WO2010073778A1 - 分光測定装置、分光測定方法、及び分光測定プログラム - Google Patents
分光測定装置、分光測定方法、及び分光測定プログラム Download PDFInfo
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- WO2010073778A1 WO2010073778A1 PCT/JP2009/065660 JP2009065660W WO2010073778A1 WO 2010073778 A1 WO2010073778 A1 WO 2010073778A1 JP 2009065660 W JP2009065660 W JP 2009065660W WO 2010073778 A1 WO2010073778 A1 WO 2010073778A1
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/645—Specially adapted constructive features of fluorimeters
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/02—Details
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- G—PHYSICS
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- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/02—Details
- G01J3/0262—Constructional arrangements for removing stray light
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- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
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- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
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- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/28—Investigating the spectrum
- G01J3/44—Raman spectrometry; Scattering spectrometry ; Fluorescence spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/28—Investigating the spectrum
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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- G—PHYSICS
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- G01N2201/065—Integrating spheres
Definitions
- the present invention relates to a spectroscopic measurement apparatus including an integrating sphere, a spectroscopic measurement method executed using the spectroscopic measurement apparatus, and a spectroscopic measurement program.
- Integrating sphere is used to measure the intensity of light emitted from the sample.
- the inner wall of the integrating sphere is made of a coating or material having a high reflectivity and excellent diffusibility, and light incident on the inner wall is subjected to multiple diffuse reflection. Then, the diffused light from the sample is detected by being incident on the photodetector through the exit opening provided at a predetermined position of the integrating sphere, thereby obtaining information such as the intensity of light emission in the sample. Can be obtained with high accuracy without depending on the light emission pattern and the angle characteristics of light emission (see, for example, Patent Documents 1 to 3).
- An example of a sample to be measured using an integrating sphere is an organic EL (electroluminescence) element.
- An organic EL element is generally a light emitting element having a structure in which an anode, an organic layer including a light emitting layer, and a cathode are laminated on a substrate made of glass or a transparent resin material. The holes injected from the anode and the electrons injected from the cathode recombine in the light emitting layer, so that photons are generated and the light emitting layer emits light.
- the external quantum efficiency defined by the ratio of the number of photons emitted outside the element to the number of injected electrons is important.
- the luminescence quantum yield (internal quantum efficiency) defined by the ratio of the number of photons emitted from the sample to the number of photons of excitation light absorbed by the sample. Is important.
- a light measuring device using an integrating sphere can be suitably used for evaluating quantum efficiency in such an organic EL element.
- next-generation displays and next-generation lighting in order to increase the light-emitting efficiency of light-emitting elements such as organic EL elements from the viewpoint of reducing power consumption, evaluation of the light-emitting quantum yield of light-emitting materials used in light-emitting elements The importance is increasing.
- a method for evaluating such a luminescence quantum yield there is a method of measuring an absolute luminescence quantum yield of a luminescent material by a photoluminescence (PL) method using a light measuring device including the integrating sphere described above.
- PL photoluminescence
- the sample of the light emitting material arranged in the integrating sphere is irradiated with excitation light of a predetermined wavelength, and the sample with respect to the number of photons of the excitation light absorbed by the sample
- the quantum yield of light emission defined by the ratio of the number of photons emitted from is measured.
- the light emitted from the sample is, for example, fluorescence emitted from the sample excited by irradiation with excitation light, and is usually light having a longer wavelength than the excitation light.
- the excitation light and the light emitted from the sample are separated and measured by using a configuration that measures the wavelength spectrum of the light to be measured using a spectroscope. (See Patent Document 1).
- the present invention has been made to solve the above problems, and provides a spectroscopic measurement apparatus, a spectroscopic measurement method, and a spectroscopic measurement program capable of reducing the influence of stray light generated in a spectroscope. For the purpose.
- the spectroscopic measurement apparatus includes: (1) a sample to be measured is disposed inside, an entrance opening for entering excitation light irradiated on the sample, and the sample; An integrating sphere having an exit opening for emitting the measured light; and (2) a spectroscopic means for obtaining a wavelength spectrum by splitting the measured light emitted from the exit opening of the integrating sphere; 3) data analysis means for performing data analysis on the wavelength spectrum acquired by the spectroscopic means, and (4) the data analysis means is the first corresponding to the excitation light in the total wavelength region measured in the wavelength spectrum.
- the sample information analysis means supplies excitation light in the absence of the sample inside the integrating sphere.
- the measurement intensity in the first target area acquired in the reference measurement for measurement is I R1
- the measurement intensity in the second target area is I R2
- the measurement intensity in the entire measurement wavelength area is I R0.
- the spectroscopic measurement method according to the present invention is (1) the sample to be measured is disposed inside, the incident opening for entering the excitation light irradiated on the sample, and the measured light from the sample are emitted. (3) using a spectroscopic measurement device comprising: an integrating sphere having a plurality of output apertures; and (2) a spectroscopic unit that splits the light to be measured emitted from the output aperture of the integrating sphere and obtains its wavelength spectrum. And (4) a spectroscopic measurement method for performing data analysis on a wavelength spectrum acquired by a spectroscopic means, and (4) a first target region corresponding to excitation light and a sample among all measurement wavelength regions in the wavelength spectrum.
- the acquired measurement intensity in the first target area is I R1
- the measurement intensity in the second target area is I R2
- the measurement intensity in the entire measurement wavelength area is I R0
- the measurement intensity in the first target region acquired in the sample measurement performed by supplying the excitation light is I S1
- the measurement intensity in the second target region is I S2
- the measurement intensity in the entire measurement wavelength region is I S0.
- the spectroscopic measurement program is (1) a sample to be measured is arranged inside, an entrance opening for entering excitation light irradiated on the sample, and light to be measured from the sample are emitted. And (2) a spectroscopic device that splits the light to be measured emitted from the exit aperture of the integrating sphere and obtains its wavelength spectrum.
- the computer executes a sample information analysis process for obtaining the emission quantum yield of the sample.
- the sample information analysis process is performed by exciting light with no sample inside the integrating sphere.
- I R1 is the measured intensity in the first target region
- I R2 is the measured intensity in the second target region
- I R0 is the measured intensity in the entire wavelength region obtained in the reference measurement.
- the measurement intensity in the first target area obtained in the sample measurement in which the excitation light is supplied in the state where the sample is present in the integrating sphere is I S1
- the measurement intensity in the second target area is I S2
- an integrating sphere configured to be capable of measurement by the PL method by providing an excitation light incident opening and a measured light emission opening
- a spectroscopic measurement apparatus is configured using spectroscopic means for spectroscopically measuring light to be measured so that the excitation light and the light emitted from the sample can be distinguished by the wavelength spectrum.
- the measurement result ⁇ of the luminescence quantum yield is used while using the two measurement results of the reference measurement without the sample and the sample measurement with the sample.
- the stray light in the spectroscope included in the measurement result is obtained by correcting the measurement value ⁇ 0 by the above formula and obtaining the analysis value ⁇ corresponding to the true value of the emission quantum yield. It is possible to reliably reduce the influence of.
- a spectroscope for decomposing the light to be measured into wavelength components, and a plurality of channels for detecting each wavelength component of the light to be measured decomposed by the spectroscope It is preferable that it is comprised as a multichannel spectrometer. In the configuration using the multi-channel spectrometer, stray light is relatively generated as described above. However, according to the method for obtaining the analysis value ⁇ corrected by the coefficients ⁇ and ⁇ , even in such a configuration, stray light is generated. The value of the light emission quantum yield with reduced influence can be suitably obtained. Further, such a method can be applied effectively in the same manner even when a spectroscope other than a multi-channel spectroscope is used.
- the spectroscopic measurement apparatus is configured using an integrating sphere and spectroscopic means for spectroscopically measuring the light to be measured to obtain a wavelength spectrum, and a sample.
- the measurement results of the reference measurement and the sample measurement are used twice, and the coefficients ⁇ and ⁇ related to the stray light are defined and corrected for the measurement value ⁇ 0 of the luminescence quantum yield from the result of the reference measurement.
- FIG. 1 is a diagram schematically illustrating a configuration of an embodiment of a spectroscopic measurement apparatus.
- FIG. 2 is a diagram schematically showing the configuration of another embodiment of the spectroscopic measurement apparatus.
- FIG. 3 is a cross-sectional view showing an example of the configuration of the integrating sphere.
- FIG. 4 is a cross-sectional view showing an example of the configuration of the integrating sphere.
- FIG. 5 is a block diagram illustrating an example of the configuration of the data analysis apparatus.
- FIG. 6 is a graph illustrating an example of a wavelength spectrum acquired by reference measurement and sample measurement.
- FIG. 7 is a diagram illustrating generation of stray light in the multichannel spectrometer.
- FIG. 8 is a graph showing a wavelength spectrum acquired by reference measurement.
- FIG. 1 is a diagram schematically illustrating a configuration of an embodiment of a spectroscopic measurement apparatus.
- FIG. 2 is a diagram schematically showing the configuration of another embodiment of the spectroscopic measurement apparatus.
- FIG. 9 is a graph showing a wavelength spectrum obtained by reference measurement.
- FIG. 10 is a graph showing a wavelength spectrum obtained by reference measurement.
- FIG. 11 is a flowchart showing an operation example of the spectroscopic measurement apparatus in the measurement mode.
- FIG. 12 is a flowchart illustrating an operation example of the spectroscopic measurement apparatus in the adjustment mode.
- FIG. 1 is a diagram schematically showing a configuration of an embodiment of a spectroscopic measurement apparatus.
- a spectroscopic measurement apparatus 1A according to the present embodiment includes an excitation light supply unit 10, an integrating sphere 20, a spectroscopic analysis device 30, and a data analysis device 50, and excitation light having a predetermined wavelength with respect to a sample S such as a luminescent material.
- the light emission characteristics such as the fluorescence characteristics of the sample S can be measured and evaluated by the photoluminescence method (PL method).
- the excitation light supply unit 10 is excitation light supply means for supplying excitation light for measuring the light emission characteristics of the sample S to the measurement target sample S accommodated in the integrating sphere 20.
- the excitation light supply unit 10 includes an excitation light source 11 and a light guide 13 that guides light from the light source 11 to the integrating sphere 20.
- a wavelength selection unit 12 for selecting a wavelength component of light used as excitation light is installed between the excitation light source 11 and the light guide 13.
- a wavelength selector 12 for example, a spectroscope can be used.
- the wavelength selection unit 12 may be omitted if unnecessary.
- the wavelength selection unit 12 may be configured to variably switch the wavelength of the excitation light.
- the integrating sphere 20 is used for measuring the light emission characteristics of the sample S disposed inside.
- the integrating sphere 20 includes an incident opening 21 for allowing the excitation light applied to the sample S to enter the integrating sphere 20, and the sample S. And an opening 23 for introducing the sample S into the integrating sphere 20 and an opening 23 for introducing the sample S into the integrating sphere 20.
- a sample holder 40 is fixed to the sample introduction opening 23.
- a sample container (sample cell) 400 that holds the sample S in a predetermined position in the integrating sphere 20 is provided at the tip of the sample holder 40.
- the exit end of the light guide 13 for exciting light incidence is fixed to the entrance opening 21 of the integrating sphere 20.
- an optical fiber can be used as the light guide 13.
- an incident end of a light guide 25 that guides light to be measured from the sample S to the subsequent spectroscopic analyzer 30 is fixed to the exit opening 22 of the integrating sphere 20.
- the light guide 25 for example, a single fiber or a bundle fiber can be used.
- the spectroscopic analyzer 30 is a spectroscopic means for spectroscopically measuring light to be measured from the sample S emitted from the exit opening 22 of the integrating sphere 20 through the light guide 25 and acquiring the wavelength spectrum thereof.
- the spectroscopic analysis device 30 includes a spectroscopic unit 31 and a spectroscopic data generation unit 32.
- the spectroscopic unit 31 includes a spectroscope for decomposing the light to be measured into wavelength components, and a multi-channel (for example, 1024 channel) detection unit for detecting each wavelength component of the light to be measured wavelength-decomposed by the spectroscope.
- the detector is configured as a multi-channel spectrometer. Specifically, for example, a CCD linear sensor in which pixels of a plurality of channels are arranged one-dimensionally can be used as the photodetector. Further, the total measurement wavelength region in which the wavelength spectrum is acquired by the spectroscopic unit 31 may be appropriately set according to a specific configuration or the like, and is, for example, 200 nm to 950 nm.
- the spectroscopic data generation unit 32 performs signal processing necessary for detection signals output from each channel of the photodetector of the spectroscopic unit 31, and generates spectroscopic data for generating wavelength spectrum data of the measured light to be dispersed. It is a generation means.
- the wavelength spectrum data generated and acquired by the spectral data generation unit 32 is output to the subsequent data analysis device 50.
- the data analysis device 50 is a data analysis unit that performs necessary data analysis on the wavelength spectrum acquired by the spectroscopic analysis device 30 and acquires information about the sample S. Details of data analysis in the analysis device 50 will be described later. Further, the data analysis device 50 is connected to an input device 61 used for inputting instructions for data analysis and the like, inputting analysis conditions, and the like, and a display device 62 used for displaying data analysis results. .
- FIG. 2 is a diagram showing a configuration of another embodiment of the spectroscopic measurement apparatus.
- the excitation light supply unit 10 selects excitation light that irradiates the sample S by selecting a predetermined wavelength component from the excitation light source 11, the light guide 13, and the light from the excitation light source 11.
- an optical filter 14 such as an interference filter.
- the integrating sphere 20 includes an incident opening 21, an exit opening 22, and a sample introduction opening 24.
- the sample holder 240 is fixed to the sample introduction opening 24, and the sample S is placed on the sample holder 240.
- FIG. 3 is a cross-sectional view showing an example of the configuration of the integrating sphere 20 used in the spectroscopic measurement apparatus 1A shown in FIG. 1, and shows the cross-sectional configuration of the integrating sphere 20 along the irradiation optical axis L of the excitation light.
- the integrating sphere 20 in this configuration example includes an integrating sphere main body 200 attached to the gantry 280 by an attaching screw 285.
- the gantry 280 is formed in an L shape having two grounding surfaces 281 and 282 orthogonal to each other.
- the irradiation optical axis L passes through the center position of the integrating sphere body 200 and extends in a direction parallel to the ground plane 281 and orthogonal to the ground plane 282.
- the integrating sphere body 200 is provided with the entrance opening 21, the exit opening 22, and the sample introduction opening 23 shown in FIG.
- the incident opening 21 is provided at a predetermined position of the integrating sphere main body 200 on one side of the optical axis L.
- the exit opening 22 is provided at a predetermined position on a plane that passes through the center position of the integrating sphere body 200 and is orthogonal to the optical axis L.
- the sample introduction opening 23 is provided at a position shifted by 90 ° from the emission opening 22 when viewed from the center position on a plane passing through the center position of the integrating sphere body 200 and orthogonal to the optical axis L.
- a second sample introduction opening 24 is provided in addition to the opening 23.
- the sample introduction opening 24 is provided on the other side of the optical axis L and at a position facing the incident opening 21.
- a light guide holder 210 for connecting the light guide 13 for exciting light incidence is inserted and attached.
- a light guide holder 220 for connecting a light guide 25 for emitting light to be measured is inserted and attached to the emission opening 22.
- the light guides 13 and 25 are not shown.
- a sample holder fixing member 230 for fixing the sample holder 40 is attached to the first sample introduction opening 23 (see FIG. 1).
- the sample holder 40 includes a hollow sample container 400 in which the sample S is accommodated (for example, a quadrangular prism shape), and a container support 401 that extends from the sample container 400.
- the container 400 is fixed to the main body 200 via the support portion 401 and the fixing member 230 in a state of being arranged at the center of the integrating sphere main body 200.
- the sample container 400 is preferably formed of a material that transmits light including excitation light and light to be measured. For example, an optical cell made of synthetic quartz glass is preferably used.
- the container support part 401 is comprised by the rod-shaped branch pipe etc. which extend in a tubular shape, for example.
- a second sample holder 240 for mounting the sample S is attached to the second sample introduction opening 24 (see FIG. 2).
- the opening 23 and the sample holder 40 can be suitably used, for example, when the solution in which the light emitting material is dissolved is the sample S.
- Such sample holder 40 can also be used when the sample S is a solid sample, a powder sample, or the like.
- the opening part 24 and the sample holder 240 can be suitably used, for example, when the sample S is a solid sample or a powder sample. In this case, for example, a sample holding substrate or a petri dish is used as the sample container.
- sample holders are selectively used according to the type of sample S, the content of spectroscopic measurement, and the like.
- the integrating sphere 20 is set with the grounding surface 281 of the gantry 280 down so that the optical axis L is along the horizontal line.
- the sample holder 240 is used, the integrating sphere 20 is set with the ground surface 282 of the gantry 280 down so that the optical axis L is along the vertical line.
- the measurement is performed with the light shielding cover 405 covered, for example, as shown in FIG.
- the light guide 13 for exciting light incidence is held in a state of being positioned by the light guide holding portion 211 of the light guide holder 210.
- Light from the excitation light source 11 (see FIG. 1) is guided to the integrating sphere 20 by the light guide 13 and is collected by the condensing lens 212 installed in the light guide holder 210 while being integrated into the integrating sphere 20.
- the held sample S is irradiated.
- the light guide 25 for emitting the light to be measured is held in a state of being positioned by the light guide holder 220.
- the light from the sample S irradiated with the excitation light is subjected to multiple diffuse reflection by the high diffuse reflection powder applied to the inner wall of the integrating sphere body 200.
- the diffusely reflected light is incident on the light guide 25 connected to the light guide holder 220, and is guided to the spectroscopic analyzer 30 as light to be measured through the light guide 25.
- the spectroscopic measurement is performed on the light to be measured from the sample S.
- the light from the sample S to be measured light includes luminescence such as fluorescence generated in the sample S by irradiation of excitation light, and scattering, reflection, etc. in the integrating sphere 20 without being absorbed by the sample S in the excitation light. There is a light component.
- FIG. 5 is a block diagram showing an example of the configuration of the data analysis apparatus 50 used in the spectroscopic measurement apparatus 1A shown in FIG.
- the data analysis apparatus 50 in this configuration example includes a spectral data input unit 51, a sample information analysis unit 52, a target region setting unit 53, and an analysis data output unit 56.
- the spectroscopic data input unit 51 is an input means for inputting wavelength spectrum data that is spectroscopic data for the sample S acquired by the spectroscopic analyzer 30.
- the wavelength spectrum data input from the spectral data input unit 51 is sent to the sample information analysis unit 52.
- the sample information analysis unit 52 is sample information analysis means for analyzing the input wavelength spectrum and acquiring information about the sample S.
- the target region setting unit 53 is a target region setting unit that sets a target region that is a wavelength region used for data analysis with respect to the acquired wavelength spectrum. Specifically, the target region setting unit 53 corresponds to the excitation light and the light emitted from the sample S included in the light to be measured, in the measurement total wavelength region in the wavelength spectrum. A corresponding first target region on the short wavelength side and a second target region on the long wavelength side corresponding to light emission from the sample S and different from the first target region are set. Such setting of the target area is executed automatically by a predetermined setting algorithm or manually based on the input content from the input device 61 by the operator.
- the analysis part 52 calculates
- the analysis data output unit 56 is an output unit that outputs data indicating the analysis result of the sample information analysis unit 52.
- the display device 62 displays the analysis result on a predetermined display screen for the operator.
- the data output destination by the output unit 56 is not limited to the display device 62, and the data may be output to other devices.
- FIG. 5 shows a configuration in which an external device 63 is connected to the analysis data output unit 56 in addition to the display device 62. Examples of the external device 63 include a printing device, an external storage device, and other terminal devices.
- the processing corresponding to the spectroscopic measurement method executed in the data analysis apparatus 50 shown in FIGS. 1 and 5 is spectroscopic measurement for causing a computer to perform data analysis on the wavelength spectrum acquired by the spectroscopic analysis apparatus 30 of the spectroscopic means. It can be realized by a program.
- the data analysis device 50 includes a CPU that operates each software program necessary for the spectroscopic measurement process, a ROM that stores the software program and the like, and a RAM that temporarily stores data during the execution of the program. Can be configured.
- the data analysis device 50 and the spectroscopic measurement device 1A described above can be realized by executing a predetermined spectroscopic measurement program by the CPU.
- the above-described program for causing the CPU to execute each process for spectroscopic measurement can be recorded on a computer-readable recording medium and distributed.
- a recording medium for example, a magnetic medium such as a hard disk and a flexible disk, an optical medium such as a CD-ROM and a DVD-ROM, a magneto-optical medium such as a floppy disk, or a program instruction is executed or stored.
- hardware devices such as RAM, ROM, and semiconductor non-volatile memory are included.
- the spectroscopic measurement performed by the excitation light supply unit 10, the integrating sphere 20, and the spectroscopic analyzer 30 and the data analysis performed by the data analyzer 50 on the wavelength spectrum acquired by the spectroscopic analyzer 30 I will explain it.
- the reference measurement in which the excitation light is supplied to the inside of the integrating sphere 20 without supplying the sample S, and the sample S is provided inside the integrating sphere 20.
- a sample measurement is performed in which excitation light is supplied and measurement is performed, and a method of obtaining a light emission quantum yield from the measurement results of these two times is used.
- the reference measurement is performed, for example, in a state where a sample container (a sample cell, a sample holding substrate, or the like) that does not contain the sample S is disposed in the integrating sphere 20.
- the sample measurement is performed in a state where the sample container containing the sample S is arranged in the integrating sphere 20.
- FIG. 6 is a graph showing an example of a wavelength spectrum acquired in the reference measurement and the sample measurement.
- a graph (a) shows a wavelength spectrum on a linear scale
- a graph (b) shows a wavelength spectrum on a log scale.
- the graph GR indicates the wavelength spectrum acquired for the excitation light in the reference measurement without the sample S.
- the graph GS shows the wavelength spectrum of excitation light + emission obtained by the sample measurement with the sample S.
- the target region setting unit 53 of the data analysis device 50 has a first target region R1 on the short wavelength side corresponding to the excitation light and a second on the long wavelength side corresponding to the light emission from the sample S.
- the target area R2 is set.
- the first target region R1 the short wavelength side region end is indicated as C1
- the long wavelength side region end is indicated as C2.
- the second target region R2 the short wavelength side region end is indicated as C3, and the long wavelength side region end is indicated as C4.
- the sample information analysis unit 52 analyzes the wavelength spectrum in the wavelength region including the target regions R1 and R2, and obtains the emission quantum yield ⁇ of the sample S.
- the measurement intensity (excitation light intensity) in the first target region R1 acquired in the reference measurement without the sample S is I R1
- the measurement intensity (emission intensity, excitation light intensity of the second target region R2) is the measurement intensity (emission intensity, excitation light intensity of the second target region R2).
- I R2 is the intensity of stray light or the like
- I R0 is the measurement intensity of the spectroscopic analyzer 30 in the entire measurement wavelength region.
- the measured intensity (excitation light intensity, intensity after absorption by the sample) in the first target region R1 obtained in the sample measurement with the sample S is I S1
- FIG. 7 is a diagram illustrating generation of stray light in the multichannel spectrometer.
- This multi-channel spectrometer is configured to include an entrance slit 311, a collimating optical system 312, a diffraction grating 313 that is a dispersive element, and a focusing optical system 314.
- stray light a case where stray light SL generated in the diffraction grating 313 is output as a wavelength component different from the original on the wavelength spectrum output surface 315 via the focusing optical system 314 is shown.
- the coefficient ⁇ is the number of photons observed in the first target region (excitation light wavelength region) with respect to the entire wavelength region, assuming that the excitation light is spread over the entire measurement wavelength region due to stray light from the spectrometer. Shows the percentage.
- the coefficient ⁇ indicates the ratio of the number of photons observed in the second target region (emission wavelength region) with respect to the entire wavelength region.
- FIGS. 8 to 10 are graphs showing wavelength spectra obtained by reference measurement in which excitation light is supplied into the integrating sphere 20 without the sample S.
- the total wavelength region measured by the spectroscopic analyzer 30 is 200 nm to 950 nm.
- the region ends C1, C2, and the like of the first target region R1 corresponding to the excitation light in the target region setting unit 53 of the data analysis device 50, the region ends C1, C2, and the like of the first target region R1 corresponding to the excitation light
- region ends C3 and C4 of the second target region R2 corresponding to light emission (for example, fluorescence) from the sample S are set.
- the light component detected in the second target region R2 is, for example, stray light caused by excitation light.
- the sample information analysis unit 52 calculates the measurement intensity in each wavelength region in the reference measurement.
- the measured intensity (integrated value of the measured intensity in the wavelength region) I R0 is obtained for the entire wavelength region of the wavelength spectrum.
- corresponding measurement intensities I R1 and I R2 are obtained for the first target region R1 and the second target region R2, respectively. Note that the measurement intensities I S0 , I S1 , and I S2 in each wavelength region in the sample measurement can be calculated by the same method.
- These stray light correction coefficients satisfy ⁇ > 0, ⁇ > 0, and ⁇ + ⁇ ⁇ 1.
- ⁇ is a value close to 1
- ⁇ is a value close to 0.
- the total intensity of the excitation light in the sample measurement is I 1
- the total intensity of the fluorescence in the sample measurement is F
- I R2 ⁇ I 0
- the measured value ⁇ 0 of the luminescence quantum yield obtained from these measured intensities is It becomes.
- ⁇ / ⁇ in the first term is measured with a small number of photons of the excitation light absorbed in the sample S due to the influence of stray light, and thus the emission quantum yield is 1 / ⁇ ( ⁇ 1) times. It shows that it is calculated greatly.
- the second term - ⁇ / ⁇ can be considered as an error given by fluorescence background subtraction.
- the measured value ⁇ 0 of the luminescence quantum yield if the influence of stray light is small and ⁇ ⁇ 1, ⁇ ⁇ 0, the measured value becomes ⁇ 0 ⁇ ⁇ with respect to the true value ⁇ of the luminescence quantum yield.
- the following formula obtained by solving the above formula in reverse Can be used to determine the analytic value ⁇ corresponding to the true value of the emission quantum yield.
- an excitation light incident opening 21 and a measured light emission opening 22 are provided to perform measurement by the PL method.
- the spectroscopic measurement apparatus 1A is configured by using the integrating sphere 20 that can be configured and the spectroscopic analysis apparatus 30 that performs spectroscopic measurement of the light to be measured so that the excitation light and the light emission from the sample S can be distinguished by the wavelength spectrum.
- the measurement result of the light emission quantum yield is used while using the two measurement results of the reference measurement without the sample S and the sample measurement with the sample S.
- the analysis value ⁇ of the rate is obtained.
- the stray light in the spectroscope included in the measurement result is obtained by correcting the measurement value ⁇ 0 by the above formula and obtaining the analysis value ⁇ corresponding to the true value of the emission quantum yield. It is possible to reliably reduce the influence of.
- the spectroscopic measurement apparatus can be realized at low cost.
- the configuration for reducing the influence of stray light by calculation as described above can be used in combination with the configuration for physically reducing stray light.
- the spectroscopic means for acquiring the wavelength spectrum of the light to be measured includes a multi-channel spectroscope having a spectroscope and a photodetector having a multi-channel detector as described above with respect to the spectroscopic analyzer 30. It is preferable that In this case, it is possible to simultaneously measure all wavelength regions necessary for the spectroscopic measurement of excitation light and light emission from the sample S without performing wavelength scanning or the like. Further, according to the above method for obtaining the analysis value ⁇ corrected by the coefficients ⁇ and ⁇ , even in the configuration using the multi-channel spectrometer in which the generation of the stray light is relatively large, the light emission in which the influence of the stray light is reduced. A quantum yield can be calculated
- Patent Document 4 Japanese Patent Laid-Open No. 11-30552 describes the removal of the influence of stray light in a spectrophotometer.
- the configuration described in Document 4 uses a method of separately preparing reference light output means including a reference spectrometer for the spectrophotometer, thereby estimating the influence of stray light as an apparatus constant.
- the coefficient ⁇ is obtained by using the measured intensities in the first target region R1 corresponding to the excitation light and the second target region R2 corresponding to the light emission of the sample S.
- FIG. 11 is a flowchart showing an operation example of the spectroscopic measurement apparatus in the measurement mode.
- the operation example of this measurement mode first, it is confirmed whether or not the reference measurement without the sample S is started (step S101). If the measurement start is instructed, the reference measurement is performed and the wavelength spectrum is obtained. Obtain (S102). Further, the setting of the first and second target regions R1 and R2 and the derivation of the coefficients ⁇ and ⁇ related to stray light are performed for the wavelength spectrum of the reference measurement (S103). Note that the setting of these target regions and the derivation of the coefficients may be performed together with the calculation of the light emission quantum yield after the sample measurement.
- step S104 is repeatedly executed.
- the sample S for which the measurement has been completed is taken out from the integrating sphere 20 (S106).
- the data analysis necessary for obtaining the emission quantum yield is performed on the wavelength spectrum acquired by the reference measurement and the sample measurement.
- the measured value ⁇ 0 of the luminescence quantum yield is calculated from the measured intensities in the respective wavelength regions in the wavelength spectrum obtained by the reference and sample measurement by the method described above (S107).
- FIG. 12 is a flowchart showing an operation example of the spectroscopic measurement apparatus in the adjustment mode.
- Such an adjustment mode is used, for example, in the configuration using the wavelength selector 12 such as a spectrometer in the excitation light supply unit 10 as shown in FIG.
- the wavelength of the excitation light is adjusted by adjusting the setting of the wavelength selection unit 12 or the like (S201), and the wavelength is determined (S202).
- the optimum exposure time for irradiating the sample S with the excitation light is determined with reference to the set characteristics of the excitation light (S203).
- the spectroscopic measurement apparatus, spectroscopic measurement method, and spectroscopic measurement program according to the present invention are not limited to the above-described embodiments and configuration examples, and various modifications are possible.
- the integrating sphere used for the spectroscopic measurement with respect to the sample S the integrating sphere 20 shown in FIGS. 3 and 4 shows an example thereof, and specifically, those having various configurations may be used.
- the specific procedure of the spectroscopic measurement is not limited to the operation examples shown in FIGS. 11 and 12, and spectroscopic measurement can be performed by various procedures.
- the present invention can be used as a spectroscopic measurement apparatus, a measurement method, and a measurement program that can reduce the influence of stray light generated in the spectroscope.
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Abstract
Description
Φ0=(IS2-IR2)/(IR1-IS1)
によって求めるとともに、リファレンス測定での迷光に関する係数β、γを
β=IR1/IR0
γ=IR2/IR0
として定義し、発光量子収率の解析値Φを
Φ=βΦ0+γ
によって求めることを特徴とする。
Φ0=(IS2-IR2)/(IR1-IS1)
によって求めるとともに、リファレンス測定での迷光に関する係数β、γを
β=IR1/IR0
γ=IR2/IR0
として定義し、発光量子収率の解析値Φを
Φ=βΦ0+γ
によって求めることを特徴とする。
Φ0=(IS2-IR2)/(IR1-IS1)
によって求めるとともに、リファレンス測定での迷光に関する係数β、γを
β=IR1/IR0
γ=IR2/IR0
として定義し、発光量子収率の解析値Φを
Φ=βΦ0+γ
によって求めることを特徴とする。
β=IR1/IR0
γ=IR2/IR0
として定義する。そして、これらの係数β、γを用い、迷光の影響が低減された発光量子収率の解析値Φを
Φ=βΦ0+γ
によって求める方法を用いている。ここで、係数βは、励起光が分光器の迷光によって測定全波長領域に広がっていると仮定して、全波長領域に対して第1対象領域(励起光波長領域)で観測される光子数の割合を示している。また、係数γは、同様に、全波長領域に対して第2対象領域(発光波長領域)で観測される光子数の割合を示している。
α=I1/I0
によって求められる。リファレンス測定及びサンプル測定において迷光の影響が無く、迷光に関する係数がβ=1、γ=0であれば、試料Sの発光量子収率の値Φは、
IR1=βI0
IR2=γI0
IS1=βI1=αβI0
IS2=F+γI1=F+αγI0
となる。
Claims (6)
- 測定対象の試料が内部に配置され、前記試料に照射される励起光を入射するための入射開口部、及び前記試料からの被測定光を出射するための出射開口部を有する積分球と、
前記積分球の前記出射開口部から出射された前記被測定光を分光して、その波長スペクトルを取得する分光手段と、
前記分光手段によって取得された前記波長スペクトルに対してデータ解析を行うデータ解析手段とを備え、
前記データ解析手段は、
前記波長スペクトルにおける測定全波長領域のうちで、前記励起光に対応する第1対象領域、及び前記試料からの発光に対応し前記第1対象領域とは異なる波長領域である第2対象領域を設定する対象領域設定手段と、
前記第1対象領域及び前記第2対象領域を含む波長領域での前記波長スペクトルを解析することで、前記試料の発光量子収率を求める試料情報解析手段とを有し、
前記試料情報解析手段は、
前記積分球の内部に前記試料無しの状態で前記励起光を供給して測定を行うリファレンス測定において取得された前記第1対象領域での測定強度をIR1、前記第2対象領域での測定強度をIR2、前記測定全波長領域での測定強度をIR0とし、
前記積分球の内部に前記試料有りの状態で前記励起光を供給して測定を行うサンプル測定において取得された前記第1対象領域での測定強度をIS1、前記第2対象領域での測定強度をIS2、前記測定全波長領域での測定強度をIS0としたときに、
発光量子収率の測定値Φ0を
Φ0=(IS2-IR2)/(IR1-IS1)
によって求めるとともに、前記リファレンス測定での迷光に関する係数β、γを
β=IR1/IR0
γ=IR2/IR0
として定義し、発光量子収率の解析値Φを
Φ=βΦ0+γ
によって求めることを特徴とする分光測定装置。 - 前記分光手段は、前記被測定光を波長成分に分解する分光器と、前記分光器によって分解された前記被測定光の各波長成分を検出するための複数チャンネルの検出部を有する光検出器とを有し、マルチチャンネル分光器として構成されていることを特徴とする請求項1記載の分光測定装置。
- 測定対象の試料が内部に配置され、前記試料に照射される励起光を入射するための入射開口部、及び前記試料からの被測定光を出射するための出射開口部を有する積分球と、前記積分球の前記出射開口部から出射された前記被測定光を分光して、その波長スペクトルを取得する分光手段とを備える分光測定装置を用い、前記分光手段によって取得された前記波長スペクトルに対してデータ解析を行う分光測定方法であって、
前記波長スペクトルにおける測定全波長領域のうちで、前記励起光に対応する第1対象領域、及び前記試料からの発光に対応し前記第1対象領域とは異なる波長領域である第2対象領域を設定する対象領域設定ステップと、
前記第1対象領域及び前記第2対象領域を含む波長領域での前記波長スペクトルを解析することで、前記試料の発光量子収率を求める試料情報解析ステップとを備え、
前記試料情報解析ステップは、
前記積分球の内部に前記試料無しの状態で前記励起光を供給して測定を行うリファレンス測定において取得された前記第1対象領域での測定強度をIR1、前記第2対象領域での測定強度をIR2、前記測定全波長領域での測定強度をIR0とし、
前記積分球の内部に前記試料有りの状態で前記励起光を供給して測定を行うサンプル測定において取得された前記第1対象領域での測定強度をIS1、前記第2対象領域での測定強度をIS2、前記測定全波長領域での測定強度をIS0としたときに、
発光量子収率の測定値Φ0を
Φ0=(IS2-IR2)/(IR1-IS1)
によって求めるとともに、前記リファレンス測定での迷光に関する係数β、γを
β=IR1/IR0
γ=IR2/IR0
として定義し、発光量子収率の解析値Φを
Φ=βΦ0+γ
によって求めることを特徴とする分光測定方法。 - 前記分光手段は、前記被測定光を波長成分に分解する分光器と、前記分光器によって分解された前記被測定光の各波長成分を検出するための複数チャンネルの検出部を有する光検出器とを有し、マルチチャンネル分光器として構成されていることを特徴とする請求項3記載の分光測定方法。
- 測定対象の試料が内部に配置され、前記試料に照射される励起光を入射するための入射開口部、及び前記試料からの被測定光を出射するための出射開口部を有する積分球と、前記積分球の前記出射開口部から出射された前記被測定光を分光して、その波長スペクトルを取得する分光手段とを備える分光測定装置に適用され、前記分光手段によって取得された前記波長スペクトルに対するデータ解析をコンピュータに実行させるためのプログラムであって、
前記波長スペクトルにおける測定全波長領域のうちで、前記励起光に対応する第1対象領域、及び前記試料からの発光に対応し前記第1対象領域とは異なる波長領域である第2対象領域を設定する対象領域設定処理と、
前記第1対象領域及び前記第2対象領域を含む波長領域での前記波長スペクトルを解析することで、前記試料の発光量子収率を求める試料情報解析処理とをコンピュータに実行させ、
前記試料情報解析処理は、
前記積分球の内部に前記試料無しの状態で前記励起光を供給して測定を行うリファレンス測定において取得された前記第1対象領域での測定強度をIR1、前記第2対象領域での測定強度をIR2、前記測定全波長領域での測定強度をIR0とし、
前記積分球の内部に前記試料有りの状態で前記励起光を供給して測定を行うサンプル測定において取得された前記第1対象領域での測定強度をIS1、前記第2対象領域での測定強度をIS2、前記測定全波長領域での測定強度をIS0としたときに、
発光量子収率の測定値Φ0を
Φ0=(IS2-IR2)/(IR1-IS1)
によって求めるとともに、前記リファレンス測定での迷光に関する係数β、γを
β=IR1/IR0
γ=IR2/IR0
として定義し、発光量子収率の解析値Φを
Φ=βΦ0+γ
によって求めることを特徴とする分光測定プログラム。 - 前記分光手段は、前記被測定光を波長成分に分解する分光器と、前記分光器によって分解された前記被測定光の各波長成分を検出するための複数チャンネルの検出部を有する光検出器とを有し、マルチチャンネル分光器として構成されていることを特徴とする請求項5記載の分光測定プログラム。
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KR20110102866A (ko) | 2011-09-19 |
EP2381240A1 (en) | 2011-10-26 |
CN102187203B (zh) | 2013-06-12 |
US20110255085A1 (en) | 2011-10-20 |
EP2381240B1 (en) | 2018-09-05 |
EP2381240A4 (en) | 2017-11-01 |
JP5161755B2 (ja) | 2013-03-13 |
JP2010151632A (ja) | 2010-07-08 |
KR101647857B1 (ko) | 2016-08-11 |
CN102187203A (zh) | 2011-09-14 |
US8462337B2 (en) | 2013-06-11 |
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