WO2020135540A1 - Procédé de mesure de rendement quantique - Google Patents

Procédé de mesure de rendement quantique 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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excitation light
spectrum
preset
photoluminescence
quantum yield
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PCT/CN2019/128494
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English (en)
Chinese (zh)
Inventor
薛占强
郭翠
潘奕
Original Assignee
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/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/255—Details, e.g. use of specially adapted sources, lighting or optical systems
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00—Features of devices classified in G01N21/00
    • G01N2201/06—Illumination; Optics
    • G01N2201/063—Illuminating optical parts
    • G01N2201/0636—Reflectors

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.

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Abstract

L'invention concerne un procédé de mesure de rendement quantique. Le procédé comprend les étapes consistant à : après avoir disposé un matériau à analyser à l'intérieur d'une sphère d'intégration (60), acquérir d'abord un spectre d'excitation de lumière d'excitation (S10) ; puis émettre une lumière d'excitation en direction du matériau à analyser, acquérir un spectre de photoluminescence et un spectre transmis par le matériau à analyser de la lumière d'excitation (S20) ; selon le spectre d'excitation, le spectre de photoluminescence et le spectre transmis, générer le rendement quantique du matériau à analyser (S30). Ainsi, il n'est pas nécessaire de retirer le matériau à analyser lors du sondage d'un spectre d'excitation, d'un spectre de photoluminescence et d'un spectre transmis, ce qui garantit que les données de mesure sont toutes obtenues dans un environnement identique, ce qui évite les erreurs provoquées par différents environnements de mesure et résout le problème rencontré dans les procédés classiques de mesure du rendement quantique, à savoir des différences dans les conditions de mesure lors du sondage d'un spectre d'excitation et d'un spectre transmis de la lumière d'excitation conduisant à certaines erreurs dans la mesure du rendement quantique.
PCT/CN2019/128494 2018-12-26 2019-12-26 Procédé de mesure de rendement quantique WO2020135540A1 (fr)

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CN118348578A (zh) * 2024-06-17 2024-07-16 中国工程物理研究院激光聚变研究中心 一种x射线图像信息的增强型读取装置和方法

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CN111982864B (zh) * 2019-05-24 2021-08-24 南京工业大学 一种激发光强相关的绝对光致发光量子效率测量方法
CN112577958B (zh) * 2019-09-29 2023-06-27 成都辰显光电有限公司 量子点检测装置和方法

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CN209400422U (zh) * 2018-12-26 2019-09-17 深圳市太赫兹科技创新研究院有限公司 一种量子产率的测试装置

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CN116256322A (zh) * 2023-02-28 2023-06-13 江苏第三代半导体研究院有限公司 一种微型发光器件的量子效率测试方法及测试系统
CN118348578A (zh) * 2024-06-17 2024-07-16 中国工程物理研究院激光聚变研究中心 一种x射线图像信息的增强型读取装置和方法

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