JPH0772011A

JPH0772011A - Scattered light measuring device and scattered light measuring method

Info

Publication number: JPH0772011A
Application number: JP649394A
Authority: JP
Inventors: Takuya Uzumaki; 拓也渦巻; Atsushi Tanaka; 厚志田中
Original assignee: Fujitsu Ltd
Current assignee: Fujitsu Ltd
Priority date: 1993-06-21
Filing date: 1994-01-25
Publication date: 1995-03-17

Abstract

(57)【要約】（修正有）【目的】散乱光についての信頼性の高い波数データや強
度データを短時間に取得し、ノイズを低減して微弱なラ
マン散乱光を確実に検出する。【構成】励起光を出射する光源１と、既知の発光線スペ
クトルを有する第１の基準光を出射する第１の基準光源
２と、既知の分光エネルギ強度を有する第２の基準光を
出射する第２の基準光源８と、励起光の照射により被測
定試料７から出射された散乱光又は基準光源２又は８か
ら出射された基準光を入射し、分光する分光器３と、基
準光源２及び８のうち基準光を出射する基準光源２又は
８を選択する選択手段１０と、分光器３への散乱光の入
射と基準光の入射とを切り換える切替え手段４ａと、分
光器３を通った散乱光又は基準光を検出する光検出器５
と、検出された散乱光の強度を強度補正因子により補正
する波数校正及び強度補正手段１１とを有する。 (57) [Summary] (Correction) [Purpose] To acquire highly reliable wave number data and intensity data for scattered light in a short time, reduce noise, and reliably detect weak Raman scattered light. A light source 1 for emitting excitation light, a first reference light source 2 for emitting a first reference light having a known emission line spectrum, and a second reference light having a known spectral energy intensity are emitted. The second reference light source 8, the spectroscope 3 for injecting and dispersing the scattered light emitted from the sample 7 to be measured by the irradiation of the excitation light or the reference light emitted from the reference light source 2 or 8, and the reference light source 2 and The selection means 10 for selecting the reference light source 2 or 8 which emits the reference light among the eight, the switching means 4a for switching the incidence of the scattered light to the spectroscope 3 and the incidence of the reference light, and the scattering through the spectroscope 3 Photodetector 5 for detecting light or reference light
And a wave number calibration and intensity correction means 11 for correcting the intensity of the scattered light detected by an intensity correction factor.

Description

【発明の詳細な説明】Detailed Description of the Invention

【０００１】[0001]

【産業上の利用分野】本発明は散乱光測定装置及び散乱
光測定方法に関し、更に詳しく言えば、励起光の照射に
より被測定体から出射した散乱光を検出する散乱光測定
装置及び散乱光測定方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a scattered light measuring device and a scattered light measuring method, and more particularly to a scattered light measuring device and scattered light measuring device for detecting scattered light emitted from an object to be measured by irradiation of excitation light. Regarding the method.

【０００２】[0002]

【従来の技術】近年、酸化物超電導体の高品質な膜及び
基板が要望されるようになり、これに伴って、より精密
な、かつより多くの情報量が得られる結晶評価技術の必
要性が高まっている。このような結晶評価技術は光を用
いたものが主流となっている。このうち、ラマン散乱光
の測定による結晶評価技術は、他の測定手段では困難な
フォノンエネルギの大きさを測定することができ、結晶
状態の情報が直接得られるため注目を集めている。その
結晶評価の原理は、レーザ光を試料に入射して媒質中の
原子や分子の運動を励起し、分子の振動エネルギや回転
エネルギにより変調を受けた微弱な散乱光を分光器に通
して波長選択等した上で光検出器で検出し、入射光に対
する散乱光の波数シフトや散乱光の強度を測定して原子
の結合状態を評価するものである。2. Description of the Related Art In recent years, there has been a demand for high-quality oxide superconductor films and substrates, and along with this, the need for a crystal evaluation technique capable of obtaining more precise and more information. Is increasing. The mainstream of such crystal evaluation technology is the use of light. Among them, the crystal evaluation technique by measuring Raman scattered light is attracting attention because it is possible to measure the magnitude of phonon energy, which is difficult with other measuring means, and information on the crystal state can be directly obtained. The principle of crystal evaluation is that laser light is incident on the sample to excite the motion of atoms and molecules in the medium, and the weak scattered light modulated by the vibrational energy and rotational energy of the molecule is passed through a spectroscope to determine the wavelength. After selecting, etc., it is detected by a photodetector, and the wave number shift of scattered light with respect to incident light and the intensity of scattered light are measured to evaluate the bonding state of atoms.

【０００３】波数シフトは分子の振動や回転の状態等を
評価するために重要なパラメータであり、散乱光の強度
は散乱分子の周囲温度や励起された分子数等を評価する
ために重要なパラメータである。従って、これらの正確
な測定が超電導体薄膜等の精度のよい評価のために不可
欠である。ところで、光検出器の感度特性は一般に波長
依存性を有し、また、分光器中の回折格子やミラーの反
射率の波長依存性も大きい。更に、極端に感度の変化が
ある場合にはピーク位置もずれる可能性がある。従っ
て、散乱光の強度の正確な測定のためには感度補正が不
可欠であり、分光器及び光検出器双方を含めた感度補正
を行う必要がある。The wave number shift is an important parameter for evaluating the state of vibration and rotation of molecules, and the intensity of scattered light is an important parameter for evaluating the ambient temperature of scattered molecules and the number of excited molecules. Is. Therefore, these accurate measurements are indispensable for accurate evaluation of the superconductor thin film and the like. By the way, the sensitivity characteristic of the photodetector generally has wavelength dependency, and the reflectance of the diffraction grating and the mirror in the spectroscope also has large wavelength dependency. Furthermore, if there is an extreme change in sensitivity, the peak position may shift. Therefore, sensitivity correction is indispensable for accurate measurement of scattered light intensity, and it is necessary to perform sensitivity correction including both the spectroscope and the photodetector.

【０００４】また、分光器が選択する波数は回折格子の
微妙なずれ等により真のラマンシフトを示さない場合が
多い。例えば、回折格子を溝1200本／ｍｍから溝2400本
／ｍｍのものに変え、更に溝1200本／ｍｍの回折格子に
戻した場合、約１０ｃｍ^-1の誤差が生ずる。これは装置
の欠陥ではなくて回折格子を回転させたことによるもの
である。従って、散乱光の波数の正確な測定のためには
波数校正が不可欠である。In many cases, the wave number selected by the spectroscope does not show a true Raman shift due to a slight shift of the diffraction grating. For example, when the diffraction grating is changed from 1200 grooves / mm to 2400 grooves / mm and is returned to the diffraction grating having 1200 grooves / mm, an error of about 10 cm ^-1 occurs. This is due to rotating the diffraction grating rather than the device defect. Therefore, wave number calibration is indispensable for accurate measurement of the wave number of scattered light.

【０００５】従来、波数校正や感度補正を行う場合、試
料の位置に基準光源を置いて波数校正データや感度補正
データを取得している。また、ラマン散乱光の測定で
は、ラマン散乱光が非常に微弱であるため、超高感度の
光検出器と明るい分光器が必要である。最近の半導体光
検出器の作成技術の発展により、超高感度のＣＣＤ（Ch
arge Coupled Device ）が製造されており、このような
超高感度のＣＣＤは、一度に数百点の測定が行えるた
め、超高感度の光検出器として脚光を浴びている。Conventionally, when performing wave number calibration or sensitivity correction, a reference light source is placed at the position of a sample to obtain wave number calibration data or sensitivity correction data. Further, in the measurement of Raman scattered light, since the Raman scattered light is extremely weak, an ultra-sensitive photodetector and a bright spectroscope are required. Due to recent developments in semiconductor photodetector fabrication technology, ultra-sensitive CCD (Ch
Arge Coupled Device) is manufactured, and such an ultra-sensitive CCD is capable of measuring several hundred points at a time, and thus is in the spotlight as an ultra-sensitive photodetector.

【０００６】更に、超電導体膜の分析の場合、温度依存
性を測定する必要がある。この場合、被測定体の温度の
均一性を向上するため、被測定体のホルダとして高熱伝
導率を有する銅が用いられる。Further, in the case of analyzing a superconductor film, it is necessary to measure the temperature dependence. In this case, in order to improve the temperature uniformity of the object to be measured, copper having a high thermal conductivity is used as the holder of the object to be measured.

【０００７】[0007]

【発明が解決しようとする課題】しかし、波数校正デー
タや感度補正データを取得するために試料と基準光源と
をいちいち取り替える必要があり、長時間を必要とす
る。このため、ルーチンワークによる測定を行う必要が
ある場合には、時間のロスが多い。更に、波数校正デー
タや感度補正データを取得する者が異なると、取得デー
タも異なってくる場合が多く、波数データや強度データ
の信頼性が確保できない。However, in order to obtain the wave number calibration data and the sensitivity correction data, it is necessary to replace the sample with the reference light source, which requires a long time. Therefore, there is a lot of time loss when it is necessary to perform measurement by routine work. Further, if the person who acquires the wave number calibration data and the sensitivity correction data is different, the acquired data often differs, and the reliability of the wave number data and the intensity data cannot be secured.

【０００８】また、超高感度のＣＣＤは宇宙線に敏感に
反応するため、測定データの中に宇宙線によるパルス状
のノイズが含まれる。従って、宇宙線によるノイズが所
望のラマン散乱光に重なったり、所望のラマン散乱光と
宇宙線によるノイズとの区別がつかなくなったりしてし
まい、分析が困難になる。更に、被測定体のホルダとし
て銅が用いられ、かつ被測定体が超電導体膜等、光透過
性の被測定体である場合、光透過性の被測定体に入射し
た光は銅のホルダにより反射され、この反射光はラマン
散乱光とともに光検出器で検出されるため、ラマン散乱
光が反射光に埋もれてしまう。Further, since the ultra-sensitive CCD reacts sensitively to cosmic rays, pulsed noise due to cosmic rays is included in the measurement data. Therefore, noise due to cosmic rays overlaps with desired Raman scattered light, or the desired Raman scattered light and noise due to cosmic rays are indistinguishable, which makes analysis difficult. Further, when copper is used as a holder for the object to be measured, and the object to be measured is a light transmissive object to be measured such as a superconductor film, the light incident on the light transmissive object is measured by the copper holder. Since the reflected light is detected by the photodetector together with the Raman scattered light, the Raman scattered light is buried in the reflected light.

【０００９】本発明はかかる従来例の問題点に鑑み創作
されたものであり、散乱光についての信頼性の高い波数
データや強度データを短時間に取得し、ノイズを低減し
て微弱なラマン散乱光を確実に検出することが可能な散
乱光測定装置及び散乱光測定方法の提供を目的とする。The present invention was created in view of the problems of the conventional example, and obtains highly reliable wave number data and intensity data of scattered light in a short time to reduce noise and weak Raman scattering. An object of the present invention is to provide a scattered light measuring device and a scattered light measuring method capable of surely detecting light.

【００１０】[0010]

【課題を解決するための手段】上記課題は、第１に、図
１に示すように、励起光を出射する光源１と、既知の発
光線スペクトルを有する第１の基準光を出射する第１の
基準光源２と、前記励起光の照射により被測定体７から
出射された散乱光又は前記第１の基準光源２から出射さ
れた前記基準光を入射し、分光する分光器３と、前記分
光器３への前記散乱光の入射と前記基準光の入射を切り
換える切替え手段４と、前記分光器３を通った前記散乱
光又は前記光を検出する光検出器５と、前記分光器３を
通った前記基準光のスペクトルと前記発光線スペクトル
との比較から波数誤差を取得して、検出された前記散乱
光の波数を前記波数誤差により校正する波数校正手段６
とを有することを特徴とする散乱光測定装置によって達
成され、第２に、図２に示すように、励起光を出射する
光源１と、既知の分光エネルギ強度を有する第２の基準
光を出射する第２の基準光源８と、前記励起光の照射に
より被測定体７から出射された散乱光又は前記第２の基
準光源８から出射された前記基準光を入射し、分光する
分光器３と、前記分光器３への前記散乱光の入射と前記
基準光の入射とを切り換える切替え手段４と、前記分光
器３を通った前記散乱光又は前記基準光を検出する光検
出器５と、前記分光器３を通った前記基準光の強度と前
記分光エネルギ強度との比較から強度補正因子を取得し
て、検出された前記散乱光の強度を前記強度補正因子に
より補正する強度補正手段９とを有することを特徴とす
る散乱光測定装置によって達成され、第３に、図３に示
すように、励起光を出射する光源１と、既知の発光線ス
ペクトルを有する第１の基準光を出射する第１の基準光
源２と、既知の分光エネルギ強度を有する第２の基準光
を出射する第２の基準光源８と、前記励起光の照射によ
り被測定試料７から出射された散乱光又は前記基準光源
２又は８から出射された前記基準光を入射し、分光する
分光器３と、前記基準光源２及び８のうち前記基準光を
出射する前記基準光源２又は８を選択する選択手段１０
と、前記分光器３への前記散乱光の入射と前記基準光の
入射とを切り換える切替え手段４ａと、前記分光器３を
通った前記散乱光又は前記基準光を検出する光検出器５
と、前記分光器３を通った前記第１の基準光のスペクト
ルと前記発光線スペクトルとの比較から波数誤差を取得
して、検出された前記散乱光の波数を前記波数誤差によ
り校正し、かつ前記分光器３を通った前記第２の基準光
の強度と前記分光エネルギ強度との比較から強度補正因
子を取得して、検出された散乱光の強度を前記強度補正
因子により補正する波数校正及び強度補正手段１１とを
有することを特徴とする散乱光測定装置によって達成さ
れ、第４に、励起光を出射する光源と、前記励起光の照
射により散乱光を出射する被測定体を保持し、前記被測
定体の保持面がカーボンで被覆されている銅基板からな
るホルダと、前記散乱光を入射し、分光する分光器と、
前記分光器を通過した散乱光を検出する光検出器とを有
する散乱光測定装置によって達成され、第５に、励起光
を出射する光源と、前記励起光の照射により散乱光を出
射する被測定体を保持するＭｇＯ単結晶からなるホルダ
と、前記散乱光を入射し、分光する分光器と、前記分光
器を通った散乱光を検出する光検出器とを有する散乱光
測定装置によって達成され、第６に、前記被測定体の周
辺部に該被測定体の冷却手段を有することを特徴とする
第４又は第５の発明に記載の散乱光測定装置によって達
成され、第７に、前記光検出器はＣＣＤであることを特
徴とする第４，第５又は第６の発明に記載の散乱光測定
装置によって達成され、第８に、前記光検出器は鉛から
なる被覆手段により被覆されていることを特徴とする第
４，第５，第６又は第７の発明に記載の散乱光測定装置
によって達成され、第９に、励起光の照射により前記被
測定体から出射された散乱光を光検出器により検出して
前記被測定体を分析する散乱光測定方法であって、前記
散乱光のうちレーリー光を前記光検出器の画素を介して
検出することにより、前記光検出器の全露光領域のう
ち、前記レーリー光により露光された画素を含む領域を
使用すべき露光領域として予め確定しておき、前記使用
すべき露光領域の画素のみ動作させ、かつ前記使用すべ
き露光領域の画素以外の画素の動作を停止した状態で、
前記被測定体からの散乱光を検出することを特徴とする
散乱光測定方法によって達成され、第１０に、励起光の
照射により前記被測定体から出射された散乱光を光検出
器により検出して前記被測定体を分析する散乱光測定方
法であって、前記光検出器に入射する宇宙線によるノイ
ズ量の経時的な蓄積量を予め測定しておき、前記散乱光
の測定に支障がない程度のノイズ量が蓄積される時間の
範囲内で前記光検出器の露光時間を設定することを特徴
とする散乱光測定方法によって達成され、第１１に、前
記被測定体は超電導体膜であることを特徴とする第９又
は第１０の発明に記載の散乱光測定方法によって達成さ
れ、第１２に、前記光検出器はＣＣＤであることを特徴
とする第９，第１０又は第１１の発明に記載の散乱光測
定方法によって達成される。First, as shown in FIG. 1, a light source 1 for emitting excitation light and a first reference light having a known emission line spectrum are emitted. Of the reference light source 2, and the spectroscope 3 for injecting and dispersing the scattered light emitted from the device under test 7 by the irradiation of the excitation light or the reference light emitted from the first reference light source 2, Switching means 4 for switching the incidence of the scattered light and the incidence of the reference light on the spectroscope 3, the photodetector 5 for detecting the scattered light or the light that has passed through the spectroscope 3, and the spectroscope 3 A wave number calibrating means 6 for acquiring a wave number error from the comparison between the spectrum of the reference light and the emission line spectrum and calibrating the wave number of the detected scattered light by the wave number error.
And a second light source 1 for emitting excitation light and a second reference light having a known spectral energy intensity, as shown in FIG. A second reference light source 8 and a spectroscope 3 for injecting the scattered light emitted from the DUT 7 by the irradiation of the excitation light or the reference light emitted from the second reference light source 8 to disperse the light. A switching means 4 for switching between the incidence of the scattered light and the incidence of the reference light on the spectroscope 3, a photodetector 5 for detecting the scattered light or the reference light passing through the spectroscope 3, and An intensity correction unit 9 for obtaining an intensity correction factor from the comparison between the intensity of the reference light that has passed through the spectroscope 3 and the spectral energy intensity and correcting the detected intensity of the scattered light by the intensity correction factor. A scattered light measuring device characterized by having Thirdly, as shown in FIG. 3, a light source 1 for emitting excitation light, a first reference light source 2 for emitting a first reference light having a known emission line spectrum, and a known spectroscopic light are achieved. A second reference light source 8 which emits a second reference light having energy intensity, and scattered light emitted from the sample 7 to be measured by irradiation of the excitation light or the reference light emitted from the reference light source 2 or 8. And a selecting means 10 for selecting the reference light source 2 or 8 which emits the reference light from the reference light sources 2 and 8 which makes the reference light incident.
A switching means 4a for switching the incident of the scattered light to the spectroscope 3 and the incident of the reference light, and a photodetector 5 for detecting the scattered light or the reference light having passed through the spectroscope 3.
A wave number error is obtained from a comparison between the spectrum of the first reference light that has passed through the spectroscope 3 and the emission line spectrum, and the wave number of the detected scattered light is calibrated by the wave number error, and A wave number calibration that acquires an intensity correction factor from a comparison between the intensity of the second reference light that has passed through the spectroscope 3 and the spectral energy intensity, and corrects the intensity of the detected scattered light by the intensity correction factor, and A fourth aspect of the present invention is achieved by a scattered light measuring device having an intensity correcting means 11, and fourthly, a light source that emits excitation light and a measured object that emits scattered light by irradiation of the excitation light are held. A holder made of a copper substrate on which the holding surface of the object to be measured is coated with carbon, and a spectroscope for injecting the scattered light and separating the light,
A scattered light measuring device having a photodetector for detecting scattered light that has passed through the spectroscope. Fifth, a light source for emitting excitation light, and a device under test for emitting scattered light by irradiation of the excitation light. It is achieved by a scattered light measuring device having a holder made of a MgO single crystal holding a body, a spectroscope for injecting the scattered light to disperse the light, and a photodetector for detecting the scattered light passing through the spectroscope. Sixth, it is achieved by the scattered light measuring device according to the fourth or fifth invention, characterized in that it has a cooling means for the object to be measured in the peripheral part of the object to be measured. The detector is a CCD, which is achieved by the scattered light measuring device according to the fourth, fifth or sixth invention, and eighthly, the photodetector is coated with a coating means made of lead. 4th, 5th, 6th or A ninth aspect of the present invention is a scattering device which is achieved by the scattered light measuring device according to the seventh invention, and ninthly, detects scattered light emitted from the object to be measured by irradiation of excitation light with a photodetector to analyze the object to be measured. A light measurement method, wherein Rayleigh light of the scattered light is detected through pixels of the photodetector, and among the entire exposure region of the photodetector, the pixels exposed by the Rayleigh light are included. The area is previously determined as the exposure area to be used, only the pixels of the exposure area to be used are operated, and the operation of the pixels other than the pixels of the exposure area to be used is stopped,
This is achieved by a scattered light measuring method characterized by detecting scattered light from the measured object, and tenthly, detecting scattered light emitted from the measured object by irradiation of excitation light with a photodetector. A method for measuring scattered light by analyzing the object to be measured, wherein the accumulated amount of noise due to cosmic rays incident on the photodetector is measured in advance so that the scattered light is not hindered. This is achieved by a scattered light measuring method, characterized in that the exposure time of the photodetector is set within a range of time in which a certain amount of noise is accumulated. Eleventh, the measured object is a superconductor film. The present invention is achieved by the scattered light measuring method according to the ninth or tenth aspect of the invention, and the twelfth aspect is that the photodetector is a CCD. Reached by the scattered light measurement method described in It is.

【００１１】[0011]

【作用】本発明に係る光散乱測定装置によれば、図１
に示すように、既知の発光線スペクトルを有する第１の
基準光を出射する第１の基準光源２を有し、かつ第１の
基準光の入射と被測定体７からの散乱光の入射とを切り
換える切替え手段４を有するので、波数校正と波数測定
の切替えを適宜行い、散乱光の波数の測定と校正を短時
間で行うことができる。[Operation] According to the light scattering measuring apparatus of the present invention,
As shown in FIG. 3, the first reference light source 2 for emitting the first reference light having a known emission line spectrum is provided, and the first reference light is incident and the scattered light is incident from the DUT 7. Since the switching unit 4 for switching between the wave number and the wave number is provided, the wave number calibration and the wave number measurement can be appropriately switched, and the wave number of the scattered light can be measured and calibrated in a short time.

【００１２】また、波数校正手段６を有するので、測定
者によらず、散乱光の波数について信頼性の高いデータ
が得られる。更に、図２に示すように、既知の分光エネ
ルギ強度を有する第２の基準光を出射する第２の基準光
源８を有し、かつ第２の基準光の入射と被測定体７から
の散乱光の入射とを切り換える切替え手段４を有するの
で、強度補正と強度測定の切替えを適宜行い、散乱光の
強度の測定と補正を短時間で行うことができる。Further, since the wave number calibrating means 6 is provided, highly reliable data on the wave number of scattered light can be obtained regardless of the operator. Further, as shown in FIG. 2, a second reference light source 8 for emitting a second reference light having a known spectral energy intensity is provided, and the second reference light is incident and scattered from the measured object 7. Since the switching means 4 for switching the incidence of light is included, the intensity correction and the intensity measurement can be appropriately switched, and the intensity and the correction of the scattered light can be performed in a short time.

【００１３】また、強度補正手段９を有するので、測定
者によらず、散乱光の強度について信頼性の高いデータ
が得られる。更に、図３に示すように、上記第１の基準
光源２と第２の基準光源８とを有し、第１の基準光源２
及び第２の基準光源８のうち基準光を出射する基準光源
２又は８を選択する選択手段１０を有するので、波数補
正と強度補正をともに行える。Further, since the intensity correction means 9 is provided, highly reliable data on the intensity of scattered light can be obtained regardless of the person who makes the measurement. Further, as shown in FIG. 3, the first reference light source 2 and the second reference light source 8 are provided, and the first reference light source 2 is provided.
Further, since the selection means 10 for selecting the reference light source 2 or 8 which emits the reference light among the second reference light sources 8 is provided, both wave number correction and intensity correction can be performed.

【００１４】また、基準光源２及び８のいずれかからの
基準光の入射と被測定試料７からの散乱光の入射とを切
り換える切替え手段４ａを有するので、波数校正及び強
度補正と、波数及び強度測定との切替えを適宜行い、散
乱光の波数及び強度の測定と校正及び補正を短時間で行
うことができる。更に、波数校正及び強度補正手段１１
を有するので、測定者によらず、散乱光の波数及び強度
について信頼性の高いデータが得られる。Further, since the switching means 4a for switching between the incidence of the reference light from any of the reference light sources 2 and 8 and the incidence of the scattered light from the sample to be measured 7 is provided, the wave number calibration and the intensity correction, the wave number and the intensity are performed. By appropriately switching between measurement and measurement, the wave number and intensity of scattered light can be measured, and calibration and correction can be performed in a short time. Further, the wave number calibration and intensity correction means 11
Therefore, highly reliable data on the wave number and intensity of scattered light can be obtained regardless of the operator.

【００１５】また、ホルダは被測定体の保持面がカーボ
ンで被覆されているので、被測定体が光透過性を有する
場合に励起光が被測定体を透過し、ホルダの被測定体の
保持面に達しても、励起光はカーボンにより吸収される
ため、反射光の強度は弱くなる。これにより、入射側に
戻ってくる測定すべき散乱光の強度は相対的に強くなる
ため、Ｓ／Ｎ比は改善され、強度の弱い散乱光がノイズ
に埋もれることなく光検出器、例えばＣＣＤに有効に検
出される。Further, since the holding surface of the object to be measured of the holder is coated with carbon, the excitation light passes through the object to be measured when the object to be measured has optical transparency, and the holder holds the object to be measured. Even when it reaches the surface, the intensity of the reflected light becomes weak because the excitation light is absorbed by the carbon. As a result, the intensity of scattered light returning to the incident side to be measured becomes relatively strong, so that the S / N ratio is improved, and scattered light of low intensity is not buried in noise and is detected by a photodetector, such as a CCD. Effectively detected.

【００１６】更に、ホルダはＭｇＯ単結晶からなるた
め、被測定体が光透過性を有する場合、励起光が被測定
体を透過し、ホルダの被測定体の保持面に達しても、励
起光はそのままホルダを透過して入射側と反対側に出射
する。従って、反射光はほとんど生じないので、Ｓ／Ｎ
比が改善され、入射側に戻ってくる測定すべき散乱光が
ノイズに埋もれることなく有効に検出される。また、Ｍ
ｇＯ単結晶は熱伝導性が良いので、銅のホルダと同じよ
うに、温度の均一性を保持することができ、温度依存性
の測定に用いることができる。Further, since the holder is made of MgO single crystal, when the measured object has optical transparency, even if the excitation light passes through the measured object and reaches the holding surface of the measured object of the holder, the excitation light Passes through the holder as it is and is emitted to the side opposite to the incident side. Therefore, since almost no reflected light is generated, S / N
The ratio is improved, and scattered light to be measured returning to the incident side is effectively detected without being buried in noise. Also, M
Since the gO single crystal has good thermal conductivity, it can maintain the temperature uniformity as in the case of the copper holder and can be used for measuring the temperature dependence.

【００１７】また、被測定体の周辺部に被測定体の冷却
手段を有しているので、例えば、被測定体が超電導体膜
の場合に、温度依存性を取得することが可能となる。更
に、光検出器が鉛からなる被覆手段により被覆されてい
るので、宇宙線を防御することができる。このため、Ｓ
／Ｎ比は改善され、ノイズに妨害されることなく強度の
弱い散乱光が有効に検出される。Further, since the cooling means for the object to be measured is provided in the peripheral portion of the object to be measured, it is possible to obtain the temperature dependence when the object to be measured is a superconductor film. Furthermore, since the photodetector is coated with lead coating means, cosmic rays can be protected. Therefore, S
The / N ratio is improved, and scattered light of low intensity is effectively detected without being disturbed by noise.

【００１８】本発明に係る光散乱測定方法によれば、散
乱光により露光される有効な露光領域の画素のみを動作
させ、その領域以外の画素の動作を停止した状態で、被
測定体からの散乱光を測定するようにしている。従っ
て、露光領域が必要最小限に制限されるため、露光され
る宇宙線の量を減少することができる。このため、強度
の弱い散乱光に対する検出感度を落とすことなく、ノイ
ズのみを減少させることができる。これにより、Ｓ／Ｎ
比は改善され、宇宙線によるノイズに妨害されることな
く強度の弱い散乱光が有効に検出される。According to the light scattering measuring method of the present invention, only the pixels in the effective exposure area exposed by the scattered light are operated, and the operation of the pixels other than the area is stopped, and I try to measure scattered light. Therefore, since the exposure area is limited to the necessary minimum, the amount of exposed cosmic rays can be reduced. For this reason, it is possible to reduce only noise without lowering the detection sensitivity for scattered light of low intensity. As a result, S / N
The ratio is improved and weakly scattered light is effectively detected without interference from cosmic ray noise.

【００１９】また、光検出器に入射する宇宙線によるノ
イズ量の経時的な蓄積量を予め測定しておき、前記散乱
光の測定に支障がない程度のノイズ量が蓄積される時間
の範囲内で露光時間を設定しているので、Ｓ／Ｎ比は改
善され、宇宙線によるノイズに妨害されることなく強度
の小さい散乱光が有効に検出される。Further, the accumulated amount of noise due to cosmic rays incident on the photodetector is measured in advance, and the accumulated noise amount is within a range of time that does not hinder the measurement of the scattered light. Since the exposure time is set by, the S / N ratio is improved, and scattered light with low intensity is effectively detected without being disturbed by noise due to cosmic rays.

【００２０】[0020]

【実施例】以下に、本発明の実施例について図面を参照
しながら説明する。（Ａ）本発明の実施例に係る散乱光測定装置の構成につ
いての説明（１）第１の実施例（ｉ）第１の実施例に係る散乱光測定装置の構成につい
ての説明図４は本発明の第１の実施例に係る波数校正及び強度補
正手段を備えた散乱光測定装置について示す構成図であ
る。Embodiments of the present invention will be described below with reference to the drawings. (A) Description of Configuration of Scattered Light Measuring Device According to Example of the Present Invention (1) First Example (i) Description of Configuration of Scattered Light Measuring Device According to First Example FIG. It is a block diagram shown about the scattered light measuring device provided with the wave number calibration and intensity | strength correction means which concerns on the 1st Example of invention.

【００２１】図４において、２１は波長５１４．５ｎｍ
のレーザ光（励起光又は光）を出射するアルゴンレーザ
（光源又は光出射手段）、２２はプリモノクロメータ
（光学手段）である。３６は被測定体で、ＭｇＯ基板28
ａ上にＡｇペーストを用いてBi-Sr-Ca-Cu-O膜（ＢＳＣ
ＣＯ膜：超電導体膜）が張りつけられている。この被測
定体３６は、クライオスタット中に保持されて、例えば
液体窒素や液体ヘリウムにより１０Ｋまで冷却され、保
温される。これにより、超電導体膜が超電導状態になる
温度の前後の超電導体膜の性質を観察することが可能に
なる。In FIG. 4, 21 is a wavelength of 514.5 nm
Is an argon laser (light source or light emitting means) that emits laser light (excitation light or light), and 22 is a pre-monochromator (optical means). 36 is a measured object, which is a MgO substrate 28
Bi-Sr-Ca-Cu-O film (BSC
A CO film: a superconductor film) is attached. The device under test 36 is held in a cryostat, cooled to 10 K by, for example, liquid nitrogen or liquid helium, and kept warm. This makes it possible to observe the properties of the superconductor film before and after the temperature at which the superconductor film becomes in the superconducting state.

【００２２】２４は被測定体からのラマン散乱光のうち
所望の波長のラマン散乱光を選択して光検出器としての
ＣＣＤ（Charge Coupled Device ）２５に導く分光器
（光学手段）である。分光器２４は多数のミラーＭ０〜
Ｍ７，回折格子Ｇ１〜Ｇ５を有し、散乱光の反射・回折
を繰り返すことにより測定すべき特定の波長のラマン散
乱光を選択する。A spectroscope (optical means) 24 selects Raman scattered light of a desired wavelength from the Raman scattered light from the object to be measured and guides it to a CCD (Charge Coupled Device) 25 as a photodetector. The spectroscope 24 includes a large number of mirrors M0 to M0.
M7 and diffraction gratings G1 to G5 are provided, and Raman scattered light having a specific wavelength to be measured is selected by repeating reflection / diffraction of scattered light.

【００２３】また、ヘリウム−ネオン（Ｈｅ−Ｎｅ）レ
ーザ３７を有し、ここから試験用のレーザ光を出射して
ミラーＭ０〜Ｍ７，回折格子Ｇ１〜Ｇ５で反射・回折さ
せることによりミラーＭ０〜Ｍ７，回折格子Ｇ１〜Ｇ５
の正しい角度等の調整を行う。ミラーＭ０〜Ｍ７のう
ち、ミラーＭ０（切替え手段）は分光器２４の入射部に
設置されており、不図示の駆動手段（切替え手段）によ
りミラーＭ０の角度を調整することができる。これによ
り、分光器２４への散乱光の入射と第１の基準光源２８
又は第２の基準光源２９からの光の入射とを切り換える
ことができる。Further, a helium-neon (He-Ne) laser 37 is provided, and a test laser beam is emitted from the laser 37 and reflected and diffracted by the mirrors M0 to M7 and the diffraction gratings G1 to G5. M7, diffraction gratings G1 to G5
Adjust the correct angle, etc. Of the mirrors M0 to M7, the mirror M0 (switching means) is installed at the entrance of the spectroscope 24, and the angle of the mirror M0 can be adjusted by driving means (switching means) not shown. As a result, the scattered light enters the spectroscope 24 and the first reference light source 28
Alternatively, the incidence of light from the second reference light source 29 can be switched.

【００２４】３８は分光器２４内に設けられた、既知の
発光線スペクトルを有する第１の基準光を出射する第１
の基準光源としてのネオン（Ｎｅ）ランプ、３９は分光
器２４内に設けられた、既知の分光エネルギ強度分布を
有する第２の基準光を出射する第２の基準光源としての
タングステン（Ｗ）ランプである。４０はＮｅランプ３
８又はＷランプ３９からミラーＭ０に至る光路に垂直な
面上に置かれたレンズで、Ｎｅランプ３８又はＷランプ
３９から出射した基準光を集め、Ｆ値が6.03になるよう
にＦマッチングする。４２は光路に垂直な面上に置か
れ、レンズ４０で集光された基準光を通過させるスリッ
トである。４１は光路に垂直な面上であって、レンズ４
０とスリット４２との間に介在する偏光解消板（スクラ
ンブラ）で、Ｎｅランプ３８又はＷランプ３９から出射
した基準光の偏光を解消することにより回折格子等の偏
光特性の影響が出ないようにするために設けられてい
る。Reference numeral 38 denotes a first reference light provided in the spectroscope 24 for emitting a first reference light having a known emission line spectrum.
Is a neon (Ne) lamp as a reference light source, and 39 is a tungsten (W) lamp as a second reference light source, which is provided in the spectroscope 24 and emits a second reference light having a known spectral energy intensity distribution. Is. 40 is Ne lamp 3
8 or a lens placed on a surface perpendicular to the optical path from the W lamp 39 to the mirror M0 collects the reference light emitted from the Ne lamp 38 or the W lamp 39 and performs F matching so that the F value becomes 6.03. Reference numeral 42 is a slit which is placed on a surface perpendicular to the optical path and which allows the reference light condensed by the lens 40 to pass therethrough. 41 is a surface perpendicular to the optical path, and the lens 4
The depolarization plate (scrambler) interposed between 0 and the slit 42 eliminates the polarization of the reference light emitted from the Ne lamp 38 or the W lamp 39 so that the polarization characteristics of the diffraction grating or the like are not affected. It is provided to

【００２５】Ｎｅランプ３８とＷランプ３９とは同軸上
に取りつけられており、レバー（選択手段）４３を操作
してＮｅランプ３８及びＷランプ３９のいずれかが光路
上に置かれるようにＮｅランプ３８とＷランプ３９を選
択する。また、Ｎｅランプ３８又はＷランプ３９から分
光器２４のミラーＭ１への基準光の入射は、基準光の入
射方向に対して平行になるようにミラーＭ０の角度を調
整することにより可能となる。一方、被測定体３６から
の散乱光の入射は、散乱光の入射方向に対してミラーＭ
０の反射面が４５°になるようにミラーＭ０の角度を調
整することにより可能である。このようなミラーＭ０の
角度調整は、例えばミラーＭ０に不図示のステップモー
タ等（切替え手段）を接続し、回動することにより可能
である。The Ne lamp 38 and the W lamp 39 are coaxially mounted, and the lever (selecting means) 43 is operated to place either the Ne lamp 38 or the W lamp 39 on the optical path. 38 and W lamp 39 are selected. Further, the reference light can be incident on the mirror M1 of the spectroscope 24 from the Ne lamp 38 or the W lamp 39 by adjusting the angle of the mirror M0 so as to be parallel to the incident direction of the reference light. On the other hand, the scattered light from the DUT 36 is incident on the mirror M in the incident direction of the scattered light.
This is possible by adjusting the angle of the mirror M0 so that the reflection surface of 0 becomes 45 °. Such an angle adjustment of the mirror M0 can be performed, for example, by connecting a step motor (not shown) (switching means) to the mirror M0 and rotating the mirror.

【００２６】２５はＮｅランプ３８又はＷランプ３９か
らの基準光やラマン散乱光を検出するＣＣＤ（光検出器
又は光検出手段）で、熱ノイズを低減するため、液体窒
素で冷却されている。４４はＣＣＤ２５により検出され
た散乱光の波数校正及び強度補正を行う波数校正及び強
度補正手段で、コンピュータからなり、分光器及びＣＣ
Ｄ２５を制御する。分光器によって分光された光はＣＣ
Ｄ２５によって計測され、ＣＣＤ２５からの信号は１６
ビット／画素で画像データとしてコンピュータ４４のメ
モリに格納される。波数校正、感度補正はこの画像デー
タに基づいて計算される。例えば、発光線スペクトルと
分光器２４を通ったＮｅランプ３８からの第１の基準光
のスペクトルとの比較から波数誤差を取得して、その波
数誤差により散乱光の波数を校正する。また、分光エネ
ルギ強度と分光器２４を通ったＷランプ３９からの第２
の基準光の強度との比較から強度補正因子を取得して、
その強度補正因子により散乱光の強度を補正する。Reference numeral 25 denotes a CCD (photodetector or photodetecting means) for detecting the reference light or Raman scattered light from the Ne lamp 38 or W lamp 39, which is cooled by liquid nitrogen in order to reduce thermal noise. Reference numeral 44 is a wave number calibrating and intensity correcting means for calibrating the wave number and the intensity of the scattered light detected by the CCD 25, which is composed of a computer and includes a spectroscope and a CC
Control D25. The light dispersed by the spectroscope is CC
Measured by D25, the signal from CCD25 is 16
It is stored in the memory of the computer 44 as image data in bits / pixel. Wave number calibration and sensitivity correction are calculated based on this image data. For example, the wave number error is acquired by comparing the emission line spectrum with the spectrum of the first reference light from the Ne lamp 38 that has passed through the spectroscope 24, and the wave number of the scattered light is calibrated by the wave number error. In addition, the second energy from the W lamp 39 passing through the spectroscopic energy intensity and the spectroscope 24.
Obtain the intensity correction factor from the comparison with the intensity of the reference light of
The intensity of the scattered light is corrected by the intensity correction factor.

【００２７】以上のように、本発明の実施例の分光測定
装置においては、分光器２４内に既知の発光線スペクト
ルを有する第１の基準光を出射するＮｅランプ３８と、
既知の分光エネルギ強度を有する第２の基準光を出射す
るＷランプ３９とが設置され、かつミラーＭ０を回動し
て適宜所定の角度調整をすることにより、Ｎｅランプ３
８又はＷランプ３９のうちいずれかの基準光源からの基
準光の入射と被測定体３６からの散乱光の入射とを切り
換え可能である。As described above, in the spectroscopic measurement apparatus of the embodiment of the present invention, the Ne lamp 38 for emitting the first reference light having the known emission line spectrum in the spectroscope 24,
The W lamp 39 that emits the second reference light having a known spectral energy intensity is installed, and the mirror M0 is rotated to appropriately adjust the predetermined angle.
It is possible to switch between the incidence of the reference light from the reference light source of either the No. 8 or W lamp 39 and the incidence of the scattered light from the DUT 36.

【００２８】従って、波数及び強度測定と波数校正及び
強度補正の切替えを適宜行うことにより、正確な波数や
強度のデータ取得を短時間で行うことができる。また、
波数校正及び強度補正手段４４を有するので、測定者に
よらず、散乱光の波数や強度について信頼性の高いデー
タが得られる。（ii）上記の散乱光測定装置を用いた波数校正及び感度
補正方法についての説明（ａ）波数校正方法についての説明次に、波数校正方法について図６を参照しながら説明す
る。Therefore, by appropriately changing the wave number / intensity measurement and the wave number calibration / intensity correction, it is possible to obtain accurate wave number / intensity data in a short time. Also,
Since the wave number calibrating and intensity correcting means 44 is provided, highly reliable data on the wave number and intensity of scattered light can be obtained regardless of the measurer. (Ii) Description of Wave Number Calibration and Sensitivity Correction Method Using the Scattered Light Measuring Device (a) Description of Wave Number Calibration Method Next, the wave number calibration method will be described with reference to FIG.

【００２９】ここでは、既知の波数スペクトルを有する
基準光源としてＮｅランプを用いた波数校正方法につい
て説明する。Ｎｅランプ３８は３００〜９００ｎｍの領
域に約３００本の発光線があり、その真空中での波数は
８桁の精度で求められている。その発光線のスペクトル
は校正データとして保存される。Here, a wave number calibration method using a Ne lamp as a reference light source having a known wave number spectrum will be described. The Ne lamp 38 has about 300 emission lines in the region of 300 to 900 nm, and the wave number in vacuum thereof is obtained with an accuracy of 8 digits. The spectrum of the emission line is stored as calibration data.

【００３０】この発光線スペクトルと、Ｎｅランプ３８
からの第１の基準光を分光器２４に通し、ＣＣＤ２５で
受光して取得された波数データとを比較することによ
り、図６に示すような波数誤差の波数依存性を表示する
グラフを作成することができる。図６において、横軸は
比例目盛で示したラマンシフト（ｃｍ^-1）を表し、縦軸
は比例目盛で示した波数誤差Erro（ｃｍ^-1）を表す。This emission line spectrum and the Ne lamp 38
The first reference light from is passed through the spectroscope 24 and compared with the wave number data received and received by the CCD 25 to create a graph showing the wave number dependence of the wave number error as shown in FIG. be able to. In FIG. 6, the horizontal axis represents the Raman shift (cm ⁻¹ ) shown in the proportional scale, and the vertical axis represents the wave number error Erro (cm ⁻¹ ) shown in the proportional scale.

【００３１】図６によれば、波数範囲３００〜７００ｃ
ｍ^-1にわたって波数誤差は波数に比例して漸増してい
る。上記の波数範囲にわたってほぼ５ｃｍ^-1前後で変化
する。詳細には、波数誤差は式で示されるような波数
の一次関数でフィッティングされる。 Erro＝ａ・λ＋ｂ・・・但し、λ：波数ａ＝0.0039094 ｂ＝−6.7425 分光器２４及びＣＣＤ２５を介して測定された散乱光の
波数は、散乱光の波数に式から導かれる波数を加減す
ることにより校正される。According to FIG. 6, the wave number range is 300 to 700c.
The wave number error gradually increases in proportion to the wave number over m ⁻¹ . It varies around 5 cm ^-1 over the above wavenumber range. In detail, the wave number error is fitted by a linear function of wave number as shown in the equation. Erro = a · λ + b ... where λ: wave number a = 0.0039094 b = −6.7425 The wave number of scattered light measured through the spectroscope 24 and the CCD 25 is the wave number of the scattered light, which is derived from the equation. Be calibrated by

【００３２】以上の計算及び校正は波数校正及び強度補
正手段２７により行われる。（ｂ）感度補正方法についての説明次に、感度補正方法について図７及び図８を参照しなが
ら説明する。感度補正には分光エネルギ強度分布が精密
に測定されている標準Ｗランプ（商品名：JPD-100-500C
S ウシオ電気製）を基準光源として用いた。The above calculation and calibration are performed by the wave number calibration and intensity correction means 27. (B) Description of Sensitivity Correction Method Next, the sensitivity correction method will be described with reference to FIGS. 7 and 8. A standard W lamp (product name: JPD-100-500C) whose spectral energy intensity distribution is precisely measured for sensitivity correction.
S Ushio Denki) was used as a reference light source.

【００３３】Ｗランプ３９の分光エネルギ強度分布Ｊは
黒体に関するプランクの式にＷランプ３９のスペクトル
発散度Ｃ１を掛けた値となり、式で表される。Ｊ＝C1/(L5・(exp(C2/L)-1))・・・但し、Ｌ：光の波長Ｃ１，Ｃ２：係数従って、既知の分光エネルギ強度分布に式がフィッテ
ィングするように、係数Ｃ１，Ｃ２を求める。図７にそ
の結果を示す。The spectral energy intensity distribution J of the W lamp 39 is a value obtained by multiplying the Planck's equation for a black body by the spectral divergence C1 of the W lamp 39 and is represented by the equation. J = C1 / (L5 ・ (exp (C2 / L) -1)), where L: wavelength of light C1, C2: coefficient Therefore, as the equation fits to the known spectral energy intensity distribution, the coefficient Find C1 and C2. The result is shown in FIG.

【００３４】図７において、横軸は比例目盛で示した波
長（ｎｍ）を表し、縦軸は比例目盛で示した分光エネル
ギ強度（μＷ・cm^-2・nm^-1）を表す。図７によれば、フ
ィッティング誤差は測定誤差以内であった。なお、上記
の分光エネルギ強度分布は色温度3111Ｋで測定された値
であるため、Ｗランプ３９に供給する電流・電圧は精密
に制御する必要がある。この場合、電流値は１ミリオー
ムの標準抵抗の両端に発生する電位差を測定して正確に
93.4Ｖ、５Ａを供給した。In FIG. 7, the horizontal axis represents the wavelength (nm) indicated on the proportional scale, and the vertical axis represents the spectral energy intensity (μW · cm ⁻² · nm ⁻¹ ) indicated on the proportional scale. According to FIG. 7, the fitting error was within the measurement error. Since the above spectral energy intensity distribution is a value measured at a color temperature of 3111K, it is necessary to precisely control the current and voltage supplied to the W lamp 39. In this case, the current value is accurately measured by measuring the potential difference across both ends of a standard resistance of 1 milliohm.
93.4V, 5A was supplied.

【００３５】このように調整されたＷランプ３９からの
第２の基準光を分光器２４に入射し、分光器２４を通過
した基準光をＣＣＤ２５により受光した。ラマンシフト
（ｃｍ^-1）に対する入射エネルギ強度分布と分光器２４
及びＣＣＤ２５を介して測定された装置全体の感度特性
を図８に示す。図８において、横軸は比例目盛で示した
ラマンシフト（ｃｍ^-1）を表し、縦軸は強度（任意単
位）を表す。The second reference light from the W lamp 39 thus adjusted is incident on the spectroscope 24, and the reference light passing through the spectroscope 24 is received by the CCD 25. Incident energy intensity distribution for Raman shift (cm ^-1 ) and spectroscope 24
FIG. 8 shows the sensitivity characteristics of the entire device measured via the CCD 25 and the CCD 25. In FIG. 8, the horizontal axis represents the Raman shift (cm ⁻¹ ) on a proportional scale, and the vertical axis represents the intensity (arbitrary unit).

【００３６】図８によれば、感度はラマンシフトの増加
に比例して高くなる。このような特性が現れるのはＣＣ
Ｄ２５の感度の波長依存性が強く現れているためである
と考えられる。式で示す入射エネルギ強度分布と感度
特性とを比較して強度補正因子を算出し、分光器２４及
びＣＣＤ２５を介して測定された散乱光の強度にこの強
度補正因子を乗じて感度補正を行う。According to FIG. 8, the sensitivity increases in proportion to the increase in Raman shift. This characteristic appears in CC
It is considered that this is because the wavelength dependence of the sensitivity of D25 appears strongly. The intensity correction factor is calculated by comparing the incident energy intensity distribution shown by the equation with the sensitivity characteristic, and the intensity of the scattered light measured through the spectroscope 24 and the CCD 25 is multiplied by this intensity correction factor to perform the sensitivity correction.

【００３７】以上の計算及び補正は波数校正及び強度補
正手段２７により行われる。（ｃ）波数校正及び感度補正方法の適用例の説明次に、上記の波数校正方法及び感度補正方法を本発明の
第１の実施例に係る散乱光測定装置に適用した例につい
て図４，図５，図６及び図８を参照しながら説明する。The above calculation and correction are performed by the wave number calibration and intensity correction means 27. (C) Description of Application Example of Wavenumber Calibration and Sensitivity Correction Method Next, an example in which the above-described wavenumber calibration method and sensitivity correction method are applied to the scattered light measuring apparatus according to the first embodiment of the present invention will be described with reference to FIGS. 5, it will be described with reference to FIGS.

【００３８】図５は波数校正及び感度補正方法を示すフ
ローチャートである。まず、既知の発光線スペクトルを
有する第１の基準光を出射するＮｅランプ３８から光を
出射し、分光器２４を介して基準光をＣＣＤ２５に受光
する。次いで、上記した（ａ）の方法により、受光され
た基準光のスペクトルを発光線スペクトルと比較して波
数に対する波数誤差を求め、式の係数ａ，ｂを算出す
る。この計算は波数校正及び強度補正手段４４により行
われる。FIG. 5 is a flowchart showing a wave number calibration and sensitivity correction method. First, light is emitted from the Ne lamp 38 that emits the first reference light having a known emission line spectrum, and the reference light is received by the CCD 25 via the spectroscope 24. Next, by the method (a) described above, the spectrum of the received reference light is compared with the emission line spectrum to obtain the wave number error with respect to the wave number, and the coefficients a and b of the equation are calculated. This calculation is performed by the wave number calibration and intensity correction means 44.

【００３９】次に、既知の分光エネルギ強度を有する第
２の基準光を出射するＷランプ３９から光を出射し、分
光器２４を介して基準光をＣＣＤ２５に受光する。次い
で、上記した（ｂ）の方法により、受光された基準光の
感度特性を分光エネルギ強度と比較して波数に対する強
度補正因子を算出する。次に、スリットＳ０，Ｓ１を閉
めて光の入射を止め、ＣＣＤ２５に流れる暗電流を測定
し、暗電流に相当する強度補正因子を算出する。この計
算は波数校正及び強度補正手段４４により行われる。な
お、暗電流を含む強度の測定値は真の散乱光の強度より
高い値になるので、測定された散乱光の強度に対して暗
電流による強度補正因子を補正する必要がある。Then, light is emitted from the W lamp 39 that emits the second reference light having a known spectral energy intensity, and the reference light is received by the CCD 25 via the spectroscope 24. Then, by the method (b) described above, the sensitivity characteristic of the received reference light is compared with the spectral energy intensity to calculate the intensity correction factor for the wave number. Next, the slits S0 and S1 are closed to stop the incidence of light, the dark current flowing through the CCD 25 is measured, and the intensity correction factor corresponding to the dark current is calculated. This calculation is performed by the wave number calibration and intensity correction means 44. Since the measured value of the intensity including the dark current is higher than the intensity of the true scattered light, it is necessary to correct the intensity correction factor due to the dark current with respect to the measured intensity of the scattered light.

【００４０】次いで、被測定体３６にレーザ光を照射し
て被測定体３６から散乱光を出射させ、その散乱光を分
光器２４を介してＣＣＤ２５に受光させる。次に、受光
した散乱光の波数を波数誤差により校正し、かつ受光し
た散乱光の強度を２つの強度補正因子により補正する。
これらの校正及び補正は波数校正及び強度補正手段４４
により行われる。Next, the measured object 36 is irradiated with laser light to cause scattered light to be emitted from the measured object 36, and the scattered light is received by the CCD 25 via the spectroscope 24. Next, the wave number of the received scattered light is calibrated by a wave number error, and the intensity of the received scattered light is corrected by two intensity correction factors.
These calibration and correction are performed by wave number calibration and intensity correction means 44.
Done by.

【００４１】図９にBi-Sr-Ca-Cu-O 膜（ＢＳＣＣＯ膜）
から出射された散乱光について波数及び強度の測定デー
タと波数校正及び強度補正した後のデータとの比較を示
す。図９において、縦軸は強度（任意単位）を表し、横
軸は比例目盛で示したラマンシフト（ｃｍ^-1）を表す。
図９によれば、波数が低い方に約５ｎｍ^-1シフトし、か
つ強度が低波数側で強くなった。FIG. 9 shows a Bi-Sr-Ca-Cu-O film (BSCCO film).
The comparison of the wave number and intensity measurement data and the data after the wave number calibration and intensity correction of the scattered light emitted from is shown. In FIG. 9, the vertical axis represents intensity (arbitrary unit), and the horizontal axis represents Raman shift (cm ⁻¹ ) on a proportional scale.
According to FIG. 9, the wave number was shifted to the lower side by about 5 nm ⁻¹ , and the intensity became stronger on the low wave number side.

【００４２】以上のように、本発明の第１の実施例に係
る散乱光測定装置を用いた波数校正及び感度補正方法に
よれば、Ｎｅランプ３８とＷランプ３９とを有し、Ｎｅ
ランプ３８及びＷランプ３９のうち基準光を出射する方
を適宜選択することにより、波数補正と強度補正をとも
に行える。また、分光器２４へのＮｅランプ３８及びＷ
ランプ３９のいずれかからの基準光の入射と被測定体３
６からの散乱光の入射とを適宜切り換えることにより、
波数及び強度測定と波数校正及び強度補正とを行い、正
確な波数及び強度のデータ取得を短時間で行うことがで
きる。As described above, according to the method of wave number calibration and sensitivity correction using the scattered light measuring apparatus according to the first embodiment of the present invention, the Ne lamp 38 and the W lamp 39 are provided, and the Ne lamp 38 is provided.
By appropriately selecting which of the lamp 38 and the W lamp 39 that emits the reference light, both the wave number correction and the intensity correction can be performed. Also, the Ne lamp 38 and W to the spectroscope 24
Incident of reference light from any of the lamps 39 and the DUT 3
By switching the incident of scattered light from 6 appropriately,
Accurate wave number and intensity data acquisition can be performed in a short time by performing wave number and intensity measurement, wave number calibration, and intensity correction.

【００４３】更に、波数校正及び強度補正手段４４を有
するので、測定者によらず、散乱光の波数及び強度につ
いて信頼性の高いデータが得られる。なお、上記の実施
例では、Ｎｅランプ３８とＷランプ３９を両方設置して
いるが、場合によりいずれか一方を設置してもよい。こ
れにより、散乱光の波数校正又は強度補正を行うことが
できる。Furthermore, since the wave number calibrating and intensity correcting means 44 is provided, highly reliable data on the wave number and intensity of scattered light can be obtained regardless of the operator. Although the Ne lamp 38 and the W lamp 39 are both installed in the above embodiment, either one of them may be installed depending on circumstances. Thereby, the wave number calibration or intensity correction of scattered light can be performed.

【００４４】（２）第２の実施例図１２は本発明の第２の実施例に係るラマン散乱光の測
定装置の全体構成図であり、図１０（ａ）は被測定体の
周辺部の詳細について説明する構成図である。図１２に
おいて、２３は三重の隔壁30ａ〜30ｃを有し、各隔壁30
ａ〜30ｃ間が断熱層及びサンプル層となっているクライ
オスタットで、被測定体３６としての超電導体膜が形成
されたＭｇＯ基板がセットされて１０Ｋまで冷却され、
保温される。これにより、超電導体膜が超伝導状態にな
る温度の前後の超電導体膜の性質を観察することが可能
になる。(2) Second Embodiment FIG. 12 is an overall configuration diagram of a Raman scattered light measuring apparatus according to a second embodiment of the present invention, and FIG. 10 (a) shows the peripheral portion of the object to be measured. It is a block diagram explaining details. In FIG. 12, reference numeral 23 has triple partition walls 30a to 30c.
With a cryostat having a heat insulating layer and a sample layer between a to 30c, the MgO substrate on which the superconductor film as the DUT 36 is formed is set and cooled to 10K,
Be kept warm. This makes it possible to observe the properties of the superconductor film before and after the temperature at which the superconductor film becomes in the superconducting state.

【００４５】２６はレーザ光の出射を制御し、ＣＣＤに
より検出された散乱光を分析する制御素子である。ま
た、図１０（ａ）において、28ｂはＭｇＯ基板28ａ上に
Ａｇペーストを用いて張りつけられた被測定体としての
Bi-Sr-Ca-Cu-O 膜（ＢＳＣＣＯ膜：超電導体膜）であ
る。２９はＢＳＣＣＯ膜28ｂの形成されたＭｇＯ基板28
ａを保持するホルダで、銅基板29ａの保持面にはスプレ
ーで塗布して形成されたカーボン膜29ｂが被覆されてい
る。Reference numeral 26 is a control element which controls the emission of the laser light and analyzes the scattered light detected by the CCD. Further, in FIG. 10 (a), 28b is a measured object which is attached to the MgO substrate 28a using Ag paste.
It is a Bi-Sr-Ca-Cu-O film (BSCCO film: superconductor film). 29 is an MgO substrate 28 on which a BSCCO film 28b is formed.
In the holder for holding a, the holding surface of the copper substrate 29a is coated with a carbon film 29b formed by spraying.

【００４６】33ａ〜33ｃはレーザ光が被測定体28ｂに入
射し、散乱光が出射する隔壁30ａ〜30ｃの部分に形成さ
れたレーザ光を透過する石英窓である。３４は液体ヘリ
ウム収納容器で、ＢＳＣＣＯ膜28ｂを冷却する。なお、
図中、図４と同じ符号で示すものは図４と同じものを示
す。上記の装置によりＢＳＣＣＯ膜28ｂのラマン散乱光
を測定した結果について、図１０（ｂ）に示す。比較の
ため、銅のホルダ，保持面に黒色のマジックインキを塗
った銅のホルダ，及び被測定体を載置していない、保持
面にカーボンを塗った銅のホルダについても同様な測定
を行った。Numerals 33a to 33c are quartz windows for transmitting the laser light formed in the partition walls 30a to 30c where the laser light is incident on the measured object 28b and the scattered light is emitted. A liquid helium container 34 cools the BSCCO film 28b. In addition,
In the figure, the same symbols as those in FIG. 4 indicate the same components as those in FIG. The result of measuring the Raman scattered light of the BSCCO film 28b by the above apparatus is shown in FIG. For comparison, the same measurement is performed on a copper holder, a copper holder coated with black magic ink on the holding surface, and a copper holder on which the holding surface is not coated with carbon. It was

【００４７】それによれば、銅のホルダ、及び保持面に
マジックインキを塗った銅のホルダでは、反射光による
ノイズの強度が強いため、ＢＳＣＣＯ膜28ｂからのラマ
ン散乱光が埋もれてしまって全く検出できない。一方、
被測定体を載置していない、保持面にカーボン膜29ｂが
形成された銅のホルダ、及びＢＳＣＣＯ膜28ｂを載置し
ている、保持面にカーボン膜29ｂが形成された銅のホル
ダ２９では、ノイズがほとんどなく、ラマン散乱光が明
確に検出されている。これは、第２の実施例に係る保持
面にカーボン膜29ｂが形成された銅のホルダ２９では、
ＢＳＣＣＯ膜28ｂ及びＭｇＯ基板28ａを透過してホルダ
２９の被測定体の保持面に達した光がカーボン膜29ｂに
より吸収され、これにより、反射光の強度は弱くなると
ともに、相対的に、測定すべきラマン散乱光の強度が強
くなったためと考えられる。According to this, in the copper holder and the copper holder whose holding surface is coated with magic ink, the intensity of the noise due to the reflected light is strong, so that the Raman scattered light from the BSCCO film 28b is buried and detected at all. Can not. on the other hand,
With the copper holder on which the carbon film 29b is formed on the holding surface and the copper holder 29 on which the carbon film 29b is formed on the holding surface, on which the BSCCO film 28b is placed , There is almost no noise, and Raman scattered light is clearly detected. This is because in the copper holder 29 having the carbon film 29b formed on the holding surface according to the second embodiment,
The light transmitted through the BSCCO film 28b and the MgO substrate 28a and reaching the holding surface of the object to be measured of the holder 29 is absorbed by the carbon film 29b, whereby the intensity of the reflected light becomes weak and the relative measurement is performed. This is probably because the intensity of the Raman scattered light that should have been increased.

【００４８】（３）第３の実施例図１１（ａ）は本発明の第３の実施例に係る被測定体の
周辺部の詳細について説明する構成図である。図１０
（ａ）に示す第２の実施例と異なるところは、被測定体
を保持するホルダ３５が光透過性のＭｇＯ単結晶からな
ることである。ＭｇＯ単結晶は熱伝導性が比較的良いの
で、銅のホルダと同じように、温度の均一性を保持する
ことができ、温度依存性の測定に用いることができる。(3) Third Embodiment FIG. 11A is a configuration diagram for explaining the details of the peripheral portion of the device under test according to the third embodiment of the present invention. Figure 10
The difference from the second embodiment shown in (a) is that the holder 35 for holding the object to be measured is made of a light-transmissive MgO single crystal. Since the MgO single crystal has relatively good thermal conductivity, it can maintain the temperature uniformity like the copper holder and can be used for measuring the temperature dependence.

【００４９】また、レーザ光の入射側の容器３０〜３２
の側壁にそれぞれ光透過性の石英窓30ａ〜30ｃを有する
ほか、被測定体に対してレーザ光の入射側と反対側の容
器３０〜３２の側壁にそれぞれ光透過性の石英窓30ｄ〜
30ｆを有する。これにより、被測定体を透過したレーザ
光は入射側に戻らずに、この石英窓30ｄ〜30ｆから出射
するようになっていることである。なお、図１１（ａ）
において、図１０（ａ）と同じ符号で示すものは、図１
０（ａ）と同じものを示す。Further, the containers 30 to 32 on the laser light incident side are provided.
In addition to having light-transmissive quartz windows 30a to 30c on their side walls, respectively, light-transmissive quartz windows 30d to 30d on the side walls of the containers 30 to 32 on the side opposite to the laser light incident side with respect to the DUT.
Has 30f. As a result, the laser light transmitted through the object to be measured is emitted from the quartz windows 30d to 30f without returning to the incident side. Note that FIG.
In FIG. 1, the same reference numerals as those in FIG.
The same as 0 (a) is shown.

【００５０】上記の装置によりＢＳＣＣＯ膜28ｂのラマ
ン散乱光を測定した結果について、図１１（ｂ）に示
す。それによれば、第２の実施例と同様に、パルス状の
ノイズがわずかに存在するだけで、ラマン散乱光は明確
に検出されている。これは、ホルダ３５として光透過性
のＭｇＯ基板が用いられているので、ＢＳＣＣＯ膜28ｂ
及びＭｇＯ基板28ｂを透過してホルダ３５の被測定体の
保持面に達した光が、そのままホルダ３５を透過して反
対側から出射し、これにより、反射光はほとんど生じな
いので、Ｓ／Ｎ比が改善され、入射側に戻ってくる微弱
なラマン散乱光がノイズに埋もれることなく検出された
ためだと考えられる。The result of measuring the Raman scattered light of the BSCCO film 28b by the above apparatus is shown in FIG. 11 (b). According to this, similarly to the second embodiment, the Raman scattered light is clearly detected with the slight presence of pulsed noise. This is because the light-transmissive MgO substrate is used as the holder 35, and thus the BSCCO film 28b is used.
And the light which has passed through the MgO substrate 28b and has reached the holding surface of the object to be measured of the holder 35, passes through the holder 35 as it is and is emitted from the opposite side, whereby almost no reflected light is generated. This is probably because the ratio was improved and the weak Raman scattered light returning to the incident side was detected without being buried in noise.

【００５１】（４）第４の実施例図１３は第４の実施例に係るＣＣＤの被覆手段を有する
ラマン散乱光の測定装置について説明する構成図であ
る。図１３において、２７はＣＣＤ（光検出手段）２５
を被覆する鉛からなる被覆手段である。なお、図中、図
１２と同じ符号で示すものは図１２と同じものを示す。(4) Fourth Embodiment FIG. 13 is a block diagram for explaining a Raman scattered light measuring apparatus having a CCD covering means according to a fourth embodiment. In FIG. 13, 27 is a CCD (light detecting means) 25.
Is a coating means made of lead. In the figure, the same reference numerals as those in FIG. 12 indicate the same parts as those in FIG.

【００５２】ところで、宇宙線はミュー粒子と電子成分
の２種類がある。ミュー粒子は７０％の割合で地表に降
り注ぎ、数センチの厚さの鉛を透過するため硬成分と呼
ばれている。また、電子成分は３０％の割合で地表に降
り注ぎ、殆ど吸収されてしまうので、軟成分と呼ばれて
いる。上記の被覆手段２７により、このような宇宙線の
ＣＣＤ２５への入射を減少させることができる。There are two types of cosmic rays, muons and electronic components. Mu particles fall on the surface of the earth at a rate of 70% and permeate lead with a thickness of a few centimeters, so it is called a hard component. In addition, the electronic component is called a soft component because it is poured into the ground surface at a rate of 30% and is almost absorbed. The coating means 27 described above can reduce the incidence of such cosmic rays on the CCD 25.

【００５３】上記の散乱光測定装置によりラマン散乱光
を測定した場合、従来と比較してノイズの発生率が約２
０％減少した。このように、宇宙線ノイズが減少するた
め、Ｓ／Ｎ比は改善され、微弱なラマン散乱光が明瞭に
検出される。（Ｂ）本発明の実施例に係るラマン散乱光の測定方法（５）第５の実施例次に、本発明の第５の実施例に係るラマン散乱光の測定
方法について図１２，図１４及び図１５を参照しながら
説明する。図１４は測定のフローチャートであり、図１
５はＣＣＤ２５の全露光領域及び実際に露光された露光
領域を示す平面図である。When Raman scattered light is measured by the above scattered light measuring device, the noise generation rate is about 2 as compared with the conventional case.
It decreased by 0%. Thus, the cosmic ray noise is reduced, the S / N ratio is improved, and the weak Raman scattered light is clearly detected. (B) Raman scattered light measuring method according to an embodiment of the present invention (5) Fifth embodiment Next, a Raman scattered light measuring method according to a fifth embodiment of the present invention will be described with reference to FIGS. This will be described with reference to FIG. FIG. 14 is a measurement flowchart, and FIG.
5 is a plan view showing the entire exposure area of the CCD 25 and the actually exposed exposure area.

【００５４】まず、図１２に示すように、散乱光のうち
比較的強度の強いレーリー光をＮＤフィルタでパワーを
減少させた後、測定に用いる分光器２４に入れ、ＣＣＤ
２５に導いて、５７８×３８５画素を有するＣＣＤ２５
の露光面を露光する。これにより、図１５に示すよう
に、中央部の帯状の露光領域で、かつ黒い部分の画素が
実際に露光される。First, as shown in FIG. 12, after the Rayleigh light of relatively high intensity among scattered light is reduced in power by the ND filter, it is put into the spectroscope 24 used for measurement, and the CCD is used.
CCD 25 with 578 x 385 pixels leading to 25
The exposed surface of. As a result, as shown in FIG. 15, pixels in the central strip-shaped exposure region and in the black portion are actually exposed.

【００５５】そして、ＣＣＤ２５の画素のうちどの部分
を使用しているかを確定するために、前記レーリー光を
ＣＣＤ２５の画素を介して検出する。これにより、ＣＣ
Ｄ２５の画素エリアのうちどの部分を使用しているかが
検出される。第５の実施例の場合、図１５に示すよう
に、中央部の帯状の露光領域であって縦方向に４０画素
程度しか使用していないことがわかる。このようにし
て、全露光領域のうち、この中央部の帯状の露光領域を
有効画素エリア（使用すべき露光領域）として予め確定
しておく。なお、中央部の露光領域以外の露光領域はラ
マン散乱光の測定において使用しない露光領域とする。Then, in order to determine which part of the pixels of the CCD 25 is used, the Rayleigh light is detected through the pixels of the CCD 25. This allows CC
Which part of the pixel area of D25 is used is detected. In the case of the fifth embodiment, as shown in FIG. 15, it is understood that only about 40 pixels are used in the vertical direction in the strip-shaped exposure region in the central portion. In this way, of all the exposure areas, the central strip-shaped exposure area is determined in advance as an effective pixel area (exposure area to be used). The exposure area other than the central exposure area is an exposure area not used in the measurement of Raman scattered light.

【００５６】続いて、使用しない露光領域の画素の動作
を停止するとともに、有効画素エリアの画素のみ動作さ
せた状態で、光学系を介して被測定体３６にＡｒレーザ
光を照射し、これにより被測定体３６から出射するラマ
ン散乱光を分光器２４によりＣＣＤ２５に導く。そし
て、動作しているＣＣＤ２５の画素を介してラマン散乱
光を検出する。Subsequently, while the operation of the pixels in the exposure area not used is stopped and only the pixels in the effective pixel area are operated, the object to be measured 36 is irradiated with the Ar laser light through the optical system. The Raman scattered light emitted from the DUT 36 is guided to the CCD 25 by the spectroscope 24. Then, the Raman scattered light is detected through the pixels of the CCD 25 which is operating.

【００５７】このようにして検出されたラマン散乱光の
測定結果を図１６（ａ）に示す。縦軸が強度（cps ）を
表し、横軸がラマンシフト（cm^-1）を表す。それによれ
ば、Ｓ／Ｎ比が向上し、微弱なラマン散乱光を確実に捉
えることができる。図１６（ｂ）の従来例の場合と比較
すると、宇宙線によるノイズが大幅に減少していること
がわかる。なお、図１６（ｂ）中、スパイク状のパルス
が宇宙線によるノイズを表している。The measurement result of the Raman scattered light thus detected is shown in FIG. 16 (a). The vertical axis represents intensity (cps) and the horizontal axis represents Raman shift (cm ^-1 ). According to this, the S / N ratio is improved, and weak Raman scattered light can be reliably captured. It can be seen that the noise due to cosmic rays is significantly reduced as compared with the case of the conventional example of FIG. Note that in FIG. 16B, spike-like pulses represent noise due to cosmic rays.

【００５８】以上のように、本発明の第５の実施例に係
る散乱光測定方法においては、レーリー光を用いた測定
により、実際に露光されるＣＣＤ２５の全露光領域のう
ち有効画素エリアを予め確定しておき、その後、微弱な
ラマン散乱光を測定する際に、有効画素エリアの画素の
み動作させ、かつ使用しない露光領域の画素の動作を停
止した状態で、強度の弱いラマン散乱光を測定するよう
にしている。As described above, in the scattered light measuring method according to the fifth embodiment of the present invention, the effective pixel area of the entire exposure area of the CCD 25 actually exposed is previously measured by the measurement using Rayleigh light. After confirming it, when measuring weak Raman scattered light, measure only weak intensity Raman scattered light while operating only the pixels in the effective pixel area and stopping the pixels in the unused exposure area I am trying to do it.

【００５９】従って、露光領域が必要最小限に制限され
るため、外部から露光領域に入ってくる宇宙線の量を減
少させることができる。このため、微弱なラマン散乱光
に対する検出感度を落とすことなく、ノイズのみを減少
させることができる。これにより、Ｓ／Ｎ比は改善さ
れ、ノイズに埋もれることなく微弱なラマン散乱光が有
効に検出される。Therefore, since the exposure area is limited to the necessary minimum, the amount of cosmic rays entering the exposure area from the outside can be reduced. Therefore, it is possible to reduce only noise without lowering the detection sensitivity for weak Raman scattered light. As a result, the S / N ratio is improved, and weak Raman scattered light is effectively detected without being buried in noise.

【００６０】（６）第６の実施例次に、本発明の第６の実施例に係るラマン散乱光の測定
方法について図１２及び図１７を参照しながら説明す
る。図１７は測定のフローチャートである。まず、図１
２に示すように、レーザ光を出射させずに、ＣＣＤ２５
のみを動作させて、降り注ぐ宇宙線の蓄積量が経時的に
どのように変化しているかを検出する。このデータから
ラマン散乱光の測定が妨げられない程度の適当なノイズ
量となる時間の範囲を決める。この時間の範囲内でＣＣ
Ｄ２５の露光時間を設定する。(6) Sixth Embodiment Next, a method for measuring Raman scattered light according to a sixth embodiment of the present invention will be described with reference to FIGS. 12 and 17. FIG. 17 is a measurement flowchart. First, Fig. 1
As shown in FIG. 2, the CCD 25 does not emit laser light.
It is operated only to detect how the accumulated amount of cosmic rays falling changes with time. From this data, the range of time that gives an appropriate amount of noise that does not interfere with the measurement of Raman scattered light is determined. CC within this time
Set the exposure time of D25.

【００６１】次に、ラマン散乱光の測定を開始する。即
ち、Ａｒレーザ２１よりレーザ光を出射させ、光学系を
介して被測定体３６に照射する。これにより、被測定体
３６からラマン散乱光が出射し、該ラマン散乱光は分光
器２４を介してＣＣＤ２５に導かれる。そして、ＣＣＤ
２５の露光面の画素を介してラマン散乱光が検出され
る。Next, the measurement of Raman scattered light is started. That is, a laser beam is emitted from the Ar laser 21 and is irradiated onto the DUT 36 via the optical system. As a result, the Raman scattered light is emitted from the DUT 36, and the Raman scattered light is guided to the CCD 25 via the spectroscope 24. And CCD
Raman scattered light is detected via 25 pixels on the exposed surface.

【００６２】以上のように、第６の実施例によれば、Ｃ
ＣＤ２５に入射する宇宙線によるノイズ量の経時的な蓄
積量を予め測定しておき、ラマン散乱光の測定が妨げら
れない程度の適当なノイズ量となる時間の範囲内で露光
時間を設定しているので、微弱なラマン散乱光がノイズ
に埋まらないようにして測定することができる。このた
め、Ｓ／Ｎ比は改善され、ノイズに埋もれることなく強
度の弱い散乱光が有効に検出される。As described above, according to the sixth embodiment, C
The accumulated amount of noise due to cosmic rays incident on the CD25 is measured in advance, and the exposure time is set within a time range that provides an appropriate amount of noise that does not interfere with the measurement of Raman scattered light. Therefore, the weak Raman scattered light can be measured without being buried in the noise. Therefore, the S / N ratio is improved, and scattered light of low intensity is effectively detected without being buried in noise.

【００６３】なお、上記の第５及び第６の実施例に係る
測定方法について測定装置をマイクロコンピュータ等に
接続することにより自動化を図ることが出きる。The measuring methods according to the fifth and sixth embodiments can be automated by connecting the measuring device to a microcomputer or the like.

【００６４】[0064]

【発明の効果】以上説明したように、本発明に係る散乱
光測定装置によれば、第１の基準光源と第２の基準光源
とを有し、第１の基準光源及び第２の基準光源のうち基
準光を出射する基準光源を選択する選択手段を有する。
従って、波数補正と強度補正をともに行える。As described above, according to the scattered light measuring apparatus of the present invention, it has the first reference light source and the second reference light source, and the first reference light source and the second reference light source. Of these, there is a selecting means for selecting a reference light source for emitting the reference light.
Therefore, both wave number correction and intensity correction can be performed.

【００６５】また、第１及び第２の基準光源のいずれか
からの基準光の入射と被測定体からの散乱光の入射とを
切り換える切替え手段を有する。従って、波数校正及び
強度補正と、波数及び強度測定との切替えを適宜行い、
正確な波数及び強度のデータ取得を短時間で行うことが
できる。また、波数校正及び強度補正手段を有するの
で、測定者によらず、散乱光の波数及び強度について信
頼性の高いデータが得られる。Further, it has a switching means for switching between the incidence of the reference light from either the first or second reference light source and the incidence of the scattered light from the object to be measured. Therefore, appropriately switch between wave number calibration and intensity correction and wave number and intensity measurement,
Accurate wave number and intensity data can be acquired in a short time. Further, since the wave number calibrating and intensity correcting means are provided, highly reliable data on the wave number and intensity of scattered light can be obtained regardless of the measurer.

【００６６】更に、被測定体のホルダは保持面にカーボ
ン膜が形成されているので、光透過性を有する被測定体
を透過した励起光はカーボン膜により吸収される。この
ため、測定すべき散乱光の強度は相対的に強くなってＳ
／Ｎ比が改善され、ノイズに埋もれることなく強度の弱
い散乱光が明瞭に検出される。また、ホルダはＭｇＯ単
結晶からなるため、被測定体が光透過性を有する場合、
被測定体を透過した励起光はホルダをも透過して入射側
と反対側に出射する。従って、測定すべき散乱光の強度
は相対的に強くなってＳ／Ｎ比が改善され、ノイズに埋
もれることなく強度の弱い散乱光が光検出器に有効に検
出される。Further, since the holder of the object to be measured has the carbon film formed on the holding surface, the excitation light transmitted through the object to be measured having light transmittance is absorbed by the carbon film. Therefore, the intensity of scattered light to be measured becomes relatively strong and S
The / N ratio is improved, and scattered light with low intensity is clearly detected without being buried in noise. In addition, since the holder is made of MgO single crystal, when the measured object has optical transparency,
The excitation light that has passed through the measured object also passes through the holder and is emitted to the side opposite to the incident side. Therefore, the intensity of scattered light to be measured becomes relatively strong, the S / N ratio is improved, and scattered light having low intensity is effectively detected by the photodetector without being buried in noise.

【００６７】更に、光検出器が鉛からなる被覆手段によ
り被覆されているので、宇宙線を防御することができ
る。このため、Ｓ／Ｎ比は改善され、ノイズに埋もれる
ことなく強度の弱い散乱光が有効に検出される。また、
本発明に係る光散乱測定方法においては、実際に散乱光
により露光される露光領域の画素のみ動作させ、使用し
ない露光領域の画素の動作を停止した状態で、散乱光を
測定している。従って、露光領域が必要最小限に縮小さ
れ、これにともなって有効な露光領域にかかる宇宙線の
量も減少するため、強度の弱い散乱光に対する検出感度
を落とすことなく、ノイズのみを減少させることができ
る。これにより、Ｓ／Ｎ比は改善され、宇宙線によるノ
イズに妨害されることなく強度の弱い散乱光が有効に検
出される。Further, since the photodetector is coated with the coating means made of lead, cosmic rays can be protected. Therefore, the S / N ratio is improved, and scattered light of low intensity is effectively detected without being buried in noise. Also,
In the light-scattering measurement method according to the present invention, only the pixels in the exposure area that are actually exposed by the scattered light are operated, and the scattered light is measured in a state where the pixels in the unused exposure area are stopped. Therefore, the exposure area is reduced to the required minimum, and the amount of cosmic rays applied to the effective exposure area is reduced accordingly, so that only noise is reduced without lowering the detection sensitivity for scattered light with low intensity. You can As a result, the S / N ratio is improved, and weakly scattered light is effectively detected without being disturbed by noise due to cosmic rays.

【００６８】また、ＣＣＤに入射する宇宙線によるノイ
ズ量の経時的な蓄積量を予め測定しておき、散乱光の測
定に支障がない程度のノイズ量が蓄積される時間の範囲
内で露光時間を設定している。このため、Ｓ／Ｎ比は改
善され、ノイズに埋もれることなく強度の弱い散乱光が
明瞭に検出される。Further, the amount of accumulated noise amount due to cosmic rays incident on the CCD is measured in advance, and the exposure time is set within the range of the amount of accumulated noise amount that does not hinder the measurement of scattered light. Is set. Therefore, the S / N ratio is improved, and scattered light of low intensity is clearly detected without being buried in noise.

[Brief description of drawings]

【図１】本発明の第１の散乱光測定装置の原理構成図で
ある。FIG. 1 is a principle configuration diagram of a first scattered light measuring device of the present invention.

【図２】本発明の第２の散乱光測定装置の原理構成図で
ある。FIG. 2 is a principle configuration diagram of a second scattered light measuring device of the present invention.

【図３】本発明の第３の散乱光測定装置の原理構成図で
ある。FIG. 3 is a principle configuration diagram of a third scattered light measuring device of the present invention.

【図４】本発明の第１の実施例に係る散乱光測定装置に
ついて示す構成図である。FIG. 4 is a configuration diagram showing a scattered light measuring device according to a first embodiment of the present invention.

【図５】本発明の第１の実施例に係る散乱光測定装置を
用いた波数校正及び強度補正方法について示すフローチ
ャートである。FIG. 5 is a flow chart showing a wave number calibration and intensity correction method using the scattered light measuring apparatus according to the first embodiment of the present invention.

【図６】本発明の第１の実施例に係る波数校正データに
ついて示す特性図である。FIG. 6 is a characteristic diagram showing wave number calibration data according to the first embodiment of the present invention.

【図７】本発明の第１の実施例に係る分光エネルギ強度
について示す特性図である。FIG. 7 is a characteristic diagram showing spectral energy intensity according to the first example of the present invention.

【図８】本発明の第１の実施例に係る強度補正データに
ついて示す特性図である。FIG. 8 is a characteristic diagram showing intensity correction data according to the first embodiment of the present invention.

【図９】本発明の第１の実施例に係る散乱光測定装置を
用いた波数校正及び強度補正結果について示す特性図で
ある。FIG. 9 is a characteristic diagram showing a result of wave number calibration and intensity correction using the scattered light measuring device according to the first embodiment of the present invention.

【図１０】本発明の第２の実施例に係る散乱光測定装置
の被測定体のホルダ周辺部の詳細な構成図である。FIG. 10 is a detailed configuration diagram of a holder peripheral portion of the measured object of the scattered light measuring apparatus according to the second embodiment of the present invention.

【図１１】本発明の第３の実施例に係る散乱光測定装置
の被測定体のホルダ周辺部の詳細な構成図である。FIG. 11 is a detailed configuration diagram of a holder peripheral portion of the measured object of the scattered light measuring apparatus according to the third embodiment of the present invention.

【図１２】本発明の第２の実施例に係る散乱光測定装置
の全体構成図である。FIG. 12 is an overall configuration diagram of a scattered light measurement device according to a second embodiment of the present invention.

【図１３】本発明の第４の実施例に係るＣＣＤの被覆手
段を有する散乱光測定装置の構成図である。FIG. 13 is a configuration diagram of a scattered light measuring device having CCD covering means according to a fourth embodiment of the present invention.

【図１４】本発明の第５の実施例に係る散乱光測定方法
について説明するフローチャートである。FIG. 14 is a flowchart illustrating a scattered light measuring method according to a fifth embodiment of the present invention.

【図１５】本発明の第５の実施例に係る散乱光測定方法
について説明するＣＣＤの露光領域の平面図である。FIG. 15 is a plan view of an exposure area of a CCD for explaining a scattered light measuring method according to a fifth embodiment of the present invention.

【図１６】本発明の第５の実施例に係る散乱光測定方法
によるラマン散乱光の検出結果について説明する特性図
である。FIG. 16 is a characteristic diagram illustrating a detection result of Raman scattered light by the scattered light measuring method according to the fifth embodiment of the present invention.

【図１７】本発明の第６の実施例に係る散乱光測定方法
について説明するフローチャートである。FIG. 17 is a flowchart illustrating a scattered light measuring method according to a sixth embodiment of the present invention.

[Explanation of symbols]

１光源（光出射手段）、２第１の基準光源、３，２４分光器（光学手段）、４，４ａ切替え手段、５光検出器、６波数校正手段、７，３６被測定体、８第２の基準光源、９強度補正手段、１０選択手段、１１，３８波数補正及び強度補正手段、２１Ａｒレーザ（光源又は光出射手段）、２２プリモノクロメータ、２３クライオスタット、２５ＣＣＤ（光検出器又は光検出手段）、２６制御素子、２７被覆手段、 28ａＭｇＯ基板、 28ｂ超電導体膜（被測定体）、２９ホルダ、 29ａ銅基板、 29ｂカーボン膜、 30ａ〜30ｃ隔壁、 33ａ〜33ｆ石英窓、３４液体ヘリウム収納容器、３５ホルダ（ＭｇＯ単結晶）、３７Ｈｅ−Ｎｅレーザ、３９Ｎｅランプ（第１の基準光源）、４０Ｗランプ（第２の基準光源）、４１レンズ、４２偏光解消板（スクランブラ）、４３スリット、４４レバー（切替え手段）。 DESCRIPTION OF SYMBOLS 1 light source (light emitting means), 2 first reference light source, 3,24 spectroscope (optical means), 4,4a switching means, 5 photodetector, 6 wave number calibration means, 7,36 measured object, 8th 2 reference light source, 9 intensity correction means, 10 selection means, 11,38 wave number correction and intensity correction means, 21 Ar laser (light source or light emitting means), 22 premonochromator, 23 cryostat, 25 CCD (photodetector or Light detecting means), 26 control element, 27 coating means, 28a MgO substrate, 28b superconducting film (measured object), 29 holder, 29a copper substrate, 29b carbon film, 30a to 30c partition wall, 33a to 33f quartz window, 34 Liquid helium container, 35 holder (MgO single crystal), 37 He-Ne laser, 39 Ne lamp (first reference light source), 40 W lamp (second reference light source), 41 Lens, 42 depolarizer (scrambler), 43 slit, 44 a lever (switching means).

Claims

[Claims]

1. A light source (1) for emitting excitation light, a first reference light source (2) for emitting a first reference light having a known emission line spectrum, and an object to be measured by the irradiation of the excitation light. A spectroscope (3) for injecting and dispersing the scattered light emitted from (7) or the reference light emitted from the first reference light source (2), and the scattered light to the spectroscope (3) Switching means (4) for switching between the incident light and the reference light, a photodetector (5) for detecting the scattered light or the reference light that has passed through the spectroscope (3), and the spectroscope (3) Scattered light measurement having wave number calibration means (6) for acquiring a wave number error from a comparison between the spectrum of the light having passed through and the emission line spectrum and calibrating the detected wave number of the scattered light by the wave number error. apparatus.

2. A light source (1) for emitting excitation light, a second reference light source (8) for emitting a second reference light having a known spectral energy intensity, and an object to be measured by the irradiation of the excitation light. A spectroscope (3) for injecting and dispersing the scattered light emitted from (7) or the reference light emitted from the second reference light source (8), and the scattered light to the spectroscope (3) Switching means (4) for switching between the incident light and the reference light, a photodetector (5) for detecting the scattered light or the reference light that has passed through the spectroscope (3), and the spectroscope (3 ), And an intensity correction means (9) for obtaining an intensity correction factor from a comparison between the intensity of the light having passed through and the spectral energy intensity and correcting the detected intensity of the scattered light by the intensity correction factor. Scattered light measurement device.

3. A light source (1) which emits excitation light, a first reference light source (2) which emits a first reference light having a known emission line spectrum, and a second which has a known spectral energy intensity. A second reference light source (8) for emitting the reference light, and scattered light emitted from the sample to be measured (7) by the irradiation of the excitation light or the reference light source (2) or (8) A spectroscope (3) that receives and disperses reference light, and a selection unit (10) that selects the reference light source (2) or (8) that emits the reference light from the reference light sources (2) and (8). ), Switching means (4a) for switching between the incidence of the scattered light and the incidence of the reference light on the spectroscope (3), and detecting the scattered light or the reference light that has passed through the spectroscope (3). A photodetector (5) for converting the first reference light passing through the spectroscope (3) A wave number error is obtained from the comparison between the spectrum and the emission line spectrum, the wave number of the detected scattered light is calibrated by the wave number error, and the second reference light of the second reference light that has passed through the spectroscope (3) is obtained. A wave number calibration and intensity correction means (11) for obtaining an intensity correction factor from a comparison between intensity and the spectral energy intensity and correcting the detected intensity of the scattered light by the intensity correction factor. Scattered light measuring device.

4. A holder made of a copper substrate that holds a light source that emits excitation light and a measurement object that emits scattered light when the excitation light is irradiated, and a holding surface of the measurement object is covered with carbon. A scattered light measuring device comprising: a spectroscope that makes the scattered light incident and disperses the light; and a photodetector that detects the scattered light that has passed through the spectroscope.

5. A light source that emits excitation light, a holder made of a MgO single crystal that holds a measured object that emits scattered light when irradiated with the excitation light, and a spectroscope that makes the scattered light incident and disperses the light. And a photodetector that detects scattered light that has passed through the spectroscope.

6. The cooling means for the object to be measured is provided in the peripheral portion of the object to be measured.
The scattered light measuring device described.

7. The photodetector is a CCD (Charge Coupled).
Device), Claim 4 and Claim 5
Alternatively, the scattered light measuring device according to claim 6.

8. The scattered light measuring device according to claim 4, wherein the photodetector is coated with a coating means made of lead.

9. A scattered light measuring method for detecting scattered light emitted from the measured object by irradiation of excitation light with a photodetector to analyze the measured object, wherein Rayleigh light of the scattered light is detected. By detecting through the pixels of the photodetector, among the entire exposure region of the photodetector, the region including the pixels exposed by the Rayleigh light is previously determined as the exposure region to be used, and Scattered light measurement characterized by detecting scattered light from the object to be measured in a state in which only pixels in the exposure area to be used are operated and operation of pixels other than the pixels in the exposure area to be used is stopped Method.

10. A scattered light measuring method for detecting scattered light emitted from the object to be measured by irradiation of excitation light with a photodetector and analyzing the object to be measured, wherein the universe is incident on the photodetector. The amount of accumulated noise due to a line is measured in advance, and the exposure time of the photodetector is set within the range of the amount of accumulated noise that does not hinder the measurement of the scattered light. And a method for measuring scattered light.

11. The scattered light measuring method according to claim 9, wherein the object to be measured is a superconductor film.

12. The photodetector is a CCD, claim 4, claim 9, claim 10 or claim 1.
1. The scattered light measuring method according to 1.