JP2006250836A - Spectrophotometer - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a spectrophotometer easy to be operated and capable of shortening an analytical time. <P>SOLUTION: A sample 20 is mounted on a rotary sample table 12, and a sample chamber cover 17 is closed thereafter. The rotary sample table 12 is irradiated with light by an illumination 4 since an inside of a sample chamber 1 gets dark. Then, a spectrometer part 7 is set to a wavelength capable of observing visibly a beam wavelength by a personal computer 24, so as to generate light. A portion passed through with a beam from the spectrometer part 7 is photographed by a CCD camera 3, and an image from the CCD camera 3 is displayed on a display 25 to confirm a positional relation between the sample 20 and the beam. The sample 20 is started to be measured after a position of the beam is confirmed and after the sample 20 is moved to a prescribed position with respect to the beam by the rotary sample table 12 and a stage 13. The illumination 4 is turned off just before starting the measurement. A measuring point is moved continuously according to an operation sequence file by the rotary sample table 12 and the stage 13, after starting the measurement, to conduct continuously the measurement. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a spectrophotometer having a large sample chamber capable of measuring, for example, the deep ultraviolet region.

  In a spectrophotometer, for example, in order to perform measurement in the deep ultraviolet region (region of 190 nm or less) with high sensitivity and low stray light, it is necessary to avoid absorption of deep ultraviolet light by air. Purging is performed. In the case of measurement by this method, after the sample is placed in the sample chamber, the sample chamber is sealed and nitrogen gas is supplied. In this case, although depending on the size (capacity) of the sample chamber, the sample in the sample chamber is usually supplied with air for 10 minutes or more for safety when replacing the sample for about 1 hour after the completion of this purge operation. The room cover is open.

In addition, in a spectrophotometer capable of measuring a large area plate-like sample or the like, usually, a support means for horizontally installing the plate-like sample and this is moved in two dimensions in the X-axis and Y-axis or in only one axis direction. Furthermore, it has a relatively large sample chamber that accommodates a driving means that can be moved by rotation on a horizontal plane, etc., thereby enabling multipoint measurement of a large area plate-like sample. This drive unit can continuously measure while moving the measurement point according to the operation sequence program. Control of the operation of the spectrophotometer and the drive unit in the sample chamber is organically coupled so as to be controlled by a computer and its software installed separately from the spectrophotometer device. Further, for the safety of the operator, the drive unit holds a safety device so as not to operate when the sample chamber cover of the sample chamber is open.
Prior art literature on spectrophotometers was investigated but not found.

  The driving unit of the sample chamber operates continuously according to the operation sequence file, can move the measurement point of the sample, and can perform continuous measurement. It is also possible to confirm and set the position of the sample at the measurement point on the monitor screen of the computer by the numerical values of the X axis, Y axis, or horizontal rotation axis. However, in order to know which position of the sample is actually irradiated with the light beam, the operator must leave the computer, open the sample chamber cover of the sample chamber, and visually confirm it.

  Further, when holding a safety device that locks the drive unit when the sample chamber cover of the sample chamber is open, the sample chamber cover of the sample chamber cannot be easily opened and closed. Similarly, when performing the above-described measurement in the deep ultraviolet region, the sample chamber must be purged with nitrogen gas, so that the sample chamber cover of the sample chamber cannot be easily opened and closed. Therefore, it takes a long time to confirm the position where the light beam is irradiated. As a result, the measurement time of the entire spectrophotometric measurement becomes long, and the burden on the operator is also great.

  The present invention provides a spectrophotometer that is easy to operate and can shorten the analysis time by enabling the state of the sample and light flux in the actual sample chamber to be confirmed without opening the sample chamber cover of the sample chamber. For the purpose.

  In order to solve the above problems, the spectrophotometer of the present invention moves the sample with respect to the optical path of the dispersed light, irradiates the sample with light, and measures the sample by the intensity of light output from the sample. The illumination means for irradiating the measured portion of the sample inside the spectrophotometer, the photographing means for photographing the measured portion of the sample, and the display means for displaying a photographed image of the photographing means are provided. .

  Furthermore, a camera is used as the imaging means. Alternatively, the imaging unit is configured by an optical system that captures an image of the measured part, and a camera that is installed at the output end of the optical system and captures an output image from the optical system.

  According to the present invention, since the camera and the illumination are installed in the sample chamber and the image taken by the imaging means is displayed on the computer, the position of the light beam can be confirmed without opening and closing the sample chamber cover of the sample chamber. It becomes. Since the spectrophotometer and drive unit are controlled by computer software, the operator usually operates while looking at the computer screen, but there is no need to wait for the sample chamber cover to be opened or closed, thus shortening the measurement time. And the operation itself becomes simple. Further, the position confirmation of the light beam can be performed simultaneously with the nitrogen gas purge operation in the sample chamber, and the analysis time can be greatly shortened in the spectrophotometric measurement in the deep ultraviolet region.

  In the present invention, a photographing means such as a camera such as a CCD camera and an illumination means such as a light are installed in the sample chamber. The CCD camera is installed so as to take an image of the state of the sample within the moving range of the sample, and an image taken by the camera is displayed on a computer monitor by software. Since the sample chamber is a dark room with the sample chamber cover closed, it is a light with low illuminance (for light flux confirmation) and low heat generation (to avoid temperature rise in the sample chamber to maintain the accuracy of the device and prevent sample deterioration) Are set so as to irradiate a CCD camera target point, that is, a measurement point where light passes through the sample and its vicinity. At this time, the spectrophotometer control software sets the light beam wavelength to a visible wavelength, and the portion through which the light beam passes is confirmed by an image from the CCD camera. Thereby, the position of the light beam can be confirmed without opening and closing the sample chamber cover of the sample chamber.

  In the case where the sample is transparent such as glass, it is difficult to see the portion through which the light beam passes even if light having a visible wavelength is irradiated. The position of the light beam can be confirmed by fixing the photographing means such as a CCD camera and clearly indicating the measurement point on the image on the computer side.

  Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings. FIG. 1 is a schematic configuration perspective view of a sample chamber of a spectrophotometer according to a first embodiment of the present invention. The sample chamber 1 according to the present invention includes a CCD camera 3, an illumination 4, a mounting beam 5, a spectroscope unit 7 that splits ultraviolet / visible light or visible / near infrared light, mirrors 8 and 9, and a rotating sample. The stage 12, the stage 13, the integrating sphere unit 14, the sample chamber cover 17 and the sealing material 18 are configured. The spectroscope unit 7 includes a light source such as a deuterium lamp and a halogen lamp, a diffraction grating, a slit, and a mirror.

  FIG. 2 shows a schematic configuration diagram of the spectrophotometer of the present invention. The details of the sample chamber 1 are as shown in FIG. In the sample chamber 1, a rotating sample stage 12 for holding a sample 20, a spectroscope unit 7, mirrors 8 and 9 as an optical system, and an integrating sphere unit 14 are provided. A sealing material 18 is attached to a joint portion of the sample chamber cover 17 with the sample chamber 1. The spectrophotometer is composed of the sample chamber 1 side, the PC interface 22, a personal computer 24, a display device 25, and an operating device 26.

  The light monochromatized by the spectroscope unit 7 is reflected by the mirror 8 and passes from the lower part of the sample 20 placed on the rotating sample stage 12 toward the upper part. The light absorbed by the sample 20 is reflected by the mirror 9 and received by the integrating sphere unit 14. The rotating sample table 12 and the stage 13 on which the rotating sample table 12 is installed are connected to the personal computer 24 via the PC interface 22 by an RS-232C cable. The stage 13 is moved in the X-axis and Y-axis directions by the control of the personal computer 24 using the operating device 26, and the rotating sample stage 12 is rotationally driven. When measuring the absorbance of different parts of the sample 20, the rotating sample stage 12 and the stage 13, which are driving units, continuously in the X axis direction, the Y axis direction, and the horizontal rotation axis direction according to the operation sequence file of the personal computer 24. It is possible to move the measurement point.

  In the sample chamber 1, a CCD camera 3 and an illumination 4 are attached to a mounting beam 5 installed in the sample chamber 1. The CCD camera 3 is connected to a personal computer 24 via a PC interface 22 by USB connection, and can be directly controlled by the personal computer 24, and is set so that the entire rotating sample stage 12 can be photographed. An image photographed by the CCD camera 3 can be displayed on the display device 25 of the personal computer 24. The illumination 4 is set so as to irradiate the entire rotating sample stage 12, and is connected to the personal computer 24 via the PC interface 22 by an RS-232C cable. And is controlled by the personal computer 24.

  The CCD camera 3 is connected to the personal computer 24 by USB connection, but other communication methods can be used without being limited to USB. Moreover, although control of the rotation sample stand 12 etc. is connected and controlled with the personal computer 24 by RS-232C cable, another communication method can be used as a connection method. As the display device 25, for example, a liquid crystal display device is applied.

  In starting the measurement of absorbance, the sample chamber cover 17 is closed after the sample 20 is placed on the rotating sample stage 12. At this time, since the inside of the sample chamber 1 is a dark room, the rotating sample stage 12 is irradiated with light by the illumination 4. Next, the spectroscope unit 7 is set with a personal computer 24 so that the light beam wavelength is visible, and light is generated. A portion where the light beam from the spectroscope unit 7 is reflected by the mirror 8 and passes through the sample 20 is photographed by the CCD camera 3, and an image from the CCD camera 3 is displayed on the display unit 25. Check the positional relationship. Since the illumination 4 only needs to be able to confirm the appearance of the sample 20 other than the portion to which the luminous flux strikes, the illumination 4 is controlled to have low illuminance. Moreover, in order to maintain the accuracy of the entire apparatus and to prevent the sample 20 from being deteriorated, a low heat generating material is used. After confirming the position of the light beam and moving the sample 20 to a predetermined position with respect to the light beam by the stage 13, the measurement is started. Immediately before the start of measurement, the illumination 4 is turned off. After the measurement is started, the rotating sample stage 12 and the stage 13 continuously move the measurement points according to the operation sequence file to perform continuous measurement.

  When performing measurement in the deep ultraviolet region, the sample chamber cover 17 is closed, and the inside of the sample chamber 1 is purged with nitrogen gas in parallel with the above operation. As described above, the seal material 18 is attached to the sample chamber cover 17 so that the inside of the sample chamber 1 can be kept in a sealed structure. Similarly, in the case of an apparatus having a safety device in which the drive unit such as the stage 13 is locked when the sample chamber cover 17 is open, after the sample chamber cover 17 is closed, The position and measurement status of the sample 20 are confirmed.

  In the case of measuring a sample that does not transmit light, the light emitted from the spectroscope unit 7 is guided by the mirror 8 to the upper part of the sample 20 and then irradiated from the upper part of the sample 20. The light irradiated and reflected on the sample 20 is introduced into the integrating sphere unit 14 by the mirror 9 and the light intensity is measured, so that it can be measured by the reflection method.

  A second embodiment provided by the present invention is as shown in FIGS. The second embodiment is different from the first embodiment in that the means for photographing the measurement point is divided. As shown in FIG. 3, a photographing lens 21 is disposed corresponding to the measurement point, and an optical fiber 23 for transmitting a photographed image is connected to the photographing lens 21. The optical fiber 23 is led out from the sample chamber 1 to the outside and connected to the image pickup device 27 as shown in FIG. The output of the imaging device 27 is input to the personal computer 24 via the lead wire 28, and finally the image of the measurement site is displayed on the display device 25. 1 and 2 are the same as those in FIGS. 1 and 2, and detailed description thereof is omitted. Although the present invention has been described with reference to the first embodiment and the second embodiment, the present invention is not limited to these embodiments, and various modifications may be made, including, for example, a digital camera can be substituted for a CCD camera. In the first and second embodiments, it is visually confirmed that the rotating sample stage 12 and the stage 13 operate in a predetermined sequence. A method of use is also possible in which a point to be measured is selected and measured by moving the stage 12 and the stage 13.

  The present invention can be applied to an analyzer that measures a large sample at multiple points.

It is a schematic structure perspective view of the sample chamber of the spectrophotometer of the 1st example of the present invention. It is a schematic block diagram of the spectrophotometer of the 1st Example of this invention. It is a schematic structure perspective view of the sample chamber of the spectrophotometer of the 2nd example of the present invention. It is a schematic block diagram of the spectrophotometer of the 2nd Example of this invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Sample chamber 3 CCD camera 4 Illumination 5 Mounting beam 7 Spectrometer part 8, 9 Mirror 12 Rotating sample stand 13 Stage 14 Integrating sphere unit 17 Sample chamber cover 18 Sealing material 20 Sample 22 PC interface 24 Personal computer 25 Display 26 Operation Machine

Claims (3)

In a spectrophotometer that moves and measures a sample with respect to the optical path of the dispersed light, an illuminating unit that irradiates a measured part of the sample inside the spectrophotometer, and an imaging unit that photographs the measured part of the sample And a display means for displaying a photographed image of the imaging means. The spectrophotometer according to claim 1, wherein the imaging means is a camera. 2. The spectrophotometer according to claim 1, wherein the imaging means comprises an optical system for imaging the part to be measured, and a photographing machine that is installed at an output end of the optical system and photographs an output image from the optical system.

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