CN108007906B - Long afterglow material phosphorescence excitation spectrum measurement system and method - Google Patents
Long afterglow material phosphorescence excitation spectrum measurement system and method Download PDFInfo
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- CN108007906B CN108007906B CN201711242248.9A CN201711242248A CN108007906B CN 108007906 B CN108007906 B CN 108007906B CN 201711242248 A CN201711242248 A CN 201711242248A CN 108007906 B CN108007906 B CN 108007906B
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
Abstract
The invention provides a long afterglow material phosphorescence excitation spectrum measuring system and a method, wherein the system comprises an excitation light source 1, a first condensing element 2, an electric optical shutter 3, a grating light splitting monochromator 4, a second condensing element 5, an optical long wave pass filter 6, a sample holder 7, a third condensing element 8, an optical band pass filter 9, a photoelectric detector 10, an electric signal amplifier 11, a data acquisition and storage unit 12, a system control unit 13 and a data analysis processing and storage unit 14. Parameters such as irradiation time, excitation wavelength, light intensity acquisition interval and the like are set in the system through a control unit; in the method, phosphorescence attenuation curves under different excitation wavelengths are measured, and then change curves of phosphorescence intensity along with the excitation wavelengths at different attenuation moments, namely phosphorescence excitation spectrum curves, are obtained. Compared with fluorescence excitation spectrum, the long afterglow material phosphorescence excitation spectrum measurement system and method provided by the invention can provide more information, and are beneficial to the research of long afterglow material luminescence mechanism.
Description
Technical Field
The invention relates to the technical field of spectral measurement, in particular to a long afterglow material phosphorescence excitation spectral measurement system and a method.
Background
The long-afterglow luminescent materials have two luminescent conditions. One is light emitted by a material while being irradiated with excitation light, which is called fluorescence; the other is the light emitted by the material after the excitation light ceases to illuminate, which is called phosphorescence. At present, the fluorescence spectrum and phosphorescence spectrum analysis technology of the long afterglow material mainly has the following forms: 1) when or after the exciting light with single wavelength or continuous wavelength irradiates the sample, a CCD spectrometer with a light splitting grating is adopted to measure the fluorescence spectrum or phosphorescence spectrum of the fluorescent powder, and the phosphorescence attenuation curve in a certain bandwidth near a certain emission wavelength can be measured; 2) after the excitation light with single wavelength or continuous wavelength is irradiated, selecting a certain emission light wavelength range by adopting the combination of a photodiode and an optical filter, and measuring the phosphorescence attenuation curve of the sample; 3) the method comprises the steps of splitting emergent light of an excitation light source by a grating splitting monochromator, changing the wavelength of the emergent light by changing the corner of a grating, irradiating a sample with the split emergent light, selecting fluorescence emitted from the sample by a band-pass optical filter or a monochromator within a certain wavelength range for detection, and measuring the curve of the intensity of the fluorescence changing along with the wavelength of the excitation light, namely an excitation spectrum. These spectroscopic analysis techniques have been used to reveal the luminescent properties and the luminescent mechanism of phosphors.
It is known that, when the excitation wavelength is different, the energy level positions of the generated photogenerated carriers in the phosphor may be different, and the paths of the generated carriers reaching the luminescent center and the defect are different at different energy level positions, and the concentration is shown on the decay curve of phosphorescence and the corresponding excitation spectrum. It is emphasized that here we divide the excitation spectrum of long afterglow materials into two categories: one is fluorescence excitation spectrum, and the other is phosphorescence excitation spectrum. The measurement of fluorescence excitation spectrum is to detect the change rule curve of fluorescence intensity along with the wavelength of excitation light while the excitation light irradiates the material. The phosphorescence excitation spectrum is measured by detecting the change rule curve of phosphorescence intensity with excitation light wavelength at a certain attenuation moment after the excitation light with different wavelengths irradiates the material. So far, no report has been made on a detection system and method of phosphorescence excitation spectrum.
Disclosure of Invention
In order to solve the above problems, the present invention provides a long afterglow material phosphorescence excitation spectrum measurement system and method, which can be used to measure the phosphorescence attenuation curve of the long afterglow material under different excitation wavelengths and the change rule curve of phosphorescence intensity with excitation wavelength at a certain phosphorescence attenuation time.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a long afterglow material phosphorescence excitation spectrum measuring system comprises an excitation light source, a first light gathering element, an electric light shutter, a grating light splitting monochromator, a second light gathering element, an optical long wave pass filter, a sample holder, a third light gathering element, an optical band pass filter, a photoelectric detector, an electric signal amplifier, a data acquisition and storage unit, a system control unit and a data analysis processing and storage unit;
the light beam emitted from the excitation light source sequentially passes through the first light-gathering element, the electric optical shutter, the grating light-splitting monochromator, the second light-gathering element and the optical long-wave pass filter and then irradiates into the long afterglow material on the sample holder, the light emitted from the long afterglow material passes through the third light focusing element and the optical band pass filter in sequence and is received by the photoelectric detector and converted into an electric signal, the electric signal is amplified by the electric signal amplifier and then is subjected to data acquisition and storage by the data acquisition and storage unit, the system control unit is used for setting and controlling the parameters of the electric optical shutter, the grating light splitting monochromator and the data acquisition and storage unit, the data analysis processing and storage unit is used for processing and storing the spectrogram of the data obtained by the data acquisition and storage unit.
Further, the band-pass wavelength range of the optical band-pass filter is within the fluorescence emission spectrum range of the analyzed long afterglow material.
Furthermore, the grating light splitting monochromator is provided with an emergent light slit and an incident light slit, the grating light splitting monochromator can split incident light with continuous wavelength into monochromatic light, and the grating light splitting monochromator can be a C-T type light splitting monochromator or a Letello type monochromator;
furthermore, the grating light splitting monochromator comprises a light splitting grating, the rotation angle of the light splitting grating is driven and adjusted through a motor, the motor is connected with the control unit, and the light splitting wavelength range of the grating light splitting monochromator is within the emission spectrum wavelength range of the excitation light source.
Furthermore, the optical long-wave pass filter is used for filtering the high-order diffracted light emitted from the exit slit of the grating light splitting monochromator.
Further, the method for measuring the phosphorescence excitation spectrum of the long afterglow material comprises the following steps:
1) setting an excitation wavelength range, a wavelength scanning interval, an irradiation time, a total phosphorescence measurement time and a time interval;
2) setting the light splitting wavelength of the grating light splitting monochromator, splitting the emergent light of the excitation light source by using the grating light splitting monochromator, and selecting the optical long-wave pass filter to remove the high-order diffraction light of the emergent light of the grating light splitting monochromator;
3) controlling the electric light shutter to be opened, enabling emergent light of the excitation light source to irradiate the long-afterglow material on the sample holder after being monochromatized, controlling the electric light shutter to be closed and starting to collect a phosphorescence attenuation curve after the irradiation within a set time, and collecting and storing phosphorescence intensity data once every other time interval until the measurement time reaches the total phosphorescence measurement time;
4) adjusting the position of a light splitting grating of the grating light splitting monochromator to change the light splitting wavelength until the light splitting wavelength of the grating light splitting monochromator reaches the set termination wavelength, repeating the step 3), and measuring phosphorescence attenuation curve data under different excitation wavelengths respectively;
5) extracting a phosphorescence intensity variation curve along with the excitation wavelength at a certain attenuation moment from the phosphorescence attenuation curve data under different excitation wavelengths obtained in the step 4), and drawing a phosphorescence excitation spectrum curve.
Furthermore, the optical long-wave pass filter adopts a mode of switching a plurality of optical long-wave pass filters according to the light splitting wavelength of the grating light splitting monochromator so as to ensure the monochromaticity of emergent light.
The invention has the advantages that the control unit can set the starting time, the irradiation time, the starting time and the ending time of data acquisition and the sampling time interval of exciting light, can control the grating position of the grating light splitting monochromator, namely the light splitting wavelength, can complete the measurement of the phosphorescence light attenuation curves under different exciting wavelengths according to the set program, and reduces the experimental measurement error; meanwhile, the system and the method can measure the change rule curve of the phosphorescence intensity of the long-afterglow material along with the excitation wavelength at a phosphorescence attenuation moment to be the phosphorescence excitation spectrum, and the phosphorescence excitation spectrum contains richer spectral information than the common fluorescence excitation spectrum, thereby being beneficial to the research of the luminescence mechanism of the long-afterglow material.
Drawings
FIG. 1 is a schematic structural diagram of a long afterglow material phosphorescence excitation spectrum measurement system of the present invention.
FIG. 2 is a flow chart of the method for measuring phosphorescence excitation spectrum of the long afterglow material.
Fig. 3 is a phosphorescence attenuation curve of the long persistence material according to an embodiment of the present invention.
FIG. 4 shows the phosphorescence excitation spectrum of the long afterglow material according to the embodiment of the present invention.
In the figure, 1-excitation light source, 2-first light-gathering element, 3-electric light shutter, 4-grating light splitting monochromator, 5-second light-gathering element, 6-optical long wave pass filter, 7-sample holder, 8-third light-gathering element, 9-optical band pass filter, 10-photoelectric detector, 11-electric signal amplifier, 12-data acquisition and storage unit, 13-system control unit, 14-data analysis processing and storage unit.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When a component is referred to as being "connected" to another component, it can be directly connected to the other component or intervening components may also be present. When a component is referred to as being "disposed on" another component, it can be directly on the other component or intervening components may also be present. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1 and fig. 2, a long afterglow material phosphorescence excitation spectrum measurement system includes: the device comprises an excitation light source 1, a first light-gathering element 2, an electric optical shutter 3, a grating light-splitting monochromator 4, a second light-gathering element 5, an optical long-wave pass filter 6, a sample holder 7, a third light-gathering element 8, an optical band-pass filter 9, a photoelectric detector 10, an electric signal amplifier 11, a data acquisition and storage unit 12, a system control unit 13 and a data analysis processing and storage unit 14.
Light beams emitted from an excitation light source 1 sequentially pass through a first light-condensing element 2, an electric light shutter 3, a grating light-splitting monochromator 4, a second light-condensing element 5 and an optical long-wave pass filter 6 and then irradiate into a long-afterglow material on a sample holder 7, the light emitted from the long-afterglow material sequentially passes through a third light-condensing element 8 and an optical band-pass filter 9 and then is received by a photoelectric detector 10 and converted into electric signals, the electric signals are amplified by an electric signal amplifier 11 and then are subjected to data acquisition and storage by a data acquisition and storage unit 12, a system control unit 13 is used for setting and controlling parameters of the electric light shutter 3, the grating light-splitting monochromator 4 and the data acquisition and storage unit 12, and a data analysis processing and storage unit 14 is used for performing data processing and storage on spectrograms of data obtained by the data acquisition and storage unit 12.
The excitation light source 1 is a light source with a continuous spectrum, such as a deuterium lamp, a bromine tungsten lamp, a xenon lamp, and the like. After the long afterglow material is irradiated with the short wavelength light emitted from the excitation light source 1, photogenerated carriers are generated in the long afterglow material.
The first condensing element 2 condenses light emitted from the excitation light source 1 on the entrance slit of the grating monochromator 3.
The electro-optical shutter 3 is used to control the time at which the sample is irradiated from the exit light of the excitation light source 1.
The grating light splitting monochromator 4 is provided with an emergent light slit and an incident light slit, and can split incident light with continuous wavelength into monochromatic light. The grating light splitting monochromator 4 is a C-T type light splitting monochromator or a littrow type monochromator. The grating light splitting monochromator 4 comprises a light splitting grating, the rotation angle of the light splitting grating is driven and adjusted by a motor, and the motor is connected with the control unit 13. The spectral wavelength range of the grating spectromonochromator 4 is within the emission spectral wavelength range of the excitation light source 1.
The second condenser element 5 condenses the light emitted from the exit slit of the grating monochromator 4 onto the long afterglow material to be analyzed.
The optical long-wavelength pass filter 6 is used to select a cutoff wavelength according to the analyzed wavelength range, pass light having a wavelength longer than the cutoff wavelength, and absorb light having a wavelength shorter than the cutoff wavelength. The purpose is to filter the high-order diffracted light exiting from the exit slit of the grating monochromator 4. In this embodiment, the monochromaticity of the irradiation light of the long afterglow material to be analyzed is ensured by switching the plurality of optical long pass filters 6 according to the target wavelength to be measured.
The sample holder 7 is used for placing the analyzed long afterglow material.
The third light focusing element 8 is used for collecting the phosphorescence excited by the analyzed long afterglow material.
The optical bandpass filter 9 has a function of passing only light in a certain wavelength range. The wavelength range of the optical bandpass is selected based on the emission wavelength range of the phosphorescence, and only the phosphorescence in the wavelength range of interest is passed through and used for reception by the photodetector 10. In this embodiment, the band-pass wavelength range of the optical band-pass filter 9 is within the fluorescence emission spectrum range of the analyzed long afterglow material.
The photodetector 10: the photoelectric detector is used for receiving phosphorescence signals and can be a semiconductor photodiode detector, a semiconductor phototriode detector, a photomultiplier tube, a surface array or line array detector and other photoelectric devices. The spectral response range of the photodetector should cover the wavelength range of the phosphorescence of the analyzed long afterglow material.
The electric signal amplifier 11 converts the photocurrent signal inputted from the photodetector into a voltage signal and amplifies it. The voltage signal output by the electrical signal amplifier 9 is proportional to the intensity of the phosphorescent light incident on the receiving surface of the photodetector 11.
The data acquisition and storage unit 12 can perform analog-to-digital conversion on the voltage signal output by the electric signal amplifier 11 and can realize a storage function.
The system control unit 13: the device is used for controlling the closing of the electric control optical shutter 3, the rotation of a grating driving motor of the grating light splitting monochromator 4, the data acquisition and storage unit 12 and the like. The starting time and the irradiation time of the exciting light, the starting time and the ending time of data acquisition and the sampling time interval can be set. And the grating position of the grating light splitting monochromator 4 can be controlled, and the measurement of the phosphorescence light attenuation curve under different excitation wavelengths can be completed according to a set program.
Data analysis processing and storage unit 14: and the method is used for analyzing, processing and storing phosphorescence attenuation curve and phosphorescence excitation spectrum data.
The long afterglow material phosphorescence excitation spectrum measurement system can also be used for fluorescence excitation spectrum measurement of long afterglow materials.
The invention relates to a method for measuring phosphorescence excitation spectrum of a long afterglow material, which comprises the following steps:
1) setting an excitation wavelength range, a wavelength scanning interval, an irradiation time, a total phosphorescence measurement time and a time interval;
2) the spectral wavelength of the grating monochromator 4 is set, the emergent light of the excitation light source 1 is split by the grating monochromator 4, and the high-order diffracted light of the emergent light of the grating monochromator 4 is removed by selecting the optical long-wave pass filter 6. According to the position of the light splitting grating and the spectral range of the excitation light source 1, a plurality of optical long-wave pass filters 6 can be switched to select a proper optical long-wave pass filter to ensure the monochromaticity of emergent light; if there is no higher order diffracted light in the exit light of the grating monochromator 4 in the wavelength range of the emission spectrum of the excitation light source 1, the optical long-wave pass filter 6 is not needed.
3) And controlling the electric optical shutter 3 to be opened, enabling emergent light of the excitation light source 1 to irradiate the long-afterglow material on the sample holder 7 after being monochromated, after the irradiation for a set time, controlling the electric optical shutter 3 to be closed and starting to collect the phosphorescence attenuation curve within the set time, and collecting and storing the phosphorescence intensity data once every other time interval until the measuring time reaches the total phosphorescence measuring time. From the moment of stopping illumination, within the set total time of phosphorescence measurement, analog-to-digital conversion is performed once every interval time to measure the phosphorescence intensity, and the closing time of the electric optical shutter 3 is taken as a time zero point, so that a phosphorescence intensity-decay-time relation curve, namely a phosphorescence decay curve, can be obtained.
4) And (3) adjusting the position of the light splitting grating of the grating light splitting monochromator 4 to change the light splitting wavelength, and repeating the step (3) until the light splitting wavelength of the grating light splitting monochromator 4 reaches the set termination wavelength to respectively obtain phosphorescence attenuation curve data under different excitation wavelengths.
5) Extracting a phosphorescence intensity variation curve along with the excitation wavelength at a certain attenuation moment from the phosphorescence attenuation curve data under different excitation wavelengths obtained in the step 4), and drawing a phosphorescence excitation spectrum curve.
In this example, the analyzed material is strontium aluminate doped with divalent europium, and the emission center wavelength is 520 nm;
the excitation light source 1 adopts a bromine tungsten lamp, and the emission wavelength range of the bromine tungsten lamp is 350 nm-30000 nm;
the first light-gathering element 2 is a glass lens with the focal length of 50mm, and the transmittance between 350nm and 500nm exceeds 90 percent;
the grating light splitting monochromator 4 adopts a C-T type grating light splitting monochromator, the blaze wavelength of the light splitting grating is 400nm, the wavelength resolution is 0.5nm, and the wavelength range is 200-800 nm;
the second light condensation element 5 is a glass lens with a focal length of 50mm, and the transmittance between 350nm and 500nm is over 90 percent;
the third light condensing element 8 is a glass lens with the focal length of 50mm, and the transmittance between 350nm and 500nm is over 90 percent;
the central wavelength of the optical band-pass filter 9 is 520nm, and the bandwidth is 10 nm;
the photodetector 10 is a silicon photodiode;
the control unit 13 is an industrial control card with analog-to-digital conversion function and I/O switch function, which is inserted into a PCI slot of a desktop computer motherboard, so as to control the opening and closing of the electrically controlled optical shutter 3, the rotation of the grating in the grating monochromator 4, the data acquisition and storage 12, and the data analysis processing and storage unit 14.
Since the wavelength scanning range of the excitation light source 1 is set to 350-500 nm, there is no influence of the higher order diffracted light corresponding to the absorption band of the analyzed material, in which case the optical long-wave pass filter 6 may not be used.
In this embodiment, the increase of the wavelength of the light split by the grating monochromator 4 is 1nm, the collection time of the phosphorescence attenuation curve is 120s, and the time interval is 50 ms.
The phosphorescence attenuation curves of europium-doped strontium aluminate are shown in FIG. 3 at excitation wavelengths of 402nm and 427nm, respectively.
The phosphorescence excitation spectrum of europium-doped strontium aluminate at the decay times of 500ms, 1000ms and 1500ms is shown in FIG. 4. It can be seen from fig. 4 that the phosphorescence excitation spectrum changes significantly at different decay times.
Claims (4)
1. The long afterglow material phosphorescence excitation spectrum measurement system is characterized by comprising an excitation light source (1), a first light gathering element (2), an electric light shutter (3), a grating light splitting monochromator (4), a second light gathering element (5), an optical long wavelength pass filter (6), a sample holder (7), a third light gathering element (8), an optical band pass filter (9), a photoelectric detector (10), an electric signal amplifier (11), a data acquisition and storage unit (12), a system control unit (13) and a data analysis processing and storage unit (14);
light beams emitted from the excitation light source (1) sequentially pass through the first light condensing element (2), the electric light shutter (3), the grating light splitting monochromator (4), the second light condensing element (5) and the optical long-wave pass filter (6) and then irradiate into the long-afterglow material on the sample holder (7), the light emitted from the long afterglow material is received by the photoelectric detector (10) and converted into an electric signal after sequentially passing through the third light condensing element (8) and the optical band pass filter (9), the electric signal is amplified by the electric signal amplifier (11) and then is subjected to data acquisition and storage by the data acquisition and storage unit (12), and the system control unit (13) is used for setting and controlling parameters of the electric light shutter (3), the grating light splitting monochromator (4) and the data acquisition and storage unit (12), the data analysis processing and storage unit (14) is used for processing and storing spectrogram data of the data acquired by the data acquisition and storage unit (12);
the grating light splitting monochromator (4) comprises a light splitting grating, the rotation angle of the light splitting grating is driven and adjusted through a motor, the motor is connected with the control unit (13), and the light splitting wavelength range of the grating light splitting monochromator (4) is within the emission spectrum wavelength range of the excitation light source (1);
the method for measuring the phosphorescence excitation spectrum of the long afterglow material comprises the following steps:
1) setting an excitation wavelength range, a wavelength scanning interval, an irradiation time, a total phosphorescence measurement time and a time interval;
2) setting the light splitting wavelength of the grating light splitting monochromator (4), splitting the emergent light of the excitation light source (1) by using the grating light splitting monochromator (4), and selecting the optical long-wave pass filter (6) to remove the high-order diffracted light of the emergent light of the grating light splitting monochromator (4); the optical long-wave pass filter (6) adopts a mode of switching a plurality of optical long-wave pass filters (6) according to the light splitting wavelength of the grating light splitting monochromator so as to ensure the monochromaticity of emergent light;
3) controlling the electric optical shutter (3) to be opened, enabling emergent light of the excitation light source (1) to irradiate the long-afterglow material on the sample holder (7) after being monochromatized, controlling the electric optical shutter (3) to be closed and starting to collect a phosphorescence attenuation curve after irradiation within a set time, and collecting and storing phosphorescence intensity data once every other time interval until the measuring time reaches the total phosphorescence measuring time;
4) adjusting the position of a light splitting grating of the grating light splitting monochromator (4) to change the light splitting wavelength until the light splitting wavelength of the grating light splitting monochromator (4) reaches the set termination wavelength, repeating the step 3), and measuring phosphorescence attenuation curve data under different excitation wavelengths respectively;
5) extracting a phosphorescence intensity variation curve along with the excitation wavelength at a certain attenuation moment from the phosphorescence attenuation curve data under different excitation wavelengths obtained in the step 4), and drawing a phosphorescence excitation spectrum curve.
2. The long afterglow material phosphorescence excitation spectrum measurement system according to claim 1, wherein: the band-pass wavelength range of the optical band-pass filter (9) is within the fluorescence emission spectrum range of the analyzed long afterglow material.
3. The long afterglow material phosphorescence excitation spectrum measurement system according to claim 1, wherein: the grating light splitting monochromator (4) is provided with an emergent light slit and an incident light slit, the grating light splitting monochromator (4) can split incident light with continuous wavelength into monochromatic light, and the grating light splitting monochromator (4) is a C-T type light splitting monochromator or a Letello type monochromator.
4. The long afterglow material phosphorescence excitation spectrum measurement system according to claim 1, wherein: the optical long-wave pass filter (6) is used for filtering high-order diffracted light emitted from the exit slit of the grating light splitting monochromator (4).
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