JPH06242005A - Method and apparatus for measuring curing reaction - Google Patents
Method and apparatus for measuring curing reactionInfo
- Publication number
- JPH06242005A JPH06242005A JP2779593A JP2779593A JPH06242005A JP H06242005 A JPH06242005 A JP H06242005A JP 2779593 A JP2779593 A JP 2779593A JP 2779593 A JP2779593 A JP 2779593A JP H06242005 A JPH06242005 A JP H06242005A
- Authority
- JP
- Japan
- Prior art keywords
- internal reflection
- reflection element
- resin
- infrared light
- measuring
- 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.)
- Granted
Links
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000011347 resin Substances 0.000 claims abstract description 28
- 229920005989 resin Polymers 0.000 claims abstract description 28
- 230000003595 spectral effect Effects 0.000 claims abstract description 7
- 238000010521 absorption reaction Methods 0.000 claims abstract description 6
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 5
- 230000000644 propagated effect Effects 0.000 claims abstract 2
- 230000001678 irradiating effect Effects 0.000 claims description 4
- 230000000149 penetrating effect Effects 0.000 claims 1
- 238000004566 IR spectroscopy Methods 0.000 abstract description 3
- 238000000862 absorption spectrum Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000002238 attenuated effect Effects 0.000 description 2
- 238000001028 reflection method Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001902 propagating effect Effects 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
Landscapes
- Spectrometry And Color Measurement (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
(57)【要約】
【目的】 本発明は、紫外線又は熱硬化型樹脂の硬化反
応を赤外分光法によって測定する方法及びその装置に関
する。
【構成】 中央部に内部反射エレメント２が貫通して設
けられ、内部反射エレメント２の前及び後に窓７，７が
設けられたセル室３の中に紫外線又は熱硬化型樹脂１を
注入し、窓７，７から紫外線又は熱線９，９を照射して
該樹脂を硬化し、同時に内部反射エレメント２の一端か
ら赤外光８を入射し、その中を全反射しながら他端に伝
播した赤外光のスペクトル吸収を測定する発明である。
(57) [Abstract] [Object] The present invention relates to a method and an apparatus for measuring the curing reaction of an ultraviolet or thermosetting resin by infrared spectroscopy. [Structure] An ultraviolet or thermosetting resin 1 is injected into a cell chamber 3 in which a central reflection portion is provided with an internal reflection element 2 and windows 7 and 7 are provided in front of and behind the internal reflection element 2. Ultraviolet rays or heat rays 9, 9 are radiated from the windows 7, 7 to cure the resin, and at the same time, infrared light 8 is made incident from one end of the internal reflection element 2, and the infrared light 8 is totally reflected therein and propagated to the other end. It is an invention for measuring the spectral absorption of external light.
Description
【０００１】[0001]
【産業上の利用分野】本発明は、光又は熱線硬化型樹脂
の硬化反応を赤外分光法によって測定する方法及びその
装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and apparatus for measuring the curing reaction of a light or heat ray curable resin by infrared spectroscopy.
【０００２】[0002]
【従来の技術】従来、樹脂の硬化反応を赤外分光法によ
って測定するには、バルク中から試験用試料を取出し、
例えば拡散反射法あるいはＡＴＲ法によって行われた。
図２はこれらの方法の構成を示す概略図であり、同図
（ａ）は粉末状の試料１−１に赤外光８を入射し、粉末
の表面反射と透過を繰返して受光された赤外光をスペク
トル分析する拡散反射法である。また、同図（ｂ）はフ
ィルム状の試料１−２と内部反射エレメント２−１の接
触面で多重反射させ、その間に減衰した赤外光８の吸収
スペクトルを測定するＡＴＲ法である。2. Description of the Related Art Conventionally, in order to measure the curing reaction of a resin by infrared spectroscopy, a test sample is taken out from the bulk,
For example, the diffuse reflection method or the ATR method is used.
FIG. 2 is a schematic diagram showing the configuration of these methods. FIG. 2 (a) shows the infrared light 8 incident on the powdery sample 1-1, and the red light received by repeating surface reflection and transmission of the powder. This is a diffuse reflection method for spectral analysis of external light. Further, FIG. 2B is an ATR method in which the absorption spectrum of infrared light 8 attenuated during multiple reflection by multiple reflection at the contact surface between the film-shaped sample 1-2 and the internal reflection element 2-1.
【０００３】[0003]
【発明が解決しようとする課題】これらの方法は、いず
れもバルクの中から試料を取出して測定するために試験
用の試料を作成しなければならず、また硬化反応が進行
している任意の状態を測定することはできない。これが
バルクの内側になるとさらにむづかしくなる。そこで本
発明は、かかる問題点を解決した硬化反応の測定方法及
び装置を提供することを目的とする。In any of these methods, a sample for testing must be prepared in order to extract and measure a sample from the bulk, and any curing reaction in progress is required. The condition cannot be measured. It becomes more difficult when this is inside the bulk. Therefore, an object of the present invention is to provide a method and apparatus for measuring a curing reaction that solves the above problems.
【０００４】[0004]
【課題を解決するための手段】本発明は、中央部に内部
反射エレメントが貫通して設けられ、内部エレメントの
前後に窓が設けられたセル室に紫外線又は熱硬化型樹脂
を注入し、窓から紫外線又は熱線を照射して前記樹脂を
硬化し、同時に内部反射エレメントの一端から紫外光を
入射し、内部反射エレメント内を全反射しながら他端に
伝播した紫外光のスペクトル吸収を測定する硬化反応の
測定方法である。SUMMARY OF THE INVENTION According to the present invention, an ultraviolet ray or thermosetting resin is injected into a cell chamber in which an internal reflection element is provided so as to penetrate through the central portion and windows are provided in front of and behind the internal element. To cure the resin by irradiating it with ultraviolet rays or heat rays, at the same time injecting ultraviolet light from one end of the internal reflection element, and measuring the spectral absorption of the ultraviolet light propagating to the other end while totally reflecting inside the internal reflection element. It is a method of measuring a reaction.
【０００５】また本発明は、中央部に内部反射エレメン
トが貫通して設けられ、内部反射エレメントの前後に窓
が設けられたセル室と、セル室に導入された樹脂を窓を
通して照射する紫外線又は熱線の発生装置と、内部反射
エレメントの一端より入射される赤外光発生装置と、内
部反射エレメントの他端で受光された赤外光のスペクト
ル分光装置とを備え、前記セル中に注入された樹脂を硬
化すると同時に硬化の程度に応じたスペクトル吸収を測
定する硬化反応の測定装置である。Further, according to the present invention, an internal reflection element is provided so as to penetrate through the central portion thereof, and a cell chamber having windows provided in front of and behind the internal reflection element, and an ultraviolet ray for irradiating the resin introduced into the cell chamber through the window. A heat ray generation device, an infrared light generation device incident from one end of the internal reflection element, and a spectrum spectroscopic device for infrared light received at the other end of the internal reflection element, were injected into the cell. It is a curing reaction measuring device that measures the spectral absorption according to the degree of curing while curing the resin.
【０００６】[0006]
【作用】上記の構成によれば、本発明は、内部反射エレ
メントと接触して粘稠性樹脂を注入し、次いで樹脂が硬
化されると同時に内部反射エレメントに赤外光を入射し
て吸収スペクトルを測定する方法である。従って、試験
をするための試料を改めて作成する必要がない。また、
樹脂の硬化反応を進行させると同時に吸収スペクトルを
測定することができるので、所望の硬化状態について適
宜測定することができる。さらに、セル室の外周から硬
化を進め、中心部で測定するのでセル室の大きさを変え
ることによって表面から所望の深さの硬化状態を測定す
ることができる。According to the above construction, according to the present invention, the viscous resin is injected into contact with the internal reflection element, and then the resin is cured. Is a method of measuring. Therefore, it is not necessary to newly prepare a sample for the test. Also,
Since the absorption spectrum can be measured at the same time as the curing reaction of the resin proceeds, the desired cured state can be appropriately measured. Further, since the curing proceeds from the outer periphery of the cell chamber and the measurement is performed at the central portion, it is possible to measure the cured state at a desired depth from the surface by changing the size of the cell chamber.
【０００７】[0007]
【実施例】以下、添付図面を参照して本発明の実施例を
測定する。図１は本実施例の構成を示す概略図であり、
内部反射エレメント２は被測定用樹脂１を収納するセル
室３の中央部に貫通して設けられ、内部反射エレメント
２の前と後のセル室側壁には紫外線あるいは熱線を通す
窓７，７が設けられている。紫外線あるいは熱線の発生
装置６，６から発射された紫外線あるいは熱線９，９
は、両側の窓７，７を通してセル室内に収納された樹脂
１を照射してこれを硬化する。一方、赤外光発生装置４
からは測定用赤外光８がミラー１０を経て内部反射エレ
メント２の一端に入射され、硬化した樹脂１と内部反射
エレメント２の接触面で多重反射して他端へ伝播し、そ
の間に減衰した赤外光はスペクトル分光装置５によって
吸収スペクトルが測定される。EXAMPLES Examples of the present invention will be measured below with reference to the accompanying drawings. FIG. 1 is a schematic diagram showing the configuration of this embodiment,
The internal reflection element 2 is provided so as to penetrate through the central portion of the cell chamber 3 accommodating the resin 1 to be measured, and windows 7 and 7 for transmitting ultraviolet rays or heat rays are provided on the side walls of the cell chamber before and after the internal reflection element 2. It is provided. Ultraviolet rays or heat rays emitted from the ultraviolet ray or heat ray generators 6,6
Irradiates the resin 1 housed in the cell chamber through the windows 7 on both sides to cure it. On the other hand, the infrared light generator 4
Infrared light 8 for measurement is incident on one end of the internal reflection element 2 via the mirror 10, is multiply reflected by the contact surface between the cured resin 1 and the internal reflection element 2, propagates to the other end, and is attenuated in the meantime. The absorption spectrum of infrared light is measured by the spectrum spectroscope 5.
【０００８】被測定樹脂１としては熱硬化型あるいは紫
外線硬化型樹脂が粘稠状態でセル室３の中に注入され、
その後硬化される。内部反射エレメント２は赤外域に吸
収がなく、被測定用樹脂１より十分屈折率の大きい Ｋ
ＲＳ−５，ＺｎＳｅ，Ｓｉ，Ｇｅが用いられる。Ｇｅは
屈折率が大きく（４．０）、また傷つきにくいので好ま
しい材料である。内部反射エレメントの両端面は赤外光
が入光面に対し直角に入射され、内面を全反射しながら
伝播して他端から出射できるよう傾斜して設けられてい
る。As the resin 1 to be measured, a thermosetting or ultraviolet curable resin is injected into the cell chamber 3 in a viscous state,
It is then cured. The internal reflection element 2 has no absorption in the infrared region and has a sufficiently higher refractive index than the resin 1 to be measured.
RS-5, ZnSe, Si, Ge is used. Ge is a preferable material because it has a large refractive index (4.0) and is hard to be scratched. Both end faces of the internal reflection element are provided so as to be inclined so that infrared light is incident at a right angle to the light incident face, propagates while being totally reflected on the inner face, and is emitted from the other end.
【０００９】内部反射エレメントとセル室内面までの距
離を変えて測定することによって樹脂内における所定の
位置の硬化反応状態を調べることができる。本発明は紫
外線等を照射して樹脂の硬化を進行せしめ、同時に内部
反射エレメントに赤外線を入射して吸収スペクトルを測
定するので測定のための試料を作成する必要がなく、ま
た、硬化反応の進行に応じたデータを得ることができ
る。By changing the distance between the internal reflection element and the inner surface of the cell, the curing reaction state at a predetermined position in the resin can be examined. In the present invention, it is not necessary to prepare a sample for measurement because the absorption spectrum is measured by irradiating the resin with ultraviolet rays or the like and at the same time making infrared rays incident on the internal reflection element, and the progress of the curing reaction. It is possible to obtain data according to.
【００１０】[0010]
【発明の効果】以上説明したように、本発明は内部反射
エレメントと接触して粘稠性樹脂を注入し、次いで樹脂
が硬化されると同時に内部反射エレメントに赤外光を入
射して吸収スペクトルを測定する方法である。従って、
試験をするための試料を改めて作成する必要がない。ま
た、樹脂の硬化反応を進行させると同時に吸収スペクト
ルを測定することができるので、所望の硬化状態につい
て適宜測定することができる。さらに、セル室の外周か
ら硬化を進め、中心部で測定するのでセル室の大きさを
変えることによって表面から所望の深さの硬化状態を測
定することができる。As described above, according to the present invention, the viscous resin is injected in contact with the internal reflection element, and then the resin is cured, and at the same time, the infrared light is incident on the internal reflection element to absorb the absorption spectrum. Is a method of measuring. Therefore,
There is no need to create a new sample for testing. Further, since the absorption spectrum can be measured at the same time as the curing reaction of the resin proceeds, it is possible to appropriately measure the desired cured state. Further, since the curing proceeds from the outer periphery of the cell chamber and the measurement is performed at the central portion, it is possible to measure the cured state at a desired depth from the surface by changing the size of the cell chamber.
【図１】本発明の実施例に係る構成を示す概略図であ
る。FIG. 1 is a schematic diagram showing a configuration according to an embodiment of the present invention.
【図２】従来の実施例に係る構成を示す概略図である。FIG. 2 is a schematic diagram showing a configuration according to a conventional example.
１，１−１，１−２：被測定用の試料（樹脂） ２，２−１：内部反射エレメント ３：セル室 ４：赤外光発生装置 ５：スペクトル分光装置 ６：紫外線又は熱線発生装置 ７：窓 ８：赤外光 ９：紫外線又は熱線 １０：ミラー １１：楕円面鏡 1, 1-1, 1-2: Sample (resin) to be measured 2, 2-1: Internal reflection element 3: Cell chamber 4: Infrared light generator 5: Spectral spectroscope 6: Ultraviolet or heat ray generator 7: Window 8: Infrared light 9: Ultraviolet rays or heat rays 10: Mirror 11: Ellipsoidal mirror
Claims (3)
設けられ、内部エレメントの前後に窓が設けられたセル
室に紫外線又は熱硬化型樹脂を注入し、窓から紫外線又
は熱線を照射して前記樹脂を硬化し、同時に内部反射エ
レメントの一部から赤外光を入射し、内部反射エレメン
ト内を全反射しながら他端に伝播した赤外光のスペクト
ル吸収を測定することを特徴とする硬化反応の測定方
法。1. An ultraviolet ray or a thermosetting resin is injected into a cell chamber having an internal reflection element penetratingly provided in a central portion thereof and windows provided in front of and behind the internal element, and the ultraviolet ray or the heat ray is irradiated from the window. Curing, characterized in that the resin is cured, at the same time infrared light is incident from a part of the internal reflection element, and the spectral absorption of the infrared light propagated to the other end while being totally reflected inside the internal reflection element is measured. How to measure reaction.
面までの距離を変えることを特徴とする請求項１記載の
硬化反応の測定方法。2. The method for measuring a curing reaction according to claim 1, wherein the distance from the surface of the internal reflection element to the inner surface of the cell is changed.
設けられ、内部反射エレメントの前後に窓が設けられた
セル室と、セル室に導入された樹脂を窓を通して照射す
る紫外線又は熱線の発生装置と、内部反射エレメントの
一端より入射される赤外光発生装置と、内部反射エレメ
ントの他端で受光された赤外光のスペクトル分光装置と
を備え、前記セル中に注入された樹脂を硬化すると同時
に硬化の程度に応じたスペクトル吸収を測定することを
特徴とする硬化反応の測定装置。3. A cell chamber having an internal reflection element penetrating through the center thereof and windows provided in front of and behind the internal reflection element, and generation of ultraviolet rays or heat rays for irradiating the resin introduced into the cell chamber through the window. An apparatus, an infrared light generation device that is incident from one end of the internal reflection element, and a spectral spectroscopic device for infrared light that is received at the other end of the internal reflection element, and cures the resin injected into the cell. At the same time, the apparatus for measuring the curing reaction is characterized by measuring the spectral absorption according to the degree of curing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2779593A JP3227866B2 (en) | 1993-02-17 | 1993-02-17 | Method and apparatus for measuring curing reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2779593A JP3227866B2 (en) | 1993-02-17 | 1993-02-17 | Method and apparatus for measuring curing reaction |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06242005A true JPH06242005A (en) | 1994-09-02 |
| JP3227866B2 JP3227866B2 (en) | 2001-11-12 |
Family
ID=12230916
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2779593A Expired - Fee Related JP3227866B2 (en) | 1993-02-17 | 1993-02-17 | Method and apparatus for measuring curing reaction |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3227866B2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997032198A1 (en) * | 1996-02-28 | 1997-09-04 | Laboratory Of Molecular Biophotonics | Method and apparatus for assaying enzymatic reaction |
| US6992759B2 (en) | 2002-10-21 | 2006-01-31 | Nippon Shokubai Co., Ltd. | Sample holder for spectrum measurement and spectrophotometer |
| JP2011220962A (en) * | 2010-04-14 | 2011-11-04 | Jasco Corp | Apparatus for measuring physical property of ultraviolet curing resin |
| JPWO2016017464A1 (en) * | 2014-07-30 | 2017-04-27 | 国立研究開発法人産業技術総合研究所 | Photocrosslinking film production equipment |
-
1993
- 1993-02-17 JP JP2779593A patent/JP3227866B2/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997032198A1 (en) * | 1996-02-28 | 1997-09-04 | Laboratory Of Molecular Biophotonics | Method and apparatus for assaying enzymatic reaction |
| US5905030A (en) * | 1996-02-28 | 1999-05-18 | Laboratory Of Molecular Biophotonics | Method and apparatus for assaying enzymatic reaction |
| US6992759B2 (en) | 2002-10-21 | 2006-01-31 | Nippon Shokubai Co., Ltd. | Sample holder for spectrum measurement and spectrophotometer |
| JP2011220962A (en) * | 2010-04-14 | 2011-11-04 | Jasco Corp | Apparatus for measuring physical property of ultraviolet curing resin |
| US8763447B2 (en) | 2010-04-14 | 2014-07-01 | Jasco Corporation | Ultraviolet curing resin property measuring apparatus |
| JPWO2016017464A1 (en) * | 2014-07-30 | 2017-04-27 | 国立研究開発法人産業技術総合研究所 | Photocrosslinking film production equipment |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3227866B2 (en) | 2001-11-12 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |