CN105403548A - Temperature variable spectral measurement device - Google Patents
Temperature variable spectral measurement device Download PDFInfo
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- CN105403548A CN105403548A CN201510898434.2A CN201510898434A CN105403548A CN 105403548 A CN105403548 A CN 105403548A CN 201510898434 A CN201510898434 A CN 201510898434A CN 105403548 A CN105403548 A CN 105403548A
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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 invention relates to a temperature variable spectral measurement device, which comprises an excitation light source, an integrating sphere, a temperature control sample stage, a temperature controller and a detector. Specifically, the temperature controller is used for controlling the temperature of the temperature control sample stage, the excitation light source and the integrating sphere and the integrating sphere and the detector are all connected through optical fiber. The excitation light sent by the excitation light source is introduced into an integrating sphere entrance port of the integrating sphere through optical fiber and is incident to the temperature control sample stage, the light sent by a sample placed on the temperature control sample stage or the light reflected by the temperature control sample stage when no sample is placed thereon is collected by optical fiber through an integrating sphere exit port and is then introduced into the detector, by comparing the difference of emission spectra detected by the detector when a sample is placed and no sample is placed, the luminescence quantum yield can be calculated, thereby realizing measurement of sample luminescence. By combining the excitation light source and the detector, the temperature variable spectral measurement device provided by the invention can realize measurement of the temperature variable emission spectrum, quantum yield and other optical properties of a luminescent material.
Description
Technical field
The present invention relates to a kind of light radiancy measuring system, be specifically related to a kind of alternating temperature spectral measurement device.
Background technology
Fluorescence spectrophotometer is also known as fluorospectrophotometer, it is a kind of instrument of qualitative and quantitative analysis, by the detection of fluorescence spectrophotometer, can obtain the excitation spectrum of material, emission spectrum, quantum yield, fluorescence intensity, fluorescence lifetime, Stokes shift, fluorescence polarization and the information such as characteristic and fluorescent quenching aspect of depolarizing, therefore it is widely used in research and the production fields such as luminescent material, illumination and display.Fluorometric investigation system is generally made up of excitation source, monochromator, integrating sphere, detector and computing machine etc.Usually, when using integrating sphere, the room temperature luminous quantum yield of luminescent material can be measured.But in a lot of application, in such as white light LEDs, the working temperature of fluorescent powder, far above room temperature, can reach 80-150 DEG C.There is significant difference in luminescent material photoluminescence quantum yield at different temperatures, usually along with its luminescence efficiency of rising of temperature can significantly decline, therefore Measurement accuracy material quantum yield at different temperatures has great importance for its application.Existing fluorescence spectrophotometer can only measure the quantum yield under room temperature, cannot measure material fluorescence quantum yield at different temperatures, is unfavorable for further investigation and the accurately screening of material.
Summary of the invention
In order to solve the problems of the technologies described above, the present invention proposes a kind of alternating temperature spectral measurement device.
A kind of alternating temperature spectral measurement device that the present invention proposes, this device comprises excitation source, integrating sphere, temperature controlled sample platform, temperature controller and detector; Wherein, temperature controller is for controlling the temperature of temperature controlled sample platform, and excitation source is connected with integrating sphere and between integrating sphere with detector by optical fiber; The exciting light that excitation source sends is incorporated into the integrating sphere entrance port of integrating sphere by optical fiber and is incident on temperature controlled sample platform, when the light that when temperature controlled sample platform being placed sample, sample sends or temperature controlled sample platform not being placed sample, the light of temperature control sample stage reflection is incorporated into detector by integrating sphere exit portal after optical fiber is collected, the difference of the emission spectrum that detector detects when placing and do not place sample by contrasting, calculate photoluminescence quantum yield, thus realize the measurement to sample luminescence.
Further, this device also comprises baffle plate, and this baffle plate is arranged between temperature controlled sample platform and integrating sphere exit portal, and the light preventing sample from sending directly penetrates from integrating sphere exit portal.
Further, described integrating sphere bottom is provided with opening, and the size of this opening is mated with the size of temperature controlled sample platform, thus when making temperature controlled sample platform be positioned at opening part and integrating sphere be formed as one overall.
Further, temperature controlled sample platform is realized and the combining closely or being separated of integrating sphere by elevating mechanism, and during measurement, this temperature controlled sample platform is risen to this opening part of integrating sphere by elevating mechanism, becomes one with integrating sphere; After measurement completes, this temperature controlled sample platform is fallen from this opening part by elevating mechanism, is convenient to change sample.
Further, this device also comprises the first monochromator, and this first monochromator is arranged between excitation source and integrating sphere.
Further, this device also comprises the second monochromator, and the second monochromator is arranged between integrating sphere and detector.
Further, this device also comprises lens, and lens are arranged on integrating sphere entrance port and/or integrating sphere exit portal place.
Further, this device also comprises catoptron, and this catoptron is between excitation source and integrating sphere.
Further, this detector selects fiber spectrometer or photomultiplier.
Further, excitation source is xenon lamp, laser instrument or LED.
Beneficial effect of the present invention: the alternating temperature spectral measurement device that the present invention proposes, in conjunction with excitation source, integrating sphere, temperature controlled sample platform and detector, can realize the measurement of the alternating temperature optical property such as emission spectrum, absolute luminescence quantum yield under luminescent material different temperatures.In addition, the present invention is by arranging baffle plate, and the light that can prevent sample from sending directly penetrates from integrating sphere exit portal.Accurately can be set and control temperature by temperature controller, thus realize the control to sample temperature; Its temperature controlling range is 77K to 673K, further at 273K to 673K.Realized and the combining closely or being separated of integrating sphere by elevating mechanism.
Accompanying drawing explanation
Fig. 1 is the structural representation of the embodiment 1 of the alternating temperature spectral measurement device that the present invention proposes.
Fig. 2 is the curve that the luminous intensity utilizing the alternating temperature spectral measurement device of embodiment 1 to measure changes along with temperature variation.
Fig. 3 is the structural representation of the embodiment 2 of the alternating temperature spectral measurement device that the present invention proposes.
Fig. 4 is the curve that the luminous intensity utilizing the alternating temperature spectral measurement device of embodiment 2 to measure changes along with temperature variation.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly understand, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.But those skilled in the art know, the present invention is not limited to accompanying drawing and following examples.
The alternating temperature spectral measurement device that the present invention proposes, comprises excitation source, integrating sphere, temperature controlled sample platform, temperature controller, detector etc.In device, excitation source is connected with integrating sphere and between integrating sphere with detector by optical fiber, and detector can be detector array, and this detector can select fiber spectrometer or photomultiplier; Excitation source can be xenon lamp, laser instrument, LED etc., if needed, exciting light first can obtain the exciting light of specific wavelength and bandwidth after monochromator, is then incorporated into integrating sphere by the mode of optical fiber or optical fiber and Lens Coupling and is incident on temperature controlled sample platform.The light that sample on temperature controlled sample platform sends is incorporated into detector after optical fiber or lens are collected, and realizes the measurement to sample luminescence, also before being incorporated into detector, first can carry out light splitting through monochromator.The extent of alternating temperature of sample stage and temperature-controlled precision can be selected according to actual needs, for general luminescent material, room temperature can be selected to the warm table of 300 DEG C.Be described for LED light source and xenon source below.
Embodiment 1
Alternating temperature spectral measurement device as shown in Figure 1, comprises integrating sphere 1, temperature controlled sample platform 2, light source 6, optical fiber head 5-1 and 5-2, baffle plate 3, fiber spectrometer 7 and temperature controller 4.
Wherein optical fiber head 5-1 is arranged on integrating sphere entrance port, for the incidence of exciting light.
Optical fiber head 5-2 is arranged on integrating sphere exit portal, for collecting emergent light and being directed into detector.
Light source 6 for wavelength be the LED of 450nm.
Integrating sphere 1 lower openings, the size of this opening is mated with the size of temperature controlled sample platform, thus when making temperature controlled sample platform be positioned at this opening part and integrating sphere be formed as one overall.
Temperature controlled sample platform 2 is for placing sample, and temperature controlled sample platform 2 is realized and the combining closely or being separated of integrating sphere by elevating mechanism, and be specially: during measurement, this temperature controlled sample platform is risen to this opening part of integrating sphere by elevating mechanism, becomes one with integrating sphere; After measurement completes, this temperature controlled sample platform is fallen from this opening part by elevating mechanism, is convenient to the replacing of sample.
Baffle plate 3 is arranged between temperature controlled sample platform 2 and integrating sphere exit portal, its objective is that the light preventing sample from sending directly penetrates from integrating sphere exit portal.
Temperature controller 4 is for controlling the temperature of temperature controlled sample platform 2, and temperature controller can accurately set and control temperature, thus realizes the control to sample temperature; Its temperature controlling range is 77K to 673K, further at 273K to 673K.
When temperature controlled sample platform 2 does not place sample, the exciting light that light source 6 sends is directed into the optical fiber head 5-1 at integrating sphere entrance port place by optical fiber and incides on sample stage 2, the light that sample stage 2 reflects is through after multiple reflections in integrating sphere, a part arrives fiber spectrometer 7 from the optical fiber head 5-2 of integrating sphere exit portal by optical fiber, and spectrometer then records emission spectrum.
When temperature controlled sample platform 2 places sample, the exciting light that light source 6 sends is directed into the optical fiber head 5-1 at integrating sphere entrance port place by optical fiber and incides on sample stage 2, the light that sample sends is through after multiple reflections in integrating sphere, a part arrives fiber spectrometer 7 from the optical fiber head 5-2 of integrating sphere exit portal by optical fiber, and spectrometer then records emission spectrum.
By the luminous intensity of material under measurement different temperatures, the fluorescent quenching information of material can be obtained; When placing and do not place sample by contrasting, the difference of the emission spectrum that spectrometer is recorded, then can calculate photoluminescence quantum yield.With commercial YAG:Ce
3+yellow fluorescent powder is example, Fig. 2 gives the curve that the luminous intensity that utilizes this alternating temperature spectral measurement device to measure changes along with temperature variation, as can see from Figure 2, along with the rising of temperature, its luminous intensity weakens gradually, at 150 DEG C, its luminous intensity is 97% under room temperature, shows good fluorescence thermal quenching characteristic; Table 1 gives the photoluminescence quantum yield under different temperatures, can see from table 1, and its photoluminescence quantum yield also reduces along with the rising of temperature.These information have important reference value for the application of material.
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, comprises integrating sphere 1, temperature controlled sample platform 2, light source 9, monochromator 10-1 and 10-2, lens 8-1 and 8-2, catoptron 12, photomultiplier 11, baffle plate 3, temperature controller 4 etc.
Wherein lens 8-1 is arranged on integrating sphere entrance port, and lens 8-2 is arranged on integrating sphere exit portal.
Light source 9 is xenon lamp.
Monochromator 10-1 is arranged between light source 9 and catoptron 12.
Monochromator 10-2 is arranged between lens 8-2 and photomultiplier 11.
Integrating sphere 1, temperature controlled sample platform 2, baffle plate 3 and temperature controller 4 are with embodiment 1.
When temperature controlled sample platform 2 does not place sample, the light that light source 9 sends obtains the exciting light of specific wavelength and bandwidth after monochromator 10-1, and this exciting light incides on temperature controlled sample platform 2 after catoptron 12 and lens 8-1.Enter into after the lens 8-2 of light through integrating sphere exit portal place that sample stage 2 reflects collects monochromator 10-2 carry out light splitting and detect by photomultiplier 11.
When temperature controlled sample platform 2 places sample, the light that light source 9 sends obtains the exciting light of continuously adjustable specific wavelength after monochromator 10-1, and this exciting light incides on temperature controlled sample platform 2 after catoptron 12 and lens 8-1.The light that sample sends through integrating sphere exit portal lens 8-2 collect after enter into monochromator 10-2 carry out light splitting and detect by photomultiplier 11.With Mn
4+the K of doping
2tiF
6red fluorescence powder (doping content is 5.56at.%) is example, Fig. 4 gives the curve that the luminous intensity that utilizes this alternating temperature spectral measurement device to measure changes along with temperature variation, therefrom can see, along with the rising of temperature, its luminous intensity weakens gradually, at 150 DEG C, its luminous intensity is 97% under room temperature, shows good fluorescence thermal quenching characteristic; The difference of the emission spectrum that photomultiplier is recorded when placing and do not place sample by contrasting, then photoluminescence quantum yield can be calculated, table 2 gives the photoluminescence quantum yield under different temperatures, therefrom can see, its photoluminescence quantum yield also reduces along with the rising of temperature, particularly when for temperature higher than 150 DEG C time, its luminescence efficiency declines fast.
Table 2
| Temperature (DEG C) | 50 | 100 | 150 | 200 | 250 | 300 |
| Fluorescence quantum yield | 98％ | 97％ | 93％ | 51％ | 23％ | 12％ |
Above, embodiments of the present invention are illustrated.But the present invention is not limited to above-mentioned embodiment.Within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. an alternating temperature spectral measurement device, is characterized in that, this device comprises excitation source, integrating sphere, temperature controlled sample platform, temperature controller and detector; Wherein, temperature controller is for controlling the temperature of temperature controlled sample platform, and excitation source is connected with integrating sphere and between integrating sphere with detector by optical fiber; The exciting light that excitation source sends is incorporated into the integrating sphere entrance port of integrating sphere by optical fiber and is incident on temperature controlled sample platform, when the light that when temperature controlled sample platform being placed sample, sample sends or temperature controlled sample platform not being placed sample, the light of temperature control sample stage reflection is incorporated into detector by integrating sphere exit portal after optical fiber is collected, the difference of the emission spectrum that detector detects when placing and do not place sample by contrasting, calculate photoluminescence quantum yield, thus realize the measurement to sample luminescence.
2. alternating temperature spectral measurement device according to claim 1, is characterized in that, this device also comprises baffle plate, and this baffle plate is arranged between temperature controlled sample platform and integrating sphere exit portal, and the light preventing sample from sending directly penetrates from integrating sphere exit portal.
3. alternating temperature spectral measurement device according to claim 1, is characterized in that, described integrating sphere bottom is provided with opening, and the size of this opening is mated with the size of temperature controlled sample platform, thus when making temperature controlled sample platform be positioned at opening part and integrating sphere be formed as one overall.
4. alternating temperature spectral measurement device according to claim 3, it is characterized in that, temperature controlled sample platform is realized and the combining closely or being separated, during measurement of integrating sphere by elevating mechanism, this temperature controlled sample platform is risen to this opening part of integrating sphere by elevating mechanism, becomes one with integrating sphere; After measurement completes, this temperature controlled sample platform is fallen from this opening part by elevating mechanism, is convenient to change sample.
5. alternating temperature spectral measurement device according to claim 1, is characterized in that, this device also comprises the first monochromator, and this first monochromator is arranged between excitation source and integrating sphere.
6. alternating temperature spectral measurement device according to claim 1, is characterized in that, this device also comprises the second monochromator, and the second monochromator is arranged between integrating sphere and detector.
7. alternating temperature spectral measurement device according to claim 1, is characterized in that, this device also comprises lens, and lens are arranged on integrating sphere entrance port and/or integrating sphere exit portal place.
8. alternating temperature spectral measurement device according to claim 1, is characterized in that, this device also comprises catoptron, and this catoptron is between excitation source and integrating sphere.
9. alternating temperature spectral measurement device according to claim 1, is characterized in that, this detector selects fiber spectrometer or photomultiplier.
10. alternating temperature spectral measurement device according to claim 1, is characterized in that, excitation source is xenon lamp, laser instrument or LED.
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