CN103411703A - Non-contact-type temperature measurement method based on cadmium telluride quantum dot photoluminescence - Google Patents
Non-contact-type temperature measurement method based on cadmium telluride quantum dot photoluminescence Download PDFInfo
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Abstract
Disclosed is a non-contact-type temperature measurement method based on cadmium telluride quantum dot photoluminescence. The method comprises the steps of assembly of a spectral imaging system, synthesis of semiconductor CdTe quantum dots, sample preparation and temperature calibration. In the spectral imaging system, the peak wavelengths, the luminous intensity and the half-peak breadths of known quantum dot spectrums at different temperatures can be obtained by adjusting the set temperature of a heating platform of a microscope, and three temperature calibration curves of peak wavelength-temperature, and luminous intensity-temperature and half-peak breadth-temperature are obtained. Microelectrode joule heat, micro-fluid heat conduction and the cell body temperature are measured, the problem that a traditional temperature measurement technology is limited by the spatial scale is solved, the operation is easy, convenient and feasible, the temperature measurement position is only required to be accurately positioned, the microelectrode temperature, the micro-channel fluid temperature, the cell body temperature and the like in the scientific research can be accurately and conveniently measured.
Description
Technical field
The invention belongs to micro/nano-scale thermometry field, be specifically related to a kind of contactless temperature-measuring method based on the cadmium telluride quantum dot photoluminescence.
Background technology
The temperature survey of research, fluid channel fluid and the biomedical sector active somatic cell of microelectronics research field integrated circuit temperature of key part characteristic is the challenge difficult problem that current engineering staff and researchers run into.The compound temperature variant relation of the band gap width of quanta point material and charge carrier is enlightened our another kind of novel temperature measurement technology.Traditional thermometric instruments comprises various temperature sensors, thermometer and thermal infrared imager etc., and they have specific application scenario and sensitivity requirement.For the temperature survey of the measurement of integrated circuit temperature of key part and biomedical sector cell body in microelectronic component, traditional thermometric instruments can't meet the demands at all, and a kind of proposition of contactless spectrum thermometry is necessary.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of contactless temperature-measuring method based on the cadmium telluride quantum dot photoluminescence, can realize the Measurement accuracy of micro-nano structure, microfluid and cell body temperature.
In order to achieve the above object, the technical scheme taked of the present invention is:
A kind of contactless temperature-measuring method based on the cadmium telluride quantum dot photoluminescence comprises the following steps:
The first step, the composition of spectrum imaging system is installed, directly over microcobjective 4, be mounted with microscope warm table 3, sample 1 is fixed on above microscope warm table 3, the real time temperature of sample 1 is recorded by thermopair 2, the ultraviolet light that mercury lamp 9 is launched obtains by excitation light filter 8 exciting light 6 that wavelength is 340～390nm, exciting light 6 focuses on sample 1 by microcobjective 4 after dichroic beam splitter 7 reflections, the utilizing emitted light 5 of sample 1 sees through dichroic beam splitter 7 and utilizing emitted light filter 10 successively after microcobjective 4 is received light, by condenser 11, focus on and reflex to image raster spectrometer 13 by plane mirror 12, image raster spectrometer optical signal transmission is the most at last done subsequent treatment to CCD camera 14,
Second step, synthetic and sample 1 preparation of semiconductor cadmium telluride (CdTe) quantum dot, the synthetic employing of semiconductor CdTe quantum dot aqueous reaction synthetic method from bottom to top, adopt cadmium acetate hydrate (Cd (CH
3COO)
22H
2O) aqueous solution is as cadmium source (Cd
2+), potassium tellurite (K
2TeO
3) aqueous solution is as tellurium source (Te
4+), both using after each 50ml of volume ratio of 1:1 mixes and add mercaptoacetic acid (TGA) 18ul as stabilizing agent, add sodium borohydride (NaBH
4) 80mg is as reductive agent, the final precursor solution that forms, by controlling the condensing reflux reaction time 4h of precursor solution, obtaining photoluminescence is green CdTe quantum dot, and the preparation of sample 1, the preparation of sample 1 select microslide as backing material, cleaning is done on its surface, at the surperficial spin coating organic polymer of transparent rigid substrate 15 silica gel material PDMS16, the CdTe quantum dot colloidal solution 19 of getting 25uL concentration and be 0.2mmol/L drops to PDMS16 layer central authorities, heats 10min under 80 ℃;
The 3rd step, temperature calibration, in spectrum imaging system, by the design temperature of regulating microscope warm table 3, can obtain peak wavelength, luminous intensity and the half-peak breadth of quantum dot spectrum under known different temperatures, photoluminescence spectra under different temperatures is carried out to Gauss curve fitting, extract peak wavelength, luminous intensity and half-peak breadth signal, the signal of extraction and temperature is corresponding and do linear fit one by one, finally obtain peak wavelength-temperature, luminous intensity-temperature and the large temperature calibration curve of half-peak breadth-temperature three;
The 4th step, measure microelectrode Joule heat, microfluid heat transfer and cell body temperature,
1) preparation of microelectrode, adopt the transparent rigid substrate 15 of surface insulation as substrate, on its surface, do cleaning, spin coating a layer thickness is the negative pattern that EPG533 photoresist 17 photoetching processes of 300nm realize microelectrode, adopting afterwards sputtering technology sputter a layer thickness is the aluminium of 200nm, finally by Lift-off technique, realize the graphic structure of microelectrode 18, by 10uL concentration, be that 0.2mmol/L CdTe quantum dot colloidal solution 19 is added drop-wise to microelectrode 18 middle parts, the electrode two ends power up the generation Joule heat;
2) preparation of fluid channel, adopt transparent rigid substrate 15 to be substrate, the organic polymer silica gel material PDMS16 that is 100um in surperficial spin coating a layer thickness after cleaning, by soft impression method, realize the fluid channel structure on PDMS, the wide 550um of fluid channel structure, dark 50um, 50uL concentration is that 0.2mmol/L CdTe quantum dot colloidal solution 19 is dispersed in fluid 21 in advance, by injecting method, fluid is introduced in fluid channel;
3) cell body is engulfed the process of quantum dot, tiling one layer of cells nutrient culture media 22 on transparent rigid substrate 15, the CdTe quantum dot that is 0.68mg/mL by 150uL concentration is distributed in cell culture medium 22, after adding cell 23, through the cultivation of 24h, the endocytosis by cell makes quantum dot dispersed at cell body.
Described image raster spectrometer 13 slit width 200um.
Described 14 time shutter of CCD camera are 1s.
Described thermometric object is microsystem, and base material is transparent, and temperature-measuring range is room temperature to 300 ℃.
The present invention takes full advantage of the susceptibility of the spectral information of semiconductor-quantum-point to temperature, has solved the problem that traditional thermometry is subjected to the space scale limitation.After quantum dot was heated, the band gap of its material reduced to cause the emission spectrum red shift, was heated and can causes the non-radiative composite strengthening of charge carrier, caused luminous intensity to reduce, and the variation of spectrum can be used for doing the temperature indication.Easy to operation, only need accurately location temperature measurement location.To in research work, carrying out accurately as the temperature of temperature, fluid channel fluid and the cell body of microelectrode and measure easily.
The accompanying drawing explanation
Fig. 1 is the front view of spectrum investigating system.
Fig. 2-1 is for spin coating PDMS in substrate and the vertical view after dripping CdTe quantum dot colloidal solution; Fig. 2-2 are for spin coating PDMS in substrate and the front view after dripping CdTe quantum dot colloidal solution.
Fig. 3-1 is the vertical view after the spin coating photoresist in substrate; Fig. 3-2 are the front view after the spin coating photoresist in substrate; 3-3 be photoetching, sputtered aluminum layer and peel off after the electrode vertical view; Fig. 3-4 for photoetching, sputtered aluminum layer and peel off after the electrode front view; Fig. 3-5 add the vertical view after CdTe quantum dot colloidal solution for electrode central authorities; Fig. 3-6 add the vertical view after CdTe quantum dot colloidal solution for electrode central authorities.
Fig. 4-1 is the vertical view after spin coating PDMS in substrate; Fig. 4-2 are the front view after spin coating PDMS in substrate; Fig. 4-3 are the fluid channel structure vertical view after soft impression; Fig. 4-4 are the fluid channel structural front view after soft impression; Fig. 4-5 are for injecting fluid channel structure vertical view after the microfluid be dispersed with the CdTe quantum dot.
The vertical view after the cell culture medium of CdTe quantum dot is contained for tiling one deck in Fig. 5-1; The front view after the cell culture medium of CdTe quantum dot is contained for tiling one deck in Fig. 5-2; Fig. 5-3 add the vertical view after cell is cultivated a period of time for cell culture medium; Fig. 5-4 add the front view after cell is cultivated a period of time for cell culture medium.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in detail.
A kind of contactless temperature-measuring method based on the cadmium telluride quantum dot photoluminescence comprises the following steps:
The first step, the composition of spectrum imaging system is installed, with reference to Fig. 1, directly over microcobjective 4, be mounted with microscope warm table 3, sample 1 is fixed on above microscope warm table 3, the real time temperature of sample 1 is recorded by thermopair 2, the ultraviolet light that mercury lamp 9 is launched obtains by excitation light filter 8 exciting light 6 that wavelength is 340～390nm, exciting light 6 focuses on sample 1 by microcobjective 4 after dichroic beam splitter 7 reflections, the utilizing emitted light 5 of sample 1 sees through dichroic beam splitter 7 and utilizing emitted light filter 10 successively after microcobjective 4 is received light, by condenser 11, focus on and reflex to image raster spectrometer 13 by plane mirror 12, image raster spectrometer optical signal transmission is the most at last done subsequent treatment to CCD camera 14,
Second step, synthetic and sample 1 preparation of semiconductor cadmium telluride (CdTe) quantum dot, the synthetic employing of semiconductor CdTe quantum dot aqueous reaction synthetic method from bottom to top, adopt cadmium acetate hydrate (Cd (CH
3COO)
22H
2O) aqueous solution is as cadmium source (Cd
2+), potassium tellurite (K
2TeO
3) aqueous solution is as tellurium source (Te
4+), both using after each 50ml of volume ratio of 1:1 mixes and add mercaptoacetic acid (TGA) 18ul as stabilizing agent, add sodium borohydride (NaBH
4) 80mg is as reductive agent, the final precursor solution that forms, by controlling the condensing reflux reaction time 4h of precursor solution, obtaining photoluminescence is green CdTe quantum dot, the preparation of sample 1, with reference to 2-1, Fig. 2-2, the preparation of sample 1 selects microslide as backing material, cleaning is done on its surface, at the surperficial spin coating organic polymer of transparent rigid substrate 15 silica gel material PDMS16, the CdTe quantum dot colloidal solution 19 of getting 25uL concentration and be 0.2mmol/L drops to PDMS16 layer central authorities, heats 10min under 80 ℃;
The 3rd step, temperature calibration, with reference to Fig. 1, in spectrum imaging system, by the design temperature of regulating microscope warm table 3, can obtain peak wavelength, luminous intensity and the half-peak breadth of quantum dot spectrum under known different temperatures, photoluminescence spectra under different temperatures is carried out to Gauss curve fitting, extract peak wavelength, luminous intensity and half-peak breadth signal, the signal of extraction and temperature is corresponding and do linear fit one by one, finally obtain peak wavelength-temperature, luminous intensity-temperature and the large temperature calibration curve of half-peak breadth-temperature three;
The 4th step, measure microelectrode Joule heat, microfluid heat transfer and cell body temperature,
1) preparation of microelectrode, with reference to Fig. 3-1, Fig. 3-2, Fig. 3-3, Fig. 3-4, Fig. 3-5 and Fig. 3-6, adopt the transparent rigid substrate 15 of surface insulation as substrate, on its surface, do cleaning, spin coating a layer thickness is the negative pattern that EPG533 photoresist 17 photoetching processes of 300nm realize microelectrode, adopting afterwards sputtering technology sputter a layer thickness is the aluminium of 200nm, finally by Lift-off technique, realize the graphic structure of microelectrode 18, by 10uL concentration, be that 0.2mmol/L CdTe quantum dot colloidal solution 19 is added drop-wise to microelectrode 18 middle parts, the electrode two ends power up the generation Joule heat,
2) preparation of fluid channel, with reference to Fig. 4-1, Fig. 4-2, Fig. 4-3, Fig. 4-4 and Fig. 4-5, adopt transparent rigid substrate 15 to be substrate, the organic polymer silica gel material PDMS16 that is 100um in surperficial spin coating a layer thickness after cleaning, by soft impression method, realize the fluid channel structure on PDMS, the wide 550um of fluid channel structure, dark 50um, 50uL concentration is that 0.2mmol/L CdTe quantum dot colloidal solution 19 is dispersed in fluid 21 in advance, by injecting method, fluid is introduced in fluid channel;
3) cell body is engulfed the process of quantum dot, with reference to Fig. 5-1, Fig. 5-2, Fig. 5-3, Fig. 5-4, tiling one layer of cells nutrient culture media 22 on transparent rigid substrate 15, the CdTe quantum dot that is 0.68mg/mL by 150uL concentration is distributed in cell culture medium 22, after adding cell 23, through the cultivation of 24h, the endocytosis by cell makes quantum dot dispersed at cell body.
Described image raster spectrometer 13 slit width 200um.
Described 14 time shutter of CCD camera are 1s.
Described thermometric object is microsystem, and base material is transparent, and temperature-measuring range is room temperature to 300 ℃.
The present invention takes full advantage of the energy gap temperature influence of semiconductor-quantum-point and the regularity of the photoluminescence spectra that causes changes, and has solved the problem that traditional thermometry is subjected to the space scale limitation.After quantum dot was heated, the band gap of its material reduced to cause the emission spectrum red shift, was heated and can causes the non-radiative composite strengthening of charge carrier, caused luminous intensity to reduce, and the variation of spectrum can be used for doing the temperature indication.Easy to operation, only need accurately location temperature measurement location.To in research work, carrying out accurately as the temperature of temperature, fluid channel fluid and the cell body of microelectrode and measure easily.
Claims (4)
1. the contactless temperature-measuring method based on the cadmium telluride quantum dot photoluminescence, is characterized in that, comprises the following steps:
The first step, the composition of spectrum imaging system is installed, directly over microcobjective (4), be mounted with microscope warm table (3), sample (1) is fixed on above microscope warm table (3), the real time temperature of sample (1) is recorded by thermopair (2), the ultraviolet light that mercury lamp (9) is launched obtains the exciting light that wavelength is 340～390nm (6) by excitation light filter (8), exciting light (6) focuses on sample (1) by microcobjective (4) after dichroic beam splitter (7) reflection, the utilizing emitted light (5) of sample (1) sees through dichroic beam splitter (7) and utilizing emitted light filter (10) successively after microcobjective (4) is received light, by condenser (11), focus on and reflex to image raster spectrometer (13) by plane mirror (12), image raster spectrometer optical signal transmission is the most at last done subsequent treatment to CCD camera (14),
Second step, synthetic and sample 1 preparation of semiconductor cadmium telluride (CdTe) quantum dot, the synthetic employing of semiconductor CdTe quantum dot aqueous reaction synthetic method from bottom to top, adopt cadmium acetate hydrate (Cd (CH
3COO)
22H
2O) aqueous solution is as cadmium source (Cd
2+), potassium tellurite (K
2TeO
3) aqueous solution is as tellurium source (Te
4+), both using after each 50ml of volume ratio of 1:1 mixes and add mercaptoacetic acid (TGA) 18ul as stabilizing agent, add sodium borohydride (NaBH
4) 80mg is as reductive agent, the final precursor solution that forms, by controlling the condensing reflux reaction time 4h of precursor solution, obtaining photoluminescence is green CdTe quantum dot, the preparation of sample (1), the preparation of sample (1) selects microslide as backing material, cleaning is done on its surface, at the surperficial spin coating organic polymer of transparent rigid substrate (15) silica gel material PDMS(16), the CdTe quantum dot colloidal solution (19) of getting 25uL concentration and be 0.2mmol/L drops to PDMS(16) layer central authorities, heat 10min under 80 ℃;
The 3rd step, temperature calibration, in spectrum imaging system, by the design temperature of regulating microscope warm table (3), can obtain peak wavelength, luminous intensity and the half-peak breadth of quantum dot spectrum under known different temperatures, photoluminescence spectra under different temperatures is carried out to Gauss curve fitting, extract peak wavelength, luminous intensity and half-peak breadth signal, the signal of extraction and temperature is corresponding and do linear fit one by one, finally obtain peak wavelength-temperature, luminous intensity-temperature and the large temperature calibration curve of half-peak breadth-temperature three;
The 4th step, measure microelectrode Joule heat, microfluid heat transfer and cell body temperature,
1) preparation of microelectrode, adopt the transparent rigid substrate (15) of surface insulation as substrate, on its surface, do cleaning, spin coating a layer thickness is the negative pattern that EPG533 photoresist (17) photoetching process of 300nm realizes microelectrode, adopting afterwards sputtering technology sputter a layer thickness is the aluminium of 200nm, finally by Lift-off technique, realize the graphic structure of microelectrode (18), by 10uL concentration, be that 0.2mmol/L CdTe quantum dot colloidal solution (19) is added drop-wise to microelectrode (18) middle part, the electrode two ends power up the generation Joule heat;
2) preparation of fluid channel, adopt transparent rigid substrate (15) to be substrate, the organic polymer silica gel material PDMS(16 that is 100um in surperficial spin coating a layer thickness after cleaning), by soft impression method, realize the fluid channel structure on PDMS, the wide 550um of fluid channel structure, dark 50um, 50uL concentration is that 0.2mmol/L CdTe quantum dot colloidal solution (19) is dispersed in fluid (21) in advance, by injecting method, fluid is introduced in fluid channel;
3) cell body is engulfed the process of quantum dot, at the upper tiling of transparent rigid substrate (15) one layer of cells nutrient culture media (22), the CdTe quantum dot that is 0.68mg/mL by 150uL concentration is distributed in cell culture medium (22), after adding cell (23), through the cultivation of 24h, the endocytosis by cell makes quantum dot dispersed at cell body.
2. a kind of contactless temperature-measuring method based on the cadmium telluride quantum dot photoluminescence according to claim 1, is characterized in that: described image raster spectrometer (13) slit width 200um.
3. a kind of contactless temperature-measuring method based on the cadmium telluride quantum dot photoluminescence according to claim 1, it is characterized in that: CCD camera (14) time shutter is 1s.
4. a kind of contactless temperature-measuring method based on the cadmium telluride quantum dot photoluminescence according to claim 1, it is characterized in that: described thermometric object is microsystem, and base material is transparent, and temperature-measuring range is room temperature to 300 ℃.
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| CN106525273B (en) * | 2016-11-24 | 2018-10-30 | 哈尔滨工业大学 | cell temperature sensor based on quantum dot film and preparation method thereof |
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| CN107525604A (en) * | 2017-08-21 | 2017-12-29 | 西安交通大学 | The rolling bearing multiple spot Warm status monitoring method of different wave length quantum point sensor |
| CN109974885A (en) * | 2019-04-28 | 2019-07-05 | 西安交通大学 | A kind of surface temperature field measuring method based on CdTe thin film |
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| CN112683417A (en) * | 2020-12-28 | 2021-04-20 | 西安交通大学 | Measuring method for temperature change of organelles |
| CN112773304A (en) * | 2020-12-28 | 2021-05-11 | 西安交通大学 | Measurable capsule scope of temperature |
| CN112683417B (en) * | 2020-12-28 | 2021-10-22 | 西安交通大学 | Measuring method for temperature change of organelles |
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