CN105403548B - A kind of alternating temperature spectral measurement device - Google Patents
A kind of alternating temperature spectral measurement device Download PDFInfo
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- CN105403548B CN105403548B CN201510898434.2A CN201510898434A CN105403548B CN 105403548 B CN105403548 B CN 105403548B CN 201510898434 A CN201510898434 A CN 201510898434A CN 105403548 B CN105403548 B CN 105403548B
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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
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
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Abstract
The present invention relates to a kind of alternating temperature spectral measurement device, which includes excitation light source, integrating sphere, temperature controlled sample platform, temperature controller and detector；Wherein, temperature controller is used to control the temperature of temperature controlled sample platform, is connected by optical fiber between excitation light source and integrating sphere and integrating sphere and detector；The exciting light that excitation light source is sent out introduces the integrating sphere entrance port of integrating sphere by optical fiber and is incident on temperature controlled sample platform, the light of temperature control sample stage reflection is introduced into detector by integrating sphere exit portal after optical fiber is collected when not placing sample on the light or temperature controlled sample platform that sample is sent out when placing sample on temperature controlled sample platform, the difference for the emission spectrum that detector detects when placing by comparing and do not place sample, photoluminescence quantum yield is calculated, to realize the measurement to shine to sample.Present invention combination excitation light source and detector, it can be achieved that the optical properties such as the alternating temperature emission spectrum of luminescent material, quantum yield measurement.
Description
Technical field
The present invention relates to a kind of light radiancy measuring systems, and in particular to a kind of alternating temperature spectral measurement device.
Background technology
Fluorescence Spectrometer is also known as sepectrophotofluorometer, is a kind of instrument of qualitative and quantitative analysis, passes through Fluorescence Spectrometer
Detection, the excitation spectrum of substance, emission spectrum, quantum yield, fluorescence intensity, fluorescence lifetime, Stokes position can be obtained
It moves, the information such as in terms of fluorescence polarization and depolarize characteristic and fluorescent quenching, therefore it is widely used in luminescent material, illumination
And researchs and the production field such as display.Fluorometric investigation system is generally by excitation light source, monochromator, integrating sphere, detector and meter
The compositions such as calculation machine.In general, when using integrating sphere, the room temperature luminous quantum yield of luminescent material can be measured.But very much
In application field, such as white light LEDs, the operating temperature of fluorescent powder is far above room temperature, can reach 80-150 DEG C.Luminescent material is not
There are significant differences for photoluminescence quantum yield under synthermal, usually under the rising of temperature its luminous efficiency meeting significantly
Drop, therefore the accurate quantum yield of material at different temperatures that measures has great importance for its application.Existing fluorescence
Spectrometer can only measure quantum yield at room temperature, can not be measured to the fluorescence quantum yield of material at different temperatures,
It is unfavorable for the further investigation of material and accurate screening.
Invention content
In order to solve the above-mentioned technical problem, the present invention proposes a kind of alternating temperature spectral measurement device.
A kind of alternating temperature spectral measurement device proposed by the present invention, the device include excitation light source, integrating sphere, temperature controlled sample
Platform, temperature controller and detector；Wherein, temperature controller is used to control the temperature of temperature controlled sample platform, excitation light source and integral
It is connected by optical fiber between ball and integrating sphere and detector；The exciting light that excitation light source is sent out is introduced into integral by optical fiber
The integrating sphere entrance port of ball is simultaneously incident on temperature controlled sample platform, the light or control that sample is sent out when placing sample on temperature controlled sample platform
The light that temperature control sample stage reflects when not placing sample on warm sample stage is introduced into spy by integrating sphere exit portal after optical fiber is collected
Device is surveyed, luminescent quantum is calculated in the difference for the emission spectrum that detector detects when placing by comparing and do not place sample
Yield, to realize the measurement to shine to sample.
Further, which further includes baffle, which prevents between temperature controlled sample platform and integrating sphere exit portal
The light that only sample is sent out directly is projected from integrating sphere exit portal.
Further, the integrating sphere lower part is equipped with opening, and the size of the opening is matched with the size of temperature controlled sample platform, from
And it is integrally formed with integrating sphere when temperature controlled sample platform being made to be located at opening.
Further, temperature controlled sample platform is realized by elevating mechanism and combining closely or detach with integrating sphere, when measurement, liter
The temperature controlled sample platform is risen to the opening of integrating sphere by descending mechanism, is become one with integrating sphere；After being measured, lifting
Mechanism falls the temperature controlled sample platform from the opening, is conveniently replaceable sample.
Further, which further includes the first monochromator, first monochromator setting excitation light source and integrating sphere it
Between.
Further, which further includes the second monochromator, and the second monochromator is arranged between integrating sphere and detector.
Further, which further includes lens, and lens are arranged at integrating sphere entrance port and/or integrating sphere exit portal.
Further, which further includes speculum, and the speculum is between excitation light source and integrating sphere.
Further, which selects fiber spectrometer or photomultiplier.
Further, excitation light source is xenon lamp, laser or LED.
Beneficial effects of the present invention：Alternating temperature spectral measurement device combination excitation light source proposed by the present invention, integrating sphere, temperature control
Sample stage and detector are, it can be achieved that the alternating temperatures such as emission spectrum, absolute luminescence quantum yield are optical under luminescent material different temperatures
The measurement of energy.In addition, the present invention can prevent the light that sample is sent out from directly being projected from integrating sphere exit portal by the way that baffle is arranged.
Temperature can be accurately set and controlled by temperature controller, to realize the control to sample temperature；Its temperature controlling range
For 77K to 673K, further in 273K to 673K.It is realized by elevating mechanism and combining closely or detach with integrating sphere.
Description of the drawings
Fig. 1 is the structural schematic diagram of the embodiment 1 of alternating temperature spectral measurement device proposed by the present invention.
Fig. 2 is that the luminous intensity measured using the alternating temperature spectral measurement device of embodiment 1 is changed with temperature change
Curve.
Fig. 3 is the structural schematic diagram of the embodiment 2 of alternating temperature spectral measurement device proposed by the present invention.
Fig. 4 is that the luminous intensity measured using the alternating temperature spectral measurement device of embodiment 2 is changed with temperature change
Curve.
Specific implementation mode
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, and reference
Attached drawing, the present invention is described in more detail.But those skilled in the art know, the invention is not limited in attached drawings and following reality
Apply example.
Alternating temperature spectral measurement device proposed by the present invention, including the control of excitation light source, integrating sphere, temperature controlled sample platform, temperature
Device, detector etc..It is connected by optical fiber between excitation light source and integrating sphere and integrating sphere and detector in device, detector
Can be detector array, which can select fiber spectrometer or photomultiplier；Excitation light source can be xenon lamp, swash
Then light device, LED etc. pass through if it is desired, exciting light obtains specific wavelength and the exciting light of bandwidth after can first passing through monochromator
The mode of optical fiber or optical fiber and Lens Coupling is introduced into integrating sphere and is incident on temperature controlled sample platform.Sample on temperature controlled sample platform
The light sent out is introduced into detector after optical fiber or lens are collected, and realizes the measurement to shine to sample, can also be visited being introduced into
Monochromator is first passed through before surveying device to be divided.The extent of alternating temperature and temperature-controlled precision of sample stage can be selected according to actual needs
It selects, for general luminescent material, room temperature may be selected to 300 DEG C of warm table.Below by taking LED light source and xenon source as an example into
Row explanation.
Embodiment 1
Alternating temperature spectral measurement device as shown in Figure 1, including integrating sphere 1, temperature controlled sample platform 2, light source 6, optical fiber head 5-1 and
5-2, baffle 3, fiber spectrometer 7 and temperature controller 4.
Wherein optical fiber head 5-1 settings are used for the incidence of exciting light in integrating sphere entrance port.
Optical fiber head 5-2 is arranged in integrating sphere exit portal, for collecting emergent light and being directed into detector.
Light source 6 is the LED that wavelength is 450nm.
The size of 1 lower openings of integrating sphere, the opening is matched with the size of temperature controlled sample platform, so that temperature controlled sample platform
It is integrally formed with integrating sphere when positioned at the opening.
Temperature controlled sample platform 2 for placing sample, realized by elevating mechanism and combined closely with integrating sphere by temperature controlled sample platform 2
Or separation, specially：When measurement, which is risen to the opening of integrating sphere by elevating mechanism, with integrating sphere collection
It is integrally formed；After being measured, elevating mechanism falls the temperature controlled sample platform from the opening, is convenient for the replacement of sample.
Baffle 3 is arranged between temperature controlled sample platform 2 and integrating sphere exit portal, and the purpose is to prevent the light that sample is sent out direct
It is projected from integrating sphere exit portal.
Temperature controller 4 is used to control the temperature of temperature controlled sample platform 2, and temperature controller can accurately set and control temperature
Degree, to realize the control to sample temperature；Its temperature controlling range is 77K to 673K, further in 273K to 673K.
When not placing sample on temperature controlled sample platform 2, the exciting light that light source 6 is sent out is directed into integrating sphere entrance port by optical fiber
The optical fiber head 5-1 at place is simultaneously incident on sample stage 2, and the light that sample stage 2 reflects is after the multiple reflections in integrating sphere, a part
Optical fiber head 5-2 from integrating sphere exit portal reaches fiber spectrometer 7 by optical fiber, and spectrometer then records emission spectrum.
When placing sample on temperature controlled sample platform 2, the exciting light that light source 6 is sent out is directed by optical fiber at integrating sphere entrance port
Optical fiber head 5-1 and be incident on sample stage 2, the light that sample is sent out is after the multiple reflections in integrating sphere, and a part is from product
Optical fiber head 5-2 at bulb separation exit portal reaches fiber spectrometer 7 by optical fiber, and spectrometer then records emission spectrum.
By measuring the luminous intensity of material under different temperatures, the fluorescent quenching information of material can be obtained；Pass through comparison
The difference for the emission spectrum that spectrometer is recorded when placing and not placing sample, then can be calculated photoluminescence quantum yield.With quotient
Use YAG:Ce3+For yellow fluorescent powder, Fig. 2 gives the luminous intensity measured using the alternating temperature spectral measurement device with temperature
The curve of variation and variation, from fig. 2 it can be seen that with the raising of temperature, luminous intensity gradually weakens, at 150 DEG C
Its luminous intensity is 97% at room temperature, shows good fluorescence thermal quenching characteristic；Table 1 gives shining under different temperatures
Quantum yield, it can be seen that, photoluminescence quantum yield is reduced also with the raising of temperature from table 1.These information are for material
The application of material has important reference value.
Table 1
| Temperature (DEG C) | 50 | 100 | 150 | 200 | 250 | 300 |
| Fluorescence quantum yield | 95% | 93% | 90% | 85% | 72% | 64% |
Embodiment 2
Alternating temperature spectral measurement device as shown in Figure 3, including integrating sphere 1, temperature controlled sample platform 2, light source 9, monochromator 10-1
With 10-2, lens 8-1 and 8-2, speculum 12, photomultiplier 11, baffle 3, temperature controller 4 etc..
Wherein lens 8-1 settings are arranged in integrating sphere entrance port, lens 8-2 in integrating sphere exit portal.
Light source 9 is xenon lamp.
Monochromator 10-1 is arranged between light source 9 and speculum 12.
Monochromator 10-2 is arranged between lens 8-2 and photomultiplier 11.
Integrating sphere 1, temperature controlled sample platform 2, baffle 3 and temperature controller 4 are the same as embodiment 1.
When sample is not placed on temperature controlled sample platform 2, light that light source 9 is sent out obtained after monochromator 10-1 specific wavelength and
The exciting light of bandwidth, the exciting light are incident on after speculum 12 and lens 8-1 on temperature controlled sample platform 2.The light that sample stage 2 reflects
Lens 8-2 at integrated ball exit portal enters monochromator 10-2 and be divided and visited by photomultiplier 11 after collecting
It surveys.
When placing sample on temperature controlled sample platform 2, the light that light source 9 is sent out obtains continuously adjustable spy after monochromator 10-1
The exciting light of standing wave length, the exciting light are incident on after speculum 12 and lens 8-1 on temperature controlled sample platform 2.The light that sample is sent out
The lens 8-2 of integrated ball exit portal enters monochromator 10-2 and be divided and detected by photomultiplier 11 after collecting.
With Mn4+The K of doping2TiF6For red fluorescence powder (doping concentration 5.56at.%), Fig. 4, which gives, utilizes the alternating temperature spectrum
The curve that changes with temperature change of luminous intensity that measuring device measures, therefrom it can be seen that, with the raising of temperature,
Luminous intensity gradually weakens, its luminous intensity is 97% at room temperature at 150 DEG C, and it is special to show good fluorescence thermal quenching
Property；The difference for the emission spectrum that photomultiplier is recorded when placing by comparing and do not place sample, then can be calculated hair
Quantum yield, table 2 give the photoluminescence quantum yield under different temperatures, therefrom it can be seen that, photoluminescence quantum yield also with
It the raising of temperature and reduces, especially when being higher than 150 DEG C for temperature, luminous efficiency rapid decrease.
Table 2
| Temperature (DEG C) | 50 | 100 | 150 | 200 | 250 | 300 |
| Fluorescence quantum yield | 98% | 97% | 93% | 51% | 23% | 12% |
More than, embodiments of the present invention are illustrated.But the present invention is not limited to the above embodiments.It is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the guarantor of the present invention
Within the scope of shield.
Claims (10)
1. a kind of alternating temperature spectral measurement device, which is characterized in that the device includes excitation light source, integrating sphere, temperature controlled sample platform, temperature
Spend controller and detector；Wherein, temperature controller is used to control the temperature of temperature controlled sample platform, between excitation light source and integrating sphere
By the first optical fiber be connected and integrating sphere and detector between be connected by the second optical fiber；What excitation light source was sent out swashs
It shines and the integrating sphere entrance port of integrating sphere is introduced by the first optical fiber and is incident on temperature controlled sample platform, put on temperature controlled sample platform
The light that temperature control sample stage reflects when not placing sample on the light or temperature controlled sample platform that sample is sent out when setting sample passes through integrating sphere
Exit portal is introduced into detector after the collection of the second optical fiber, by measuring the luminous intensity of sample under different temperatures, obtains sample
Fluorescent quenching information；The difference for the emission spectrum that detector detects when placing by comparing and do not place sample, calculates
To photoluminescence quantum yield, to which alternating temperature spectral measurement device is realized to sample luminous intensity at different temperatures and luminous quantity
The measurement of sub- yield.
2. alternating temperature spectral measurement device according to claim 1, which is characterized in that the device further includes baffle, the baffle
It is arranged between temperature controlled sample platform and integrating sphere exit portal, prevents the light that sample is sent out from directly being projected from integrating sphere exit portal.
3. alternating temperature spectral measurement device according to claim 1, which is characterized in that the integrating sphere lower part is equipped with opening,
The size of the opening is matched with the size of temperature controlled sample platform, so that temperature controlled sample platform is formed when being located at opening with integrating sphere
It is integral.
4. alternating temperature spectral measurement device according to claim 3, which is characterized in that temperature controlled sample platform passes through elevating mechanism reality
It now combining closely or detaching with integrating sphere, when measurement, which is risen to the opening of integrating sphere by elevating mechanism
Place, becomes one with integrating sphere；After being measured, elevating mechanism falls the temperature controlled sample platform from the opening, convenient for more
Vary product.
5. alternating temperature spectral measurement device according to claim 1, which is characterized in that the device further includes the first monochromator,
First monochromator is arranged between excitation light source and integrating sphere.
6. alternating temperature spectral measurement device according to claim 1, which is characterized in that the device further includes the second monochromator,
Second monochromator is arranged between integrating sphere and detector.
7. alternating temperature spectral measurement device according to claim 1, which is characterized in that the device further includes lens, and lens are set
It sets at integrating sphere entrance port and/or integrating sphere exit portal.
8. alternating temperature spectral measurement device according to claim 1, which is characterized in that the device further includes speculum, this is anti-
Mirror is penetrated between excitation light source and integrating sphere.
9. alternating temperature spectral measurement device according to claim 1, which is characterized in that the detector select fiber spectrometer or
Photomultiplier.
10. alternating temperature spectral measurement device according to claim 1, which is characterized in that excitation light source be xenon lamp, laser or
LED。
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| JP3287775B2 (en) * | 1996-02-29 | 2002-06-04 | 松下電器産業株式会社 | Method and apparatus for measuring quantum efficiency of phosphor |
| CN1584553A (en) * | 2004-06-04 | 2005-02-23 | 湖南大学 | Measuring apparatus and method for fluorescent material temperature-changing characteristic |
| CN201110883Y (en) * | 2007-12-05 | 2008-09-03 | 杭州浙大三色仪器有限公司 | Semiconductor lighting device thermal performance measuring apparatus |
| JP5148387B2 (en) * | 2008-06-30 | 2013-02-20 | 浜松ホトニクス株式会社 | Spectrometer, spectroscopic method, and spectroscopic program |
| CN101430278A (en) * | 2008-12-04 | 2009-05-13 | 中国计量学院 | Apparatus for measuring luminous efficiency of photoluminescent body |
| CN102175428B (en) * | 2011-01-10 | 2013-08-21 | 杭州远方光电信息股份有限公司 | Device and method for measuring internal quantum efficiency of light emitting diode (LED) |
| CN102359817B (en) * | 2011-03-08 | 2015-11-18 | 中国科学院福建物质结构研究所 | A kind of system for testing yield of up-conversion luminescence absolute quantum |
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