CN105348550B - A kind of preparation method of the PDMS film with temperature-sensing property - Google Patents
A kind of preparation method of the PDMS film with temperature-sensing property Download PDFInfo
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- CN105348550B CN105348550B CN201510809938.2A CN201510809938A CN105348550B CN 105348550 B CN105348550 B CN 105348550B CN 201510809938 A CN201510809938 A CN 201510809938A CN 105348550 B CN105348550 B CN 105348550B
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Abstract
A kind of preparation method of the PDMS film with temperature-sensing property, water phase cadmium telluride quantum dot prepared by hydro-thermal method is after rotary evaporation concentrates, after the purification process settled with isopropanol, it is dispersed in absolute ethyl alcohol, pass through PDMS performed polymers and the affinity interaction of aqueous phase quantum point, so that cadmium telluride quantum dot is uniformly dispersed in PDMS performed polymers, then by adding in curing agent, it carries out mixing cured, obtain PDMS film of the optical clear but also with temperature-sensing property, raw material used in the present invention is conveniently easy to get, required experimental facilities is simple, technical process is easy to grasp, it is uniform photic zone can be prepared, the good temperature sensitive PDMS film of film forming.
Description
Technical field
The invention belongs to the technical field of temperature measurement of flexibility, more particularly to a kind of PDMS film with temperature-sensing property
Preparation method.
Background technology
In mechanical engineering field, temperature is the important measurement index of an equipment operation, in cell biology, temperature
Also it is an important instruction standard for distinguishing sick cell and normal cell, on the integrated, excessively high temperature shows
Integrated circuit operation troubles.Film with temperature-sensing property, in mechanical engineering, biological medicine and integrated circuit etc. tool
Have wide practical use.There is temperature-sensing property doped with the PDMS film of quantum dot, more than every field temperature can be used as
Responsive probe can monitor the thermal information of testee in due course.At present, it with the method for Layer-by-Layer, can make
It is standby go out film-like temperature-sensing property quantum dot film, and temperature sensitive film prepared by this method due to its exposure in air,
It is poor to be easy to oxidation photostability, it is easy to photobleaching can occur so as to reduce its temperature-sensing property, and Layer-by-Layer
Method prepares temperature sensitive film process complexity, expends the time.
Invention content
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide a kind of PDMS with temperature-sensing property
The preparation method of film is prepared with temperature sensitive probe function and the good PDMS film of film forming, and equipment is simple, technique mistake
Journey is easy to grasp, and it is short to expend the time.
In order to achieve the above object, inventing the technical solution taken is：
A kind of preparation method of the PDMS film with temperature-sensing property, includes the following steps：
The first step, the preparation of temperature sensitive cadmium telluride quantum dot：46mL ultra-pure waters is taken to be placed in three neck round bottom flask, pass through bubbling
Method carry out nitrogen deoxygenation 30min, then by the cadmium acetate aqueous solution of 0.04mol/L, 0.01mol/L potassium tellurites aqueous solution according to
Volume ratio 1：1 ratio is separately added into 4mL, then sequentially add the sodium citrate of 400mg, the dimercaptosuccinic acid of 100mg and
The sodium borohydride of 50mg, finally forms precursor solution, and condensing reflux reacts under 90 DEG C~100 DEG C oil baths, anti-by controlling
9h between seasonable, obtains temperature sensitive cadmium telluride quantum dot；
Second step, the purifying of cadmium telluride quantum dot and redisperse：Cadmium telluride quantum dot prepared by the first step is rotated
Evaporation, when the 1/5 of volume concentration to original volume, adds in isopropanol thereto, wherein between concentration quantum dot and isopropanol
Volume ratio is 1:3, eccentric cleaning is then carried out, most quantum dot is redispersed in isometric absolute ethyl alcohol at last, is purified
Quantum dot ethanol solution afterwards；
Third walks, the preparation of temperature sensitive PDMS film：By PDMS performed polymers with quantum dot ethanol solution after purification according to 4g：
The ratio of 1mL is mixed, and persistently stirs 20min, then adds in curing agent, and the mass ratio of wherein performed polymer and curing agent is
10:1, stirring 8min is then proceeded to, mixture is placed in vacuum glove box be filtered by vacuum and removes bubble removing 20min, is taken mixed
It closes object to be coated on the glass slide Jing Guo cleaning treatment, then places it in baking oven and cured that obtain temperature sensitive PDMS thin
Film.
The rotating speed of rotary evaporation in the second step is 200 revs/min, and temperature is 70 DEG C.
Curing agent in the third step is 296 catalyst of Essil.
The solidification temperature of baking oven is 70 DEG C in the third step, keeps 30min.
Advantages of the present invention：Raw material used in the present invention is conveniently easy to get, and required experimental facilities is simple, and technical process is easy to
It grasps, it is short to expend the time, can prepare that film forming is good, the good PDMS film with temperature-sensing property of photostability can
It is widely used in various complex working condition fields.
Description of the drawings
Fig. 1 is the fluorescence spectrum for the quantum dot that embodiment one obtains.
Fig. 2 is the fluorescence spectrum for the quantum dot that embodiment two obtains.
Fig. 3 is the fluorescence spectrum for the quantum dot that embodiment three obtains.
Fig. 4 for embodiment one, embodiment two, embodiment three under white light illumination, the temperature sensitive PDMS film having been cured
Digital photograph.
Fig. 5 is embodiment one, embodiment two, embodiment three are under ultraviolet light, the temperature sensitive PDMS film having been cured
Digital photograph.
Fig. 6 be one temperature sensitive PDMS film of embodiment at different temperature, the distribution of fluorescence spectrum.
Fig. 7 is the synthermal correspondence of the peak wavelength for the fluorescence spectrum that embodiment one extracts, and wherein point diagram is real
Data are tested, solid line is the straight line of fitting.
Specific embodiment
With reference to embodiment, the present invention will be further described.
Embodiment one：
A kind of preparation method of the PDMS film with temperature-sensing property, includes the following steps：
The first step, the preparation of temperature sensitive cadmium telluride quantum dot：46mL ultra-pure waters is taken to be placed in three neck round bottom flask, pass through bubbling
Method carry out nitrogen deoxygenation 30min, then by the cadmium acetate aqueous solution of 0.04mol/L, 0.01mol/L potassium tellurites aqueous solution according to
Volume ratio 1：1 ratio is separately added into 4mL, then sequentially add the sodium citrate of 400mg, the dimercaptosuccinic acid of 100mg and
The sodium borohydride of 50mg, finally forms precursor solution, and condensing reflux reacts under 90 DEG C of oil baths, by controlling the reaction time
9h obtains temperature sensitive cadmium telluride quantum dot；
Second step, the purifying of cadmium telluride quantum dot and redisperse：Cadmium telluride quantum dot prepared by the first step is rotated
Evaporation, the rotating speed of rotary evaporation is 200 revs/min, and temperature is 70 DEG C, when the 1/5 of volume concentration to original volume, is added in thereto
Isopropanol, wherein the volume ratio between concentration quantum dot and isopropanol is 1:3, eccentric cleaning is then carried out, most quantum dot at last
It is redispersed in isometric absolute ethyl alcohol, obtains quantum dot ethanol solution after purification；
Third walks, the preparation of temperature sensitive PDMS film：By PDMS performed polymers with quantum dot ethanol solution after purification according to 4g：
The ratio of 1mL is mixed, and persistently stirs 20min, then adds in curing agent, and the mass ratio of wherein performed polymer and curing agent is
10:1, the curing agent be 296 catalyst of Essil, then proceed to stirring 8min, by mixture be placed in vacuum glove box into
Row vacuum filtration removes bubble removing 20min, and mixture is taken to hang Tu on the glass slide Jing Guo cleaning treatment, then places it in baking oven
In cured to obtain temperature sensitive PDMS film, the solidification temperature of baking oven is 70 DEG C, keep 30min.
The fluorescence emission spectrum of temperature sensitive quantum dot manufactured in the present embodiment is as shown in Figure 1, by cadmium telluride quantum dot obtained
After being doped in PDMS, outstanding Tu is cured on glass slide, such as the glass slide on Fig. 4 left sides under white light, under ultraviolet light, is obtained
The glass slide on the left of photo such as Fig. 5 arrived, it can be seen that obtained than more uniform outstanding Tu effect, and fluorescent emission intensity is very
Stablize.Temperature calibration has been carried out to it, has obtained the temperature spectra curve of Fig. 6, spectrum peak data therein have been extracted
It is compareed with temperature, has obtained the fitted figure of Fig. 7, from the figure, it can be seen that in the range of measured temperature, spectrum peak and temperature
Degree is in certain linear relationship, and sensitivity is good, spectrum-stable.
Embodiment two：
A kind of preparation method of the PDMS film with temperature-sensing property, includes the following steps：
The first step, the preparation of temperature sensitive cadmium telluride quantum dot：46mL ultra-pure waters is taken to be placed in three neck round bottom flask, pass through bubbling
Method carry out nitrogen deoxygenation 30min, then by the cadmium acetate aqueous solution of 0.04mol/L, 0.01mol/L potassium tellurites aqueous solution according to
Volume ratio 1：1 ratio is separately added into 4mL, then sequentially add the sodium citrate of 400mg, the dimercaptosuccinic acid of 100mg and
The sodium borohydride of 50mg, finally forms precursor solution, and condensing reflux reacts under 95 DEG C of oil baths, by controlling the reaction time
9h obtains temperature sensitive cadmium telluride quantum dot；
Second step, the purifying of cadmium telluride quantum dot and redisperse：Cadmium telluride quantum dot prepared by the first step is rotated
Evaporation, the rotating speed of rotary evaporation is 200 revs/min, and temperature is 70 DEG C, when the 1/5 of volume concentration to original volume, is added in thereto
Isopropanol, wherein the volume ratio between concentration quantum dot and isopropanol is 1:3, eccentric cleaning is then carried out, most quantum dot at last
It is redispersed in isometric absolute ethyl alcohol, obtains quantum dot ethanol solution after purification；
Third walks, the preparation of temperature sensitive PDMS film：By PDMS performed polymers with quantum dot ethanol solution after purification according to 4g：
The ratio of 1mL is mixed, and persistently stirs 20min, then adds in curing agent, and the mass ratio of wherein performed polymer and curing agent is
10:1, the curing agent be 296 catalyst of Essil, then proceed to stirring 8min, by mixture be placed in vacuum glove box into
Row vacuum filtration removes bubble removing 20min, and mixture is taken to hang Tu on the glass slide Jing Guo cleaning treatment, then places it in baking oven
In cured to obtain temperature sensitive PDMS film, the solidification temperature of baking oven is 70 DEG C, keep 30min.
The fluorescence emission spectrum of temperature sensitive quantum dot manufactured in the present embodiment is as shown in Fig. 2, opposite with embodiment one, quantum dot
Emission spectrum certain red shift has occurred.After cadmium telluride quantum dot obtained is doped in PDMS, Tu is hanged on glass slide
Cured, such as the glass slide among Fig. 4 under white light, under ultraviolet light, the obtained glass slide among photo such as Fig. 5 can
To see having obtained than more uniform outstanding Tu effect, and fluorescent emission intensity is very stable.
Embodiment three：
A kind of preparation method of the PDMS film with temperature-sensing property, includes the following steps：
The first step, the preparation of temperature sensitive cadmium telluride quantum dot：46mL ultra-pure waters is taken to be placed in three neck round bottom flask, pass through bubbling
Method carry out nitrogen deoxygenation 30min, then by the cadmium acetate aqueous solution of 0.04mol/L, 0.01mol/L potassium tellurites aqueous solution according to
Volume ratio 1：1 ratio is separately added into 4mL, then sequentially add the sodium citrate of 400mg, the dimercaptosuccinic acid of 100mg and
The sodium borohydride of 50mg, finally forms precursor solution, and condensing reflux reacts under 100 DEG C of oil baths, by controlling the reaction time
9h obtains temperature sensitive cadmium telluride quantum dot；
Second step, the purifying of cadmium telluride quantum dot and redisperse：Cadmium telluride quantum dot prepared by the first step is rotated
Evaporation, the rotating speed of rotary evaporation is 200 revs/min, and temperature is 70 DEG C, when the 1/5 of volume concentration to original volume, is added in thereto
Isopropanol, wherein the volume ratio between concentration quantum dot and isopropanol is 1:3, eccentric cleaning is then carried out, most quantum dot at last
It is redispersed in isometric absolute ethyl alcohol, obtains quantum dot ethanol solution after purification；
Third walks, the preparation of temperature sensitive PDMS film：By PDMS performed polymers with quantum dot ethanol solution after purification according to 4g：
The ratio of 1mL is mixed, and persistently stirs 20min, then adds in curing agent, and the mass ratio of wherein performed polymer and curing agent is
10:1, the curing agent be 296 catalyst of Essil, then proceed to stirring 8min, by mixture be placed in vacuum glove box into
Row vacuum filtration removes bubble removing 20min, and mixture is taken to hang Tu on the glass slide Jing Guo cleaning treatment, then places it in baking oven
In cured to obtain temperature sensitive PDMS film, the solidification temperature of baking oven is 70 DEG C, keep 30min.
The fluorescence emission spectrum of temperature sensitive quantum dot manufactured in the present embodiment is as shown in figure 3, opposite with embodiment one and implement
Example two, other than red shift occurs for the emission spectrum of quantum dot, the half-peak breadth of quantum dot gradually broadens.By cadmium telluride amount obtained
After son point is doped in PDMS, outstanding Tu is cured on glass slide, the glass slide under white light on the right of Fig. 4, in ultraviolet light
Under, the obtained glass slide on the right of photo such as Fig. 5, it can be seen that obtained than more uniform outstanding Tu effect, and fluorescent emission
Intensity is very stable, is suitable as the temperature sensitive probe of two dimension.
Fig. 1 is at 90 DEG C, has obtained the launch wavelength of 541nm, and Fig. 2 is under the conditions of 95 DEG C, has obtained 557nm's
Launch wavelength, Fig. 3 are then the launch wavelengths that 574nm can be obtained at 100 DEG C.Under different reaction temperatures, quantum dot
The speed of growth difference, with the raising of reaction temperature, the nucleation rate of quantum dot is accelerated, and the speed of growth also becomes faster.Transmitting
The red shift of spectrum peak means that becoming larger for grain size.Comparison diagram 1, Fig. 2 and Fig. 3, the half-peak breadth of quantum dot also become larger, mainly
Be grain size increase can cause photon-phonon coupling effect enhance.The quantum dot of gained is entrained in PDMS respectively, Tu is then hanged and exists
On glass slide, it can be seen that can obtain than more uniform quantum dot PDMS film, and under the irradiation of excitation light source, such as
Very stable emission spectrum has been obtained shown in Fig. 5.Fig. 6 is one cadmium telluride quantum dot PDMS film emission spectrum of embodiment and temperature
Between correspondence figure, Fig. 7 is relationship between one peak wavelength of embodiment and temperature and data fitted figure, from Fig. 7 i.e.
It can see good temperature-sensing property.
Claims (3)
1. a kind of preparation method of the PDMS film with temperature-sensing property, which is characterized in that include the following steps：
The first step, the preparation of temperature sensitive cadmium telluride quantum dot：46mL ultra-pure waters is taken to be placed in three neck round bottom flask, by bubbling method into
Row nitrogen deoxygenation 30min, then by the cadmium acetate aqueous solution of 0.04mol/L, 0.01mol/L potassium tellurite aqueous solutions according to volume
Than 1：1 ratio is separately added into 4mL, then sequentially adds the sodium citrate of 400mg, the dimercaptosuccinic acid of 100mg and 50mg
Sodium borohydride, finally form precursor solution, under 90 DEG C~100 DEG C oil baths condensing reflux react, by control react when
Between 9h, obtain temperature sensitive cadmium telluride quantum dot；
Second step, the purifying of cadmium telluride quantum dot and redisperse：Cadmium telluride quantum dot prepared by the first step carries out rotary evaporation,
When the 1/5 of volume concentration to original volume, isopropanol is added in thereto, wherein the volume ratio between concentration quantum dot and isopropanol
It is 1:3, eccentric cleaning is then carried out, most quantum dot is redispersed in isometric absolute ethyl alcohol at last, obtains amount after purification
Son point ethanol solution；
Third walks, the preparation of temperature sensitive PDMS film：By PDMS performed polymers with quantum dot ethanol solution after purification according to 4g：1mL
Ratio mixed, persistently stir 20min, then add in curing agent, the mass ratio of wherein performed polymer and curing agent is 10:1,
Stirring 8min is then proceeded to, mixture is placed in vacuum glove box be filtered by vacuum and removes bubble removing 20min, mixture is taken to hang
Then Tu places it in baking oven to be cured and obtains temperature sensitive PDMS film on the glass slide Jing Guo cleaning treatment.
2. a kind of preparation method of PDMS film with temperature-sensing property according to claim 1, it is characterised in that：It is described
The rotating speed of rotary evaporation in second step is 200 revs/min, and temperature is 70 DEG C.
3. a kind of preparation method of PDMS film with temperature-sensing property according to claim 1, it is characterised in that：It is described
The solidification temperature of baking oven is 70 DEG C in third step, keeps 30min.
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| CN105885419B (en) * | 2016-04-29 | 2018-11-20 | 河南大学 | A kind of preparation method of cadmium compound quantum dot fluorescence film |
| JP7152854B2 (en) * | 2016-12-28 | 2022-10-13 | 東京応化工業株式会社 | Silicon-containing resin composition, silicon-containing resin film, silica film, light-emitting display element panel, and light-emitting display device |
| 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 |
| 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 |
| CN110218329B (en) | 2018-03-04 | 2021-03-19 | 南京大学 | 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 |
| 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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| 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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Patent Citations (5)
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| CN101431148A (en) * | 2008-10-13 | 2009-05-13 | 同济大学 | Method for improving illumination intensity of CdTe nano compound film |
| CN102877149A (en) * | 2012-10-25 | 2013-01-16 | 黑龙江东方学院 | In-situ preparation method for cadmium telluride/polyvinyl alcohol fluorescent fiber |
| CN103411703A (en) * | 2013-07-18 | 2013-11-27 | 西安交通大学 | Non-contact-type temperature measurement method based on cadmium telluride quantum dot photoluminescence |
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