WO2020135540A1 - Quantum yield measurement method - Google Patents

Quantum yield measurement method Download PDF

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Publication number
WO2020135540A1
WO2020135540A1 PCT/CN2019/128494 CN2019128494W WO2020135540A1 WO 2020135540 A1 WO2020135540 A1 WO 2020135540A1 CN 2019128494 W CN2019128494 W CN 2019128494W WO 2020135540 A1 WO2020135540 A1 WO 2020135540A1
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Prior art keywords
excitation light
spectrum
preset
photoluminescence
quantum yield
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PCT/CN2019/128494
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French (fr)
Chinese (zh)
Inventor
薛占强
郭翠
潘奕
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深圳市太赫兹科技创新研究院有限公司
华讯方舟科技有限公司
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Publication of WO2020135540A1 publication Critical patent/WO2020135540A1/en

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/255Details, e.g. use of specially adapted sources, lighting or optical systems
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00Features of devices classified in G01N21/00
    • G01N2201/06Illumination; Optics
    • G01N2201/063Illuminating optical parts
    • G01N2201/0636Reflectors

Definitions

  • the embodiment of the present application belongs to the technical field of quantum yield, and particularly relates to a quantum yield testing method.
  • Quantum yield is an important parameter for evaluating the performance of luminescent materials.
  • the measurement of quantum yield mainly uses a spectrometer to detect the excitation light spectrum, photoluminescence spectrum, and transmission spectrum of the excitation light in the integrating sphere. It is obtained by calculating the ratio of the total number of emitted photons to the number of absorbed photons. Among them, the number of emitted photons It can be obtained by measuring the photoluminescence spectrum. The number of absorbed photons is the difference between the number of excitation photons and the number of transmitted excitation photons.
  • the embodiments of the present application provide a quantum yield test method, which aims to solve the difference between the measurement state when detecting the excitation light spectrum and the excitation light transmission spectrum in the traditional method for measuring quantum yield, resulting in the measured quantum yield There is a certain error problem.
  • the embodiments of the present application provide a quantum yield test method, including:
  • the quantum yield of the material to be measured is generated according to the excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum.
  • the acquiring the excitation light spectrum of the excitation light includes:
  • the excitation light spectrum of the excitation light emitted from the exit of the integrating sphere is detected.
  • irradiating the excitation light on the surface of the material to be measured to obtain the photoluminescence spectrum of the material to be tested and the transmission spectrum of the excitation light include:
  • the adjusting the incident angle of the excitation light so that the excitation light irradiates the surface of the material to be measured includes:
  • the angle of incidence of the excitation light into the integrating sphere is adjusted by adjusting the angle of the rotatable angle mirror device, so that the excitation light irradiates the surface of the material to be measured.
  • the angle of incidence of the excitation light into the integrating sphere is adjusted by adjusting the angle of the rotatable angle mirror device, so that the excitation light irradiates the surface of the material to be measured, and include:
  • a focusing lens is provided between the rotatable angle mirror device and the integrating sphere;
  • the angle of the rotatable angle mirror device is adjusted so that the excitation light irradiates the surface of the material to be measured after passing through a focusing lens.
  • the rotatable angle mirror device includes:
  • An optical mirror is used to receive the excitation light and reflect the excitation light
  • a mirror support rod for fixing the optical mirror, and the mirror support rod is connected to the optical mirror;
  • An electric rotating table is used to adjust the angle of the optical mirror through the mirror support rod, and the electric rotating table is connected with the mirror support rod.
  • the generating the quantum yield of the material to be measured according to the excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum further includes:
  • the area between the preset excitation light spectrum band and the horizontal axis of wavelength is set as the number of photons in the excitation light spectrum, and the area between the preset photoluminescence spectrum band and the horizontal axis of wavelength is For the photon number of the photoluminescence spectrum, the area between the preset transmission spectrum band and the horizontal axis of the wavelength is taken as the photon number of the transmission spectrum.
  • the generating the quantum yield of the material to be tested according to the excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum includes:
  • the excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum are generated by a preset quantum yield relationship, and the preset quantum yield relationship is:
  • Ne is the number of photons in the photoluminescence spectrum
  • Na is the difference between the number of photons in the excitation light spectrum and the number of photons in the transmission spectrum.
  • the setting of the area between the preset excitation light spectrum band and the horizontal axis of wavelength as the number of photons in the excitation light spectrum includes:
  • the energy value of the excitation light spectrum is calculated by the preset photon number relationship of the excitation light spectrum, and the preset photon number relationship of the excitation light spectrum is:
  • ⁇ N P( ⁇ )* ⁇ /Ea1;
  • Ea1 is the energy value of the excitation light spectrum
  • h is the Planck constant
  • c is the speed of light
  • ⁇ 1 is the first wavelength in the preset wavelength range
  • ⁇ 2 is the second in the preset wavelength range Wavelength
  • P ( ⁇ ) is the absolute power.
  • the setting of the area between the preset photoluminescence spectrum band and the horizontal axis of wavelength as the photon number of the photoluminescence spectrum includes:
  • the energy value of the photoluminescence spectrum is calculated by a preset photon number relationship of photoluminescence spectrum, and the photon number relationship of the preset photoluminescence spectrum is:
  • ⁇ N P( ⁇ )* ⁇ /Ee
  • Ee is the energy value of the photoluminescence spectrum
  • h is the Planck constant
  • c is the speed of light
  • ⁇ 1 is the first wavelength in the preset wavelength range
  • ⁇ 2 is the first in the preset wavelength range
  • P( ⁇ ) is the absolute power
  • Ne is the number of photons in the photoluminescence spectrum.
  • the embodiments of the present application provide a method for measuring quantum yield.
  • the excitation light spectrum of the excitation light is obtained first, and then the excitation light is irradiated on the material to be tested to obtain the material to be tested.
  • the photoluminescence spectrum and the transmission spectrum of the excitation light, and the quantum yield of the material to be tested is generated according to the excitation light spectrum, the photoluminescence spectrum and the transmission spectrum, so that when the excitation light spectrum, the photoluminescence spectrum and the transmission spectrum are detected No need to take out the material to be tested, to ensure that the test data are obtained in the same environment, to avoid errors caused by different test environments, to solve the traditional method of measuring quantum yield, in the detection of excitation light spectrum and excitation light transmission spectrum There is a difference in the measurement state at the time, which causes a certain error in the quantum yield of the measurement.
  • FIG. 1 is a schematic diagram of a quantum yield test method provided by an embodiment of this application.
  • FIG. 2 is a schematic structural diagram of a quantum yield testing device provided by an embodiment of the present application.
  • FIG. 3 is a schematic diagram of a quantum yield test method provided by another embodiment of the present application.
  • FIG. 4 is a schematic diagram of a quantum yield test method provided by another embodiment of the present application.
  • FIG. 5 is a schematic diagram of a quantum yield test method provided by another embodiment of the present application.
  • FIG. 6 is a schematic diagram of a quantum yield test method provided by another embodiment of the present application.
  • FIG. 7 is a schematic structural diagram of a rotatable angle mirror device provided by an embodiment of the present application.
  • FIG. 8 is a schematic diagram of the excitation light provided to the inner wall of the integrating sphere provided by an embodiment of the present application.
  • FIG. 9 is a schematic diagram of the excitation light provided to the surface of the material to be measured provided by an embodiment of the present application.
  • 10 is a schematic diagram of excitation light spectrum, transmission spectrum and photoluminescence spectrum when the excitation light provided by one embodiment of the present application is irradiated to the surface of the material to be measured.
  • FIG. 1 is a schematic flowchart of a quantum yield test method provided by an embodiment of the present application. As shown in FIG. 1, the quantum yield test method in this embodiment includes:
  • Step S10 Put the material to be tested inside the integrating sphere, and obtain the excitation light spectrum of the excitation light;
  • Step S20 irradiate the excitation light on the surface of the material to be measured to obtain a photoluminescence spectrum of the material to be tested and a transmission spectrum of the excitation light;
  • Step S30 Generate a quantum yield of the material to be measured according to the excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum.
  • the user can put the material to be tested inside the integrating sphere in advance, and after the excitation light is generated, irradiate the excitation light to the inner wall of the integrating sphere to detect the excitation light spectrum of the excitation light, and then adjust the incident angle of the excitation light , So that the excitation light is irradiated on the surface of the material to be tested, so as to obtain the photoluminescence spectrum of the material to be tested and the transmission spectrum of the excitation light after passing the material to be tested.
  • the entire test process there is no need to frequently take out the material to be tested and Put in, to avoid the inconsistency of the test state of the material to be tested in the integrating sphere.
  • the material to be tested can be placed on a sample stage, which is preset in the integrating sphere.
  • the incident angle of the excitation light due to a certain deflection of the incident angle of the excitation light, it fails to illuminate the sample surface, but illuminates the whiteboard at the bottom of the integrating sphere, and the excitation light undergoes uniform diffuse reflection inside the integrating sphere. Therefore, it is emitted through the exit of the integrating sphere. Therefore, the optical spectrum of the light beam emitted from the exit of the integrating sphere can be detected by providing an optical detection module at the exit of the integrating sphere.
  • the material to be measured may be a luminescent material.
  • FIG. 2 is a quantum yield testing device used in a quantum yield testing method in this embodiment.
  • the quantum yield testing method in this embodiment may further include:
  • a monochromator 20 is used to separate a series of narrow-band light beams from a wide-band light beam
  • the collimating lens 30 converges into parallel light to emit excitation light.
  • the optical collimating lens 30 collects and collimates the divergent monochromatic light output by the monochromator 20 into a parallel beam.
  • the optical collimating lens 30 is dispersed by a diffraction grating into separate single wavelengths.
  • the optical detection module 70 may be connected to the exit of the integrating sphere 60 to detect the spectrum of the light beam emitted from the exit of the integrating sphere 60.
  • FIG. 3 is a flowchart of another quantum yield test method provided by an embodiment of the present application.
  • the excitation light for acquiring the excitation light Spectrum including:
  • the excitation light is irradiated to the inner wall of the integrating sphere through the entrance of the integrating sphere, thereby detecting the excitation light spectrum of the excitation light emitted at the exit of the integrating sphere. At this time, the detection of the excitation light spectrum is completed.
  • irradiating the excitation light on the surface of the material to be measured to obtain the photoluminescence spectrum of the material to be tested and the transmission spectrum of the excitation light include:
  • the incident angle of the excitation light and irradiating the excitation light to the surface of the material to be measured it is possible to avoid moving the material to be measured when acquiring the photoluminescence spectrum of the material to be tested and the transmission spectrum of the excitation light.
  • Moving includes adjusting the position of the material to be tested or removing the material to be tested. The user can directly detect the light beam emitted by the exit of the integrating sphere 60 through the optical detection module 70 to obtain the photoluminescence spectrum of the material to be measured and the transmission spectrum of the excitation light.
  • the adjusting the incident angle of the excitation light so that the excitation light irradiates the surface of the material to be measured includes:
  • Step S211 receiving the excitation light through a rotatable angle mirror device
  • Step S212 Adjust the angle of incidence of the excitation light into the integrating sphere by adjusting the angle of the rotatable angle mirror device, so that the excitation light irradiates the surface of the material to be measured.
  • the incident angle of the excitation light can be adjusted by adjusting the angle of the rotatable angle mirror device 40 to adjust the incident angle of the excitation light to the integrating sphere 60.
  • the angle of incidence of the excitation light into the integrating sphere is adjusted by adjusting the angle of the rotatable angle mirror device, so that The irradiation of the excitation light onto the surface of the material to be measured includes:
  • Step S2121 adjust the angle of the rotatable angle mirror device
  • Step S2122 setting a focusing lens between the rotatable angle mirror device and the integrating sphere;
  • Step S2123 Adjust the angle of the rotatable angle mirror device so that the excitation light irradiates the surface of the material to be measured after passing through a focusing lens.
  • the excitation light can be focused by the focusing lens 50 so that the excitation light entering the integrating sphere 60 can be completely irradiated to the sample surface.
  • FIG. 7 is a schematic structural diagram of a rotatable angle mirror device 40 according to an embodiment of the present application. As shown in FIG. 7, the rotatable angle mirror device 40 in this embodiment includes:
  • the optical reflector 41 is used to receive the excitation light and reflect the excitation light
  • a mirror support rod 42 for fixing the optical mirror, and the mirror support rod is connected with the optical mirror;
  • the electric rotating table 43 is used to adjust the angle of the optical mirror through the mirror support rod, and the electric rotating table is connected to the mirror support rod.
  • the electric rotating table 43 can rotate clockwise or counterclockwise, driving the optical mirror 41 to rotate a certain angle, thereby changing the angle of excitation light incident into the integrating sphere 60, so that the excitation light deviates from the material to be measured or irradiates Measure the surface of the material.
  • FIG. 8 is a schematic diagram of the excitation light irradiating the inner wall of the integrating sphere provided by an embodiment of the present application. As shown in FIG. There is a certain deflection, which fails to illuminate the surface of the sample, but illuminates the whiteboard at the bottom of the integrating sphere. The excitation light uniformly diffuses inside the integrating sphere, and the excitation light entering the integrating sphere 60 is emitted from the exit of the integrating sphere 60. Then the optical detection module 7 measures the spectrum of the light beam.
  • the rotation direction here is defined as clockwise, the rotation direction is related to the actual optical path layout, and the clockwise direction is not limited.
  • FIG. 9 is a schematic diagram of the excitation light irradiating the surface of the material to be measured provided by an embodiment of the present application.
  • the electric rotating table 43 rotates counterclockwise by a certain angle, and the excitation light passes through the focusing lens 50 and enters the integrating sphere 60. Because the incident angle of the excitation light is deflected, it can be irradiated on the surface of the sample to be tested, and the sample to be tested can be excited to produce a photoluminescence spectrum.
  • the optical detection module 70 the photoluminescence spectrum and the transmission spectrum of the excitation light are measured.
  • the rotation direction here is defined as counterclockwise, the rotation direction depends on the actual optical path layout, and the rotation direction may be opposite to the rotation direction described in FIG. 3.
  • FIG. 10 is a schematic diagram of a photoluminescence spectrum, excitation light spectrum, and transmission spectrum of excitation light of a material to be tested provided by an embodiment of the present application.
  • the horizontal axis of the spectrum diagram is the wavelength.
  • the vertical axis in the spectrum diagram is the absolute energy distribution of the spectrum.
  • the generating the quantum yield of the material to be tested according to the excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum includes:
  • the area between the preset excitation light spectrum band and the horizontal axis of wavelength is set as the number of photons in the excitation light spectrum, and the area between the preset photoluminescence spectrum band and the horizontal axis of wavelength is For the photon number of the photoluminescence spectrum, the area between the preset transmission spectrum band and the horizontal axis of the wavelength is taken as the photon number of the transmission spectrum.
  • the preset wavelength range includes a first wavelength and a second wavelength, where the second wavelength is greater than the first wavelength.
  • the second wavelength may be the upper limit of the preset wavelength range
  • the first wavelength may be The lower limit of the preset wavelength range.
  • the area between each spectrum and the horizontal axis is calculated, and the area can be the number of photons corresponding to each spectrum.
  • the preset wavelength range is 400nm-600nm
  • the first wavelength is 400nm
  • the second wavelength is 600nm
  • the area of each spectrum in the range of 400nm-600nm can be calculated to obtain the number of photons corresponding to each spectrum.
  • the area between each spectrum and the horizontal axis can be obtained by integrating the spectral absolute energy of each spectrum.
  • the generating the quantum yield of the material to be tested according to the excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum further includes:
  • the excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum are generated by a preset quantum yield relationship, and the preset quantum yield relationship is:
  • Ne is the number of photons in the photoluminescence spectrum
  • Na is the difference between the number of photons in the excitation light spectrum and the number of photons in the transmission spectrum.
  • the setting of the area between the preset excitation light spectrum band and the horizontal axis of wavelength as the number of photons in the excitation light spectrum includes:
  • the energy value of the excitation light spectrum is calculated by the preset photon number relationship of the excitation light spectrum, and the preset photon number relationship of the excitation light spectrum is:
  • ⁇ N P( ⁇ )* ⁇ /Ea1;
  • Ea1 is the energy value of the excitation light spectrum
  • h is the Planck constant
  • c is the speed of light
  • ⁇ 1 is the first wavelength in the preset wavelength range
  • ⁇ 2 is the second in the preset wavelength range
  • P( ⁇ ) is the absolute power
  • Na1 is the number of photons in the excitation light spectrum.
  • the area between each spectrum and the horizontal axis can be obtained by integrating the spectral absolute energy of each spectrum.
  • the setting of the area between the preset transmission spectrum band and the horizontal axis of wavelength as the number of photons in the excitation light spectrum includes:
  • the energy value of the transmission spectrum is calculated by the preset photon number relationship of the transmission spectrum, and the preset photon number relationship of the transmission spectrum is:
  • ⁇ N P( ⁇ )* ⁇ /Ea2;
  • Ea2 is the energy value of the transmission spectrum
  • h is the Planck constant
  • c is the speed of light
  • ⁇ 1 is the first wavelength in the preset wavelength range
  • ⁇ 2 is the second wavelength in the preset wavelength range
  • P( ⁇ ) is the absolute power
  • Na2 is the number of photons in the transmission spectrum.
  • the setting of the area between the preset photoluminescence spectrum band and the horizontal axis as the number of photons in the photoluminescence spectrum includes:
  • the energy value of the photoluminescence spectrum is calculated by a preset photon number relationship of photoluminescence spectrum, and the photon number relationship of the preset photoluminescence spectrum is:
  • ⁇ N P( ⁇ )* ⁇ /Ee
  • Ee is the energy value of the photoluminescence spectrum
  • h is the Planck constant
  • c is the speed of light
  • ⁇ 1 is the first wavelength in the preset wavelength range
  • ⁇ 2 is the first in the preset wavelength range
  • P( ⁇ ) is the absolute power
  • Ne is the number of photons in the photoluminescence spectrum.
  • the embodiments of the present application provide a method for measuring quantum yield.
  • the excitation light spectrum of the excitation light is obtained first, and then the excitation light is irradiated on the material to be tested to obtain the material to be tested.
  • the photoluminescence spectrum and the transmission spectrum of the excitation light, and the quantum yield of the material to be tested is generated according to the excitation light spectrum, the photoluminescence spectrum and the transmission spectrum, so that when the excitation light spectrum, the photoluminescence spectrum and the transmission spectrum are detected No need to take out the material to be tested, to ensure that the test data are obtained in the same environment, to avoid errors caused by different test environments, to solve the traditional method of measuring quantum yield, in the detection of excitation light spectrum and excitation light transmission spectrum There is a difference in the measurement state at the time, which causes a certain error in the quantum yield of the measurement.

Abstract

A quantum yield measurement method. By means of placing a material to be detected inside an integration sphere (60), first acquiring an excitation spectrum of excitation light (S10); then, emitting excitation light onto the material to be detected, acquiring a photoluminescence spectrum and an excitation light transmitted spectrum of the material to be detected (S20); according to the excitation spectrum, photoluminescence spectrum and transmitted spectrum, generating a quantum yield of the material to be detected (S30). Thus, it is not necessary to remove the material to be detected when probing an excitation spectrum, a photoluminescence spectrum and a transmitted spectrum, ensuring that measurement data is all obtained in an identical environment, preventing errors caused by different measurement environments, and solving the problem in conventional methods of measuring quantum yield of differences in measurement conditions when probing excitation spectrum and excitation light transmitted spectrum, leading to certain errors in quantum yield measurement.

Description

一种量子产率的测试方法Method for testing quantum yield 技术领域Technical field
本申请实施例属于量子产率技术领域,尤其涉及一种量子产率的测试方法。The embodiment of the present application belongs to the technical field of quantum yield, and particularly relates to a quantum yield testing method.
背景技术Background technique
量子产率是评价发光材料性能的重要参数。量子产率的测定,主要利用光谱仪探测积分球内的激发光光谱、光致发光光谱、激发光的透射光谱,通过计算发射的光子总数与吸收的光子数的比值得到,其中,发射的光子数可通过测量光致发光光谱得到,吸收的光子数为激发光的光子数与透射的激发光光子数之差。Quantum yield is an important parameter for evaluating the performance of luminescent materials. The measurement of quantum yield mainly uses a spectrometer to detect the excitation light spectrum, photoluminescence spectrum, and transmission spectrum of the excitation light in the integrating sphere. It is obtained by calculating the ratio of the total number of emitted photons to the number of absorbed photons. Among them, the number of emitted photons It can be obtained by measuring the photoluminescence spectrum. The number of absorbed photons is the difference between the number of excitation photons and the number of transmitted excitation photons.
然而,传统测定量子产率的方法中,在探测激发光的光谱和激发光透射光谱时的测量状态存在差异,导致测定的量子产率出现一定的误差。However, in the traditional method for measuring quantum yield, there is a difference in the measurement state when detecting the excitation light spectrum and the excitation light transmission spectrum, resulting in a certain error in the measured quantum yield.
发明内容Summary of the invention
本申请实施例提供一种量子产率的测试方法,旨在解决传统测定量子产率的方法中,在探测激发光的光谱和激发光透射光谱时的测量状态存在差异,导致测定的量子产率出现一定的误差的问题。The embodiments of the present application provide a quantum yield test method, which aims to solve the difference between the measurement state when detecting the excitation light spectrum and the excitation light transmission spectrum in the traditional method for measuring quantum yield, resulting in the measured quantum yield There is a certain error problem.
本申请实施例提供了一种量子产率的测试方法,包括:The embodiments of the present application provide a quantum yield test method, including:
将待测材料放入积分球内部,并获取激发光的激发光光谱;Put the material to be tested inside the integrating sphere and obtain the excitation light spectrum of the excitation light;
将所述激发光照射在所述待测材料表面,获取所述待测材料的光致发光光谱以及所述激发光的透射光谱;Irradiating the excitation light on the surface of the material to be measured to obtain a photoluminescence spectrum of the material to be tested and a transmission spectrum of the excitation light;
根据所述激发光光谱、所述光致发光光谱以及所述透射光谱生成所述待测材料的量子产率。The quantum yield of the material to be measured is generated according to the excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum.
可选的,所述获取所述激发光的激发光光谱,包括:Optionally, the acquiring the excitation light spectrum of the excitation light includes:
将所述激发光通过积分球的入口照射在所述积分球的内壁;Irradiating the excitation light on the inner wall of the integrating sphere through the entrance of the integrating sphere;
检测从所述积分球的出口发出的激发光的激发光光谱。The excitation light spectrum of the excitation light emitted from the exit of the integrating sphere is detected.
可选的,将所述激发光照射在所述待测材料表面,获取所述待测材料的光致发光光谱以及所述激发光的透射光谱,包括:Optionally, irradiating the excitation light on the surface of the material to be measured to obtain the photoluminescence spectrum of the material to be tested and the transmission spectrum of the excitation light include:
调整所述激发光的入射角度,以使所述激发光照射到所述待测材料表面;Adjusting the incident angle of the excitation light so that the excitation light irradiates the surface of the material to be measured;
检测从所述积分球的出口发出的所述待测材料的光致发光光谱以及所述激发光的透射光谱。Detecting the photoluminescence spectrum of the material to be tested and the transmission spectrum of the excitation light emitted from the exit of the integrating sphere.
可选的,所述调整所述激发光的入射角度,以使所述激发光照射到所述待测材料表面,包括:Optionally, the adjusting the incident angle of the excitation light so that the excitation light irradiates the surface of the material to be measured includes:
通过可旋转角度反射镜装置接收所述激发光;Receiving the excitation light through a rotatable angle mirror device;
通过调节所述可旋转角度反射镜装置的角度对所述激发光进入所述积分球的入射角进行调节,以使得所述激发光照射到所述待测材料表面。The angle of incidence of the excitation light into the integrating sphere is adjusted by adjusting the angle of the rotatable angle mirror device, so that the excitation light irradiates the surface of the material to be measured.
可选的,所述通过调节所述可旋转角度反射镜装置的角度对所述激发光进入所述积分球的入射角进行调节,以使得所述激发光照射到所述待测材料表面,还包括:Optionally, the angle of incidence of the excitation light into the integrating sphere is adjusted by adjusting the angle of the rotatable angle mirror device, so that the excitation light irradiates the surface of the material to be measured, and include:
对所述可旋转角度反射镜装置的角度进行调节;Adjust the angle of the rotatable angle mirror device;
在所述可旋转角度反射镜装置与所述积分球之间设置聚焦透镜;A focusing lens is provided between the rotatable angle mirror device and the integrating sphere;
调节所述可旋转角度反射镜装置的角度,以使得所述激发光通过聚焦透镜后照射到所述待测材料表面。The angle of the rotatable angle mirror device is adjusted so that the excitation light irradiates the surface of the material to be measured after passing through a focusing lens.
可选的,所述可旋转角度反射镜装置,包括:Optionally, the rotatable angle mirror device includes:
光学反射镜,用于接收所述激发光,并对所述激发光进行反射;An optical mirror is used to receive the excitation light and reflect the excitation light;
反射镜支杆,用于固定所述光学反射镜,所述反射镜支杆与所述光学反射镜连接;以及A mirror support rod for fixing the optical mirror, and the mirror support rod is connected to the optical mirror; and
电动旋转台,用于通过所述反射镜支杆调整所述光学反射镜的角度,所述电动旋转台与所述反射镜支杆连接。An electric rotating table is used to adjust the angle of the optical mirror through the mirror support rod, and the electric rotating table is connected with the mirror support rod.
可选的,所述根据所述激发光光谱、所述光致发光光谱以及所述透射光谱生成所述待测材料的量子产率,还包括:Optionally, the generating the quantum yield of the material to be measured according to the excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum, further includes:
按照预设波长范围分别从所述激发光光谱中获取预设激发光光谱波段、从所述光致发光光谱中获取预设光致发光光谱波段以及从所述透射光谱中获取预设透射光谱波段;Obtaining a preset excitation light spectrum band from the excitation light spectrum, a preset photoluminescence spectrum band from the photoluminescence spectrum, and a preset transmission spectrum band from the transmission spectrum according to a preset wavelength range ;
将所述预设激发光光谱波段与波长横轴之间的面积设为所述激发光光谱的光子数,将所述预设光致发光光谱波段与所述波长横轴之间的面积设为所述光致发光光谱的光子数,将所述预设透射光谱波段与所述波长横轴之间的面积设为所述透射光谱的光子数。The area between the preset excitation light spectrum band and the horizontal axis of wavelength is set as the number of photons in the excitation light spectrum, and the area between the preset photoluminescence spectrum band and the horizontal axis of wavelength is For the photon number of the photoluminescence spectrum, the area between the preset transmission spectrum band and the horizontal axis of the wavelength is taken as the photon number of the transmission spectrum.
可选的,所述根据所述激发光光谱、所述光致发光光谱以及所述透射光谱生成所述待测材料的量子产率,包括:Optionally, the generating the quantum yield of the material to be tested according to the excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum includes:
将所述激发光光谱、所述光致发光光谱以及所述透射光谱通过预设量子产率关系式生成量子产率,所述预设量子产率关系式为:The excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum are generated by a preset quantum yield relationship, and the preset quantum yield relationship is:
η=Ne/Na;η=Ne/Na;
其中,η为所述待测材料的量子产率,Ne为所述光致发光光谱的光子数,Na为所述激发光光谱的光子数与所述透射光谱的光子数的差值。Where η is the quantum yield of the material to be measured, Ne is the number of photons in the photoluminescence spectrum, and Na is the difference between the number of photons in the excitation light spectrum and the number of photons in the transmission spectrum.
可选的,所述将所述预设激发光光谱波段与波长横轴之间的面积设为所述激发光光谱的光子数,包括:Optionally, the setting of the area between the preset excitation light spectrum band and the horizontal axis of wavelength as the number of photons in the excitation light spectrum includes:
通过所述激发光光谱获取所述激发光光谱的能量值;Obtaining the energy value of the excitation light spectrum through the excitation light spectrum;
将所述激发光光谱的能量值通过预设的所述激发光光谱的光子数关系式计算所述激发光光谱的光子数,所述预设的所述激发光光谱的光子数关系式为:The energy value of the excitation light spectrum is calculated by the preset photon number relationship of the excitation light spectrum, and the preset photon number relationship of the excitation light spectrum is:
Ea1=h*c/λ;Ea1=h*c/λ;
△N=P(λ)*△λ/Ea1;△N=P(λ)*△λ/Ea1;
Figure PCTCN2019128494-appb-000001
Figure PCTCN2019128494-appb-000001
其中,Ea1为所述激发光光谱的能量值,h为普朗克常量,c为光速,λ1为所述预设波长范围中的第一波长,λ2为所述预设波长范围中的第二波长,P (λ)为绝对功率。Where Ea1 is the energy value of the excitation light spectrum, h is the Planck constant, c is the speed of light, λ1 is the first wavelength in the preset wavelength range, and λ2 is the second in the preset wavelength range Wavelength, P (λ) is the absolute power.
可选的,所述将所述预设光致发光光谱波段与所述波长横轴之间的面积设为所述光致发光光谱的光子数,包括:Optionally, the setting of the area between the preset photoluminescence spectrum band and the horizontal axis of wavelength as the photon number of the photoluminescence spectrum includes:
通过所述光致发光光谱获取所述光致发光光谱的能量值;Obtaining the energy value of the photoluminescence spectrum through the photoluminescence spectrum;
将所述光致发光光谱的能量值通过预设的光致发光光谱的光子数关系式计算所述光致发光光谱的光子数,所述预设的光致发光光谱的光子数关系式为:The energy value of the photoluminescence spectrum is calculated by a preset photon number relationship of photoluminescence spectrum, and the photon number relationship of the preset photoluminescence spectrum is:
Ee=h*c/λ;Ee=h*c/λ;
△N=P(λ)*△λ/Ee;△N=P(λ)*△λ/Ee;
Figure PCTCN2019128494-appb-000002
Figure PCTCN2019128494-appb-000002
其中,Ee为所述光致发光光谱的能量值,h为普朗克常量,c为光速,λ1为所述预设波长范围中的第一波长,λ2为所述预设波长范围中的第二波长,P(λ)为绝对功率,Ne为所述光致发光光谱的光子数。Where Ee is the energy value of the photoluminescence spectrum, h is the Planck constant, c is the speed of light, λ1 is the first wavelength in the preset wavelength range, and λ2 is the first in the preset wavelength range At two wavelengths, P(λ) is the absolute power, and Ne is the number of photons in the photoluminescence spectrum.
本申请实施例提供了一种量子产率的测试方法,通过将待测材料放入积分球内部,先获取激发光的激发光光谱,然后将激发光照射在待测材料上,获取待测材料的光致发光光谱以及激发光的透射光谱,并根据激发光光谱、光致发光光谱以及透射光谱生成待测材料的量子产率,从而使得在探测激发光光谱、光致发光光谱以及透射光谱时无需取出待测材料,保证了测试数据均在同一环境下取得,避免了因为测试环境不同而产生的误差,解决了传统测定量子产率的方法中,在探测激发光的光谱和激发光透射光谱时的测量状态存在差异,导致测定的量子产率出现一定的误差的问题。The embodiments of the present application provide a method for measuring quantum yield. By placing the material to be tested inside the integrating sphere, the excitation light spectrum of the excitation light is obtained first, and then the excitation light is irradiated on the material to be tested to obtain the material to be tested The photoluminescence spectrum and the transmission spectrum of the excitation light, and the quantum yield of the material to be tested is generated according to the excitation light spectrum, the photoluminescence spectrum and the transmission spectrum, so that when the excitation light spectrum, the photoluminescence spectrum and the transmission spectrum are detected No need to take out the material to be tested, to ensure that the test data are obtained in the same environment, to avoid errors caused by different test environments, to solve the traditional method of measuring quantum yield, in the detection of excitation light spectrum and excitation light transmission spectrum There is a difference in the measurement state at the time, which causes a certain error in the quantum yield of the measurement.
附图说明BRIEF DESCRIPTION
为了更清楚地说明本申请实施例中的技术方案,下面将对实施例描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图是本申请的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。In order to more clearly explain the technical solutions in the embodiments of the present application, the following will briefly introduce the drawings used in the description of the embodiments. Obviously, the drawings in the following description are some embodiments of the present application. Those of ordinary skill in the art can obtain other drawings based on these drawings without creative work.
图1为本申请的一个实施例提供的量子产率的测试方法的示意图;FIG. 1 is a schematic diagram of a quantum yield test method provided by an embodiment of this application;
图2为本申请的一个实施例提供的量子产率的测试装置的结构示意图;2 is a schematic structural diagram of a quantum yield testing device provided by an embodiment of the present application;
图3是本申请的另一个实施例提供的量子产率的测试方法的示意图;3 is a schematic diagram of a quantum yield test method provided by another embodiment of the present application;
图4是本申请的另一个实施例提供的量子产率的测试方法的示意图;4 is a schematic diagram of a quantum yield test method provided by another embodiment of the present application;
图5是本申请的另一个实施例提供的量子产率的测试方法的示意图;5 is a schematic diagram of a quantum yield test method provided by another embodiment of the present application;
图6是本申请的另一个实施例提供的量子产率的测试方法的示意图;6 is a schematic diagram of a quantum yield test method provided by another embodiment of the present application;
图7是本申请的一个实施例提供的可旋转角度反射镜装置的结构示意图;7 is a schematic structural diagram of a rotatable angle mirror device provided by an embodiment of the present application;
图8是本申请的一个实施例提供的激发光照射到积分球内壁的示意图;8 is a schematic diagram of the excitation light provided to the inner wall of the integrating sphere provided by an embodiment of the present application;
图9是本申请的一个实施例提供的激发光照射到待测材料表面的示意图;9 is a schematic diagram of the excitation light provided to the surface of the material to be measured provided by an embodiment of the present application;
图10是本申请的一个实施例提供的激发光照射到待测材料表面时的激发光光谱、透射光谱以及光致发光光谱的示意图。10 is a schematic diagram of excitation light spectrum, transmission spectrum and photoluminescence spectrum when the excitation light provided by one embodiment of the present application is irradiated to the surface of the material to be measured.
具体实施方式detailed description
为了使本技术领域的人员更好地理解本申请方案,下面将结合本申请实施例中的附图,对本申请实施例中的技术方案进行清楚地描述,显然,所描述的实施例是本申请一部分的实施例,而不是全部的实施例。基于本申请中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都应当属于本申请保护的范围。In order to enable those skilled in the art to better understand the solutions of the present application, the technical solutions in the embodiments of the present application will be described clearly in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are the present application Some embodiments, not all embodiments. Based on the embodiments in this application, all other embodiments obtained by a person of ordinary skill in the art without creative work shall fall within the scope of protection of this application.
本申请的说明书和权利要求书及上述附图中的术语“包括”以及它们任何变形,意图在于覆盖不排他的包含。例如包含一系列步骤或单元的过程、方法或系统、产品或设备没有限定于已列出的步骤或单元,而是可选地还包括没有列出的步骤或单元,或可选地还包括对于这些过程、方法、产品或设备固有的其它步骤或单元。此外,术语“第一”、“第二”和“第三”等是用于区别不同对象,而非用于描述特定顺序。The term "comprising" and any variations thereof in the description and claims of the present application and the above drawings are intended to cover non-exclusive inclusion. For example, a process, method or system, product, or device that includes a series of steps or units is not limited to the listed steps or units, but optionally includes steps or units that are not listed, or optionally includes Other steps or units inherent to these processes, methods, products, or equipment. In addition, the terms "first", "second", "third", etc. are used to distinguish different objects, not to describe a specific order.
图1为本申请实施例提供的一种量子产率的测试方法的流程示意图,如图1所示,本实施例中的量子产率的测试方法包括:FIG. 1 is a schematic flowchart of a quantum yield test method provided by an embodiment of the present application. As shown in FIG. 1, the quantum yield test method in this embodiment includes:
步骤S10:将待测材料放入积分球内部,并获取激发光的激发光光谱;Step S10: Put the material to be tested inside the integrating sphere, and obtain the excitation light spectrum of the excitation light;
步骤S20:将所述激发光照射在所述待测材料表面,获取所述待测材料的光致发光光谱以及所述激发光的透射光谱;Step S20: irradiate the excitation light on the surface of the material to be measured to obtain a photoluminescence spectrum of the material to be tested and a transmission spectrum of the excitation light;
步骤S30:根据所述激发光光谱、所述光致发光光谱以及所述透射光谱生成所述待测材料的量子产率。Step S30: Generate a quantum yield of the material to be measured according to the excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum.
在本实施例中,用户可以预先将待测材料放入积分球内部,并在生成激发光后将激发光照射到积分球内壁,以检测激发光的激发光光谱,然后调整激发光的入射角度,使得激发光照射在待测材料表面,从而获取待测材料的光致发光光谱以及所述激发光通过待测材料后的透射光谱,在整个测试流程中,无需频繁的将待测材料取出和放入,避免了待测材料在积分球内测试状态的不一致性。In this embodiment, the user can put the material to be tested inside the integrating sphere in advance, and after the excitation light is generated, irradiate the excitation light to the inner wall of the integrating sphere to detect the excitation light spectrum of the excitation light, and then adjust the incident angle of the excitation light , So that the excitation light is irradiated on the surface of the material to be tested, so as to obtain the photoluminescence spectrum of the material to be tested and the transmission spectrum of the excitation light after passing the material to be tested. In the entire test process, there is no need to frequently take out the material to be tested and Put in, to avoid the inconsistency of the test state of the material to be tested in the integrating sphere.
在一个实施例中,待测材料可以放置在样品台上,该样品台预先设置于积分球内。In one embodiment, the material to be tested can be placed on a sample stage, which is preset in the integrating sphere.
在一个实施例中,由于激发光的入射角度有一定的偏转,其未能照射在样品表面,而是照射在积分球底部的白板,激发光在积分球内部发生均匀的漫反射。从而通过积分球的出口发出,因此,通过在积分球的出口设置光学探测模块即可探测从积分球的出口发出的光束的光谱。In one embodiment, due to a certain deflection of the incident angle of the excitation light, it fails to illuminate the sample surface, but illuminates the whiteboard at the bottom of the integrating sphere, and the excitation light undergoes uniform diffuse reflection inside the integrating sphere. Therefore, it is emitted through the exit of the integrating sphere. Therefore, the optical spectrum of the light beam emitted from the exit of the integrating sphere can be detected by providing an optical detection module at the exit of the integrating sphere.
在一个实施例中,所述待测材料可以为发光材料。In one embodiment, the material to be measured may be a luminescent material.
在一个实施例中,图2为本实施例中的一种量子产率的测试方法所采用的量子产率测试装置,本实施例中的量子产率的测试方法还可以包括:In one embodiment, FIG. 2 is a quantum yield testing device used in a quantum yield testing method in this embodiment. The quantum yield testing method in this embodiment may further include:
通过氙灯10辐射光谱能量;Radiation of spectral energy through xenon lamp 10;
采用单色仪20从宽波段的光束中分离出一系列狭窄波段的光束;A monochromator 20 is used to separate a series of narrow-band light beams from a wide-band light beam;
当一束复合光线进入单色仪20的入射狭缝后,由光学准直透镜30汇聚成平行光,从而发出激发光。When a beam of composite light enters the entrance slit of the monochromator 20, the collimating lens 30 converges into parallel light to emit excitation light.
在本实施例中,光学准直透镜30是将单色仪20输出的发散单色光进行收集并准直成一束平行光。In this embodiment, the optical collimating lens 30 collects and collimates the divergent monochromatic light output by the monochromator 20 into a parallel beam.
在一个实施例中,光学准直透镜30通过衍射光栅色散为分开的单个波长。In one embodiment, the optical collimating lens 30 is dispersed by a diffraction grating into separate single wavelengths.
如图2所示,在一个实施例中,可以通过将光学探测模块70与积分球60的出口相连,从而对积分球60出口发出的光束的光谱进行检测。As shown in FIG. 2, in one embodiment, the optical detection module 70 may be connected to the exit of the integrating sphere 60 to detect the spectrum of the light beam emitted from the exit of the integrating sphere 60.
在一个实施例中,图3为本申请实施例提供的另一种量子产率测试方法的实现流程图,如图3所示,在本实施例中,所述获取所述激发光的激发光光谱,包括:In one embodiment, FIG. 3 is a flowchart of another quantum yield test method provided by an embodiment of the present application. As shown in FIG. 3, in this embodiment, the excitation light for acquiring the excitation light Spectrum, including:
S11:将所述激发光通过积分球的入口照射在所述积分球的内壁;S11: irradiate the excitation light on the inner wall of the integrating sphere through the entrance of the integrating sphere;
S12:检测从所述积分球的出口发出的激发光的激发光光谱。S12: Detect the excitation light spectrum of the excitation light emitted from the exit of the integrating sphere.
在本实施例中,激发光通过积分球的入口照射在积分球的内壁,从而检测在积分球的出口发出的激发光的激发光光谱,此时,完成激发光光谱的检测,在需要检测待测材料的光致发光光谱和激发光的透射光谱时,通过调节激发光的入射角度即可,避免了样品的取出和放入。In this embodiment, the excitation light is irradiated to the inner wall of the integrating sphere through the entrance of the integrating sphere, thereby detecting the excitation light spectrum of the excitation light emitted at the exit of the integrating sphere. At this time, the detection of the excitation light spectrum is completed. When measuring the photoluminescence spectrum of the material and the transmission spectrum of the excitation light, it is sufficient to adjust the incident angle of the excitation light to avoid taking out and putting in the sample.
在一个实施例中,如图4所示,将所述激发光照射在所述待测材料表面,获取所述待测材料的光致发光光谱以及所述激发光的透射光谱,包括:In one embodiment, as shown in FIG. 4, irradiating the excitation light on the surface of the material to be measured to obtain the photoluminescence spectrum of the material to be tested and the transmission spectrum of the excitation light include:
S21:调整所述激发光的入射角度,以使所述激发光照射到所述待测材料表面;S21: Adjust the incident angle of the excitation light so that the excitation light irradiates the surface of the material to be measured;
S22:检测从所述积分球的出口发出的所述待测材料的光致发光光谱以及所述激发光的透射光谱。S22: Detect the photoluminescence spectrum of the material to be tested and the transmission spectrum of the excitation light emitted from the exit of the integrating sphere.
在本实施例中,通过调整激发光的入射角度,将激发光照射到待测材料表面,可以避免在获取待测材料的光致发光光谱和激发光的透射光谱时对待测材料进行移动,该移动包括调整待测材料的位置,或者取出待测材料。用户可以直接通过光学探测模块70对积分球60的出口发出的光束进行检测,以获取所述待测材料的光致发光光谱以及所述激发光的透射光谱。In this embodiment, by adjusting the incident angle of the excitation light and irradiating the excitation light to the surface of the material to be measured, it is possible to avoid moving the material to be measured when acquiring the photoluminescence spectrum of the material to be tested and the transmission spectrum of the excitation light. Moving includes adjusting the position of the material to be tested or removing the material to be tested. The user can directly detect the light beam emitted by the exit of the integrating sphere 60 through the optical detection module 70 to obtain the photoluminescence spectrum of the material to be measured and the transmission spectrum of the excitation light.
在一个实施例中,如图5所示,所述调整所述激发光的入射角度,以使所述激发光照射到所述待测材料表面,包括:In one embodiment, as shown in FIG. 5, the adjusting the incident angle of the excitation light so that the excitation light irradiates the surface of the material to be measured includes:
步骤S211:通过可旋转角度反射镜装置接收所述激发光;Step S211: receiving the excitation light through a rotatable angle mirror device;
步骤S212:通过调节所述可旋转角度反射镜装置的角度对所述激发光进入所述积分球的入射角进行调节,以使得所述激发光照射到所述待测材料表面。Step S212: Adjust the angle of incidence of the excitation light into the integrating sphere by adjusting the angle of the rotatable angle mirror device, so that the excitation light irradiates the surface of the material to be measured.
在本实施例中,调整所述激发光的入射角度可以通过调整可旋转角度反射镜装置40角度对激发光入射到积分球60的入射角度进行调节。In this embodiment, the incident angle of the excitation light can be adjusted by adjusting the angle of the rotatable angle mirror device 40 to adjust the incident angle of the excitation light to the integrating sphere 60.
在一个实施例中,如图6所示,在本实施例中,所述通过调节所述可旋转角度反射镜装置的角度对所述激发光进入所述积分球的入射角进行调节,以使得所述激发光照射到所述待测材料表面,包括:In one embodiment, as shown in FIG. 6, in this embodiment, the angle of incidence of the excitation light into the integrating sphere is adjusted by adjusting the angle of the rotatable angle mirror device, so that The irradiation of the excitation light onto the surface of the material to be measured includes:
步骤S2121:对所述可旋转角度反射镜装置的角度进行调节;Step S2121: adjust the angle of the rotatable angle mirror device;
步骤S2122:在所述可旋转角度反射镜装置与所述积分球之间设置聚焦透镜;Step S2122: setting a focusing lens between the rotatable angle mirror device and the integrating sphere;
步骤S2123:调节所述可旋转角度反射镜装置的角度,以使得所述激发光通过聚焦透镜后照射到所述待测材料表面。Step S2123: Adjust the angle of the rotatable angle mirror device so that the excitation light irradiates the surface of the material to be measured after passing through a focusing lens.
在本实施中,通过聚焦透镜50可以将激发光聚焦,从而使得进入积分球60内的激发光可以完全照射到样品表面。In this embodiment, the excitation light can be focused by the focusing lens 50 so that the excitation light entering the integrating sphere 60 can be completely irradiated to the sample surface.
图7为本申请一个实施例提供的一种可旋转角度反射镜装置40的结构示意图,如图7所示,本实施例中的可旋转角度反射镜装置40包括:7 is a schematic structural diagram of a rotatable angle mirror device 40 according to an embodiment of the present application. As shown in FIG. 7, the rotatable angle mirror device 40 in this embodiment includes:
光学反射镜41,用于接收所述激发光,并对所述激发光进行反射;The optical reflector 41 is used to receive the excitation light and reflect the excitation light;
反射镜支杆42,用于固定所述光学反射镜,所述反射镜支杆与所述光学反射镜连接;以及A mirror support rod 42 for fixing the optical mirror, and the mirror support rod is connected with the optical mirror; and
电动旋转台43,用于通过所述反射镜支杆调整所述光学反射镜的角度,所述电动旋转台与所述反射镜支杆连接。The electric rotating table 43 is used to adjust the angle of the optical mirror through the mirror support rod, and the electric rotating table is connected to the mirror support rod.
在本实施例中,电动旋转台43可以顺时针或者逆时针旋转,带动光学反射镜41旋转一定的角度,从而改变激发光入射进入积分球60角度,使激发光偏离待测材料或者照射在待测材料表面。In this embodiment, the electric rotating table 43 can rotate clockwise or counterclockwise, driving the optical mirror 41 to rotate a certain angle, thereby changing the angle of excitation light incident into the integrating sphere 60, so that the excitation light deviates from the material to be measured or irradiates Measure the surface of the material.
图8为本申请的一个实施例提供的激发光照射在积分球内壁的示意图,如图8所示,电动旋转台43顺时针旋转一定角度,激发光进入积分球3,由于激 发光的入射角度有一定的偏转,其未能照射在样品表面,而是照射在积分球底部的白板,激发光在积分球内部发生均匀的漫反射,进入积分球60内部的激发光从积分球60的出口发出后通过光学探测模块7测出光束的光谱。虽然定义此处的旋转方向为顺时针,但是旋转方向根据实际光路布局有关,不限制顺时针方向。FIG. 8 is a schematic diagram of the excitation light irradiating the inner wall of the integrating sphere provided by an embodiment of the present application. As shown in FIG. There is a certain deflection, which fails to illuminate the surface of the sample, but illuminates the whiteboard at the bottom of the integrating sphere. The excitation light uniformly diffuses inside the integrating sphere, and the excitation light entering the integrating sphere 60 is emitted from the exit of the integrating sphere 60. Then the optical detection module 7 measures the spectrum of the light beam. Although the rotation direction here is defined as clockwise, the rotation direction is related to the actual optical path layout, and the clockwise direction is not limited.
图9为本申请的一个实施例提供的激发光照射在待测材料表面的示意图,如图9所示,电动旋转台43逆时针旋转一定角度,激发光通过聚焦透镜50,进入积分球60。由于激发光的入射角度有一定的偏转,其恰能照射在待测样品表面,激发待测样品产生光致发光光谱。使用光学探测模块70,测出光致发光光谱、激发光的透射光谱。虽然定义此处的旋转方向为逆时针,但是旋转方向根据实际光路布局有关,旋转方向与图3所述的旋转方向相反即可。9 is a schematic diagram of the excitation light irradiating the surface of the material to be measured provided by an embodiment of the present application. As shown in FIG. 9, the electric rotating table 43 rotates counterclockwise by a certain angle, and the excitation light passes through the focusing lens 50 and enters the integrating sphere 60. Because the incident angle of the excitation light is deflected, it can be irradiated on the surface of the sample to be tested, and the sample to be tested can be excited to produce a photoluminescence spectrum. Using the optical detection module 70, the photoluminescence spectrum and the transmission spectrum of the excitation light are measured. Although the rotation direction here is defined as counterclockwise, the rotation direction depends on the actual optical path layout, and the rotation direction may be opposite to the rotation direction described in FIG. 3.
图10为本申请的一个实施例提供的一种待测材料的光致发光光谱、激发光光谱以及激发光的透射光谱的光谱示意图,如图10所示,该光谱示意图的横轴为波长,光谱示意图中的纵轴为光谱绝对能量分布,激发光偏离待测样品时,激发光没有被待测样品吸收,探测得到的激发光强度很大。激发光照射在待测样品时,激发光能量被待测样品吸收,待测样品产生光致发光光谱。激发光能量被吸收之后,变为激发光透射光光谱,其波长仍与激发光保持一致。10 is a schematic diagram of a photoluminescence spectrum, excitation light spectrum, and transmission spectrum of excitation light of a material to be tested provided by an embodiment of the present application. As shown in FIG. 10, the horizontal axis of the spectrum diagram is the wavelength. The vertical axis in the spectrum diagram is the absolute energy distribution of the spectrum. When the excitation light deviates from the sample to be measured, the excitation light is not absorbed by the sample to be measured, and the intensity of the excitation light obtained by detection is large. When the excitation light is irradiated on the sample to be tested, the excitation light energy is absorbed by the sample to be tested, and the sample to be tested generates a photoluminescence spectrum. After the excitation light energy is absorbed, it becomes the transmission light spectrum of the excitation light, and its wavelength is still consistent with the excitation light.
在一个实施例中,所述根据所述激发光光谱、所述光致发光光谱以及所述透射光谱生成所述待测材料的量子产率,包括:In one embodiment, the generating the quantum yield of the material to be tested according to the excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum includes:
按照预设波长范围分别从所述激发光光谱中获取预设激发光光谱波段、从所述光致发光光谱中获取预设光致发光光谱波段以及从所述透射光谱中获取预设透射光谱波段;Obtaining a preset excitation light spectrum band from the excitation light spectrum, a preset photoluminescence spectrum band from the photoluminescence spectrum, and a preset transmission spectrum band from the transmission spectrum according to a preset wavelength range ;
将所述预设激发光光谱波段与波长横轴之间的面积设为所述激发光光谱的光子数,将所述预设光致发光光谱波段与所述波长横轴之间的面积设为所述光致发光光谱的光子数,将所述预设透射光谱波段与所述波长横轴之间的面积设为所述透射光谱的光子数。The area between the preset excitation light spectrum band and the horizontal axis of wavelength is set as the number of photons in the excitation light spectrum, and the area between the preset photoluminescence spectrum band and the horizontal axis of wavelength is For the photon number of the photoluminescence spectrum, the area between the preset transmission spectrum band and the horizontal axis of the wavelength is taken as the photon number of the transmission spectrum.
在本实施例中,该预设波长范围包括第一波长和第二波长,其中,第二波长大于第一波长,具体的,第二波长可以为预设波长范围的上限,第一波长可以为预设波长范围的下限。In this embodiment, the preset wavelength range includes a first wavelength and a second wavelength, where the second wavelength is greater than the first wavelength. Specifically, the second wavelength may be the upper limit of the preset wavelength range, and the first wavelength may be The lower limit of the preset wavelength range.
在一个实施例中,通过选取图10中的中的预设波长范围,然后截取对应的光谱,计算各个光谱与横轴之间的面积,该面积即可以为各个光谱对应的光子数。例如,若预设波长范围为400nm-600nm,此时,第一波长为400nm,第二波长为600nm,计算各个光谱在400nm-600nm的面积,即可得到各个光谱对应的光子数。In one embodiment, by selecting the preset wavelength range in FIG. 10 and then intercepting the corresponding spectrum, the area between each spectrum and the horizontal axis is calculated, and the area can be the number of photons corresponding to each spectrum. For example, if the preset wavelength range is 400nm-600nm, at this time, the first wavelength is 400nm and the second wavelength is 600nm, the area of each spectrum in the range of 400nm-600nm can be calculated to obtain the number of photons corresponding to each spectrum.
在一个实施例中,各个光谱与横轴之间的面积可以通过对各个光谱的光谱绝对能量进行积分得到。In one embodiment, the area between each spectrum and the horizontal axis can be obtained by integrating the spectral absolute energy of each spectrum.
在一个实施例中,所述根据所述激发光光谱、所述光致发光光谱以及所述透射光谱生成所述待测材料的量子产率,还包括:In one embodiment, the generating the quantum yield of the material to be tested according to the excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum, further includes:
将所述激发光光谱、所述光致发光光谱以及所述透射光谱通过预设量子产率关系式生成量子产率,所述预设量子产率关系式为:The excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum are generated by a preset quantum yield relationship, and the preset quantum yield relationship is:
η=Ne/Na;η=Ne/Na;
其中,η为所述待测材料的量子产率,Ne为所述光致发光光谱的光子数,Na为所述激发光光谱的光子数与所述透射光谱的光子数的差值。Where η is the quantum yield of the material to be measured, Ne is the number of photons in the photoluminescence spectrum, and Na is the difference between the number of photons in the excitation light spectrum and the number of photons in the transmission spectrum.
在一个实施例中,所述将所述预设激发光光谱波段与波长横轴之间的面积设为所述激发光光谱的光子数,包括:In one embodiment, the setting of the area between the preset excitation light spectrum band and the horizontal axis of wavelength as the number of photons in the excitation light spectrum includes:
通过所述激发光光谱获取所述激发光光谱的能量值;Obtaining the energy value of the excitation light spectrum through the excitation light spectrum;
将所述激发光光谱的能量值通过预设的所述激发光光谱的光子数关系式计算所述激发光光谱的光子数,所述预设的所述激发光光谱的光子数关系式为:The energy value of the excitation light spectrum is calculated by the preset photon number relationship of the excitation light spectrum, and the preset photon number relationship of the excitation light spectrum is:
Ea1=h*c/λ;Ea1=h*c/λ;
△N=P(λ)*△λ/Ea1;△N=P(λ)*△λ/Ea1;
Figure PCTCN2019128494-appb-000003
Figure PCTCN2019128494-appb-000003
其中,Ea1为所述激发光光谱的能量值,h为普朗克常量,c为光速,λ1 为所述预设波长范围中的第一波长,λ2为所述预设波长范围中的第二波长,P(λ)为绝对功率,Na1为所述激发光光谱的光子数。Where Ea1 is the energy value of the excitation light spectrum, h is the Planck constant, c is the speed of light, λ1 is the first wavelength in the preset wavelength range, and λ2 is the second in the preset wavelength range The wavelength, P(λ) is the absolute power, and Na1 is the number of photons in the excitation light spectrum.
在一个实施例中,各个光谱与横轴之间的面积可以通过对各个光谱的光谱绝对能量进行积分得到。In one embodiment, the area between each spectrum and the horizontal axis can be obtained by integrating the spectral absolute energy of each spectrum.
在一个实施例中,所述将所述预设透射光谱波段与波长横轴之间的面积设为所述激发光光谱的光子数,包括:In one embodiment, the setting of the area between the preset transmission spectrum band and the horizontal axis of wavelength as the number of photons in the excitation light spectrum includes:
通过所述透射光谱获取所述透射光谱的能量值;Acquiring the energy value of the transmission spectrum through the transmission spectrum;
将所述透射光谱的能量值通过预设的所述透射光谱的光子数关系式计算所述透射光谱的光子数,所述预设的所述透射光谱的光子数关系式为:The energy value of the transmission spectrum is calculated by the preset photon number relationship of the transmission spectrum, and the preset photon number relationship of the transmission spectrum is:
Ea2=h*c/λ;Ea2=h*c/λ;
△N=P(λ)*△λ/Ea2;△N=P(λ)*△λ/Ea2;
Figure PCTCN2019128494-appb-000004
Figure PCTCN2019128494-appb-000004
其中,Ea2为所述透射光谱的能量值,h为普朗克常量,c为光速,λ1为所述预设波长范围中的第一波长,λ2为所述预设波长范围中的第二波长,P(λ)为绝对功率,Na2为所述透射光谱的光子数。Where Ea2 is the energy value of the transmission spectrum, h is the Planck constant, c is the speed of light, λ1 is the first wavelength in the preset wavelength range, and λ2 is the second wavelength in the preset wavelength range , P(λ) is the absolute power, and Na2 is the number of photons in the transmission spectrum.
在一个实施例中,Na为所述激发光光谱的光子数与所述透射光谱的光子数的差值,即Na=Na1-Na2。In one embodiment, Na is the difference between the number of photons in the excitation light spectrum and the number of photons in the transmission spectrum, that is, Na=Na1-Na2.
在一个实施例中,所述将所述预设光致发光光谱波段与所述波长横轴之间的面积设为所述光致发光光谱的光子数,包括:In one embodiment, the setting of the area between the preset photoluminescence spectrum band and the horizontal axis as the number of photons in the photoluminescence spectrum includes:
通过所述光致发光光谱获取所述光致发光光谱的能量值;Obtaining the energy value of the photoluminescence spectrum through the photoluminescence spectrum;
将所述光致发光光谱的能量值通过预设的光致发光光谱的光子数关系式计算所述光致发光光谱的光子数,所述预设的光致发光光谱的光子数关系式为:The energy value of the photoluminescence spectrum is calculated by a preset photon number relationship of photoluminescence spectrum, and the photon number relationship of the preset photoluminescence spectrum is:
Ee=h*c/λ;Ee=h*c/λ;
△N=P(λ)*△λ/Ee;△N=P(λ)*△λ/Ee;
Figure PCTCN2019128494-appb-000005
Figure PCTCN2019128494-appb-000005
其中,Ee为所述光致发光光谱的能量值,h为普朗克常量,c为光速,λ1为所述预设波长范围中的第一波长,λ2为所述预设波长范围中的第二波长,P(λ)为绝对功率,Ne为所述光致发光光谱的光子数。Where Ee is the energy value of the photoluminescence spectrum, h is the Planck constant, c is the speed of light, λ1 is the first wavelength in the preset wavelength range, and λ2 is the first in the preset wavelength range At two wavelengths, P(λ) is the absolute power, and Ne is the number of photons in the photoluminescence spectrum.
本申请实施例提供了一种量子产率的测试方法,通过将待测材料放入积分球内部,先获取激发光的激发光光谱,然后将激发光照射在待测材料上,获取待测材料的光致发光光谱以及激发光的透射光谱,并根据激发光光谱、光致发光光谱以及透射光谱生成待测材料的量子产率,从而使得在探测激发光光谱、光致发光光谱以及透射光谱时无需取出待测材料,保证了测试数据均在同一环境下取得,避免了因为测试环境不同而产生的误差,解决了传统测定量子产率的方法中,在探测激发光的光谱和激发光透射光谱时的测量状态存在差异,导致测定的量子产率出现一定的误差的问题。The embodiments of the present application provide a method for measuring quantum yield. By placing the material to be tested inside the integrating sphere, the excitation light spectrum of the excitation light is obtained first, and then the excitation light is irradiated on the material to be tested to obtain the material to be tested The photoluminescence spectrum and the transmission spectrum of the excitation light, and the quantum yield of the material to be tested is generated according to the excitation light spectrum, the photoluminescence spectrum and the transmission spectrum, so that when the excitation light spectrum, the photoluminescence spectrum and the transmission spectrum are detected No need to take out the material to be tested, to ensure that the test data are obtained in the same environment, to avoid errors caused by different test environments, to solve the traditional method of measuring quantum yield, in the detection of excitation light spectrum and excitation light transmission spectrum There is a difference in the measurement state at the time, which causes a certain error in the quantum yield of the measurement.
以上所述仅为本申请的可选实施例而已,并不用以限制本申请,凡在本申请的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本申请的保护范围之内。The above are only optional embodiments of this application and are not intended to limit this application. Any modification, equivalent replacement and improvement made within the spirit and principle of this application should be included in the protection of this application Within range.

Claims (10)

  1. 一种量子产率的测试方法,其特征在于,所述测试方法包括:A quantum yield test method, characterized in that the test method includes:
    将待测材料放入积分球内部,并获取激发光的激发光光谱;Put the material to be tested inside the integrating sphere and obtain the excitation light spectrum of the excitation light;
    将所述激发光照射在所述待测材料表面,获取所述待测材料的光致发光光谱以及所述激发光的透射光谱;Irradiating the excitation light on the surface of the material to be measured to obtain a photoluminescence spectrum of the material to be tested and a transmission spectrum of the excitation light;
    根据所述激发光光谱、所述光致发光光谱以及所述透射光谱生成所述待测材料的量子产率。The quantum yield of the material to be measured is generated according to the excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum.
  2. 如权利要求1所述的测试方法,其特征在于,所述获取所述激发光的激发光光谱,包括:The test method according to claim 1, wherein the acquiring the excitation light spectrum of the excitation light comprises:
    将所述激发光通过积分球的入口照射在所述积分球的内壁;Irradiating the excitation light on the inner wall of the integrating sphere through the entrance of the integrating sphere;
    检测从所述积分球的出口发出的激发光的激发光光谱。The excitation light spectrum of the excitation light emitted from the exit of the integrating sphere is detected.
  3. 如权利要求1所述的测试方法,其特征在于,将所述激发光照射在所述待测材料表面,获取所述待测材料的光致发光光谱以及所述激发光的透射光谱,包括:The test method according to claim 1, wherein irradiating the excitation light on the surface of the material to be measured to obtain the photoluminescence spectrum of the material to be tested and the transmission spectrum of the excitation light include:
    调整所述激发光的入射角度,以使所述激发光照射到所述待测材料表面;Adjusting the incident angle of the excitation light so that the excitation light irradiates the surface of the material to be measured;
    检测从所述积分球的出口发出的所述待测材料的光致发光光谱以及所述激发光的透射光谱。Detecting the photoluminescence spectrum of the material to be tested and the transmission spectrum of the excitation light emitted from the exit of the integrating sphere.
  4. 如权利要求3所述的测试方法,其特征在于,所述调整所述激发光的入射角度,以使所述激发光照射到所述待测材料表面,包括:The test method according to claim 3, wherein the adjusting the incident angle of the excitation light so that the excitation light irradiates the surface of the material to be measured includes:
    通过可旋转角度反射镜装置接收所述激发光;Receiving the excitation light through a rotatable angle mirror device;
    通过调节所述可旋转角度反射镜装置的角度对所述激发光进入所述积分球的入射角进行调节,以使得所述激发光照射到所述待测材料表面。The angle of incidence of the excitation light into the integrating sphere is adjusted by adjusting the angle of the rotatable angle mirror device, so that the excitation light irradiates the surface of the material to be measured.
  5. 如权利要求4所述的测试方法,其特征在于,所述通过调节所述可旋转角度反射镜装置的角度对所述激发光进入所述积分球的入射角进行调节,以使得所述激发光照射到所述待测材料表面,包括:The test method according to claim 4, wherein the angle of incidence of the excitation light into the integrating sphere is adjusted by adjusting the angle of the rotatable angle mirror device so that the excitation light Irradiation to the surface of the material to be measured includes:
    对所述可旋转角度反射镜装置的角度进行调节;Adjust the angle of the rotatable angle mirror device;
    在所述可旋转角度反射镜装置与所述积分球之间设置聚焦透镜;A focusing lens is provided between the rotatable angle mirror device and the integrating sphere;
    调节所述可旋转角度反射镜装置的角度,以使得所述激发光通过聚焦透镜后照射到所述待测材料表面。The angle of the rotatable angle mirror device is adjusted so that the excitation light irradiates the surface of the material to be measured after passing through a focusing lens.
  6. 如权利要求4所述的测试方法,其特征在于,所述可旋转角度反射镜装置,包括:The test method according to claim 4, wherein the rotatable angle mirror device includes:
    光学反射镜,用于接收所述激发光,并对所述激发光进行反射;An optical mirror is used to receive the excitation light and reflect the excitation light;
    反射镜支杆,用于固定所述光学反射镜,所述反射镜支杆与所述光学反射镜连接;以及A mirror support rod for fixing the optical mirror, and the mirror support rod is connected to the optical mirror; and
    电动旋转台,用于通过所述反射镜支杆调整所述光学反射镜的角度,所述电动旋转台与所述反射镜支杆连接。An electric rotating table is used to adjust the angle of the optical mirror through the mirror support rod, and the electric rotating table is connected with the mirror support rod.
  7. 如权利要求1所述的测试方法,其特征在于,所述根据所述激发光光谱、所述光致发光光谱以及所述透射光谱生成所述待测材料的量子产率,包括:The test method according to claim 1, wherein the generating the quantum yield of the material to be tested according to the excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum includes:
    按照预设波长范围从所述激发光光谱中获取预设激发光光谱波段、从所述光致发光光谱中获取预设光致发光光谱波段以及从所述透射光谱中获取预设透射光谱波段;Obtaining a preset excitation light spectrum band from the excitation light spectrum according to a preset wavelength range, a preset photoluminescence spectrum band from the photoluminescence spectrum, and a preset transmission spectrum band from the transmission spectrum;
    将所述预设激发光光谱波段与波长横轴之间的面积设为所述激发光光谱的光子数,将所述预设光致发光光谱波段与所述波长横轴之间的面积设为所述光致发光光谱的光子数,将所述预设透射光谱波段与所述波长横轴之间的面积设为所述透射光谱的光子数。The area between the preset excitation light spectrum band and the horizontal axis of wavelength is set as the number of photons in the excitation light spectrum, and the area between the preset photoluminescence spectrum band and the horizontal axis of wavelength is For the photon number of the photoluminescence spectrum, the area between the preset transmission spectrum band and the horizontal axis of the wavelength is taken as the photon number of the transmission spectrum.
  8. 如权利要求7所述的测试方法,其特征在于,所述根据所述激发光光谱、所述光致发光光谱以及所述透射光谱生成所述待测材料的量子产率,还包括:The test method according to claim 7, wherein the generating the quantum yield of the material to be tested according to the excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum further comprises:
    将所述激发光光谱、所述光致发光光谱以及所述透射光谱通过预设量子产率关系式生成量子产率,所述预设量子产率关系式为:The excitation light spectrum, the photoluminescence spectrum, and the transmission spectrum are generated by a preset quantum yield relationship, and the preset quantum yield relationship is:
    η=Ne/Na;η=Ne/Na;
    其中,η为所述待测材料的量子产率,Ne为所述光致发光光谱的光子数, Na为所述激发光光谱的光子数与所述透射光谱的光子数的差值。Where η is the quantum yield of the material to be measured, Ne is the number of photons in the photoluminescence spectrum, and Na is the difference between the number of photons in the excitation light spectrum and the number of photons in the transmission spectrum.
  9. 如权利要求7所述的测试方法,其特征在于,所述将所述预设激发光光谱波段与波长横轴之间的面积设为所述激发光光谱的光子数,包括:The test method according to claim 7, wherein the area between the preset excitation light spectrum band and the horizontal axis of wavelength is set as the number of photons in the excitation light spectrum, including:
    通过所述激发光光谱获取所述激发光光谱的能量值;Obtaining the energy value of the excitation light spectrum through the excitation light spectrum;
    将所述激发光光谱的能量值通过预设的所述激发光光谱的光子数关系式计算所述激发光光谱的光子数,所述预设的所述激发光光谱的光子数关系式为:The energy value of the excitation light spectrum is calculated by the preset photon number relationship of the excitation light spectrum, and the preset photon number relationship of the excitation light spectrum is:
    Ea1=h*c/λ;Ea1=h*c/λ;
    △N=P(λ)*△λ/Ea1;△N=P(λ)*△λ/Ea1;
    Figure PCTCN2019128494-appb-100001
    Figure PCTCN2019128494-appb-100001
    其中,Ea1为所述激发光光谱的能量值,h为普朗克常量,c为光速,λ1为所述预设波长范围中的第一波长,λ2为所述预设波长范围中的第二波长,P(λ)为绝对功率。Where Ea1 is the energy value of the excitation light spectrum, h is the Planck constant, c is the speed of light, λ1 is the first wavelength in the preset wavelength range, and λ2 is the second in the preset wavelength range Wavelength, P(λ) is absolute power.
  10. 如权利要求7所述的测试方法,其特征在于,所述将所述预设光致发光光谱波段与所述波长横轴之间的面积设为所述光致发光光谱的光子数,包括:The test method according to claim 7, wherein the area between the preset photoluminescence spectrum band and the horizontal axis of wavelength is set as the number of photons in the photoluminescence spectrum, including:
    通过所述光致发光光谱获取所述光致发光光谱的能量值;Obtaining the energy value of the photoluminescence spectrum through the photoluminescence spectrum;
    将所述光致发光光谱的能量值通过预设的光致发光光谱的光子数关系式计算所述光致发光光谱的光子数,所述预设的光致发光光谱的光子数关系式为:The energy value of the photoluminescence spectrum is calculated by a preset photon number relationship of photoluminescence spectrum, and the photon number relationship of the preset photoluminescence spectrum is:
    Ee=h*c/λ;Ee=h*c/λ;
    △N=P(λ)*△λ/Ee;△N=P(λ)*△λ/Ee;
    Figure PCTCN2019128494-appb-100002
    Figure PCTCN2019128494-appb-100002
    其中,Ee为所述光致发光光谱的能量值,h为普朗克常量,c为光速,λ1为所述预设波长范围中的第一波长,λ2为所述预设波长范围中的第二波长,P(λ)为绝对功率,Ne为所述光致发光光谱的光子数。Where Ee is the energy value of the photoluminescence spectrum, h is the Planck constant, c is the speed of light, λ1 is the first wavelength in the preset wavelength range, and λ2 is the first in the preset wavelength range At two wavelengths, P(λ) is the absolute power, and Ne is the number of photons in the photoluminescence spectrum.
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