CN104502319A - Measurement device and measurement method of fluorescence quantum efficiency of half integrating spheres - Google Patents
Measurement device and measurement method of fluorescence quantum efficiency of half integrating spheres Download PDFInfo
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- CN104502319A CN104502319A CN201410819732.3A CN201410819732A CN104502319A CN 104502319 A CN104502319 A CN 104502319A CN 201410819732 A CN201410819732 A CN 201410819732A CN 104502319 A CN104502319 A CN 104502319A
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Abstract
The invention discloses a measurement device and a measurement method of the fluorescence quantum efficiency of half integrating spheres. The measurement device comprises a constant-current and constant-pressure source, a patch LED light source, a half integrating sphere optical cavity, an optical fiber spectrometer and a computer, wherein the constant-current and constant-pressure source is used for supplying stable current to the LED light source; the half integrating sphere optical cavity is surrounded by a half integrating sphere shell and a half integrating sphere reflector with the high reflectivity; the inner wall of the half integrating sphere shell is coated by a diffuse reflection coating with the high reflectivity; the half integrating sphere reflector penetrates through the sphere centers; the plane reflector is provided with a round hole which is used for fixing the patch LED light source and a to-be-detected sample; the to-be-detected sample is arranged on the patch LED light source; and a detection hole is formed in the half integrating sphere shell, and is used for coupling connection of an optical probe of the optical fiber spectrometer. A spectrum signal is detected by virtue of the optical fiber spectrometer; the to-be-detected sample is arranged out of an optical fiber numerical value aperture region to prevent primary direct light from entering a detector; and the use of a baffle plate is avoided, and thus the uniformity of light distribution in the integrating spheres is improved.
Description
Technical field
The present invention relates to a kind of quantum efficiency measuring device and measuring method thereof, particularly relate to a kind of semi-integral ball fluorescence quantum efficiency measurement mechanism using transparent fluorescent material as measuring object and measuring method thereof.
Background technology
In recent years, along with developing rapidly of LED illumination device, be more and more subject to people's attention the research of fluorescent material, quantum efficiency enjoys the concern of people as the important indicator evaluating fluorescent material luminescent properties.Usually, the quantum efficiency of fluorescent material is defined as the ratio of photon number that material launches and the photon number that material absorbs.
Fluorescent samples to be measured often causes its luminous intensity presentation space feature pockety due to its factor such as internal chemical composition and physical dimension, and prior art and involved measurement mechanism all adopt integrating sphere to collect the fluorescence sent from measuring object for this reason.Prior art, usual use laser as excitation source, and imports exciting light by the aperture offered at integrating sphere wall, and this kind of mode has following shortcoming: first, the relative distance of light source and sample is comparatively far away, adjust the process that exciting light can be irradiated on sample more loaded down with trivial details; The second, offer light hole at integrating sphere wall and easily make interior lights also easily be subject to the interference of exterior light from light hole escape.Monochromatic excitation light imports in integrating sphere for using optical fiber by another kind of technology, irradiates fluorescent samples and sends fluorescence.The shortcoming of this kind of method is, more weak by the exciting light energy of coupling fiber progradation bulb separation.
In addition, in existing integrating sphere measuring technique, in order to avoid a direct light enters detector, measurement result is impacted, be provided with baffle plate mostly before the detectors, but baffle plate self also can participate in absorption, the scattering of light in integrating sphere, the ideal behavior having broken integrating sphere makes integrating sphere effect reduce.
Summary of the invention
For there is incidence hole, baffle plate in prior art to the impact of measuring accuracy, the invention provides and a kind ofly need not offer incidence hole, semi-integral ball fluorescence quantum efficiency measurement mechanism without the need to baffle plate.
Meanwhile, present invention also offers a kind of corresponding semi-integral ball fluorescence quantum efficiency measuring method.
In order to solve the problems of the technologies described above, present invention employs following technical scheme:
A kind of semi-integral ball fluorescence quantum efficiency measurement mechanism, comprises constant current constant voltage source, semi-integral ball optics cavity, fiber spectrometer, computing machine and adopting surface mounted LED light source; Described semi-integral ball optics cavity is scribbled the semi-integral global shell of the diffuse coatings of high reflectance and is horizontally disposed with and is surrounded by the plane mirror of the center of curvature of semi-integral global shell by inwall; Described adopting surface mounted LED light source be positioned at semi-integral ball optics cavity sphere center position and with the center superposition of plane mirror, the fibre-optical probe of described fiber spectrometer is positioned on the inwall of semi-integral global shell, and the testing sample be placed on adopting surface mounted LED light source is positioned at outside the numerical aperture region of fibre-optical probe; Described constant current constant voltage source provides steady current for adopting surface mounted LED light source; The information output of described fiber spectrometer is connected with computing machine.
Correspondingly, a kind of semi-integral ball fluorescence quantum efficiency measuring method provided by the invention, have employed above-mentioned a kind of semi-integral ball fluorescence quantum efficiency measurement mechanism in the method, the steps include:
1) open constant current constant voltage source and set predetermined current/voltage value driving adopting surface mounted LED light source luminescent, when not laying testing sample, Deng adopting surface mounted LED light source luminescent stable after, fiber spectrometer detects by detection mouth the excitation spectrum obtained and saves as P
excite 1(λ), the wavelength coverage of this exciting light is λ
1L-λ
1H, wherein λ
1Lthe start wavelength of excitation spectrum, λ
1Hit is the cutoff wavelength of excitation spectrum;
2) semi-integral ball is opened, testing sample to be placed on adopting surface mounted LED light source and outside the numerical aperture region being positioned at fibre-optical probe, its light that can be excited is made to irradiate and send fluorescence, then close semi-integral ball optics cavity, now spectrometer detection to semi-integral ball optics cavity space in unabsorbed excitation spectrum save as P
excite 2(λ) spectrum that, sample launches fluorescence saves as P
launch(λ) wavelength coverage of, launching fluorescence is λ
2L-λ
2H, wherein λ
2Lthe start wavelength of emission spectrum, λ
2Hit is the cutoff wavelength of emission spectrum;
3) the quantum efficiency η automatically calculating sample by computing machine is:
In above-mentioned: h is Planck constant, c is the light velocity.
The present invention adopts adopting surface mounted LED light source as excitation source, and volume is little, is directly placed in semi-integral ball optics cavity space, short distance can acts on testing sample, ensure that the intensity excited, also without the need to loaded down with trivial details incident light coupling process.Meanwhile, adopting surface mounted LED light source is utilized more to be added with researching value as quantum efficiency measured by excitation source to the fluorescent material for LED.Testing sample is configured at outside fiber numerical aperture region, can ensures that the fluorescence that testing sample sends directly cannot enter spectrometer thus eliminate the use of baffle plate.
Compared with prior art, a kind of semi-integral ball fluorescence quantum efficiency measurement mechanism of the present invention and measuring method thereof have following beneficial effect:
1, adopt fibre-optical probe as detecting devices, outside numerical aperture region testing sample being configured at fibre-optical probe, restrained effectively direct light and enter the impact that detector causes measurement result, thus avoid the use of baffle plate.
2, this quantum efficiency measuring device adopts adopting surface mounted LED light source as excitation source, be placed in plane mirror center position, can closely act on testing sample and ensure that excitation intensity, semi-integral ball optics cavity interior volume can be placed in because adopting surface mounted LED light source volume is very little simultaneously, therefore need not offer light hole on ball wall.By selecting the LED monochromatic source of different centre wavelength, realize to identical fluorescent material under different excitation wavelength and the quantum efficiency of different fluorescent material under different excitation wavelength measure.
3, design transmission-type optical path, carry out quantum efficiency measurement for transparent fluorescent material, as fluorescent glass, transparent fluorescent ceramic, can disperse in a liquid fluorescent powder etc.
4, this quantum efficiency measuring device solves existing fluorescence efficiency integral ball measuring device structure the accessory such as sample clamp, optical baffle causes integrating sphere lack of homogeneity because using, sample is difficult to the problem of fixing.
Accompanying drawing explanation
Fig. 1 is a kind of structural representation of semi-integral ball fluorescence quantum efficiency measurement mechanism;
Excitation spectrum instrumentation plan one when Fig. 2 is not setting-out product;
Excitation spectrum instrumentation plan two when Fig. 3 is not setting-out product;
Fig. 4 is the structural representation that fluorescent glass or microslide are placed in semi-integral ball optics cavity;
Fig. 5 is the structural representation that fluorescent liquid is placed in semi-integral ball optics cavity;
Fig. 6 is the schematic diagram that the quantum efficiency of not placing testing sample is measured;
Fig. 7 is the fluorescence spectrum figure that when not placing testing sample, measurement obtains;
Fig. 8 is the schematic diagram that the quantum efficiency of placing testing sample is measured;
Fig. 9 is the fluorescence spectrum figure that when placing testing sample, measurement obtains.
In accompanying drawing: 1-constant current constant voltage source; 2-semi-integral ball optics cavity; 3-fiber spectrometer; 4-computing machine; 5-adopting surface mounted LED light source; 6-electrode holder; 7-testing sample; 8-plane mirror; 9-fibre-optical probe; 10-semi-integral global shell; 11-cuvette; 12-microslide; 13-optical fiber; 14-light source.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
As shown in Figure 1, a kind of semi-integral ball fluorescence quantum efficiency measurement mechanism, comprises constant current constant voltage source 1, semi-integral ball optics cavity 2, fiber spectrometer 3, computing machine 4 and adopting surface mounted LED light source 5.Semi-integral ball optics cavity 2 is scribbled the semi-integral global shell 10 of the diffuse coatings of high reflectance by inwall and is horizontally disposed with and is surrounded by the plane mirror 8 of the semi-integral centre of spherical curvature.The medium position of plane mirror 8 is provided with circular port, is provided with the electrode holder 6 for fixed L ED in circular port, adopting surface mounted LED light source is arranged on the end face that stretches in semi-integral global shell 10.Adopting surface mounted LED light source 5 be positioned at semi-integral ball optics cavity 2 sphere center position and with the center superposition of plane mirror 8, the fibre-optical probe 9 of fiber spectrometer 3 is positioned on the inwall of semi-integral global shell 10, and the testing sample be placed on adopting surface mounted LED light source 5 is positioned at outside the numerical aperture region of fibre-optical probe 9.Constant current constant voltage source 1 for driving adopting surface mounted LED light source 5 luminous, and by regulating electric current to regulate LED luminous intensity, to adapt to the sample with different fluorescence intensity, avoids output signal saturated.Measured by the spectrum of fibre-optical probe 9 to the integration space in half integrating sphere optics cavity 2, the information input computing machine 4 that fiber spectrometer 3 records, computing machine 4 calculates the fluorescence quantum efficiency of measuring object according to the first spectrum and the second spectrum.Fibre-optical probe is positioned at the ball wall of semi-integral ball optics cavity 2, by the angle configurations of fibre-optical probe, the sample being in sphere center position is in outside fiber numerical aperture region.This kind of detection mode can effectively suppress a direct light to enter detector.Fibre-optical probe position can be realized by modes such as probe positions or probe inclinations, as shown in Figure 2,3.
The semi-integral ball of this measurement mechanism uses a plane mirror 8 and semi-integral global shell 10 to carry out imaging, and then semi-integral global shell in kind and virtual image semi-integral global shell are combined into a spheroid completed in space.While this device ensure that integrating sphere effect, overcome the shortcoming because gravity factor needs unit clamp to support sample.Simple fixture can be used can to realize measuring the sample under the states such as solid, liquid, powder.Fluorescent glass or microslide 12 are placed as shown in Figure 4, and fluorescent glass can directly be placed on above adopting surface mounted LED light source, or is tested on microslide by fluorescent powder uniform application.As shown in Figure 5, fluorescent liquid is in cuvette 11 the placement schematic diagram of fluorescent liquid, and LED light is incident from the bottom of cuvette 11.
The feature of this measurement mechanism is: 1. adopt monochromatic adopting surface mounted LED light source as excitation source, carry out quantum efficiency measurement by transmission-type optical path to transparent fluorescent sample.The transmitted light path adopted refers to: LED monochromatic light is incident from sample side, and after absorption of sample, residue luminous energy is from the outgoing of sample opposite side.By selecting the LED monochromatic source of different centre wavelength, realize to identical fluorescent material under different excitation wavelength and the quantum efficiency of different fluorescent material under different excitation wavelength measure.2. adopt fiber spectrometer detecting light spectrum signal, testing sample is configured in fiber numerical aperture angular zone external suppression direct light and enters detector, avoid the use of baffle plate, thus improve photodistributed homogeneity in integrating sphere.3. adopting surface mounted LED light source is positioned at the sphere center position of semi-integral ball optics cavity, with the center superposition of plane mirror; Detector is positioned at the ball wall of semi-integral ball optics cavity 2, by the angle configurations of fibre-optical probe, the sample being in sphere center position is in outside fiber numerical aperture region.
Meanwhile, this covering device can also by computing machine according to detect twice spectroscopic data obtained and directly calculate quantum efficiency, namely semi-integral ball fluorescence quantum efficiency measuring method, the steps include:
1) adopting surface mounted LED light source 5 is arranged on electrode holder 6, as shown in Figure 6, open constant current constant voltage source and set predetermined current/voltage value driving adopting surface mounted LED light source 5 luminescence, when not laying testing sample 7, after adopting surface mounted LED light source 5 stable luminescence, it is P that fiber spectrometer 3 detects by fibre-optical probe 9 excitation spectrum obtained
excite 1(λ), the wavelength coverage of exciting light is λ
1L-λ
1H, wherein λ
1Lthe start wavelength of excitation spectrum, λ
1Hit is the cutoff wavelength of excitation spectrum; This excitation spectrum P
excite 1(λ) as the first spectrum.The spectrum that first spectrum is obtained by spectrometer measurement when being and not putting sample and standard diffusion sheet be configured in sample position, as shown in Figure 7.
2) semi-integral ball optics cavity 2 is opened, testing sample 7 to be placed on adopting surface mounted LED light source 5 and outside the numerical aperture region being positioned at fibre-optical probe 9, as shown in Figure 8, its light that can be excited is made to irradiate and send fluorescence, then close semi-integral ball optics cavity 2, now in semi-integral ball optics cavity 2 space detected of fiber spectrometer 3, unabsorbed excitation spectrum saves as P
excite 2(λ), sample launches the spectrum of fluorescence is P
launch(λ) wavelength coverage of, launching fluorescence is λ
2L-λ
2H, wherein λ
2Lthe start wavelength of emission spectrum, λ
2Hit is the cutoff wavelength of emission spectrum; This excitation spectrum is P
excite 2(λ) with spectrum P
launch(λ) as the second spectrum.The spectrum that second spectrum is obtained by spectrometer measurement when being and sample being configured in assigned position place, as shown in Figure 9.
3) computing machine calculates the quantum efficiency of testing sample automatically by the data of the first spectrum and the second spectrum, and the quantum efficiency η that computing machine calculates sample is automatically:
In above-mentioned: h is Planck constant, c is the light velocity.
Utilize above-mentioned semi-integral ball fluorescence quantum efficiency measurement mechanism and measuring method, quantum efficiency measurement is carried out to the YAG aluminate LED yellow fluorescent powder of Ying Temei YAG-04 model.Utilize the blue chip that centre wavelength is 450nm to excite fluorescent powder, take multiple measurements under passing to the electric current of 25mA, 50mA, 75mA, 100mA respectively.The quantum efficiency obtained as shown in Table 1.
Table one: the quantum efficiency of fluorescent powder under different excitating light strength
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (2)
1. a semi-integral ball fluorescence quantum efficiency measurement mechanism, is characterized in that: comprise constant current constant voltage source (1), semi-integral ball optics cavity (2), fiber spectrometer (3), computing machine (4) and adopting surface mounted LED light source (5); Described semi-integral ball optics cavity (2) is scribbled the semi-integral global shell (10) of the diffuse coatings of high reflectance and is horizontally disposed with and is surrounded by the plane mirror (8) of the center of curvature of semi-integral global shell (10) by inwall; Described adopting surface mounted LED light source (5) be positioned at semi-integral ball optics cavity (2) sphere center position and with the center superposition of plane mirror (8), the fibre-optical probe (9) of described fiber spectrometer (3) is positioned on the inwall of semi-integral global shell (10), and the testing sample be placed on adopting surface mounted LED light source (5) is positioned at outside the numerical aperture region of fibre-optical probe (9); Described constant current constant voltage source (1) provides steady current for adopting surface mounted LED light source (5); The information output of described fiber spectrometer (3) is connected with computing machine (4).
2. a semi-integral ball fluorescence quantum efficiency measuring method, is characterized in that, have employed a kind of semi-integral ball fluorescence quantum efficiency measurement mechanism according to claim 1 in the method, the steps include:
1. open constant current constant voltage source and set predetermined current/voltage value driving adopting surface mounted LED light source (5) luminescence, when not laying testing sample (7), after adopting surface mounted LED light source (5) stable luminescence, fiber spectrometer (3) detects by fibre-optical probe (9) excitation spectrum obtained and saves as P
excite 1(λ), the wavelength coverage of this exciting light is λ
1L-λ
1H, wherein λ
1Lthe start wavelength of excitation spectrum, λ
1Hit is the cutoff wavelength of excitation spectrum;
2. semi-integral ball optics cavity (2) is opened, testing sample (7) to be placed on adopting surface mounted LED light source (5) and outside the numerical aperture region being positioned at fibre-optical probe (9), its light that can be excited is made to irradiate and send fluorescence, then close semi-integral ball optics cavity (2), now in semi-integral ball optics cavity (2) space detected of spectrometer (3), unabsorbed excitation spectrum saves as P
excite 2(λ) spectrum that, sample launches fluorescence saves as P
launch(λ) wavelength coverage of, launching fluorescence is λ
2L-λ
2H, wherein λ
2Lthe start wavelength of emission spectrum, λ
2Hit is the cutoff wavelength of emission spectrum;
3. the quantum efficiency η automatically calculating sample by computing machine is:
In above-mentioned: h is Planck constant, c is the light velocity.
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Application publication date: 20150408 |