JPH087331B2 - Infrared absorption spectrum measurement microscope device - Google Patents
Infrared absorption spectrum measurement microscope deviceInfo
- Publication number
- JPH087331B2 JPH087331B2 JP5915888A JP5915888A JPH087331B2 JP H087331 B2 JPH087331 B2 JP H087331B2 JP 5915888 A JP5915888 A JP 5915888A JP 5915888 A JP5915888 A JP 5915888A JP H087331 B2 JPH087331 B2 JP H087331B2
- Authority
- JP
- Japan
- Prior art keywords
- sample
- infrared
- absorption spectrum
- measured
- focusing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
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- Investigating Or Analysing Materials By Optical Means (AREA)
- Microscoopes, Condenser (AREA)
- Spectrometry And Color Measurement (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、微小部分の赤外吸収スペクトル測定を行う
装置に係わり、特に、微小部分の観察も同時に可能な、
赤外吸収スペクトル測定顕微鏡装置に関するものであ
る。TECHNICAL FIELD The present invention relates to an apparatus for measuring an infrared absorption spectrum of a minute portion, and in particular, it is possible to observe the minute portion at the same time.
The present invention relates to an infrared absorption spectrum measuring microscope device.
一般に用いられている赤外吸収スペクトル測定装置
は、赤外線光源、赤外線の各波長又は波数毎の測定信号
を得るためのモノクロメータ又は干渉計、検出器及び試
料室等から構成されている。A commonly used infrared absorption spectrum measuring apparatus is composed of an infrared light source, a monochromator or interferometer for obtaining a measurement signal for each wavelength or wave number of infrared rays, a detector, a sample chamber, and the like.
しかし、微小部分の測定装置としては、微小部分の赤
外吸収スペクトルの測定には干渉計を用いたフーリエ変
換赤外分光光度計が高感度であるため、フーリエ変換赤
外分光光度計と顕微鏡とを組み合せた装置が用いられて
いる。However, as a measuring device for a minute portion, a Fourier transform infrared spectrophotometer using an interferometer has high sensitivity for measuring an infrared absorption spectrum of the minute portion, and therefore, a Fourier transform infrared spectrophotometer and a microscope are used. A device that combines the two is used.
この装置では、干渉計からの赤外線は楕円面及び双曲
面反射鏡からなる集光鏡でXYZステージ上の被測定試料
（以下試料と称する）面上に集光され、試料を透過した
赤外線はこの集光鏡と対称的に配置された対物レンズで
集光され、検出される。試料の観察は可視光で行ない対
物レンズの焦点の調整はXYZステージのＺ軸を調節して
行う。可視光線と赤外光線とでは集光鏡及び対物レンズ
の焦点距離が異なるため、赤外吸収スペクトルの測定の
際にＺ軸をさらに調節する。このようにすることによ
り、粒子径が20μｍ〜500μｍの試料の測定が出来る。In this device, the infrared rays from the interferometer are condensed on the surface of the sample to be measured (hereinafter referred to as the sample) on the XYZ stage by the condenser mirror consisting of the ellipsoidal surface and the hyperbolic reflector, and the infrared rays transmitted through the sample are It is condensed and detected by an objective lens symmetrically arranged with the condenser mirror. The sample is observed with visible light, and the focus of the objective lens is adjusted by adjusting the Z axis of the XYZ stage. Since the focal lengths of the condenser mirror and the objective lens are different between visible light and infrared light, the Z axis is further adjusted when measuring the infrared absorption spectrum. By doing so, it is possible to measure a sample having a particle size of 20 μm to 500 μm.
なお、関連する技術は、例えば、ジヨン・エイ・レフ
ナー他（John A.Reffner,John P.Coates and Robert G.
Messerschmidt）、フーリエ変換赤外顕微鏡による微小
部の化学分析（Chemical microscopy with FTIR micros
pectrometry）、インターナシヨナル ラボラトリ（Int
ernational Laboratory）1987年7/8月号P18〜25に開示
されている。In addition, related techniques include, for example, John A. Reffner, John P. Coates and Robert G.
Messerschmidt), Chemical analysis with FTIR micros
pectrometry), internal laboratory (Int
ernational Laboratory) 1987 July / August issue P18 ~ 25.
上述の従来技術では集光鏡の赤外線の焦点はXYZステ
ージ上の一定の高さに固定されており、試料面の高さが
異なる試料に対する配慮がなされてない。そのため、試
料によつては集光鏡の焦点の位置に測定面がないので、
試料の測定粒子径が20μｍ以下の場合には赤外吸収スペ
クトルが測定出来ない。In the above-mentioned conventional technique, the focus of infrared rays of the condenser mirror is fixed at a fixed height on the XYZ stage, and no consideration is given to samples having different sample surface heights. Therefore, depending on the sample, there is no measurement surface at the focal point of the condenser mirror,
If the measured particle size of the sample is 20 μm or less, the infrared absorption spectrum cannot be measured.
本発明は、どのような試料の場合でも集光鏡の焦点と
対物レンズの焦点と試料の測定点の３者を常に合致させ
てることを可能とし、５μｍ〜20μｍの極微小の試料の
赤外吸収スペクトルの測定を可能にすることを目的とす
るものである。INDUSTRIAL APPLICABILITY The present invention makes it possible to always match the focus of the condenser mirror, the focus of the objective lens, and the measurement point of the sample, regardless of the type of sample, and the infrared of a microscopic sample of 5 μm to 20 μm. The purpose is to enable measurement of absorption spectra.
上述の問題点を解決するためにとられた本発明の構成
は、被測定試料を三次元的に移動させるXYZステージ
と、前記被測定試料に赤外線を集光、照明する赤外線集
光系と、前記被測定試料を透過する赤外線を集光する対
物レンズと、前記被測定試料の赤外吸収スペクトルの測
定を行うスペクトル測定系及び可視光による顕微鏡像の
検出系とを有する装置において、前記対物レンズの焦点
合せ用の第１の焦点合せ手段と該第１の焦点合せ手段と
独立に操作される前記赤外線集光系の焦点合せ用の第２
の焦点合せ手段とが設けてあることを特徴とするもので
ある。The configuration of the present invention taken to solve the above-mentioned problems is an XYZ stage that moves a sample to be measured three-dimensionally, an infrared light condensing system that collects and irradiates infrared light on the sample to be measured, An objective lens comprising: an objective lens that collects infrared rays that pass through the sample to be measured; and a spectrum measurement system that measures an infrared absorption spectrum of the sample to be measured and a microscope image detection system using visible light. First focusing means for focusing and a second focusing means for the infrared focusing system which is operated independently of the first focusing means.
And a focusing means are provided.
すなわち、本発明は、XYZステージ上の試料の測定点
の高さが異なつても、赤外線の集光鏡の焦点と対物レン
ズの焦点が合致するような調節機構を設けることにより
両者の焦点の合致を達成することが出来る点に着目し、
対物レンズと赤外線集光鏡の焦点を合せる機構とその焦
点に試料の測定面を合せる機構とをそれぞれ独立にする
ことにより所期の目的を達成可能としたものである。That is, according to the present invention, even if the heights of the measurement points of the sample on the XYZ stage are different, an adjusting mechanism is provided so that the focus of the infrared condenser mirror and the focus of the objective lens match, so that the two focus points match. Focusing on the ability to achieve
By making the mechanism for focusing the objective lens and the infrared condenser mirror and the mechanism for aligning the measurement surface of the sample at the focal point independent from each other, the intended purpose can be achieved.
本発明の作用を第２図の光路図を用いて説明する。こ
の図で、１はXYZステージ、２は放物面鏡2aと双曲面鏡2
bを有するカセグレン型対物レンズ（以下対物レンズと
称する）、３は集光反射法、４はXYZステージ１上の試
料、５はタングステンランプ、６及び７はタングステン
ランプ５の光を双曲面鏡2bに導くための切換ミラー及び
部分ミラー、８は対物レンズ２と集光反射鏡の焦点、９
は試料４の測定点、F0及びFlはそれぞれ、対物レンズ２
及び集光反射鏡３の焦点距離を示している。The operation of the present invention will be described with reference to the optical path diagram of FIG. In this figure, 1 is an XYZ stage, 2 is a parabolic mirror 2a and a hyperboloidal mirror 2
Cassegrain type objective lens having b (hereinafter referred to as objective lens), 3 is a condensing reflection method, 4 is a sample on the XYZ stage 1, 5 is a tungsten lamp, 6 and 7 are lights of the tungsten lamp 5 are hyperbolic mirrors 2b A switching mirror and a partial mirror for guiding the beam to the lens, 8 is the focal point of the objective lens 2 and the condenser mirror, 9
Is the measurement point of the sample 4, and F 0 and Fl are the objective lens 2 respectively.
And the focal length of the condenser mirror 3.
集光反射鏡３は干渉計からの赤外線を試料４の測定点
に集光させるもので、上下動の可能な機構を持つてお
り、この機構を動作させることにより検出器で受ける赤
外線の強度が最大となるように調節し、それによつて対
物レンズ２と集光反射鏡３の集点８を合致させることが
出来る。次にタングステンランプ５を点灯し可視光を部
分ミラー７側から対物レンズ２試料面を照射し可視光の
焦点をXYZステージ１のＺ軸を調節して試料の測定点９
を出す。測定点９は焦点８に比べて対物レンズ２に近い
所にある。（この間隔は一定で36倍のカセグレン型対物
レンズで80μｍである。）以上の様な操作の後、赤外線
を集光反射鏡３側から入射させることにより試料２の測
定点９に赤外線の対物レンズ２と集光反射鏡３の焦点８
の３者を合致させて測定することが出来る。The condensing reflecting mirror 3 focuses the infrared light from the interferometer on the measurement point of the sample 4, and has a mechanism capable of moving up and down. By operating this mechanism, the intensity of the infrared light received by the detector is It can be adjusted to the maximum, and thereby the objective lens 2 and the focusing point 8 of the condenser mirror 3 can be matched. Next, the tungsten lamp 5 is turned on, the visible light is irradiated from the side of the partial mirror 7 to the objective lens 2 sample surface, the focus of the visible light is adjusted by adjusting the Z axis of the XYZ stage 1, and the measurement point 9 of the sample is measured.
Give out. The measurement point 9 is closer to the objective lens 2 than the focal point 8. (This interval is constant and is 80 μm for a 36 × Cassegrain type objective lens.) After the above operation, the infrared rays are made incident on the measuring point 9 of the sample 2 by making the infrared rays incident from the side of the condensing reflecting mirror 3. Focus 8 of lens 2 and condenser reflector 3
It is possible to match and measure the three.
以下、実施例について説明する。 Hereinafter, examples will be described.
第１図は一実施例の要部を示す構成図で、第２図と同
一部分には同一の符号が付してある。図において、10及
び11は平面反射鏡で、フーリエ変換赤外分光光度計の干
渉計（図示せず）から出た平行な赤外線を集光反射鏡３
へ照射させるように配置されている。12は集光反射鏡３
の上下駆動装置で集光反射鏡３と平面反射鏡11は上下駆
動装置12によつて一体となつて同時に上下するようにな
つている。13,14及び15は、それぞれ接眼レンズ、TVモ
ニタ及び赤外線検出器を示している。集光反射鏡３は焦
点距離の短かい放物面反射鏡で90度の軸外し角度で使用
する。XYZステージ１は回転体1bを回すことにより試料
台1aが上下するようになつている。切換ミラー６はタン
グステンランプから出た可視光を対物レンズ２に照射す
るための平面反対鏡で、この切換ミラー６をレバー操作
で入れることで可視光を照射できる。部分ミラー７は可
視光を対物レンズ２側に照射し、また試料４から反射し
てきた可視光を接眼レンズ13,TVモニタ14,赤外線検出器
15へ導くためのものである。FIG. 1 is a configuration diagram showing a main part of one embodiment, and the same parts as those in FIG. 2 are designated by the same reference numerals. In the figure, 10 and 11 are plane reflecting mirrors for collecting parallel infrared rays emitted from an interferometer (not shown) of a Fourier transform infrared spectrophotometer.
It is arranged to irradiate. 12 is a condenser reflector 3
With the vertical driving device, the condensing reflecting mirror 3 and the plane reflecting mirror 11 are integrally moved by the vertical driving device 12 so as to move up and down at the same time. Reference numerals 13, 14 and 15 denote an eyepiece lens, a TV monitor and an infrared detector, respectively. The condensing reflector 3 is a parabolic reflector having a short focal length and is used at an off-axis angle of 90 degrees. In the XYZ stage 1, the sample stage 1a is moved up and down by rotating the rotating body 1b. The switching mirror 6 is a flat mirror for irradiating the objective lens 2 with visible light emitted from a tungsten lamp, and visible light can be irradiated by inserting the switching mirror 6 by operating a lever. The partial mirror 7 irradiates visible light to the objective lens 2 side, and the visible light reflected from the sample 4 is an eyepiece lens 13, a TV monitor 14, an infrared detector.
It is for guiding to 15.
この実施例の赤外吸収スペクトル測定顕微鏡装置を用
いて測定を行なうには、まず、平面反射鏡10,11を通し
て集光反射鏡３に赤外線を通し、上下駆動装置12を操作
し赤外線検出器15で受ける赤外線の強度が最大となるよ
う調節し、この際にXYZステージ１の高さも調節する。
次に切換ミラー６を切換えてタングステンランプ５から
の可視光を部分ミラー７を介して対物レンズ２に入射さ
せ、試料台1aの上に試料４をのせる。回転体1bのつまみ
を回し、試料台1aを上下動させまた、XY軸を動かして試
料の測定点９に焦点８を合せる。次に切換ミラー６を外
し回転体1bを回し赤外線検出器15で受ける赤外線の強度
が最大となるように調節する。そして、ピン1cで試料台
1aの回転は固定する。In order to perform measurement using the infrared absorption spectrum measuring microscope apparatus of this embodiment, first, infrared rays are passed through the flat reflecting mirrors 10 and 11 to the condensing reflecting mirror 3, and the vertical drive unit 12 is operated to operate the infrared detector 15. Adjust so that the intensity of infrared rays received at is maximum, and at this time, adjust the height of the XYZ stage 1.
Next, the switching mirror 6 is switched so that visible light from the tungsten lamp 5 is made incident on the objective lens 2 via the partial mirror 7, and the sample 4 is placed on the sample table 1a. The knob of the rotator 1b is turned to move the sample table 1a up and down, and the XY axes are moved to bring the focus 8 to the measurement point 9 of the sample. Next, the switching mirror 6 is removed and the rotating body 1b is rotated so that the intensity of infrared rays received by the infrared detector 15 is adjusted to the maximum. Then, use pin 1c to mount the sample
The rotation of 1a is fixed.
このような操作によつて測定した結果を例示したのが
第３図で、粒子径５μｍφのポリスチレンの赤外吸収ス
ペクトルで、倍率52倍、絞り４μｍφの対物レンズを用
い、積算回数2000回で測定したもので、横軸、縦軸にそ
れぞれ波数、透過率（％）がとつてある。Fig. 3 exemplifies the result of measurement by such an operation. Infrared absorption spectrum of polystyrene with a particle size of 5 μmφ is measured with an objective lens with a magnification of 52 times and an aperture of 4 μmφ, and the number of integration is 2000 times. The horizontal axis and the vertical axis respectively show the wave number and the transmittance (%).
以上の如く、この実施例の装置によれば、いかなる試
料でも、赤外線の焦点にその測定点を合せて測定するこ
とができ、高精度の赤外吸収スペクトル測定顕微鏡装置
を実現することができる。As described above, according to the apparatus of this embodiment, any sample can be measured by aligning its measurement point with the infrared focus, and a highly accurate infrared absorption spectrum measuring microscope apparatus can be realized.
本発明は、どのような試料の場合でも、集光反射鏡の
焦点と対物レンズの焦点と試料の測定点の３者を常に合
致させることを可能とし、５μｍ〜20μｍの極微小の試
料の赤外吸収スペクトルの測定を可能とするもので、産
業上の効果の大なるものである。INDUSTRIAL APPLICABILITY The present invention makes it possible to always match the focal point of the condenser mirror, the focal point of the objective lens, and the measurement point of the sample, regardless of the type of sample, and the red color of the extremely small sample of 5 to 20 μm. It is possible to measure the external absorption spectrum and has great industrial effect.
第１図は本発明の赤外吸収スペクトル測定顕微鏡装置の
一実施例の要部の説明図、第２図は同じく作用の説明
図、第３図は第１図の実施例によつて得られた赤外吸収
スペクトルの一例の線図である。 １……XYZステージ、２……カセグレン型対物レンズ、
３……集光反射鏡、４……試料（被測定試料）、５……
タングステンランプ、６……切換ミラー、７……部分ミ
ラー、８……焦点、９……（試料の）測定点、10,11…
…平面反射鏡、12……（集光反射鏡の）上下駆動装置。FIG. 1 is an explanatory view of a main part of an embodiment of an infrared absorption spectrum measuring microscope apparatus of the present invention, FIG. 2 is an explanatory view of the same operation, and FIG. 3 is obtained by the embodiment of FIG. It is a diagram of an example of an infrared absorption spectrum. 1 ... XYZ stage, 2 ... Cassegrain type objective lens,
3 ... Focusing reflector, 4 ... Sample (sample to be measured), 5 ...
Tungsten lamp, 6 ... Switching mirror, 7 ... Partial mirror, 8 ... Focus, 9 ... (Sample) measuring point, 10, 11 ...
… Plane reflector, 12 …… Vertical drive device (of condensing reflector).
Claims (2)
テージと、前記被測定試料に赤外線を集光、照明する赤
外線集光系と、前記被測定試料を透過する赤外線を集光
する対物レンズと、前記被測定試料の赤外吸収スペクト
ルの測定を行うスペクトル測定系及び可視光による顕微
鏡像の検出系とを有する装置において、前記対物レンズ
の焦点合せ用の第１の焦点合せ手段と、該第１の焦点合
せ手段と独立に操作される前記赤外線集光系の焦点合せ
用の第２の焦点合せ手段とが設けてあることを特徴とす
る赤外吸収スペクトル測定顕微鏡装置。1. An XYZ stage for moving a sample to be measured three-dimensionally, an infrared light condensing system for collecting and illuminating infrared light on the sample to be measured, and an objective for collecting infrared light passing through the sample to be measured. In a device having a lens, a spectrum measuring system for measuring an infrared absorption spectrum of the sample to be measured, and a system for detecting a microscope image by visible light, a first focusing means for focusing the objective lens, An infrared absorption spectrum measuring microscope apparatus comprising: a first focusing means and a second focusing means for focusing the infrared focusing system which is operated independently.
部に位置する集光反射鏡と、該集光反射鏡に赤外線を入
射させる互いに平行に配置された第１及び第２の平面反
射鏡とよりなり、前記第２の焦点合せ手段が、前記集光
反射鏡と前記第２の平面反射鏡とを一体として前記対物
レンズの光軸方向に移動させる駆動装置よりなつている
特許請求の範囲第１項記載の赤外吸収スペクトル測定顕
微鏡装置。2. The infrared ray condensing system has a condenser reflecting mirror located below the sample to be measured, and first and second planes arranged in parallel with each other for making infrared rays incident on the condenser reflecting mirror. A second mirror focusing means comprises a driving device for moving the condensing reflecting mirror and the second flat reflecting mirror in the optical axis direction of the objective lens. Infrared absorption spectrum measuring microscope apparatus according to item 1 above.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5915888A JPH087331B2 (en) | 1988-03-12 | 1988-03-12 | Infrared absorption spectrum measurement microscope device |
| US07/277,964 US4922104A (en) | 1987-11-30 | 1988-11-30 | Infrared microspectrometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5915888A JPH087331B2 (en) | 1988-03-12 | 1988-03-12 | Infrared absorption spectrum measurement microscope device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01232316A JPH01232316A (en) | 1989-09-18 |
| JPH087331B2 true JPH087331B2 (en) | 1996-01-29 |
Family
ID=13105278
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5915888A Expired - Fee Related JPH087331B2 (en) | 1987-11-30 | 1988-03-12 | Infrared absorption spectrum measurement microscope device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH087331B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1096691A (en) * | 1991-03-19 | 1998-04-14 | Tokai Rika Co Ltd | Method and apparatus for analyzing plane |
| WO2013007726A1 (en) * | 2011-07-11 | 2013-01-17 | Facultes Universitaires Notre-Dame De La Paix | Method for high resolution sum-frequency generation and infrared microscopy |
| WO2014106657A1 (en) | 2013-01-04 | 2014-07-10 | University Of Limerick | Differential infra red nanoscopy system and method |
-
1988
- 1988-03-12 JP JP5915888A patent/JPH087331B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01232316A (en) | 1989-09-18 |
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| Date | Code | Title | Description |
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| LAPS | Cancellation because of no payment of annual fees |