CN105348550A - Preparation method of PDMS film with thermosensitivity - Google Patents

Preparation method of PDMS film with thermosensitivity Download PDF

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CN105348550A
CN105348550A CN201510809938.2A CN201510809938A CN105348550A CN 105348550 A CN105348550 A CN 105348550A CN 201510809938 A CN201510809938 A CN 201510809938A CN 105348550 A CN105348550 A CN 105348550A
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quantum dot
preparation
temperature
pdms film
pdms
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CN105348550B (en
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江新兵
李本强
于伟
杨欢
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Xian Jiaotong University
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Xian Jiaotong University
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Abstract

A preparation method of a PDMS film with thermosensitivity comprises the following steps: carrying out rotary evaporative concentration on aqueous-phase cadmium telluride quantum dots prepared by a hydrothermal method, carrying out purification treatment by settling with isopropanol, dispersing the purified product in anhydrous ethanol, uniformly dispersing the cadmium telluride quantum dots in a PDMS prepolymer through the affinity interaction between the PDMS prepolymer and aqueous-phase quantum dots, mixing and curing by adding a curing agent, so as to obtain optically transparent PDMS film with thermosensitivity. The raw materials used in the invention are easily available, required experimental equipment is simple, and the technological process is easy to master. By the preparation method, a thermosensitive PDMS film having uniform euphotic layer and with good film-forming ability can be prepared.

Description

A kind of preparation method with the PDMS film of temperature-sensing property
Technical field
The invention belongs to the technical field of temperature measurement of flexibility, particularly a kind of preparation method with the PDMS film of temperature-sensing property.
Background technology
In mechanical engineering field, temperature is the important measurement index that an equipment runs, and in cytobiology, temperature is also one and distinguishes sick cell and a Normocellular important instruction standard, on the integrated, too high temperature shows unicircuit operation troubles.There is the film of temperature-sensing property, be with a wide range of applications in mechanical engineering, biological medicine and unicircuit etc.PDMS film doped with quantum dot has temperature-sensing property, can as above every field temperature sensing probe, the thermal information monitoring testee that can be in good time.At present, by the method for Layer-by-Layer, the temperature-sensing property quantum dot film of film-like can be prepared, and temperature sensitive film prepared by this method due to its expose in atmosphere, be easy to oxidation light stability poor, be easy to photobleaching to occur thus reduce its temperature-sensing property, and Layer-by-Layer method prepares temperature sensitive film process complexity, expends time in.
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 preparation method with the PDMS film of temperature-sensing property, prepare and have temperature sensitive probe function and the good PDMS film of film-forming properties, equipment is simple, technological process is easy to grasp, and expends time in short.
In order to achieve the above object, inventing the technical scheme taked is:
There is a preparation method for the PDMS film of temperature-sensing property, comprise the following steps:
The first step, the preparation of temperature sensitive cadmium telluride quantum dot: get 46mL ultrapure water and be placed in three mouthfuls of round-bottomed flasks, nitrogen deoxygenation 30min is carried out by bubbling method, then the cadmium acetate aqueous solution of 0.04mol/L, the 0.01mol/L potassium tellurite aqueous solution are added 4mL respectively according to the ratio of volume ratio 1:1, add the sodium borohydride of the Trisodium Citrate of 400mg, the dimercaptosuccinic acid of 100mg and 50mg subsequently successively, final composition precursor solution, condensing reflux reaction under 90 DEG C ~ 100 DEG C oil baths, by controlling reaction times 9h, obtain temperature sensitive cadmium telluride quantum dot;
Second step, the purifying of cadmium telluride quantum dot and redispersion: the cadmium telluride quantum dot the first step prepared carries out rotary evaporation, until volume concentration to original volume 1/5 time, add Virahol wherein, wherein concentrated volume ratio between quantum dot and Virahol is 1:3, then carry out eccentric cleaning, quantum dot is redispersed in isopyknic dehydrated alcohol the most at last, obtains the quantum dot ethanolic soln after purifying;
3rd step, the preparation of temperature sensitive PDMS film: PDMS performed polymer is mixed according to the ratio of 4g:1mL with the quantum dot ethanolic soln after purifying, Keep agitation 20min, add solidifying agent subsequently, wherein the mass ratio of performed polymer and solidifying agent is 10:1, then continue to stir 8min, mixture is placed in vacuum glove box and carries out vacuum filtration removal bubble 20min, getting mixture is coated with on the slide glass through clean, is then placed in baking oven to be cured namely to obtain temperature sensitive PDMS film.
The rotating speed of the rotary evaporation in described second step is 200 revs/min, and temperature is 70 DEG C.
Solidifying agent in described 3rd step is Essil296 catalyzer.
In described 3rd step, the solidification value of baking oven is 70 DEG C, keeps 30min.
Advantage of the present invention: raw material used in the present invention is conveniently easy to get, required experimental installation is simple, and technological process is easy to grasp, expend time in short, can prepare film-forming properties good, the PDMS film of what light stability was good have temperature-sensing property, can be widely used in various complex working condition field.
Accompanying drawing explanation
Fig. 1 is the fluorescence spectrum of the quantum dot that embodiment one obtains.
Fig. 2 is the fluorescence spectrum of the quantum dot that embodiment two obtains.
Fig. 3 is the fluorescence spectrum of the quantum dot that embodiment three obtains.
Fig. 4 be embodiment one, embodiment two, embodiment three under white light illumination, the digital photograph of the temperature sensitive PDMS film had cured.
Fig. 5 be embodiment one, embodiment two, embodiment three under UV-irradiation, the digital photograph of the temperature sensitive PDMS film had cured.
Fig. 6 be the temperature sensitive PDMS film of embodiment one at different temperature, the distribution of fluorescence spectrum.
Fig. 7 is the synthermal corresponding relation of peak wavelength of the fluorescence spectrum that embodiment one extracts, and wherein point diagram is experimental data, and solid line is the straight line of matching.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment one:
There is a preparation method for the PDMS film of temperature-sensing property, comprise the following steps:
The first step, the preparation of temperature sensitive cadmium telluride quantum dot: get 46mL ultrapure water and be placed in three mouthfuls of round-bottomed flasks, nitrogen deoxygenation 30min is carried out by bubbling method, then the cadmium acetate aqueous solution of 0.04mol/L, the 0.01mol/L potassium tellurite aqueous solution are added 4mL respectively according to the ratio of volume ratio 1:1, add the sodium borohydride of the Trisodium Citrate of 400mg, the dimercaptosuccinic acid of 100mg and 50mg subsequently successively, final composition precursor solution, condensing reflux reaction under 90 DEG C of oil baths, by controlling reaction times 9h, obtain temperature sensitive cadmium telluride quantum dot;
Second step, the purifying of cadmium telluride quantum dot and redispersion: the cadmium telluride quantum dot the first step prepared carries out rotary evaporation, the rotating speed of rotary evaporation is 200 revs/min, temperature is 70 DEG C, until volume concentration to original volume 1/5 time, add Virahol wherein, wherein concentrated volume ratio between quantum dot and Virahol is 1:3, then carry out eccentric cleaning, quantum dot is redispersed in isopyknic dehydrated alcohol the most at last, obtains the quantum dot ethanolic soln after purifying;
3rd step, the preparation of temperature sensitive PDMS film: PDMS performed polymer is mixed according to the ratio of 4g:1mL with the quantum dot ethanolic soln after purifying, Keep agitation 20min, add solidifying agent subsequently, wherein the mass ratio of performed polymer and solidifying agent is 10:1, described solidifying agent is Essil296 catalyzer, then continue to stir 8min, mixture is placed in vacuum glove box and carries out vacuum filtration removal bubble 20min, get mixture and hang Tu on the slide glass through clean, then be placed in baking oven to be cured and obtain temperature sensitive PDMS film, the solidification value of baking oven is 70 DEG C, keep 30min.
The fluorescence emission spectrum of temperature sensitive quantum dot prepared by the present embodiment as shown in Figure 1, obtained cadmium telluride quantum dot is doped to after in PDMS, outstanding Tu is cured on slide glass, as the slide glass on Fig. 4 left side under white light, under ultraviolet light, the photo obtained, as the slide glass on the left of Fig. 5, can see and obtain more outstanding Tu effect, and fluorescent emission intensity is very stable.Temperature calibration has been carried out to it, obtain the temperature spectra curve of Fig. 6, spectrum peak data are wherein extracted and contrasts with temperature, obtain the fitted figure of Fig. 7, as we can see from the figure, within the scope of measured temperature, spectrum peak and temperature are certain linear relationship, sensitivity is good, spectrum-stable.
Embodiment two:
There is a preparation method for the PDMS film of temperature-sensing property, comprise the following steps:
The first step, the preparation of temperature sensitive cadmium telluride quantum dot: get 46mL ultrapure water and be placed in three mouthfuls of round-bottomed flasks, nitrogen deoxygenation 30min is carried out by bubbling method, then the cadmium acetate aqueous solution of 0.04mol/L, the 0.01mol/L potassium tellurite aqueous solution are added 4mL respectively according to the ratio of volume ratio 1:1, add the sodium borohydride of the Trisodium Citrate of 400mg, the dimercaptosuccinic acid of 100mg and 50mg subsequently successively, final composition precursor solution, condensing reflux reaction under 95 DEG C of oil baths, by controlling reaction times 9h, obtain temperature sensitive cadmium telluride quantum dot;
Second step, the purifying of cadmium telluride quantum dot and redispersion: the cadmium telluride quantum dot the first step prepared carries out rotary evaporation, the rotating speed of rotary evaporation is 200 revs/min, temperature is 70 DEG C, until volume concentration to original volume 1/5 time, add Virahol wherein, wherein concentrated volume ratio between quantum dot and Virahol is 1:3, then carry out eccentric cleaning, quantum dot is redispersed in isopyknic dehydrated alcohol the most at last, obtains the quantum dot ethanolic soln after purifying;
3rd step, the preparation of temperature sensitive PDMS film: PDMS performed polymer is mixed according to the ratio of 4g:1mL with the quantum dot ethanolic soln after purifying, Keep agitation 20min, add solidifying agent subsequently, wherein the mass ratio of performed polymer and solidifying agent is 10:1, described solidifying agent is Essil296 catalyzer, then continue to stir 8min, mixture is placed in vacuum glove box and carries out vacuum filtration removal bubble 20min, get mixture and hang Tu on the slide glass through clean, then be placed in baking oven to be cured and obtain temperature sensitive PDMS film, the solidification value of baking oven is 70 DEG C, keep 30min.
As shown in Figure 2, relative and embodiment one, the emmission spectrum of quantum dot there occurs certain red shift to the fluorescence emission spectrum of temperature sensitive quantum dot prepared by the present embodiment.Obtained cadmium telluride quantum dot is doped to after in PDMS, outstanding Tu is cured on slide glass, as the slide glass in the middle of Fig. 4 under white light, under ultraviolet light, the photo obtained is as the slide glass in the middle of Fig. 5, can see and obtain more outstanding Tu effect, and fluorescent emission intensity is very stable.
Embodiment three:
There is a preparation method for the PDMS film of temperature-sensing property, comprise the following steps:
The first step, the preparation of temperature sensitive cadmium telluride quantum dot: get 46mL ultrapure water and be placed in three mouthfuls of round-bottomed flasks, nitrogen deoxygenation 30min is carried out by bubbling method, then the cadmium acetate aqueous solution of 0.04mol/L, the 0.01mol/L potassium tellurite aqueous solution are added 4mL respectively according to the ratio of volume ratio 1:1, add the sodium borohydride of the Trisodium Citrate of 400mg, the dimercaptosuccinic acid of 100mg and 50mg subsequently successively, final composition precursor solution, condensing reflux reaction under 100 DEG C of oil baths, by controlling reaction times 9h, obtain temperature sensitive cadmium telluride quantum dot;
Second step, the purifying of cadmium telluride quantum dot and redispersion: the cadmium telluride quantum dot the first step prepared carries out rotary evaporation, the rotating speed of rotary evaporation is 200 revs/min, temperature is 70 DEG C, until volume concentration to original volume 1/5 time, add Virahol wherein, wherein concentrated volume ratio between quantum dot and Virahol is 1:3, then carry out eccentric cleaning, quantum dot is redispersed in isopyknic dehydrated alcohol the most at last, obtains the quantum dot ethanolic soln after purifying;
3rd step, the preparation of temperature sensitive PDMS film: PDMS performed polymer is mixed according to the ratio of 4g:1mL with the quantum dot ethanolic soln after purifying, Keep agitation 20min, add solidifying agent subsequently, wherein the mass ratio of performed polymer and solidifying agent is 10:1, described solidifying agent is Essil296 catalyzer, then continue to stir 8min, mixture is placed in vacuum glove box and carries out vacuum filtration removal bubble 20min, get mixture and hang Tu on the slide glass through clean, then be placed in baking oven to be cured and obtain temperature sensitive PDMS film, the solidification value of baking oven is 70 DEG C, keep 30min.
As shown in Figure 3, relatively and embodiment one and embodiment two, except the emmission spectrum generation red shift of quantum dot, the peak width at half height of quantum dot broadens the fluorescence emission spectrum of temperature sensitive quantum dot prepared by the present embodiment gradually.Obtained cadmium telluride quantum dot is doped to after in PDMS, outstanding Tu is cured on slide glass, as the slide glass on the right of Fig. 4 under white light, under ultraviolet light, the photo obtained is as the slide glass on the right of Fig. 5, can see and obtain more outstanding Tu effect, and fluorescent emission intensity is very stable, is suitable as the temperature sensitive probe of two dimension.
Fig. 1 is 90 DEG C time, obtain the emission wavelength of 541nm, and Fig. 2 is under 95 DEG C of conditions, obtains the emission wavelength of 557nm, and Fig. 3 is then the emission wavelength that can obtain 574nm at 100 DEG C.Under different temperature of reaction, the speed of growth difference to some extent of quantum dot, along with the rising of temperature of reaction, the nucleation rate of quantum dot is accelerated, and the speed of growth also accelerates.The red shift of Emission Spectrum Peals just means that the change of particle diameter is large.Comparison diagram 1, Fig. 2 and Fig. 3, the peak width at half height of quantum dot has also become greatly, and mainly the increase of particle diameter can make photon-phonon coupling effect strengthen.Be entrained in respectively in PDMS by the quantum dot of gained, then outstanding Tu is on slide glass, can see, all can obtain more uniform quantum dot PDMS film, and under the irradiation of excitation light source, obtain very stable emmission spectrum as shown in Figure 5.Fig. 6 relation that to be the corresponding relation figure between embodiment one cadmium telluride quantum dot PDMS film emmission spectrum and temperature, Fig. 7 be between embodiment one peak wavelength and temperature and data fitting figure, can see good temperature-sensing property from Fig. 7.

Claims (4)

1. there is a preparation method for the PDMS film of temperature-sensing property, it is characterized in that, comprise the following steps:
The first step, the preparation of temperature sensitive cadmium telluride quantum dot: get 46mL ultrapure water and be placed in three mouthfuls of round-bottomed flasks, nitrogen deoxygenation 30min is carried out by bubbling method, then the cadmium acetate aqueous solution of 0.04mol/L, the 0.01mol/L potassium tellurite aqueous solution are added 4mL respectively according to the ratio of volume ratio 1:1, add the sodium borohydride of the Trisodium Citrate of 400mg, the dimercaptosuccinic acid of 100mg and 50mg subsequently successively, final composition precursor solution, condensing reflux reaction under 90 DEG C ~ 100 DEG C oil baths, by controlling reaction times 9h, obtain temperature sensitive cadmium telluride quantum dot;
Second step, the purifying of cadmium telluride quantum dot and redispersion: the cadmium telluride quantum dot the first step prepared carries out rotary evaporation, until volume concentration to original volume 1/5 time, add Virahol wherein, wherein concentrated volume ratio between quantum dot and Virahol is 1:3, then carry out eccentric cleaning, quantum dot is redispersed in isopyknic dehydrated alcohol the most at last, obtains the quantum dot ethanolic soln after purifying;
3rd step, the preparation of temperature sensitive PDMS film: PDMS performed polymer is mixed according to the ratio of 4g:1mL with the quantum dot ethanolic soln after purifying, Keep agitation 20min, add solidifying agent subsequently, wherein the mass ratio of performed polymer and solidifying agent is 10:1, then continue to stir 8min, mixture is placed in vacuum glove box and carries out vacuum filtration removal bubble 20min, get mixture and hang Tu on the slide glass through clean, be then placed in baking oven to be cured and namely obtain temperature sensitive PDMS film.
2. a kind of preparation method with the PDMS film of temperature-sensing property according to claim 1, is characterized in that: the rotating speed of the rotary evaporation in described second step is 200 revs/min, and temperature is 70 DEG C.
3. a kind of preparation method with the PDMS film of temperature-sensing property according to claim 1, is characterized in that: the solidifying agent in described 3rd step is Essil296 catalyzer.
4. a kind of preparation method with the PDMS film of temperature-sensing property according to claim 1 or 3, is characterized in that: in described 3rd step, the solidification value of baking oven is 70 DEG C, keeps 30min.
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Cited By (7)

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CN106929000A (en) * 2017-03-31 2017-07-07 厦门大学 A kind of quantum dot dimethyl silicone polymer composite and preparation method thereof
CN108117870A (en) * 2017-12-18 2018-06-05 吉林师范大学 A kind of method for improving manganese and mixing perovskite quantum dot light emitting thermal stability
CN108250754A (en) * 2016-12-28 2018-07-06 东京应化工业株式会社 Containing silicone resin composition, containing silicone resin film, silica membrane, illuminated display element panel and luminous display unit
CN109738403A (en) * 2019-01-03 2019-05-10 必欧瀚生物技术(合肥)有限公司 A kind of preparation method of fluorescence standard card and fluorescence standard card fluorescent film
CN111171570A (en) * 2020-01-15 2020-05-19 常熟理工学院 Quick-response oil-sensitive deformable film and preparation method thereof
US11591441B2 (en) 2018-03-04 2023-02-28 Nanjing University Modified polysiloxane and application thereof

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CN103439027A (en) * 2013-08-08 2013-12-11 西安交通大学 High-speed bearing temperature measurement method based on quantum dot film photoluminescence
CN104926155A (en) * 2015-05-28 2015-09-23 福州大学 Preparation method for metal/organic shell core quantum dot-semiconductor quantum dot composite luminous film

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Publication number Priority date Publication date Assignee Title
CN105885419A (en) * 2016-04-29 2016-08-24 河南大学 Method for preparing cadmium compound quantum dot fluorescent thin film
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CN108250754A (en) * 2016-12-28 2018-07-06 东京应化工业株式会社 Containing silicone resin composition, containing silicone resin film, silica membrane, illuminated display element panel and luminous display unit
CN106929000A (en) * 2017-03-31 2017-07-07 厦门大学 A kind of quantum dot dimethyl silicone polymer composite and preparation method thereof
CN108117870A (en) * 2017-12-18 2018-06-05 吉林师范大学 A kind of method for improving manganese and mixing perovskite quantum dot light emitting thermal stability
CN108117870B (en) * 2017-12-18 2020-05-12 吉林师范大学 Method for improving photothermal stability of manganese-doped perovskite quantum dots
US11591441B2 (en) 2018-03-04 2023-02-28 Nanjing University Modified polysiloxane and application thereof
CN109738403A (en) * 2019-01-03 2019-05-10 必欧瀚生物技术(合肥)有限公司 A kind of preparation method of fluorescence standard card and fluorescence standard card fluorescent film
CN111171570A (en) * 2020-01-15 2020-05-19 常熟理工学院 Quick-response oil-sensitive deformable film and preparation method thereof
CN111171570B (en) * 2020-01-15 2021-08-31 常熟理工学院 Quick-response oil-sensitive deformable film and preparation method thereof

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