicate the degree of cure of each sample. FIG. 2 shows the relationship between the measurement results, that is, the UV irradiation amount and the gel fraction and Tg of the resin at that time. Here, the symbol A in the figure indicates the relationship between the dose and the Tg, and the symbol B indicates the relationship between the dose and the gel fraction.
第２図より、この樹脂においては、Tgが120℃以上で
あれば、樹脂の硬化度は十分であることが判断される。From FIG. 2, it is determined that the degree of cure of the resin is sufficient if the Tg is 120 ° C. or higher.
「発明の効果」 以上、説明したように、本発明は、紫外線硬化型樹脂
の誘電緩和スペクトルの値から、この樹脂のTgを求め、
得られたTgの値から上記紫外線硬化型樹脂の硬化度を知
ることを特徴とする紫外線硬化型樹脂の硬化度測定方法
であるので、誘電緩和スペクトルから得られるTgの精度
が高いことから、このTgを用いたUV硬化型樹脂の硬化度
の測定が精度良く行える。さらに、光ファイバに被覆さ
れた状態のUV硬化型樹脂でも測定できることから、短時
間で容易に測定試料が調製できる。"Effects of the Invention" As described above, the present invention determines the Tg of this resin from the value of the dielectric relaxation spectrum of the ultraviolet-curable resin,
Since the method for measuring the degree of cure of the ultraviolet-curable resin is characterized by knowing the degree of cure of the ultraviolet-curable resin from the obtained value of Tg, the accuracy of Tg obtained from the dielectric relaxation spectrum is high, The degree of cure of UV-curable resin using Tg can be measured with high accuracy. Furthermore, since measurement can be performed even on a UV-curable resin coated on an optical fiber, a measurement sample can be easily prepared in a short time.
従って、本発明は、製造工程等においてUV硬化型樹脂
の硬化度を正確にしかも迅速に測定できるという効果を
有するもので、光ファイバの製造工程の管理等に有用な
測定法である。Therefore, the present invention has an effect that the degree of curing of a UV curable resin can be accurately and quickly measured in a manufacturing process or the like, and is a useful measuring method for controlling the manufacturing process of an optical fiber.
第１図は本発明に用いられる誘電緩和スペクトルを示す
グラフ、第２図は本発明の実施例におけるUV照射量と樹
脂のTgおよびゲル分率との関係を示すグラフである。FIG. 1 is a graph showing the dielectric relaxation spectrum used in the present invention, and FIG. 2 is a graph showing the relationship between the UV irradiation amount and the Tg and gel fraction of the resin in the example of the present invention.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平３−242525（ＪＰ，Ａ) 特開 平３−96843（ＪＰ，Ａ) 特開 平３−95428（ＪＰ，Ａ) 特開 平３−63557（ＪＰ，Ａ) 特開 平３−51751（ＪＰ，Ａ) 特開 平３−23240（ＪＰ，Ａ) 特開 昭61−62853（ＪＰ，Ａ) 特開 昭55−146033（ＪＰ，Ａ) ────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP-A-3-242525 (JP, A) JP-A-3-96843 (JP, A) JP-A-3-95428 (JP, A) JP-A-3-95428 63557 (JP, A) JP-A-3-51751 (JP, A) JP-A-3-23240 (JP, A) JP-A-61-62853 (JP, A) JP-A-54-146033 (JP, A)
Claims (1)
測定し、この誘電緩和スペクトルからこの樹脂のTg（ガ
ラス転移点）を求め、得られたTgの値から上記紫外線硬
化型樹脂の硬化度を知ることを特徴とする紫外線硬化型
樹脂の硬化度測定方法。1. The dielectric relaxation spectrum of an ultraviolet-curable resin is measured, the Tg (glass transition point) of the resin is determined from the dielectric relaxation spectrum, and the degree of curing of the ultraviolet-curable resin is determined from the obtained Tg value. A method for measuring the degree of curing of an ultraviolet curable resin, characterized by knowing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1188327A JP2742450B2 (en) | 1989-07-20 | 1989-07-20 | Method for measuring the degree of cure of UV-curable resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1188327A JP2742450B2 (en) | 1989-07-20 | 1989-07-20 | Method for measuring the degree of cure of UV-curable resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0353152A JPH0353152A (en) | 1991-03-07 |
| JP2742450B2 true JP2742450B2 (en) | 1998-04-22 |
Family
ID=16221669
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1188327A Expired - Fee Related JP2742450B2 (en) | 1989-07-20 | 1989-07-20 | Method for measuring the degree of cure of UV-curable resin |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2742450B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20210002738A (en) * | 2018-06-12 | 2021-01-08 | 토요잉크Sc홀딩스주식회사 | Electromagnetic shielding sheet |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH063299A (en) * | 1992-06-22 | 1994-01-11 | Showa Electric Wire & Cable Co Ltd | Method for judging hardness of ultraviolet curing resin covering optical fiber |
| CA2975586A1 (en) * | 2015-02-05 | 2016-08-11 | Tatsuya Iwamoto | Interlayer film for laminated glass, and laminated glass |
| JP7099365B2 (en) * | 2019-03-01 | 2022-07-12 | 東洋インキＳｃホールディングス株式会社 | Electromagnetic wave shield sheet, component mounting board, and electronic equipment |
-
1989
- 1989-07-20 JP JP1188327A patent/JP2742450B2/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20210002738A (en) * | 2018-06-12 | 2021-01-08 | 토요잉크Sc홀딩스주식회사 | Electromagnetic shielding sheet |
| KR102311989B1 (en) * | 2018-06-12 | 2021-10-13 | 토요잉크Sc홀딩스주식회사 | electromagnetic shielding sheet |
| US11990420B2 (en) | 2018-06-12 | 2024-05-21 | Artience Co., Ltd. | Electromagnetic wave shielding sheet |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0353152A (en) | 1991-03-07 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |