CN108645803A - A kind of optical coupled test device of alternating temperature integrating sphere - Google Patents
A kind of optical coupled test device of alternating temperature integrating sphere Download PDFInfo
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- CN108645803A CN108645803A CN201810565487.6A CN201810565487A CN108645803A CN 108645803 A CN108645803 A CN 108645803A CN 201810565487 A CN201810565487 A CN 201810565487A CN 108645803 A CN108645803 A CN 108645803A
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- integrating sphere
- temperature
- alternating temperature
- test device
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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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
Abstract
The present invention provides a kind of optical coupled test devices of alternating temperature integrating sphere, including:Temperature-control units change for controlling within the temperature range of solid sample;Integrating sphere, light are beaten by the unthreaded hole on integrating sphere on sample, are reflected into integrating sphere after carrying out realization diffusing reflection and are exported by optical fiber;Optical fiber connects integrating sphere and spectrometer, diffuses through alternating temperature spectroscopic assay, obtain optical parameter measurement of the solid sample under condition of different temperatures.The present invention takes full advantage of the reapective features of integrating sphere and temperature control equipment, and efficient coupling connection, simple structure is efficient, and test result is accurate, and test speed is fast, can be used for the detection of photosensitive functional material and correlative technology field.
Description
Technical field
The invention belongs to field of optical measuring technologies, it particularly relates under the conditions of a wide range of temperature change, effectively survey
Try optical parameter a kind of optical coupled test device of alternating temperature integrating sphere, for measure optical material under condition of different temperatures
Optics diffusing reflection and the parameter measurements such as luminous quantum efficiency.
Background technology
In recent years, it with semiconductor lighting, shines, the fields such as display and bio-imaging are flourished, high-performance solid-state
Luminescent material is by information technology, the extensive concern of the high-end technical field such as new material and new energy.Currently, from basic research angle
Degree analysis, the routine test of solid luminescent material cannot meet the needs of researcher assesses material property, such as
Low temperature/alternating temperature under deoxygenation test condition, some special physics and chemical phenomenon can occur, while near infrared region (800-
1700 nanometers) detection demand it is also bigger.On the other hand, engineering technology application field (as illuminated, display etc.), shine material
The physical property of material is subjected to the influence of external operation condition (such as temperature), it is therefore desirable to develop and establish novel test means with
Meet the demand.
Solid sample (such as powder and film) luminous absolute quantum yield test be develop in recent years faster function it
One, and weigh the core index of luminescent material performance quality.Photoluminescence quantum yield (also referred to as quantum efficiency, PLQY) refers to substance
Light emitted number of photons and the ratio between the excitation light subnumber absorbed, characterize the size of material luminescence ability after extinction.Currently,
The test of absolute quantum efficiency is also only limitted to normal temperature condition, cannot achieve and is analysed in depth to the optical characteristics under specific condition
And research, this is tested with alternating temperature emission spectrum developed in recent years and the test of alternating temperature luminescent lifetime is inconsistent.
The low temperature quantum yield measurement that relents on a large scale is currently in blank stage, and this respect demand is very big, as long as doing alternating temperature
Optic test will be related to the needs of alternating temperature absolute luminescence quantum yield.
Integrating sphere refers to the hollow ball that inner surface has high reflectivity, is mainly dissipated to light to being put in sample in ball
It penetrates and reflex, or to a kind of Efficient devices that the light that light source itself is sent out is collected.Light passes through with coating
The reflection of ball inner homogeneous and diffusion, and projected by delivery outlet after being integrated inside integrating sphere, be a kind of ideal
Light uniforming device is diffused, it can outgoing beam caused by by eliminating light source itself in internal repeatedly unrestrained transmitting be uneven or band
There is the problem of polarization direction, can accurately measure the performances such as optical reflection, transmission, brightness, radiancy and the coloration of material, commonly uses
In LED, laser, energy-saving lamp, in the photochromic test of luminescent screen etc..The good optic test ability of integrating sphere and accuracy height etc.
Advantage makes it be widely applied in optical engineering, chemistry and material science.In recent years, integrating sphere measurement optics is utilized
The parameters such as the UV, visible light near-infrared diffusing reflection spectrum of material, fluorescence absolute quantum yield are more and more extensive.Meanwhile in low temperature and
Testing requirement under temperature match curing conditions is bigger.
Now widely used is that direct method surveys the absolute quantum yield that shines, that is, utilizes integrating sphere and spectrometer directly to survey
Amount, the test of room temperature absolute luminescence quantum yield may be implemented in this method, and alternating temperature control is still in the exploratory stage.It is general to think
Method, which is low temperature, can directly use liquid nitrogen frozen sample, and changing device can be placed in integrating sphere by when alternating temperature, but for integral
It is difficult to realize that changing device is placed in regular integral ball for ball, first, volume is larger, second is that integrating sphere is not easy to seal,
Third, changing device is placed on the scattering that can seriously affect light in integrating sphere;Second scheme be by sample bin accretion bulb separation directly into
Row alternating temperature controls, and this mode difficulty is big, and sample bin is accomplished to be completely closed, and this method is not for current device
Reality.
However, current diffusing reflection spectrum spectrum and absolute quantum yield test are largely only limitted to room temperature, in order to meet
Spectral information technical testing growth requirement, it is necessary to realize alternating temperature integrating sphere optic testing system.Especially a wide range of alternating temperature product
Ball-dividing device is but in blank stage so far.Meanwhile low temperature and alternating temperature control are also different, low temperature can pass through liquid nitrogen frozen sample
It realizes, and alternating temperature controlling difficulties are after introducing regulating and controlling temperature device, how to be further effectively combined into and set with integrating sphere
Count difficult point.
Invention content
In order to solve the above technical problems, the present invention provides a kind of optical coupled test device of alternating temperature integrating sphere, technical side
Case is as follows:
A kind of optical coupled test device of alternating temperature integrating sphere, which is characterized in that including:
Temperature-control units, the temperature range for controlling solid sample change;
Integrating sphere, light are beaten by the unthreaded hole on integrating sphere on sample, are reflected into integrating sphere after carrying out realization diffusing reflection
It is exported by optical fiber;
Optical fiber connects integrating sphere and spectrometer, diffuses through alternating temperature spectroscopic assay, obtain solid sample in not equality of temperature
Optical parameter measurement under the conditions of degree.
Preferably, the temperature-control units include electricity refrigeration and electrical heating temperature control device, are being located at integrating sphere opening just
Lower section 1-2mm, the temperature range for controlling solid sample are 4K-500K.
Preferably, the solid sample is located in the temperature-control units, is powder or film sample.
Preferably, the fiber lengths ranging from 1 to 5m.
Preferably, the spectrometer is any one in ultraviolet, visible, near-infrared fluorescent spectrometer or absorption spectrometer
Kind.
Preferably, the optical parameter to be measured is diffusing reflection spectrum and fluorescence absolute quantum yield.Preferably, described
Temperature-control units are the microstat devices of Oxford company.
Preferably, the spectrometer is the FLS980 of Edinburg company.
The present invention takes full advantage of the reapective features of integrating sphere and temperature control equipment, and efficient coupling connects, simple structure,
Efficient, test result is accurate, and test speed is fast, can be used for the detection of photosensitive functional material and correlative technology field.
Description of the drawings
Fig. 1 is the structural schematic diagram of the optical coupled test device of alternating temperature integrating sphere in embodiment 1.
In Fig. 2, A, C figures are 1, Isosorbide-5-Nitrae, and 4- tetraphenyl 1,3-butadiene samples and reference sample barium sulfate are in 100 Kelvins
And 300 Kelvin light scattering spectrum;B, D figure are sample and reference sample barium sulfate in 100 Kelvins and 300 Kelvins
Emission spectrum.
In Fig. 3, A, C figures are the light scattering of anthracene sample and reference sample barium sulfate in 170 Kelvins and 370 Kelvins
Spectrum;B, D figure are the emission spectrum of sample and reference sample barium sulfate in 170 Kelvins and 370 Kelvins.
Reference sign:
Spectrometer 1, optical fiber 2, integrating sphere 3, temperature-control units 4, solid sample 5.
Specific implementation mode
The optical coupled test device of alternating temperature integrating sphere of the present invention is done further with reference to specific embodiment
Illustrate, but protection scope of the present invention is not limited to this.
Embodiment 1
A kind of optical coupled test device of alternating temperature integrating sphere, including:Temperature-control units 4, the temperature for controlling solid sample 5
Variation in range;Integrating sphere 3, light are beaten by the unthreaded hole on integrating sphere 3 on sample, be reflected into integrating sphere 3 realize it is unrestrained
It is exported by optical fiber 2 after reflection;Optical fiber 2 connects integrating sphere 3 and spectrometer 1, diffuses through alternating temperature spectroscopic assay, obtain
Optical parameter measurement of the solid sample 5 under condition of different temperatures.
Temperature-control units 4 include electricity refrigeration and electrical heating temperature control device, are located at 1-2mm immediately below 3 opening of integrating sphere,
The temperature range for controlling solid sample 5 is 4K-500K.Solid sample 5 is located in the temperature-control units 4, is powder or film sample
Product.2 length range of optical fiber is 1 to 5m.Spectrometer 1 is times in ultraviolet, visible, near-infrared fluorescent spectrometer or absorption spectrometer
Meaning is a kind of.
The optical parameter to be measured is diffusing reflection spectrum and fluorescence absolute quantum yield.
Solid sample 5 can be anthracene or 1,1,4,4- tetraphenyl 1,3- butadiene.
Most preferably, temperature-control units 4 are the microstat devices of Oxford company, and spectrometer 1 is Edinburg company
FLS980。
Embodiment 2
Utilize the alternating temperature integrating sphere device system testing alternating temperature luminous quantum efficiency in embodiment 1:
1) 150 milligrams of luminescent sample anthracene is weighed, it is evenly laid out in temperature-control units microstat, it is at integrating sphere
Immediately below opening;
2) 1m optical fiber is utilized to combine above-mentioned temperature-control units and molding Fluorescence Spectrometer (FLS980 of Edinburg company);
3) sample temperature is controlled respectively in 157K, 257K, 317K using temperature regulating device, arrange parameter swashs on spectrometer
It is 360 nanometers to send out wavelength, and exciting slit is 10 nanometers, and transmite slit is 10 nanometers, is surveyed to the absolute luminescence quantum yield of sample
Examination, result is respectively 27.4%, 26.5% and 23.2%.
Embodiment 3
Utilize the alternating temperature integrating sphere device system testing alternating temperature luminous quantum efficiency in embodiment 1:
1) 300 milligrams of luminescent sample anthracene is weighed, it is evenly laid out in temperature-control units microstat, it is at integrating sphere
Immediately below opening;
2) optical fiber of 5m long is utilized to tie above-mentioned temperature-control units and molding Fluorescence Spectrometer (FLS980 of Edinburg company)
It closes, as shown in Figure 1;
3) sample temperature is controlled respectively in 137 and 297K using temperature regulating device, the arrange parameter excitation wave on spectrometer
A length of 360 nanometers, exciting slit is 5 nanometers, and transmite slit is 5 nanometers, is tested the absolute luminescence quantum yield of sample, knot
Fruit is respectively 26.3% and 24.0%.
Embodiment 4
Utilize the alternating temperature integrating sphere device system testing alternating temperature luminous quantum efficiency in embodiment 1:
1) luminescent sample 1, Isosorbide-5-Nitrae are weighed, 200 milligrams of 4- tetraphenyls 1,3-butadiene is uniformly positioned over temperature-control units
It in microstat, is at immediately below integrating sphere opening, distance is 1 millimeter;
2) 2m optical fiber is utilized to combine above-mentioned apparatus and molding Fluorescence Spectrometer (FLS980 of Edinburg company);
3) low temperature temperature control is utilized to control temperature in 100K, arrange parameter excitation wavelength is 360 nanometers on spectrometer, is swashed
It is 5 nanometers to send out slit, and transmite slit is 5 nanometers, is tested the absolute luminescence quantum yield of sample, as a result 65.9%;
4) temperature is controlled to 300K using heat riser, arrange parameter excitation wavelength is 360 nanometers on spectrometer, is swashed
It is 5 nanometers to send out slit, and transmite slit is 5 nanometers, and 65.1% is tested to the absolute luminescence quantum yield of sample.
In Fig. 2, A, C figures are 1, Isosorbide-5-Nitrae, and 4- tetraphenyl 1,3-butadiene samples and reference sample barium sulfate are in 100 Kelvins
And 300 Kelvin light scattering spectrum;B, D figure are sample and reference sample barium sulfate in 100 Kelvins and 300 Kelvins
Emission spectrum.The quantum yield that 100 and 300 Kelvin's conditions are calculated by two figures is respectively 65.9% and 65.1%.
Embodiment 5
1) 100 milligrams of luminescent sample anthracene is weighed, it is evenly laid out in temperature-control units microstat, it is at integrating sphere
Immediately below opening, distance is 2 millimeters;
2) 2m optical fiber is utilized to combine above-mentioned temperature-control units and molding Fluorescence Spectrometer (FLS980 of Edinburg company);
3) low temperature temperature control is utilized to control temperature in 170K, arrange parameter excitation wavelength is 360 nanometers on spectrometer, is swashed
It is 5 nanometers to send out slit, and transmite slit is 5 nanometers, is tested the absolute luminescence quantum yield of sample, as a result 28.4%;
4) temperature is controlled to 370K using heat riser, arrange parameter excitation wavelength is 360 nanometers on spectrometer, is swashed
It is 5 nanometers to send out slit, and transmite slit is 5 nanometers, and 22.1% is tested to the absolute luminescence quantum yield of sample.
In Fig. 3, A, C figures are the light scattering of anthracene sample and reference sample barium sulfate in 170 Kelvins and 370 Kelvins
Spectrum;B, D figure are the emission spectrum of sample and reference sample barium sulfate in 170 Kelvins and 370 Kelvins.It is calculated by two figures
The quantum yield for obtaining 170 and 370 Kelvin's conditions is respectively 28.4% and 22.1%.
Claims (8)
1. a kind of optical coupled test device of alternating temperature integrating sphere, which is characterized in that including:
Temperature-control units change for controlling within the temperature range of solid sample;
Integrating sphere, light are beaten by the unthreaded hole on integrating sphere on sample, be reflected into integrating sphere after carrying out realization diffusing reflection by
Optical fiber exports;
Optical fiber connects integrating sphere and spectrometer, diffuses through alternating temperature spectroscopic assay, obtain solid sample in different temperatures item
Optical parameter measurement under part.
2. the optical coupled test device of alternating temperature integrating sphere according to claim 1, which is characterized in that the temperature-control units packet
Electricity refrigeration and electrical heating temperature control device are included, is located at 1-2mm immediately below integrating sphere opening, controls the temperature model of solid sample
It encloses for 4K-500K.
3. the optical coupled test device of alternating temperature integrating sphere according to claim 2, which is characterized in that the solid-like grade
It is powder or film sample in the temperature-control units.
4. the optical coupled test device of alternating temperature integrating sphere according to claim 3, which is characterized in that the fiber lengths model
Enclose is 1 to 5m.
5. the optical coupled test device of alternating temperature integrating sphere according to claim 4, which is characterized in that the spectrometer is purple
Outside, any one in visible, near-infrared fluorescent spectrometer or absorption spectrometer.
6. the optical coupled test device of alternating temperature integrating sphere according to claim 5, which is characterized in that the light to be measured
It is diffusing reflection spectrum and fluorescence absolute quantum yield to learn parameter.
7. the optical coupled test device of alternating temperature integrating sphere according to claim 6, which is characterized in that the temperature-control units are
The microstat devices of Oxford company.
8. the optical coupled test device of alternating temperature integrating sphere according to claim 7, which is characterized in that the spectrometer is love
The FLS980 of Ding Bao companies.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112014319A (en) * | 2020-08-26 | 2020-12-01 | 中山大学新华学院 | Detector for dynamically detecting influence of illumination on ultraviolet absorbance of substance |
CN113218629A (en) * | 2021-04-26 | 2021-08-06 | 爱丁堡仪器有限公司 | Variable-temperature electroluminescent quantum efficiency testing system |
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CN102269701A (en) * | 2011-07-04 | 2011-12-07 | 中国科学院化学研究所 | Surface albedo measurement system for laboratory |
CN102830064A (en) * | 2012-08-20 | 2012-12-19 | 中国科学院宁波材料技术与工程研究所 | Middle/high-temperature infrared emissivity testing device |
CN105403548A (en) * | 2015-12-08 | 2016-03-16 | 厦门稀土材料研究所 | Temperature variable spectral measurement device |
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2018
- 2018-06-04 CN CN201810565487.6A patent/CN108645803A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102269701A (en) * | 2011-07-04 | 2011-12-07 | 中国科学院化学研究所 | Surface albedo measurement system for laboratory |
CN102830064A (en) * | 2012-08-20 | 2012-12-19 | 中国科学院宁波材料技术与工程研究所 | Middle/high-temperature infrared emissivity testing device |
CN105403548A (en) * | 2015-12-08 | 2016-03-16 | 厦门稀土材料研究所 | Temperature variable spectral measurement device |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112014319A (en) * | 2020-08-26 | 2020-12-01 | 中山大学新华学院 | Detector for dynamically detecting influence of illumination on ultraviolet absorbance of substance |
CN112014319B (en) * | 2020-08-26 | 2021-11-23 | 中山大学新华学院 | Detector for dynamically detecting influence of illumination on ultraviolet absorbance of substance |
CN113218629A (en) * | 2021-04-26 | 2021-08-06 | 爱丁堡仪器有限公司 | Variable-temperature electroluminescent quantum efficiency testing system |
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Application publication date: 20181012 |