JP2012207935A - Raman spectrometer and identification device using the same - Google Patents

Raman spectrometer and identification device using the same Download PDF

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JP2012207935A
JP2012207935A JP2011071675A JP2011071675A JP2012207935A JP 2012207935 A JP2012207935 A JP 2012207935A JP 2011071675 A JP2011071675 A JP 2011071675A JP 2011071675 A JP2011071675 A JP 2011071675A JP 2012207935 A JP2012207935 A JP 2012207935A
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JP5425131B2 (en
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Hiroshi Kurokawa
博志 黒川
Jiro Naka
慈朗 中
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Mitsubishi Electric Corp
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Abstract

【課題】プラスチックからのラマン信号に対する蛍光信号を低減または除去するラマン分光装置およびそれを用いた識別装置を得る。
【解決手段】ラマン分光装置は、照射したレーザ光がラマン散乱された散乱光を分光するラマン分光装置において、前記レーザ光の照射に先立って蛍光除去用レーザ光を照射する蛍光除去用レーザを、または、前記レーザ光の照射に先立って紫外線を照射する紫外線照射手段を備える。また、識別装置は、このラマン分光装置を用いてプラスチックを識別する。
【選択図】図１A Raman spectroscopic device that reduces or eliminates a fluorescence signal with respect to a Raman signal from plastic and an identification device using the same are obtained.
A Raman spectroscopic device is a Raman spectroscopic device that scatters scattered light obtained by Raman scattering of an irradiated laser beam. A fluorescence removing laser that irradiates a fluorescence removing laser beam prior to the irradiation of the laser light, Alternatively, an ultraviolet irradiation means for irradiating ultraviolet light prior to the laser light irradiation is provided. The identification device identifies the plastic using this Raman spectroscopic device.
[Selection] Figure 1

Description

この発明は、プラスチックにレーザ光を照射することにより生起するラマン信号を分光するラマン分光装置およびそれを用いたプラスチックの種類を識別する装置に関するものである。   The present invention relates to a Raman spectroscopic device that separates a Raman signal generated by irradiating a plastic with laser light, and an apparatus for identifying the type of plastic using the Raman spectroscopic device.

従来のラマン分光装置を用いた識別装置は、試料にはファイバヘッドを介して６４０ｎｍから９５０ｎｍの範囲の波長のレーザ光が照射される。ファイバヘッドは、光ファイバによりレーザに結合されている。試料から反射された光は、０．６より大きい開口数を有するファイバヘッド対物レンズによって集光され、光ファイバを介して分光写真器に送られる。分光写真器におけるラマン分光法による分析により、重合体の種類及び一定の添加物の存在を同定するための分光データが与えられる（例えば、特許文献１参照）。   In an identification device using a conventional Raman spectrometer, a sample is irradiated with laser light having a wavelength in the range of 640 nm to 950 nm via a fiber head. The fiber head is coupled to the laser by an optical fiber. The light reflected from the sample is collected by a fiber head objective lens having a numerical aperture greater than 0.6 and sent to the spectrograph through the optical fiber. Analysis by Raman spectroscopy in a spectrograph gives spectroscopic data for identifying the type of polymer and the presence of certain additives (see, for example, Patent Document 1).

特開２０００−３５６５９５号公報JP 2000-356595 A

しかし、従来の識別装置においては、移動する測定対象物をラマン分光するとき、同時に生起する蛍光信号がラマン測定信号に対するノイズとなるという問題がある。
従来の蛍光除去用レーザを用いない構成とした場合には、散乱光中に蛍光も含まれるため、蛍光信号もラマン信号と同時に検出される。そのため、識別制度が低下したり、識別できなかったりという問題が発生する。 However, the conventional identification device has a problem in that when a moving measurement object is subjected to Raman spectroscopy, a fluorescent signal generated simultaneously becomes noise with respect to the Raman measurement signal.
When the conventional laser for removing fluorescence is used, since the scattered light includes fluorescence, the fluorescence signal is detected simultaneously with the Raman signal. For this reason, there arises a problem that the identification system is lowered or cannot be identified.

この発明は、前記のような課題を解決するためになされたものであり、プラスチックからのラマン信号に対する蛍光信号を低減または除去するラマン分光装置およびそれを用いた識別装置を得ることを目的とする。   The present invention has been made to solve the above-described problems, and an object of the present invention is to obtain a Raman spectroscopic device that reduces or eliminates a fluorescence signal with respect to a Raman signal from plastic, and an identification device using the same. .

この発明に係るラマン分光装置は、照射したレーザ光がラマン散乱された散乱光を分光するラマン分光装置において、前記レーザ光の照射に先立って蛍光除去用レーザ光を照射する蛍光除去用レーザを備える。   The Raman spectroscopic device according to the present invention is a Raman spectroscopic device that scatters the scattered light in which the irradiated laser light is Raman-scattered, and includes a fluorescence removing laser that emits the fluorescence removing laser light prior to the laser light irradiation. .

この発明に係るラマン分光装置は、ラマン信号測定のレーザ照射部及び散乱光検出部と、その前段に蛍光除去用のレーザ照射部を備えた構成である。前段でのレーザ照射により蛍光発光強度を低減した後、ラマン散乱測定を行うことにより、蛍光の妨害を低減してＳ／Ｎ比の良好なラマン信号を得ることができるため、プラスチックの識別精度を向上させることができる。   The Raman spectroscopic device according to the present invention is configured to include a laser irradiation unit and a scattered light detection unit for Raman signal measurement, and a laser irradiation unit for removing fluorescence in the preceding stage. After reducing the fluorescence emission intensity by laser irradiation in the previous stage, the Raman scattering measurement can be performed to reduce the interference of fluorescence and obtain a Raman signal with a good S / N ratio. Can be improved.

本発明の実施の形態１に係るラマン分光装置を用いた識別装置の構成を示す図である。It is a figure which shows the structure of the identification device using the Raman spectroscopy apparatus which concerns on Embodiment 1 of this invention. 本発明の実施の形態１に係る識別装置で事前のレーザ照射による蛍光発光強度低減効果を示す図である。It is a figure which shows the fluorescence emission intensity | strength reduction effect by the prior laser irradiation in the identification device which concerns on Embodiment 1 of this invention. 蛍光除去用レーザ光の照射時間と発光する蛍光の強度の関係を示すグラフである。It is a graph which shows the relationship between the irradiation time of the laser beam for fluorescence removal, and the intensity | strength of emitted fluorescence. 本発明の実施の形態２に係るラマン分光装置を用いた識別装置の構成を示す図である。It is a figure which shows the structure of the identification device using the Raman spectroscopy apparatus which concerns on Embodiment 2 of this invention.

以下、本発明のラマン分光装置の好適な実施の形態につき図面を用いて説明する。
実施の形態１．
図１は、本発明の実施の形態１に係るラマン分光装置を用いた識別装置の構成を示す図である。
この発明の実施の形態１に係る識別装置は、図１に示すように、測定対象物４を第１ステージから第２ステージに順次搬送する試料台２０、第１ステージの直上に配置され入射された蛍光除去用レーザ光を第１ステージに向けて光路を変える除去用レーザ反射ミラー３、除去用レーザ反射ミラー３に蛍光除去用レーザ光を集光する除去用レーザ集光レンズ２、蛍光除去用レーザ光を発光する蛍光除去用レーザ１を備える。 Hereinafter, preferred embodiments of the Raman spectroscopic device of the present invention will be described with reference to the drawings.
Embodiment 1 FIG.
FIG. 1 is a diagram showing a configuration of an identification device using the Raman spectroscopic device according to Embodiment 1 of the present invention.
As shown in FIG. 1, the identification device according to Embodiment 1 of the present invention is arranged and incident on a sample stage 20 that sequentially conveys the measurement object 4 from the first stage to the second stage, and immediately above the first stage. The removal laser reflecting mirror 3 which changes the optical path by directing the removed fluorescence removal laser light to the first stage, the removal laser condensing lens 2 for condensing the fluorescence removal laser light on the removal laser reflection mirror 3, and the fluorescence removal A fluorescence removing laser 1 that emits laser light is provided.

また、識別装置は、第２ステージの直上に配置され入射された測定用レーザ光を第２ステージに向けて光路を変える測定用レーザ反射ミラー８、測定用レーザ反射ミラー８に測定用レーザ光を集光する測定用レーザ集光レンズ９、測定用レーザ光を発光する測定用レーザ５、測定用レーザ光の照射により発生する散乱光を集光する第１集光レンズ６及び第２集光レンズ７、入射された散乱光を分光してラマン信号を出力する分光器１０を備える。   Further, the identification device places the measurement laser light on the measurement laser reflection mirror 8 and the measurement laser reflection mirror 8 that changes the optical path of the measurement laser light that is arranged and incident directly above the second stage toward the second stage. Measuring laser condensing lens 9 for condensing, measuring laser 5 for emitting measuring laser light, first condensing lens 6 and second condensing lens for condensing scattered light generated by irradiation of the measuring laser light 7. A spectroscope 10 that splits the incident scattered light and outputs a Raman signal is provided.

蛍光除去用レーザ１は、発光するレーザの波長に制限は特になく、例えば、５１４．５ｎｍ、４８８．０ｎｍ（いずれもＡｒレーザ）、６３２．８ｎｍ（Ｈｅ−Ｎｅレーザ）、６４７．１ｎｍ（Ｋｒレーザ）、７８５ｎｍ（半導体レーザ）などを使用することができる。
また、蛍光除去用レーザ１と測定用レーザ５とを同一のものを用いても構わない。
なお、蛍光除去用レーザ１のパワーとしては、１〜５ｍＷ程度のものが使用可能であるが、測定対象物４の移動速度、測定対象物４までの距離によりパワーを変える必要があることは自明であり、特にこの値にとらわれない。装置構成により適切な値とする。 The laser 1 for removing fluorescence is not particularly limited in the wavelength of the emitted laser. For example, 514.5 nm, 488.0 nm (both Ar laser), 632.8 nm (He-Ne laser), 647.1 nm (Kr laser) ), 785 nm (semiconductor laser) or the like can be used.
Further, the same fluorescence removing laser 1 and measuring laser 5 may be used.
The power of the fluorescence removing laser 1 can be about 1 to 5 mW, but it is obvious that the power needs to be changed depending on the moving speed of the measuring object 4 and the distance to the measuring object 4. And is not particularly limited by this value. Use an appropriate value depending on the device configuration.

また、識別装置は、試料台２０、蛍光除去用レーザ１、測定用レーザ５及び分光器１０を制御する制御装置２１を備える。   The identification device also includes a control device 21 that controls the sample stage 20, the fluorescence removal laser 1, the measurement laser 5, and the spectrometer 10.

次に、この識別装置の動作について説明する。
試料台２０に測定対象物４を載せ、照射箇所が第１ステージに位置するように試料台２０を移動する。次に、蛍光除去用レーザ１から所定の時間、例えば２０秒間に亘って蛍光除去用レーザ光を発光する。これにより照射箇所に２０秒間蛍光除去用レーザ光が照射される。 Next, the operation of this identification device will be described.
The measurement object 4 is placed on the sample stage 20, and the sample stage 20 is moved so that the irradiation location is located on the first stage. Next, the fluorescence removal laser light is emitted from the fluorescence removal laser 1 for a predetermined time, for example, 20 seconds. Thereby, the laser beam for removing fluorescence is irradiated to the irradiated portion for 20 seconds.

次に、照射箇所が第２ステージに位置するように試料台２０を移動する。次に、測定用レーザ５から所定の時間、例えば５秒間に亘って測定用レーザ光を発光する。これにより照射箇所からラマン散乱光が発光する。このラマン散乱光が第１集光レンズ６及び第２集光レンズ７により分光器１０に集光される。
このように集光されて入射されたラマン散乱光は分光器１０により分光されて、プラスチックの素材や添加物に特有なラマン信号が得られる。 Next, the sample stage 20 is moved so that the irradiation location is located on the second stage. Next, the measurement laser beam is emitted from the measurement laser 5 for a predetermined time, for example, 5 seconds. Thereby, Raman scattered light is emitted from the irradiated portion. This Raman scattered light is condensed on the spectroscope 10 by the first condenser lens 6 and the second condenser lens 7.
The Raman scattered light that has been collected and incident in this manner is dispersed by the spectroscope 10 to obtain a Raman signal that is specific to plastic materials and additives.

図２は、蛍光除去用レーザ光を測定対象物４に照射した場合と照射しない場合での蛍光の発光強度を示すグラフである。
蛍光除去用レーザ光を照射しない場合のスペクトルでは、波数５００ｃｍ−１付近をピークとするブロードな蛍光信号であるが、事前に２０秒間蛍光除去用レーザ光を照射した場合のスペクトルでは、蛍光信号の強度が大きく低下している。
また、図３に示すように、蛍光信号は蛍光除去用レーザ光の照射時間とともに発光強度が低減する特徴を有している。これは発光に寄与する準位がキャリアで埋められていくための現象であるが、この特徴に着目して蛍光を低減するという本発明に至った。
尚、蛍光除去用レーザ光のパワーを強くした場合、プラスチック片が溶ける恐れがあるため、装置にあわせ適宜設計する必要があることはいうまでもない。 FIG. 2 is a graph showing the emission intensity of fluorescence when the measurement object 4 is irradiated with the laser light for fluorescence removal and when it is not irradiated.
In the spectrum when the laser beam for removing fluorescence is not irradiated, it is a broad fluorescence signal having a peak near the wave number of 500 cm −1 , but in the spectrum when irradiated with the laser beam for removing fluorescence for 20 seconds in advance, the fluorescence signal The strength is greatly reduced.
Further, as shown in FIG. 3, the fluorescence signal has a feature that the emission intensity decreases with the irradiation time of the fluorescence removal laser light. This is a phenomenon in which the level contributing to light emission is filled with carriers, but the present invention of reducing fluorescence by focusing on this feature has been achieved.
Needless to say, if the power of the laser light for removing fluorescence is increased, the plastic piece may be melted, so that it is necessary to design appropriately according to the apparatus.

この発明の実施の形態１に係るラマン分光装置では、蛍光除去用レーザ光の照射をラマン測定前に行われ、これにより蛍光の強度が低減される。従って、信号としてのラマン信号とノイズとしての蛍光との比が蛍光の強度が減少することにより改善されてラマン信号を確実に検出することができる。
また、このラマン分光装置を用いてプラスチックを識別して分けることにより、単一の種類のプラスチックだけ分けられるので、リサイクルを容易にする。
なお、蛍光除去用レーザ光に関してはレンズ、ミラーのいずれか、あるいは両方を無くして照射してもよい。 In the Raman spectroscopic device according to Embodiment 1 of the present invention, the irradiation of the fluorescence removing laser light is performed before the Raman measurement, thereby reducing the intensity of the fluorescence. Therefore, the ratio of the Raman signal as the signal and the fluorescence as the noise is improved by decreasing the intensity of the fluorescence, so that the Raman signal can be reliably detected.
Also, by identifying and separating plastics using this Raman spectroscopic device, only a single type of plastic can be separated, which facilitates recycling.
Note that the fluorescence removing laser light may be irradiated without either the lens or the mirror, or both.

実施の形態２．
図４は、本発明の実施の形態２によるラマン分光装置を用いた識別装置の構成を示す図である。
この発明の実施の形態１に係るラマン分光装置では、蛍光を減少するためにレーザ光をラマン分光に先だって照射させていたが、この発明の実施の形態２に係るラマン分光装置では、蛍光を減少するために紫外線をラマン分光に先立って照射させている。
この発明の実施の形態２に係る識別装置では、図４に示すように、紫外線照射部２２で測定対象物４に紫外線が照射される。この紫外線照射はラマン測定前に行われ、これにより蛍光の強度が低減される。これに続いて測定用レーザ５から照射された光がレンズ８、ミラー９を介して測定対象物４に照射される。 Embodiment 2. FIG.
FIG. 4 is a diagram showing a configuration of an identification device using the Raman spectroscopic device according to the second embodiment of the present invention.
In the Raman spectroscopic device according to the first embodiment of the present invention, the laser beam is irradiated prior to the Raman spectroscopy in order to reduce the fluorescence. However, in the Raman spectroscopic device according to the second embodiment of the present invention, the fluorescence is decreased. In order to do this, ultraviolet rays are irradiated prior to Raman spectroscopy.
In the identification device according to Embodiment 2 of the present invention, as shown in FIG. 4, the ultraviolet ray irradiation unit 22 irradiates the measurement object 4 with ultraviolet rays. This ultraviolet irradiation is performed before the Raman measurement, whereby the intensity of fluorescence is reduced. Subsequently, the light irradiated from the measurement laser 5 is irradiated to the measurement object 4 through the lens 8 and the mirror 9.

このレーザ照射により発生する散乱光は第１集光レンズ６と第２集光レンズ７により集光され、分光器に導かれ、ラマン信号が得られる。散乱光には蛍光も含まれるため、蛍光信号もラマン信号と同時に検出される。
なお、紫外線の照射時間、照射距離等は識別装置の構成により適宜設計すればよい。
移動に通常用いられるベルトコンベアライン全体に用いても構わないし、一部分に用いても構わない。
但し、あまり照射時間を長くしたり、照射距離を短くしたりすれば、プラスチック片の変質等を起こす恐れがあるため、変質等が起こらない適切照射量を調整する必要がある。 Scattered light generated by this laser irradiation is condensed by the first condenser lens 6 and the second condenser lens 7 and guided to the spectroscope to obtain a Raman signal. Since the scattered light includes fluorescence, the fluorescence signal is detected simultaneously with the Raman signal.
Note that the ultraviolet irradiation time, irradiation distance, and the like may be appropriately designed depending on the configuration of the identification device.
You may use for the whole belt conveyor line normally used for a movement, and you may use for a part.
However, if the irradiation time is too long or the irradiation distance is shortened, the plastic piece may be deteriorated. Therefore, it is necessary to adjust an appropriate irradiation amount that does not cause deterioration.

１ 蛍光除去用レーザ、２、９ レンズ、３、８ ミラー、４ 測定対象物、５ 測定用レーザ、６ 第１集光レンズ、７ 第２集光レンズ、１０ 分光器、２０ 試料台、２１ 制御装置、２２ 紫外線照射部。   DESCRIPTION OF SYMBOLS 1 Fluorescence removal laser, 2, 9 lens, 3, 8 mirror, 4 measurement object, 5 measurement laser, 6 1st condensing lens, 7 2nd condensing lens, 10 Spectroscope, 20 Sample stand, 21 Control Device, 22 UV irradiation unit.

Claims (3)

照射したレーザ光がラマン散乱された散乱光を分光するラマン分光装置において、
前記レーザ光の照射に先立って蛍光除去用レーザ光を照射する蛍光除去用レーザを備えることを特徴とするラマン分光装置。 In the Raman spectroscopic device that scatters the scattered light in which the irradiated laser light is Raman scattered,
A Raman spectroscopic apparatus comprising: a fluorescence removal laser that emits fluorescence removal laser light prior to the laser light irradiation. 照射したレーザ光がラマン散乱された散乱光を分光するラマン分光装置において、
前記レーザ光の照射に先立って紫外線を照射する紫外線照射手段を備えることを特徴とするラマン分光装置。 In the Raman spectroscopic device that scatters the scattered light in which the irradiated laser light is Raman scattered,
A Raman spectroscopic device comprising ultraviolet irradiation means for irradiating ultraviolet light prior to the laser light irradiation. 請求項１または２に記載のラマン分光装置を用いてプラスチックを識別することを特徴とする識別装置。   An identification device, wherein plastic is identified using the Raman spectroscopic device according to claim 1.
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