WO2021201237A1 - 計測治具およびそれを用いた校正方法、テラヘルツ波の測定方法 - Google Patents
計測治具およびそれを用いた校正方法、テラヘルツ波の測定方法 Download PDFInfo
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- WO2021201237A1 WO2021201237A1 PCT/JP2021/014188 JP2021014188W WO2021201237A1 WO 2021201237 A1 WO2021201237 A1 WO 2021201237A1 JP 2021014188 W JP2021014188 W JP 2021014188W WO 2021201237 A1 WO2021201237 A1 WO 2021201237A1
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Images
Classifications
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3581—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using far infrared light; using Terahertz radiation
- G01N21/3586—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using far infrared light; using Terahertz radiation by Terahertz time domain spectroscopy [THz-TDS]
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3581—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using far infrared light; using Terahertz radiation
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/27—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration
- G01N21/274—Calibration, base line adjustment, drift correction
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G01N2201/12—Circuits of general importance; Signal processing
- G01N2201/127—Calibration; base line adjustment; drift compensation
Definitions
- the present invention relates to a measuring jig, a calibration method using the same, and a method for measuring a terahertz wave.
- the present invention relates to a measuring jig used for measuring the characteristics of the terahertz wave, a calibration method using the measuring jig, and a terahertz wave measuring method.
- Electromagnetic waves are called ultraviolet rays, infrared rays, terahertz waves, microwaves, etc., depending on their wavelength.
- One of the techniques for measuring various properties of a substance using electromagnetic waves is called spectroscopic measurement or spectroscopic method, and the measuring device is called a spectroscopic device.
- the measurable characteristics vary greatly depending on the wavelength region of the electromagnetic wave used here. For example, in terms of molecular characteristics, it is possible to observe the electronic state with ultraviolet rays, the molecular vibration / rotation state with infrared rays, the rotational state of the electric dipole of the molecule with microwaves, and the interaction between molecules in the terahertz wave region. Is. Therefore, when measuring a liquid in which the interaction between molecules controls the state, spectroscopic measurement in the terahertz wave region is suitable.
- spectroscopy an electromagnetic wave is incident on a sample, and the physical and chemical properties of the sample are measured from the change in the electromagnetic wave caused by the interaction between the electromagnetic wave and the sample during passage or reflection.
- a spectroscopic device using such electromagnetic waves the reproducibility of the results of measuring the same sample under the same conditions is guaranteed, and adjustments are made to the device or the results output from the device so that the values are as true as possible. It is said.
- This is called calibration.
- the difference is corrected by comparing the data output from the device using a reference standard or standard sample with the data of a known standard or standard sample in advance.
- a sample is placed in a container (generally called a spectroscopic cell) made of a material that transmits electromagnetic waves, and electromagnetic waves are incident from the outside of the spectroscopic cell to transmit, reflect, and scatter.
- a container generally called a spectroscopic cell
- electromagnetic waves are incident from the outside of the spectroscopic cell to transmit, reflect, and scatter.
- a spectroscopic cell for inserting the liquid sample is required in order to always measure the temperature and shape of the liquid sample under constant conditions.
- the necessary conditions for the spectroscopic cell are that the material sufficiently transmits the terahertz wave and that the shape is stable.
- the liquid sample is filled by a human, it is necessary to use a material having transparency in the visible light region so that the process of filling the spectroscopic cell with the liquid can be visually confirmed in consideration of workability.
- Resin is an inexpensive material that meets these conditions and can be industrially mass-produced in large quantities.
- the problem of the spectroscopic cell using the resin material is that the gap interval (hereinafter referred to as the cell gap thickness) for filling the liquid sample inside the spectroscopic cell, which is the most basic performance of the spectroscopic cell, is a resin material, so that the entire structure of the spectroscopic cell is The measurement data of the sample to be inspected was not constant or varied among the individual spectroscopic cells due to the individual deformation due to bending or the like and the variation in the cell gap thickness. Even if liquid samples in the same state are measured, there is a high possibility that the results will change, which has been a major issue in terms of measurement reproducibility.
- Patent Document 1 as an example of the measurement method of the terahertz wave spectroscope, one terahertz wave beam is divided into two beams, and a reference sample is placed on the other beam and a sample to be measured is placed on the other. A method for accurately measuring the difference between the sample to be measured and the sample is described.
- This optical system can detect only the difference with higher sensitivity by interfering the terahertz wave beam after passing from the reference sample and the sample to be inspected, respectively.
- the characteristics such as the cell gap thickness of each spectroscopic cell filled with the reference sample and the sample to be inspected are the same, it can be said that the detected difference accurately represents the characteristic difference of the sample.
- the difference in the spectroscopic cell is reflected in the measurement result and the measurement result becomes inaccurate.
- Patent Document 2 describes that terahertz wave measurement is performed using a spectroscopic cell made of a glass plate as an example of a measurement method of a terahertz wave spectroscopic device.
- a spectroscopic cell made of a glass plate As an example of a measurement method of a terahertz wave spectroscopic device.
- the transparency of terahertz waves is poor, so the thickness of the glass plate must be made thinner to create a spectroscopic cell. There was a problem that the operability was poor.
- the present invention has been made to solve such a problem, and an object of the present invention is to perform highly accurate terahertz measurement.
- the measuring jig of the present invention includes a spectroscopic cell provided with one or more plate-shaped spaces for an object to be measured that transmits or reflects terahertz waves, and the object to be measured of the spectroscopic cell.
- the spectroscopic cell is made of a resin material that allows terahertz waves to pass through, and the spectroscopic cell is loaded into the holder.
- the holder has the function of holding the spectroscopic cell and the ability to correct one or more of the strains, twists and bends of the spectroscopic cell.
- the present invention configured as described above, it is possible to mechanically correct the bending of the spectroscopic cell due to a plurality of other factors such as the bending generated during the production of the resin product and the secular change occurring during the storage of the resin product. As a result, the cell gap thickness inside the spectroscopic cell is guaranteed, and accurate spectroscopic information of the sample can be measured.
- FIG. 1 It is a figure which shows the appearance shape example of a spectroscopic cell. It is a figure which shows the combination of a spectroscopic cell and a holder, (a) is an overall outline view, (b) is a sectional view. It is a figure which shows the structural example of the cross section of the spectroscopic cell. It is a figure which shows the structural example of the terahertz wave spectroscope. It is a figure which shows the example of the spectroscopic cell, (a) shows the whole outer shape figure, (b) shows the sectional view.
- FIG. 1 It is a figure which shows the example of the spectroscopic cell, (a) shows the whole outer shape example 1, (b) shows the whole outer shape example 2, and (c) shows the cross-sectional view. It is an exploded view of a spectroscopic cell and a holder. It is a schematic diagram of the positional relationship between the spectroscopic cell and the terahertz wave beam at the time of measurement. It is a figure which shows the example of the terahertz wave absorption spectrum of a photonic crystal structure. It is a figure which shows the example which combined the holder and the spectroscopic cell when two absorption objects are attached to the holder.
- FIG. 1 is a diagram showing an example of an external shape of a spectroscopic cell 100 used in the terahertz wave spectroscopic apparatus according to the present embodiment.
- the spectroscopic cell 100 filled with the liquid sample is used in combination with the holder as shown in FIG. 2, and this is arranged in the path where the terahertz wave propagates as shown in FIG. 4, and the liquid sample is placed.
- the characteristics of the liquid sample are measured from the transmitted terahertz wave.
- Examples of the liquid sample described here include various other liquids such as saline solution and silicone oil.
- the absorption coefficient of terahertz waves varies depending on the characteristics of the liquid sample, but the cell gap thickness of the spectroscopic cell suitable for measurement may be selected.
- the material forming the spectroscopic cell 100 is transparent in the visible light region in order to secure the function of visually confirming the liquid filling operation and to allow the measurement by transmitting the terahertz wave. It is necessary to be. As a result, the filling amount in the spectroscopic cell 100 during the filling operation can be confirmed visually or with a visible camera, and terahertz wave measurement becomes possible. Glass can be mentioned as a material, but since glass absorbs terahertz waves not a little, it is necessary to reduce the thickness of the plate in order to ensure sufficient transparency for measurement, but this makes it fragile and difficult to handle. .. Therefore, the materials satisfying these conditions including the ease of handling are some resin materials, and the problem can be solved by manufacturing the spectroscopic cell 100 using the resin materials. Examples of this resin material include cycloolefin polymer and polymethylpentene.
- the spectroscopic cell 100 when the spectroscopic cell 100 is made of resin, it is easily deformed such as bent. Therefore, as shown in FIG. 2, in order to correct one or more of distortion, twist, and bending of the resin-molded spectroscopic cell 100. Invented the holder 6.
- the holder 6 has a function of attaching and detaching the spectroscopic cell 100, and the spectroscopic cell 100 and the holder 6 are always combined, and a mechanism used in the terahertz wave spectroscopic device is also invented.
- an object that absorbs a certain amount of terahertz waves (hereinafter referred to as a terahertz wave absorbing object 7) is arranged in a part of the holder 6.
- the terahertz wave absorbing object 7 has a known terahertz wave absorption amount or can be calculated from calculations or the like. Then, by measuring the terahertz wave absorbing object 7 at the same time as, before, or after measuring the object to be measured such as a liquid, the entire measurement system including the terahertz wave spectroscope, the measuring jig, and the computer (not shown) can be used. Calibration can be performed at the same time or before or after that. That is, it becomes possible to perform calibration every time the object to be measured is measured, and more accurate measurement becomes possible.
- the signal is supplied to a computer (not shown).
- processing including calibration is performed by a computer, and the characteristics of the object to be measured are analyzed from the information of the amplitude and phase of each frequency of the terahertz wave.
- calibration is performed with at least one of transmittance, reflectance, phase difference, intensity, and phase as the calibration amount.
- calibration is performed using three terahertz signals measured by transmitting a terahertz wave through the three spectroscopic cell windows 2, 4 and 5 (details will be described later) of the spectroscopic cell 100. It is also possible to perform calibration based on not only linear but also non-linear functions.
- the terahertz wave absorbing object 7 an absorbing object having a photonic structure, it is possible to artificially design its absorption characteristics, and to perform a configuration suitable for a measurement target such as a frequency band or an absorption region. Is possible. This can be designed according to the sample to be measured, and is a very effective means when there is no suitable standard or standard sample.
- the spectroscopic cell 100 includes a spectroscopic cell main body 1 which is a base of mechanical strength, a spectroscopic cell window 2 through which a terahertz wave passes (corresponding to a cell through hole in the range of patent claims), and a spectroscopic cell window. 4. Consists of a spectroscopic cell window 5, and a spectroscopic cell window cover plate 3.
- FIG. 3 shows an example of a cross-sectional view of the spectroscopic cell 100.
- the spectroscopic cell main body 1 has the same depth as the liquid filling portion 8 having a uniform depth on a plate having a thickness of 12 and the liquid filling portion 8. It has a recess of the liquid filling portion 10 and has a through hole 2, and is resin-molded.
- the spectroscopic cell window cover plate 3 is adhered in close contact with the surface of the spectroscopic cell main body 1 side in parallel.
- the liquid filling portion 10 covered with the same spectroscopic cell window cover plate 3 can also be filled with liquid in the same manner.
- the cell gap thickness 11 of each of the spectroscopic cell window 4 and the spectroscopic cell window 5 can be the same and uniform within the range of molding accuracy.
- One end of the flow path 15 and the flow path 16 formed inside the spectroscopic cell main body 1 is connected to the liquid injection port 13 and the air vent hole 14, and the other end is connected to the liquid filling portion 8 in the spectroscopic cell window 4.
- the liquid filling portion 10 in the spectroscopic cell window 5 is connected to the liquid injection port and the air vent hole via the two flow paths.
- the liquid filling portions 8 and 10 correspond to the "plate-shaped space in which the object to be measured is placed" in the claims.
- the material of the spectroscopic cell main body 1 and the spectroscopic cell window cover plate 3 needs to sufficiently transmit terahertz waves. Further, when a person visually confirms the liquid filling, either one or both of the materials of the spectroscopic cell main body 1 and the spectroscopic cell window cover plate 3 are transparent not only in the terahertz wave but also in the visible light region. Have. Of course, in the case of confirming the liquid filling by a camera or the like, the transparency in the wavelength region observable by the camera may be used.
- the spectroscopic cell window cover plate 3 and the spectroscopic cell main body 1 are bonded to each other except for the spectroscopic cell windows 4 and 5 by using a fusion or an adhesive.
- the resin material examples include cycloolefin polymer and polymethylpentene, and the spectroscopic cell 100 is manufactured using these.
- various other surface treatments such as hydrophilicity / hydrophobicity or low protein adsorption on the part where these resin materials come into contact with the liquid, it is easy to inject the liquid into the filling part and the deterioration of the filled liquid is suppressed.
- By providing a surface function that matches the properties of the liquid stable terahertz waves can be measured.
- FIG. 2 shows an example in which the spectroscopic cell main body 1 is loaded in the holder 6.
- the holder 6 is designed to have a function of correcting the distortion of the spectroscopic cell main body 1. The details of the mechanism will be described later in the description of FIG.
- Corresponds to the first holder through hole in the claims and is designed to coincide with the positions of the spectral cell window 2, the spectral cell window 4, and the spectral cell window 5, respectively.
- the spectroscopic cell 100 is a transparent medium with respect to the terahertz wave, when the terahertz wave touches the outer edges of the spectroscopic cell window 2, the spectroscopic cell window 4, the spectroscopic cell window 5, etc., complicated diffracted light is generated. , It interferes with the accuracy and reproducibility of measurement. Therefore, it is preferable that the holder window 6a, the holder window 6b, and the holder window 6c are smaller than the spectroscopic cell window 2, the spectroscopic cell window 4, and the spectroscopic cell window 5, respectively.
- the material of the holder 6 is preferably opaque to terahertz waves such as metal, and the edges of the holder window 6a, the holder window 6b, and the holder window 6c are devised to prevent diffraction (for example, corners). Has an R shape) and the like are preferable.
- the terahertz wave absorbing object 7 may be provided outside the holder window 6a, or may be provided inside the holder that does not mechanically interfere with the spectroscopic cell main body 1.
- FIG. 4 shows an example of the configuration of the terahertz wave spectroscope.
- the terahertz wave spectroscope includes a femtosecond laser light source 17, a laser light spectroscopic unit 19, a condenser lens 22, a semiconductor for generating terahertz waves 23, a terahertz wave focusing unit 24, a holder movable unit 26, a terahertz wave focusing unit 27, and a terahertz wave detection. It is configured to include a semiconductor 28 for light, a condenser lens 29, a terahertz signal detection device 30, reflection mirrors 31a, 31b, 31c, and a variable optical delay unit 32 for time delay.
- the laser light spectroscopic unit 19 uses the laser light (femtosecond laser pulse) emitted from the femtosecond laser light source 17 as a pump light 20 for operating the terahertz wave generation semiconductor 23, which is a terahertz wave light source, and terahertz wave detection. It is divided into two parts, a sampling light 21 for increasing the weak current generated by the terahertz wave by incident on the terahertz wave detection semiconductor 28, which is a part.
- the laser light spectroscopic unit 19 is composed of a semi-transmissive mirror.
- the terahertz wave 25 generated from the terahertz wave generating semiconductor 23 is any of the spectroscopic cell windows 2, 4 and 5 of the spectroscopic cell main body 1 mounted on the holder 6 by the terahertz wave focusing unit 24 composed of a focusing mirror. It is focused on the crab. Details of the three spectroscopic cell windows 2, the spectroscopic cell window 4, the spectroscopic cell window 5, and the focused terahertz wave will be described later.
- an LED light is installed on the terahertz wave generation semiconductor 23, the terahertz wave detection semiconductor 28, or the holder movable portion 26 in order to confirm with high visibility that the spectroscopic cell 100 has been installed. By doing so, when the spectroscopic cell main body 1 is loaded in the holder 6, the upper part of the spectroscopic cell main body 1 can be seen to shine.
- the terahertz wave focusing unit 27 focuses the terahertz wave transmitted through the spectroscopic cell main body 1 on the terahertz wave detecting semiconductor 28 by the condensing mirror 27a.
- the terahertz wave detection semiconductor 28 detects the terahertz wave focused by the terahertz wave focusing unit 27, and outputs a terahertz wave signal current representing the waveform.
- the terahertz signal detection device 30 detects the terahertz wave signal current and Fourier transforms the detected signal to obtain information on the amplitude and phase of each terahertz wave frequency.
- the variable optical delay unit 32 for time delay is provided in the path through which the sampling light 21, which is one of the laser lights dispersed by the laser light spectroscopic unit 19, propagates, and the sampled light reaches the terahertz wave detection semiconductor 28.
- Variable setting of the time delay amount The variable optical delay unit 32 for time delay has two movable reflection mirrors 32a and 32b with respect to the fixed reflection mirrors 31a, 31b and 31c, and the reflection mirrors 32a and 32b are directed in the direction of the arrow A. It is configured so that it can be physically translated. As a result, the delay time of the sampling light is made variable.
- the time delay variable optical delay unit 32 is used to measure the time waveform of the terahertz wave while shifting the timing at which the sampled light reaches the terahertz wave detection semiconductor 28.
- the holder movable portion 26 can be physically translated in the direction of the arrow B, and is moved to the respective positions of the holder window 6a, the holder window 6b, and the holder window 6c of the holder 6 so that the terahertz wave beam can pass therethrough. It is controlled by a computer so that it can be.
- the controlling computer is not included in FIG.
- the holder window 6a, the holder window 6b, the holder window 6c, and the spectroscopic cell main body are taken as an example in which the spectroscopic cell 100 in which the liquid filling portions 8 and 10 are filled with the sample liquid is mounted on the holder 6.
- the relationship between the spectroscopic cell window 2, the spectroscopic cell window 4, and the spectroscopic cell window 5 of Part 1 and the focused terahertz wave will be described.
- the holder window 6a, the holder window 6b, and the holder window 6c, and the spectroscopic cell window 2, the spectroscopic cell window 4, and the spectroscopic cell window 5 of the spectroscopic cell main body 1 are each in a state where the spectroscopic cell 100 is mounted on the holder 6. It is manufactured so that the centers match.
- the terahertz wave When the terahertz wave is focused on the holder window 6a by moving the holder movable portion 26, the terahertz wave passes through the terahertz wave absorbing object 7 installed on the side surface of the holder 6 and is a spectroscopic cell window. Pass through 2. At this time, since the spectroscopic cell window 2 is hollow as shown in FIG. 1, the terahertz wave that has passed through the terahertz wave absorbing object 7 measures the characteristics of only the terahertz wave absorbing object 7.
- the terahertz wave passing through the spectroscopic cell window 4 measures the characteristics of the sample liquid filled in the liquid filling section 8. Will be done.
- the terahertz wave passing through the spectroscopic cell window 5 measures the characteristics of the sample liquid filled in the liquid filling section 10. Will be done.
- FIG. 5 shows an example of another form of the spectroscopic cell 100A.
- the spectroscopic cell body 33 shown in FIG. 5 has the same material and external dimensions as the spectroscopic cell body 1 shown in FIGS. 1 and 3, but the spectroscopic cell window 33a is not hollow and is similar to the spectroscopic cell window 4.
- the spectroscopic cell windows 33b and 33c have the same structure as the spectroscopic cell windows 4 and 5, respectively.
- the spectroscopic cell window cover plate 34 is longer than the spectroscopic cell window cover plate 3 and covers the three spectroscopic cell windows 33a, 33b, 33c, and forms a space in which the solution can be filled inside the spectroscopic cell window 33a. .. FIG.
- the spectroscopic cell 100A has the same configuration as the flow path 15, the flow path 16, the liquid injection port 13, and the air vent hole 14 in FIG. 3, and the spectroscopic cell window 33a, It is connected to the spectroscopic cell window 33b and the spectroscopic cell window 33c. Further, the spectroscopic cell window 33a can be used by sealing the liquid sample.
- the spectroscopic cell window 33a is filled with a liquid having a complex dielectric constant (or absorption coefficient and refractive index, etc.) known in the terahertz wave frequency band that can be used as a reference. It has the same function as the terahertz wave absorbing object 7 made of the solid material mounted on the holder 6, and can be calibrated immediately before the measurement of the liquid sample as described above.
- a complex dielectric constant or absorption coefficient and refractive index, etc.
- FIG. 6 shows an example of spectroscopic cells 100B and 100C having different structures.
- FIG. 6C shows a cross-sectional view of the spectroscopic cells 100B and 100C.
- the spectroscopic cell body 35 shown in FIG. 6A has the same material and external dimensions as the spectroscopic cell body 1 shown in FIGS. 1 and 3, but the spectroscopic cell window 36 is not hollow, and FIG. As shown in c), it is composed of an absorption reference unit 41.
- the spectroscopic cell window 37 and the spectroscopic cell window 38 have the same structure as the spectroscopic cell windows 4 and 5, respectively.
- the spectroscopic cells 100B and 100C are provided with a flow path, a liquid injection port, an air vent hole, and the like as in FIG. 3, and are not shown.
- the absorption reference portion 41 has a photonic crystal structure formed of the same resin as the material for molding the spectroscopic cell main body portion 35.
- the spectroscopic data due to the terahertz wave passing through this portion has absorption characteristics and phase characteristics that depend on the molding material due to the design of the geometric groove pattern formed in the absorption reference unit 41. It is possible to assign a specific index to a frequency axis, a transmittance axis, and a phase axis different from those of the above.
- the spectroscopic cell window 36 has the same function as the terahertz wave absorbing object 7 made of the solid material mounted on the holder 6, and can be calibrated immediately before the measurement of the liquid sample as described above.
- the case of molding with the same resin has been described, but of course, as long as it has the same characteristics by adjusting the photonic crystal structure, it may be molded with different resins, and the same resin material may be used. It is not limited. Further, since the material of the photonic crystal structure may be a metal having geometric holes, the material is not limited to the resin. Further, in the above, the case where a geometric structure is formed by a groove pattern to form a photonic crystal has been described, but this is a photonic crystal structure in which spheres having different refractive indexes such as air are arranged in a resin. However, the photonic crystal structure is not limited to the geometric groove pattern.
- the absorption reference unit 41 has a structure formed of the same resin as the material for molding the terahertz wave absorbing object 7.
- the spectroscopic cell window 40 has the same function as the terahertz wave absorbing object 7 made of the solid material mounted on the holder 6, and can be calibrated immediately before the measurement of the liquid sample as described above.
- FIG. 7 shows an example of the internal structure of the holder 6.
- 7 (b) shows the spectroscopic cell 100
- FIG. 7 (a) shows the holder front surface 42
- FIG. 7 (c) shows the holder back surface 44.
- the holder front portion 42 has a holder window 42a, a holder window 42b, and a holder window 42c, each of which is a through hole, and is designed to coincide with the positions of the spectral cell windows 2, 4, and 5 of the spectral cell 100, respectively. There is.
- the terahertz wave absorbing object 7 is adhered to the outside of the holder window 42a.
- the screw hole 49 is used to connect the holder front surface portion 42 and the holder back surface portion 44.
- the tap holes of the holder back surface 44 corresponding to the screw holes 49 are not shown.
- the holder back surface 44 has a holder window 45a, a holder window 45b, and a holder window 45c, each of which is a through hole, and is designed to coincide with the positions of the spectral cell windows 2, 4, and 5 of the spectral cell 100, respectively. There is.
- the back surface portion 44 of the holder is provided with connection holes 46 at a plurality of locations, and by arranging the spectroscopic cell pushing units 47 (pressing mechanisms) at a plurality of locations through the connection holes 46, a function of correcting the distortion of the spectroscopic cell 100 is provided. There is.
- the spectroscopic cell pushing unit 47 is provided with a pin 48 that is pushed out at a constant pressure by an internal spring mechanism. By arranging the spectroscopic cell pushing units 47 in the connection holes 46 at a plurality of positions on the back surface portion 44 of the holder, the base plate on the back surface of the spectroscopic cell main body portion 1 can be pressed with a constant pressure by the urging force of the pin 48.
- the groove 43 on the back surface of the holder front surface 42 is formed in the spectroscopic cell body 1 in consideration of the thickness of the spectroscopic cell body 1 when the holder front surface 42 and the holder back surface 44 are in close contact with each other.
- the depth is optimized so that the contact of the pin 48 with respect to the back surface of the base plate provides an appropriate pressure.
- the connection hole 46 and the spectroscopic cell pushing unit 47 have a screw mechanism that can be moved back and forth, and the position of the spectroscopic cell pushing unit 47 arranged in the connection hole 46 (separation of the spectroscopic cell main body 1 from the back surface of the base plate). By adjusting the distance), the pressure with which the pin 48 pushes the back surface of the base plate of the spectroscopic cell main body 1 can be finely adjusted.
- Calibration can be performed by arranging the spectroscopic cell pushing unit 47 at any or all points and fine-tuning the pressure of the pin 48.
- FIG. 8A shows a state in which the incident terahertz wave beam 50 passes through the spectroscopic cell window 36, and the transmitted terahertz wave beam 51 influenced by the photonic crystal structure, which is a function of the spectroscopic cell window 36, is used for terahertz wave detection. Enter the semiconductor 28.
- An example of the resulting terahertz wave absorbance spectrum is shown in FIG.
- the terahertz wave passing through the spectroscopic cell window 36 in which the photonic crystal structure is formed can generate an absorbance spectrum having a plurality of peaks having a specific peak absorbance at a specific frequency. can. That is, since an index showing the known absorbance with respect to the frequency can be obtained for each spectroscopic cell 100B, this can be used for calibration.
- the phase difference can be calibrated in the same manner.
- the spectroscopic cell 100B having this characteristic, it is possible to always measure the same absorption spectrum for each spectroscopic cell 100B within the range of processing accuracy of the resin molded product, and it is possible to calibrate each spectroscopic cell 100B. Become. As a result, by measuring the frequency and intensity deviations and drifts of the measuring device factors in FIG. 4 as shown in FIG. 8A, it is possible to calibrate each spectroscopic cell 100B each time, resulting in higher accuracy and higher accuracy. Highly reproducible measurement is possible.
- the measurement procedure for passing the terahertz wave beam through the spectroscopic cell window 37 and the spectroscopic cell window 38 formed in the same spectroscopic cell main body 35 is sequentially performed. do. Since the calibration has already been performed at the time of the measurement, it is possible to measure the sample to be inspected more accurately. As a result, it is possible to minimize errors between individual measuring devices and errors in measurement date and time. Of course, as described above, the calibration is performed after the terahertz signals measured by passing the terahertz through the spectroscopic cell windows 36 to 38 are taken into the computer, so FIG. 8A is shown in FIG. 8B. And may be performed after FIG. 8 (c), and the order is not specified.
- FIG. 10 shows an example of a holder 63 having a different structure.
- the holder 63 is provided with two objects 64 and 65 that absorb a certain amount of terahertz waves like the terahertz wave absorbing object 7, and measures the terahertz waves to obtain two different frequency-dependent absorbances and phase differences. It has a function that can be used as a calibration amount. As a result, more accurate calibration becomes possible as compared with the case where one terahertz wave absorbing object 7 is provided as shown in FIG. Further, although two terahertz wave absorbing objects 64 and 65 have been described here, although not shown, by arranging and using terahertz wave absorbing objects having a larger number of different characteristics such as three or more, further Highly accurate configuration is possible.
- FIG. 11 shows an example of spectroscopic cells 100D and 100E having different structures.
- the uppermost spectroscopic cell window 67 and the lowermost spectroscopic cell window 70 provided in the spectroscopic cell main body 66 have different characteristics as shown in FIG. 11 (c). It is composed of an absorption reference unit 73 and an absorption reference unit 74 made of a terahertz wave absorbing object.
- the uppermost spectroscopic cell window 71 and the lowermost spectroscopic cell window 72 provided in the spectroscopic cell main body 66 are respectively as shown in FIG. 11C.
- the spectroscopic cell window cover plate 69 is provided only for the spectroscopic cell window 68 arranged in the center.
- terahertz wave measurement using the spectroscopic cells 100D and 100E configured in this way, it is possible to obtain different frequency-dependent absorbances and phase differences of the absorption reference unit 73 and the absorption reference unit 74 as calibration amounts. As a result, more accurate calibration can be performed as compared with the case where one terahertz wave absorbing object 7 is provided as shown in FIG. Further, although two terahertz wave absorbing objects have been described here, although not shown, by arranging and using terahertz wave absorbing objects having a larger number of different characteristics such as three or more, the accuracy is further improved. Configuration is possible.
- FIG. 12 shows an example of a spectroscopic cell 100A'with another structure.
- components having the same function as the components shown in FIG. 5 are designated by the same reference numerals.
- the spectroscopic cell 100A'shown in FIG. 12 columns 35a, 35b, 35c are provided in the spectroscopic cell windows 33a, 33b, 33c, respectively.
- the spectroscopic cell window cover plate 34 of the liquid filling portions 36a, 36b, 36c can be prevented from being dented or protruding after the liquid filling portions 36a, 36b, 36c are filled with the liquid.
- the columns 35a, 35b, and 35c are provided in the configuration shown in FIG. 5 has been described here, the same can be applied to FIGS. 3, 6, and 11.
- the above embodiment it is possible to mechanically correct the bending of the spectroscopic cell due to a plurality of other factors such as the bending generated during the production of the resin product and the secular change occurring during the storage of the resin product. .. As a result, the cell gap thickness inside the spectroscopic cell is guaranteed, and accurate spectroscopic information of the sample can be measured.
- the variation in the cell gap thickness of each filling portion is as follows: one having a plurality of filling portions and one having one filling portion in one spectroscopic cell.
- the one having a plurality of filling portions has the effect of significantly reducing the filling portion, and is a feature of measuring accurate spectral information.
- an object that absorbs a certain amount of terahertz waves used for calibration is placed in the window through which the terahertz wave beam of the holder passes, so that calibration data is obtained for each measurement. Can be measured, and more accurate measurement becomes possible.
- the spectroscopic cell made of an opaque material is significantly compared with the spectroscopic cell. Since it has good operability and high reliability, it greatly contributes to industrial use sites where continuous inspection work is performed.
- a gas sample or a solid sample may be used. Even in this case, the same effect as in the case of the liquid sample can be obtained. Further, the spectroscopic cell made of a resin material can be made not only by resin molding but also by cutting, and the same effect can be obtained by other resin processing methods. In addition, although an object that absorbs a certain amount of terahertz waves has been described as a solid or a liquid, the present invention is not limited to this.
- 13 (a) to 13 (c) show an outline of the embodiment of reflection.
- the components having the same functions as the components shown in FIG. 5 are designated by the same reference numerals.
- the liquid-filled portion 36c of the spectroscopic cell 100A can be filled with an object to be measured (for example, mercury) that reflects terahertz waves, and the object to be measured can be measured. ..
- the reflective surface may be the bottom of the object to be measured instead of the surface of the object to be measured, depending on the object to be measured filled in the liquid filling portion 36c.
- not only all of the object to be measured may be reflected on the surface of the object to be measured, but also a part of the object may be reflected and a part of the object may be transmitted. Furthermore, these may be repeated and multiple reflected in the object to be measured.
- FIG. 13C shows an example in which the reflection acquisition method is different.
- the incident on the object to be reflected is transmitted through the half mirror from the terahertz wave generating semiconductor.
- the reflection is configured to detect the terahertz wave reflected by the half mirror with the terahertz wave detection semiconductor.
- the terahertz wave absorbing object 7 may be filled inside the second holder through hole.
- the holder window 45a provided on the back surface portion 44 of the holder may be filled with the terahertz wave absorbing object 7.
- the holder window 42a provided on the front surface portion 42 of the holder may be filled with the terahertz wave absorbing object 7.
- the present invention relates to a spectroscopic device measuring jig and a calibration method thereof for improving accuracy, reproducibility and operability in spectroscopic measurement using a terahertz wave.
- a spectroscopic device measuring jig and a calibration method thereof for improving accuracy, reproducibility and operability in spectroscopic measurement using a terahertz wave.
- the spectroscopic cell capable of simultaneously calibrating the present invention greatly improves the reliability of measured values.
- the difference between the models of the terahertz wave measuring device can be minimized, and the correction between production lines and the correction between factories, which has been difficult until now, can be easily performed within the organization. Is subject to consistent management.
- transparency in the visible light region is one of the features of the present invention, which significantly improves the operability of the measuring operator and makes it possible to prevent mistakes in filling the liquid sample in advance, which in turn makes it possible to prevent mistakes in filling the liquid sample. By improving measurement accuracy, it greatly contributes to sampling inspections at factories.
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Abstract
Description
2 分光セル窓
3 分光セル窓カバー板
4 分光セル窓
5 分光セル窓
6 ホルダー
6a ホルダー窓
6b ホルダー窓
6c ホルダー窓
7 テラヘルツ波を一定量吸収する物体
8 液体充填部
9 液体充填部の底面
10 液体充填部
11 セルギャップ厚
12 厚さ
13 流路
14 流路
15 液体注入口
16 エアー抜き穴
17 フェムト秒レーザ光源
18 サンプリング光
19 レーザ光分光部
20 ポンプ光
21 サンプリング光
22 集光レンズ
23 テラヘルツ波発生用半導体
24 テラヘルツ波集束部
25 テラヘルツ波
26 ホルダー可動部
27 テラヘルツ波集束部
27a 集光ミラー
28 テラヘルツ波検出用半導体
29 集光レンズ
30 テラヘルツ信号検出装置
31a 反射ミラー
31b 反射ミラー
31c 反射ミラー
32 時間遅延用可変光学遅延部
32a 反射ミラー
32b 反射ミラー
33 分光セル本体部
34 分光セル窓カバー板
35 分光セル本体部
36 分光セル窓
37 分光セル窓
38 分光セル窓
39 分光セル窓カバー板
40 分光セル窓
41 吸収基準部
42a ホルダー窓
42b ホルダー窓
42c ホルダー窓
43 ホルダー前面部背面にある溝
44 ホルダー背面部
45a ホルダー窓
45b ホルダー窓
45c ホルダー窓
46 接続穴
47 分光セル押ユニット
48 ピン
49 ビス穴
50 入射テラヘルツ波ビーム
51 透過テラヘルツ波ビーム
52 入射テラヘルツ波ビーム
53 透過テラヘルツ波ビーム
54 入射テラヘルツ波ビーム
55 透過テラヘルツ波ビーム
56 基準周波数1
57 基準周波数2
58 基準周波数3
59 基準吸光度1
60 基準吸光度2
61 基準吸光度3
62 分光セル
63 ホルダー
63a ホルダー窓
63b ホルダー窓
63c ホルダー窓
64 テラヘルツ波を一定量吸収する物体
65 テラヘルツ波を一定量吸収する物体
66 分光セル
67 分光セル窓
68 分光セル窓
69 分光セル窓カバー板
70 分光セル窓
71 分光セル窓
72 分光セル窓
73 吸収基準部
74 吸収基準部
100,100A~100E 分光セル
Claims (16)
- テラヘルツ波分光装置で使用する計測治具であって、
テラヘルツ波を透過または反射させる被測定物を入れる板状の空間を1つ以上備えている容器としての分光セルと、
前記分光セルの前記被測定物を入れる空間に対応した位置に配置される1つ以上の第1ホルダー貫通孔を持つホルダーとを備え、
前記分光セルはテラヘルツ波が透過する樹脂材料でできており、前記分光セルを前記ホルダーに装填させて使用するようになされ、
前記ホルダーは、前記分光セルを保持する機能と、前記分光セルの歪み、捻れ、曲がりの1つ以上を補正することができる機能とを持つ
ことを特徴とする計測治具。 - 前記分光セルが、前記被測定物を入れる空間以外にセル貫通孔を更に備え、
前記ホルダーが、前記セル貫通孔に対応した位置に配置される第2ホルダー貫通孔を更に持つことを特徴とする請求項1に記載の計測治具。 - 前記第2ホルダー貫通孔に対して、前記テラヘルツ波を一定量吸収する物体が配置されていることを特徴とする請求項2に記載の計測治具。
- 前記テラヘルツ波を一定量吸収する物体は、前記第2ホルダー貫通孔の外部に配置され、前記ホルダーに接着されていることを特徴とする請求項3に記載の計測治具。
- 前記テラヘルツ波を一定量吸収する物体は、前記第2ホルダー貫通孔の内部に充填されていることを特徴とする請求項3に記載の計測治具。
- 前記セル貫通孔の内部に、前記テラヘルツ波を一定量吸収する物体が配置されていることを特徴とする請求項2に記載の計測治具。
- 前記テラヘルツ波を一定量吸収する物体が、フォトニック結晶構造をもつことを特徴とする請求項3または6に記載の計測治具。
- 前記テラヘルツ波を一定量吸収する物体は、前記分光セルの本体部を成形する材料と同一の樹脂材料で成形されるフォトニック結晶構造を有する吸収基準部により構成されることを特徴とする請求項6に記載の計測治具。
- 前記分光セルは、前記セル貫通孔を少なくとも2つ有し、当該少なくとも2つの前記セル貫通孔には、異なる種類のテラヘルツ波を一定量吸収する物体が配置されていることを特徴とする請求項2に記載の計測治具。
- 前記異なる種類のテラヘルツ波を一定量吸収する物体が、少なくともその1つがフォトニック結晶構造をもつことを特徴とし、2つ以上のフォトニック結晶構造がある場合は、その2つ以上のフォトニック結晶構造がすべて異なることを特徴とする請求項9に記載の計測治具。
- 前記ホルダーが、前記分光セルの着脱機能を有したことを特徴とする請求項1に記載の計測治具。
- 前記分光セルは、前記被測定物を入れる空間を複数備えるとともに、前記セル貫通孔を1つ備え、
前記被測定物を入れる複数の空間は、前記セル貫通孔を間に挟まずに並べて配置されている
ことを特徴とする請求項2に記載の計測治具。 - 前記ホルダーは、前記分光セルの歪み、捻れ、曲がりの1つ以上を補正することができる機能として、前記ホルダーの背面部の複数箇所に配置される押圧機構を備え、
前記押圧機構は、内部のバネ機構が有する付勢力によって押し出されるピンにより、前記分光セルの本体部を押圧する
ことを特徴とする請求項1に記載の計測治具。 - 前記押圧機構は、前記ホルダーの背面部の複数箇所に設けられた接続穴内に配置され、
前記押圧機構および前記接続穴は、前記接続穴内に配置される前記押圧機構の位置をネジ機構により調整可能に構成され、前記ピンが前記分光セルの本体部を押す圧力を微調整できるようになっている
ことを特徴とする請求項13に記載の計測治具。 - テラヘルツ波分光装置のテラヘルツ波光路の途中に、請求項1~14の何れか1項に記載の計測治具を設置して、上記テラヘルツ波分光装置により被測定物の特性を分光計測するテラヘルツ波の測定方法。
- テラヘルツ波分光装置のテラヘルツ波光路の途中に、請求項1~14の何れか1項に記載の計測治具を設置して、上記テラヘルツ波分光装置により測定物の特性を分光計測し、透過率、反射率、位相差、強度、あるいは位相の内、少なくとも1つを校正量として使用することを特徴とする校正方法。
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US17/770,394 US20220390364A1 (en) | 2020-04-03 | 2021-04-01 | Measuring jig, and calibration method and terahertz wave measuring method using same |
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JP2011127950A (ja) | 2009-12-16 | 2011-06-30 | Hikari Physics Kenkyusho:Kk | 液体薄膜化装置 |
JP2013190423A (ja) * | 2012-02-16 | 2013-09-26 | Univ Of Tsukuba | 試料透過光検出方法および試料透過光検出装置 |
JP2017078599A (ja) | 2015-10-19 | 2017-04-27 | フェムトディプロイメンツ株式会社 | テラヘルツ時間分解分光装置 |
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JP7465578B2 (ja) | 2024-04-11 |
KR20220163347A (ko) | 2022-12-09 |
EP4130716A1 (en) | 2023-02-08 |
US20220390364A1 (en) | 2022-12-08 |
JPWO2021201237A1 (ja) | 2021-10-07 |
TW202138786A (zh) | 2021-10-16 |
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