CN114349782A - Temperature sensor and preparation method thereof - Google Patents
Temperature sensor and preparation method thereof Download PDFInfo
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- CN114349782A CN114349782A CN202110381451.4A CN202110381451A CN114349782A CN 114349782 A CN114349782 A CN 114349782A CN 202110381451 A CN202110381451 A CN 202110381451A CN 114349782 A CN114349782 A CN 114349782A
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Abstract
The invention discloses a temperature sensor and a preparation method thereof, and relates to the technical field of sensors. The temperature sensor includes: the flexible substrate is made of polyimide; the metal interdigital electrode is plated on the flexible substrate; and the modified graphene oxide/epoxy resin composite temperature sensing film is coated on the upper surface of the metal interdigital electrode. The temperature sensor prepared by the invention has the advantages of good flexibility, high sensitivity, good stability and microminiaturization, and the application range of the sensor is greatly widened; and the sensor has simple structure and low cost, and can realize large-scale mass production.
Description
Technical Field
The invention belongs to the technical field of sensors, and particularly relates to a temperature sensor and a preparation method thereof.
Background
The temperature sensor is a device capable of identifying temperature, and is crucial to temperature measurement and monitoring in many fields, such as accurate temperature control in a temperature control module of a fluorescence quantitative PCR instrument and other instruments. However, the conventional temperature sensors generally use metal materials as sensitive elements, and these sensors often have certain limitations. The requirements for a temperature sensor are that it is highly stable, simple in manufacturing process, accurate, highly sensitive, etc. This has prompted researchers to explore new high performance temperature sensor materials.
The research on novel temperature sensor materials mainly focuses on conductive composite materials, in particular to polymer-based composite materials based on carbon-based nano conductive fillers. The composite material has good conductive performance of filler particles and processability of a high polymer material, and has certain thermal resistance performance. When the temperature sensor is manufactured, the temperature can be reversely deduced from the resistance by the resistance change of the sensor caused by the environmental temperature change under the direct current environment, which is a common manufacturing strategy of the temperature sensor. At present, certain research achievements exist on a composite material temperature sensor, but the achievements can not meet the requirements of scientific research and markets, and further research and exploration are needed for the development of novel high-performance temperature sensor materials.
Disclosure of Invention
The invention aims to provide a temperature sensor and a preparation method thereof, wherein the temperature sensor has the advantages of simple structure, convenience in processing, high sensitivity, good linearity and excellent stability, and can realize miniaturization.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a modified silane coupling agent has the following structural formula:
The preparation method of the modified silane coupling agent comprises the following steps:
dissolving eupatorin in toluene, reacting, heating to 50-60 ℃, adding a karstedt catalyst, and continuously stirring for 30-50 min; then adding methoxysilane into the constant-pressure dropping funnel, slowly dropping the methoxysilane into the solution, and reacting at a constant temperature of 75-85 ℃ for 22-28 h after the dropping is finished; and carrying out suction filtration while the solution is hot, cooling to room temperature, carrying out rotary evaporation, drying, and recrystallizing with ethanol to obtain the modified silane coupling agent.
The mass ratio of eupatorin to methoxysilane is 1: 0.6 to 0.8.
The invention also discloses application of the modified silane coupling agent in preparation of a temperature sensing film or a temperature sensor.
A composite temperature sensing film is made of modified graphene oxide/epoxy resin, wherein the modified graphene oxide is the modified silane coupling agent functionalized graphene oxide.
Further, the preparation method of the modified graphene oxide specifically comprises the following steps:
dispersing graphene oxide in a mixed solution of water and ethanol (the volume ratio is 2-3: 1), dispersing graphene oxide in the mixed solution by ultrasonic treatment for 30min, adding a modified silane coupling agent, stirring for 3-4 h under stable reflux in a water bath at 70-75 ℃, cleaning for 2-3 times by using the mixed solution of water and ethanol in the same proportion, and drying in an oven at 55-60 ℃ to obtain the modified graphene oxide.
The mass ratio of the graphene oxide to the modified silane coupling agent is 1: 12 to 14.
The invention also discloses the application of the composite temperature sensing film in a temperature sensor.
A temperature sensor, comprising:
the flexible substrate is made of polyimide;
the metal interdigital electrode is plated on the flexible substrate;
the composite temperature sensing film is coated on the upper surface of the metal interdigital electrode. The temperature sensor is manufactured on the basis of the modified graphene oxide/epoxy resin composite material, the negative temperature coefficient effect is shown, the resistance of the temperature sensor shows a good linear reduction trend along with the temperature rise, and the cycling stability performance is excellent. The modified graphene oxide/epoxy resin composite temperature-sensing film has good flexibility, the metal interdigital electrode and the flexible temperature-sensing film form a temperature-sensing unit of the sensor, and the sensor has the advantages of good flexibility, high sensitivity, good stability and miniaturization, so that the application range of the sensor is greatly widened; and the sensor has simple structure and low cost, and can realize large-scale mass production.
The metal interdigital electrode is a metal layer formed of one of Cu and Au, or an alloy layer formed of both.
The thickness of the flexible substrate is 0.02-0.08 mm; the thickness of the metal interdigital electrode is 0.03-0.1 mm; the thickness of the composite temperature sensing film is 0.08-0.16 mm.
A method of making a temperature sensor, comprising:
dispersing functionalized graphene oxide in acetone, adding the dispersed functionalized graphene oxide into an epoxy resin monomer at the temperature of 50-60 ℃, performing ultrasonic treatment for 20-30 min, performing stable stirring at the temperature of 50-60 ℃ for 10-12 h, volatilizing the acetone, adding a curing agent DDM, stirring, and then putting into a vacuum box to remove bubbles; and then coating the metal interdigital electrode on a flexible substrate plated with the metal interdigital electrode, and curing to obtain the temperature sensor.
The addition amount of the modified graphene oxide is 0.8-1.2 wt% of the epoxy resin; the mass ratio of the curing agent to the epoxy resin is 1: 3 to 3.5.
The conditions for carrying out the curing are as follows: curing for 2-4 h at 70-80 ℃, or curing for 40-46 h at room temperature.
The preparation method is characterized in that 4- [2- (2-methoxy-5-chlorobenzoylamino) ethyl ] benzenesulfonamide is added in the preparation process, and the addition amount of the 4- [2- (2-methoxy-5-chlorobenzoylamino) ethyl ] benzenesulfonamide is 1.2-2.5 wt% of the epoxy resin. The addition of the 4- [2- (2-methoxy-5-chlorobenzoylamino) ethyl ] benzene sulfonamide enhances the conductivity of the composite material; meanwhile, the flame retardant is compounded with other components, so that the flame retardant property of the composite material can be obviously improved. The linearity of the resistance of the prepared temperature sensor along with the temperature change curve is obviously improved, and the performance of the sensor is improved; and the sensitivity of the sensor can be further enhanced by compounding the nano-particles with other components.
Compared with the prior art, the invention has the following beneficial effects:
the eupatorium odoratum modified silane coupling agent is adopted, so that the interface of graphene oxide and epoxy resin can be regulated and controlled, the electrical conductivity of the composite material is enhanced, the thermal conductivity coefficient is improved, and the mechanical property of the material is improved. The temperature sensor is manufactured on the basis of the modified graphene oxide/epoxy resin composite material, the negative temperature coefficient effect is shown, the resistance of the temperature sensor shows a good linear reduction trend along with the temperature rise, and the cycling stability performance is excellent. The temperature sensor has the advantages that the sensitivity of the temperature sensor is remarkably improved and the recycling stability is enhanced due to the existence of the modified graphene oxide/epoxy resin composite temperature sensing film. In addition, the addition of the 4- [2- (2-methoxy-5-chlorobenzoylamino) ethyl ] benzene sulfonamide further enhances the conductivity of the composite material; the flame retardant property of the composite material can be obviously improved; meanwhile, the linearity and the sensitivity of the resistance of the temperature sensor along with the temperature change are enhanced, and the performance of the sensor is further improved. The temperature sensor prepared by the invention can realize the advantage of miniaturization, thereby greatly widening the application range of the sensor; and the structure is simple, the cost is low, and large-scale mass production can be realized.
Therefore, the invention provides the temperature sensor and the preparation method thereof, the temperature sensor has the advantages of simple structure, convenient processing, high sensitivity, good linearity and excellent stability, and can realize miniaturization.
Drawings
FIG. 1 shows the results of the flame retardancy test in test example 1 of the present invention;
FIG. 2 is a resistance-temperature curve in test example 2 of the present invention.
Detailed Description
The technical solution of the present invention is further described in detail below with reference to the following detailed description and the accompanying drawings:
the epoxy resin used in the embodiment of the invention is as follows: bisphenol a NPEL-128, south asian reagent; graphene oxide used was purchased from Sigma-Aldrich.
Example 1:
preparation of modified silane coupling agent:
dissolving eupatorin in toluene, reacting, heating to 55 ℃, adding karstedt catalyst, and continuously stirring for 35 min; then adding methoxysilane (the mass ratio of eupatorium round leaf to methoxysilane is 1: 0.74) into a constant-pressure dropping funnel, slowly dropping into the solution, and reacting at a constant temperature of 80 ℃ for 25 hours after dropping; and carrying out suction filtration while the solution is hot, cooling to room temperature, carrying out rotary evaporation, drying, and recrystallizing with ethanol to obtain the modified silane coupling agent.
Preparing modified graphene oxide:
dispersing 1g of graphene oxide in 800mL of mixed solution of water and ethanol (volume ratio is 3: 1), performing ultrasonic treatment for 30min, dispersing in the mixed solution, adding 13g of modified methoxysilane, performing stable reflux stirring for 3h in a water bath at 75 ℃, cleaning for 3 times by using the mixed solution of water and ethanol in the same proportion, and drying in an oven at 60 ℃ to obtain the modified graphene oxide.
Preparation of a temperature sensor:
dispersing functionalized graphene oxide (the addition amount is 1.1 wt% of epoxy resin) in acetone, adding the dispersed functionalized graphene oxide into an epoxy resin monomer at the temperature of 55 ℃, carrying out ultrasonic treatment for 30min, carrying out stable stirring at the temperature of 60 ℃ for 12h, volatilizing the acetone, adding a curing agent DDM (the mass ratio of the curing agent to the epoxy resin is 1: 3.24), stirring, and then placing the obtained product in a vacuum box to remove bubbles; and then coating the metal oxide film on a flexible substrate plated with a Cu interdigital electrode, and curing for 4 hours at 75 ℃ to obtain the temperature sensor.
Wherein the thickness of the flexible substrate is 0.06 mm; the thickness of the metal interdigital electrode is 0.08 mm; the thickness of the composite temperature sensing film is set to be 0.12 mm.
Example 2:
the modified silane coupling agent was prepared differently from example 1 in that: the mass ratio of eupatorin to methoxysilane is 1: 0.79.
the preparation of modified graphene oxide differs from example 1 in that: the modified silane coupling agent was obtained in this example.
A temperature sensor was prepared differently from example 1 in that: the modified graphene oxide was prepared in this example; the addition amount of the modified graphene oxide is 0.9 wt% of the epoxy resin; the mass ratio of the curing agent to the epoxy resin is 1: 3.2.
example 3:
the modified silane coupling agent and the modified graphene oxide were prepared in the same manner as in example 1.
A temperature sensor was prepared differently from example 1 in that: the addition amount of the modified graphene oxide is 1 wt% of the epoxy resin; the mass ratio of the curing agent to the epoxy resin is 1: 3.42.
example 4:
the modified silane coupling agent and the modified graphene oxide were prepared in the same manner as in example 1.
A temperature sensor was prepared differently from example 1 in that: the addition amount of the modified graphene oxide is 1.2 wt% of the epoxy resin; the mass ratio of the curing agent to the epoxy resin is 1: 3.36.
example 5:
the modified silane coupling agent and the modified graphene oxide were prepared in the same manner as in example 1.
A temperature sensor was prepared differently from example 1 in that: in the process, 4- [2- (2-methoxy-5-chlorobenzoylamino) ethyl ] benzenesulfonamide is added, and the addition amount is 1.8 wt% of the epoxy resin.
Comparative example 1:
a temperature sensor was prepared differently from example 1 in that: the modified graphene oxide is replaced by graphene oxide.
Comparative example 2:
the preparation of modified graphene oxide differs from example 1 in that: methoxy silane coupling agent is adopted to replace modified silane coupling agent.
A temperature sensor was prepared differently from example 1 in that: the modified graphene oxide was prepared in this comparative example.
Comparative example 3:
the preparation of modified graphene oxide differs from example 1 in that: KH560 was used instead of the modified silane coupling agent.
A temperature sensor was prepared differently from example 1 in that: the modified graphene oxide was prepared in this comparative example.
Comparative example 4:
a temperature sensor was prepared differently from example 1 in that: the carbon nano tube is adopted to replace the modified graphene oxide.
Test example 1:
1. characterization of nuclear magnetic resonance (1H NMR)
3mg of modified methoxysilane is weighed and dissolved in deuterated DMSO to prepare a sample solution, the sample solution is placed in a nuclear magnetic tube, and the nuclear magnetic resonance instrument is used for measurement. The operating conditions of the instrument are as follows: AVANCE III 400 nuclear magnetic resonance apparatus (Bruker). And analyzing the type and the amount of hydrogen in the target product through the data of the hydrogen spectrum.
The modified methoxysilane prepared in example 1 was subjected to nuclear magnetic hydrogen spectrum test, and the characterization results were as follows:
example 1:1h NMR (400MHz, DMSO-d 6): 6.17(m, 1H, C ═ C-H), 5.56(d, 1H, C ═ C-H), 4.42(d, 1H, O ═ C-O-CH), 4.01 to 4.11(m, 2H, O ═ C-O-CH and HO-CH), 3.71(s, 1H, -OH), 3.60(s, 9H, O-CH)3)，2.85(d，1H，-OH)，2.32～2.66(m，5H，CH、CH2)，2.45、1.85(s，6H，-CH3)，2.09(d，3H，-CH3)，1.79、1.63(d，2H，-CH2)，1.11、0.86(m，2H，Si-CH2). Indicating that the modified methoxysilane is successfully prepared.
2. Thermal conductivity test
After adding the curing agent, pouring the mixed solution into a polytetrafluoroethylene mold for vacuum defoamation (the curing process conditions are 60 ℃/2h +100 ℃/3h +150 ℃/2h) to obtain the composite material. The thermal conductivity of the composite material was measured using a laser thermal conductivity tester (Netsch, LFA447) from relaxation corporation, which allowed the thermal diffusivity of the material to be measured in a non-contact manner, which eliminated the problem of thermal contact resistance. The test process is as follows: liquid nitrogen is filled into a cavity of the LFA447, the testing temperature (generally 25 ℃) is set, when the temperature difference between the temperature and the set temperature is about 0.1 ℃, the testing is started, and different lasers are set to ensure that the curve obtained by the testing can reflect the real thermal performance of the material. After the test, the thermal conductivity was calculated.
The mechanical property test was performed after curing the adhesives prepared in comparative examples 1 to 4 and examples 1 to 5, and the results are shown in table 1:
table 1 results of thermal conductivity test
| Sample (I) | Thermal conductivity/[ W. (mK)-1] |
| Comparative example 1 | 0.247 |
| Comparative example 2 | 0.271 |
| Comparative example 3 | 0.263 |
| Comparative example 4 | 0.254 |
| Example 1 | 0.334 |
| Example 2 | 0.349 |
| Example 3 | 0.321 |
| Example 4 | 0.337 |
| Example 5 | 0.351 |
The analysis in table 1 shows that the thermal conductivity of the composite material prepared in example 1 is equivalent to that of comparative examples 1-4, and that the composite material prepared by compounding eupatorium odoratum modified methoxysilane and functionalized graphene oxide with epoxy resin has good thermal conductivity, and the presence of eupatorium odoratum can significantly improve the thermal conductivity of the composite material. The effect of example 5 is significantly higher than that of example 1, indicating that the addition of 4- [2- (2-methoxy-5-chlorobenzamido) ethyl ] benzenesulfonamide has no negative effect on the thermal conductivity of the composite.
3. Mechanical Property test
The test instrument was a Universal Testing machine 5567 from instron corporation, usa. The mechanical properties of the samples were measured with a gauge length of 50mm and tested at a tensile speed of 20 mm/min. After adding the curing agent, pouring the mixed solution into a polytetrafluoroethylene mold for vacuum defoamation (the curing process conditions are 60 ℃/2h +100 ℃/3h +150 ℃/2h) to obtain the composite material, shearing the sample into a dumbbell shape, measuring the thickness of each sample by using a micrometer in each measurement, inputting the thickness into software for testing, measuring each sample at least 8 times, and taking an average value.
The mechanical property test was performed after curing the adhesives prepared in comparative examples 1 to 4 and examples 1 to 5, and the results are shown in table 2:
TABLE 2 mechanical Property test results
From the analysis in table 2, it can be seen that the tensile strength of the composite material prepared in example 1 is significantly higher than that of comparative examples 1 to 4, which indicates that the composite material prepared by compounding eupatorium odoratum modified methoxysilane and functionalized graphene oxide with epoxy resin has good mechanical properties, and the presence of eupatorium odoratum can significantly improve the tensile strength of the material. The effect of example 5 is comparable to example 1, indicating that the addition of 4- [2- (2-methoxy-5-chlorobenzamido) ethyl ] benzenesulfonamide has no negative effect on the mechanical properties of the composite.
4. Conductivity test
Conductivity is generally used to characterize the conductivity of a material, and a value for conductivity can be calculated after knowing the dimensions and resistance of the material. After the curing agent is added, pouring the mixed solution into a prepared circular hole silica gel mold and curing to obtain composite material small cylinders with the diameter of 8mm and the thickness of 6mm and different graphene contents. The method comprises the following steps of polishing two bottom surfaces of a sample to be detected by using sand paper to erase surface impurities, uniformly coating conductive silver paste to serve as an electrode, carrying out room-temperature volume resistance test on the electrode by using a digital multimeter to obtain a resistance value, and then obtaining the conductivity of the sample by calculation, wherein the calculation formula is as follows:
ρ＝RS/h
in the formula, rho is volume resistivity, omega m; r is the resistance between the upper electrode and the lower electrode, omega; s-floor area, m2(ii) a h is the distance between the upper electrode and the lower electrode, m.
Conductivity σ 1/ρ
The results of the above tests on the composites prepared in comparative examples 1 to 4 and examples 1 to 5 are shown in Table 3:
table 3 conductivity test results
As can be seen from table 3, the conductivity of the composite material prepared in example 1 is significantly better than that of comparative examples 1 to 4, which indicates that the composite material prepared by re-functionalizing graphene oxide with eupatorium odoratum modified methoxysilane has good conductivity, and the presence of eupatorium odoratum can significantly improve the conductivity of the material. Example 5 is more effective than example 1, indicating that the addition of 4- [2- (2-methoxy-5-chlorobenzamido) ethyl ] benzenesulfonamide has a synergistic effect.
5. Test for flame retardancy
After adding the curing agent, pouring the mixed solution into a polytetrafluoroethylene mold for vacuum defoamation (the curing process conditions are 60 ℃/2h +100 ℃/3h +150 ℃/2h) to obtain the composite material. Cutting the composite material into a square shape of 1.5cm/1.5cm, burning for 90s under an alcohol lamp, recording the mass before and after burning, and calculating the residual rate of the sample.
The results of the above tests on the composite materials prepared in comparative examples 1 to 2 and examples 1 to 5 are shown in FIG. 1. As can be seen from FIG. 1, the residual rate of the composite material prepared in example 1 is equivalent to that of comparative example 2, while the effect of example 5 is obviously better than that of example 1, which shows that the addition of 4- [2- (2-methoxy-5-chlorobenzamide) ethyl ] benzenesulfonamide has a synergistic enhancement effect, and the flame retardant property of the composite material can be remarkably improved.
Test example 2:
thermal resistance performance test of temperature sensor
And (3) putting the sample to be tested into a temperature control test box, connecting the electrode with the LCR analyzer through a lead and reducing the constraint of the lead on the test piece as much as possible. After the temperature is stable, the resistance values of the sensors at different temperatures can be read in real time. Then setting temperature-rise parameters of a temperature-control test box, wherein the humidity of the temperature-control test box is 40%, the temperature is heated from 30 ℃ to 100 ℃ at the temperature-rise rate of 1 ℃/min, and every 10 ℃ is taken as a temperature measurement point. And the temperature stays for 5min when reaching each temperature measurement point, so that the whole sensor is ensured to completely reach the temperature to be measured, and the reliability of the measured data is ensured. And when the sensor reaches the temperature to be measured and stays for 5min, measuring the resistance of the sensor by using an LCR analyzer and recording data to obtain the thermal resistance performance of the sensor under direct current.
1. Resistance-temperature relationship
The above-described test was performed on the sensors obtained in examples 1 and 5, and the results are shown in fig. 2. As can be seen from FIG. 2, the sensors prepared in the embodiments 1 and 5 of the present invention have resistance decreasing with increasing temperature in the temperature range of 30-100 ℃, show NTC effect, and have resistance showing good linear decreasing trend. Wherein example 5 has better linearity than example 1, it is shown that the addition of 4- [2- (2-methoxy-5-chlorobenzamido) ethyl ] benzenesulfonamide enhances the linear change in resistance and improves the performance of the sensor.
2. Temperature coefficient of resistance
The Temperature Coefficient of Resistance (TCR) refers to the relative change in resistance when the temperature changes by 1 ℃, and is generally divided into positive temperature coefficient and negative temperature coefficient. The resistance temperature coefficient is an important index for measuring the performance of the temperature sensor, and the absolute value of the resistance temperature coefficient can reflect the sensitivity. The calculation formula is as follows:
TCR＝(R2－R1)/[R0(T1－T2)]
in the formula, R1Temperature T1The resistance of the time sensor; r2Temperature T2The resistance of the time sensor; r0Resistance of the sensor at 30 ℃. In order to reduce the influence of difference brought by the initial resistance of the sensor, the resistance change rate is used for replacing the resistance to characterize the thermal resistance performance of the sensor. As the rate of change of resistance (Δ R/R)0，R0The TCR is obtained by fitting and calculating a resistance-temperature relation curve of the sensor at 30 ℃.
The results of the above tests on the temperature sensors prepared in comparative examples 1 to 4 and examples 1 to 5 are shown in Table 4:
TABLE 4 temperature coefficient of resistance test results
| Sample (I) | TCR(/℃) |
| Comparative example 1 | -0.0050 |
| Comparative example 2 | -0.0063 |
| Comparative example 3 | -0.0059 |
| Comparative example 4 | -0.0055 |
| Example 1 | -0.0080 |
| Example 2 | -0.0075 |
| Example 3 | -0.0078 |
| Example 4 | -0.0079 |
| Example 5 | -0.0089 |
From the analysis in table 4, it can be seen that the absolute value of the TCR value of the temperature sensor prepared in example 1 is significantly higher than that of comparative examples 1 to 4, which indicates that the obtained sensor has good temperature-sensitive performance when the composite material prepared by compounding the eupatorium odoratum modified methoxysilane and the epoxy resin is used for preparing the temperature sensor, the absolute value of the TCR value of the obtained sensor is higher than that of the temperature sensor (about 0.0040/° c) prepared from common metals such as copper and platinum, and the existence of eupatorium odoratum can significantly improve the sensitivity of the material. The effect of example 5 is equivalent to that of example 1, and shows that the addition of 4- [2- (2-methoxy-5-chlorobenzamide) ethyl ] benzenesulfonamide has a positive influence on the temperature-sensitive performance of the sensor.
3. Thermal cycling stability testing of temperature sensors
And carrying out 16 times of resistance-temperature tests on the temperature sensor with stable performance within the temperature range of 30-100 ℃. In order to ensure that the sensor can be completely restored to the initial state after each test, the sensor is placed in the room temperature for 12h after each test to serve as a cooling restoration stage. The cycle stability of the temperature sensor is characterized by the change of the 16 th resistance-temperature linearity compared with the 1 st resistance-temperature linearity.
The results of the above tests on the temperature sensors prepared in comparative examples 1 to 4 and examples 1 to 5 are shown in Table 5:
TABLE 5 Linearity Change
From the analysis in table 5, it can be seen that the linearity reduction rate of the temperature sensor prepared in example 1 after 16 thermal cycles is significantly lower than that of comparative examples 1 to 4, which indicates that the eupatorium odoratum modified methoxysilane is re-functionalized with graphene oxide, and the graphene oxide is compounded with epoxy resin to prepare a composite material, and the obtained sensor has good cycle stability when the temperature sensor is prepared, and the existence of eupatorium odoratum can significantly improve the cycle performance of the sensor. The effect of example 5 is comparable to example 1, indicating that the presence of 4- [2- (2-methoxy-5-chlorobenzamido) ethyl ] benzenesulfonamide has no negative impact on temperature sensor cycling performance.
Conventional techniques in the above embodiments are known to those skilled in the art, and therefore, will not be described in detail herein.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. A modified silane coupling agent has the following structural formula:
2. use of the modified silane coupling agent according to claim 1 for the preparation of a temperature sensitive film or a temperature sensor.
3. A composite temperature sensing film, the material of which is modified graphene oxide/epoxy resin, wherein the modified graphene oxide is the modified silane coupling agent functionalized graphene oxide of claim 1.
4. Use of the composite temperature sensitive film of claim 3 in a temperature sensor.
5. A temperature sensor, comprising:
the flexible substrate is made of polyimide;
the metal interdigital electrode is plated on the flexible substrate;
the composite temperature sensing film of claim 3 coated on the upper surface of the metal interdigital electrode.
6. A temperature sensor according to claim 5, wherein: the metal interdigital electrode is a metal layer formed by one of Cu or Au or an alloy layer formed by the two.
7. A temperature sensor according to claim 5, wherein: the thickness of the flexible substrate is 0.02-0.08 mm;
the thickness of the metal interdigital electrode is 0.03-0.1 mm;
the thickness of the composite temperature sensing film is 0.08-0.16 mm.
8. A method of making a temperature sensor according to claim 5, comprising:
dispersing modified graphene oxide in acetone, adding the acetone into an epoxy resin monomer at the temperature of 50-60 ℃, performing ultrasonic treatment for 20-30 min, stably stirring at the temperature of 50-60 ℃ for 10-12 h, volatilizing the acetone, adding a curing agent DDM, stirring, and then putting into a vacuum box to remove bubbles; and then coating the metal interdigital electrode on a flexible substrate plated with the metal interdigital electrode, and curing to obtain the temperature sensor.
9. The method for manufacturing a temperature sensor according to claim 8, wherein: the addition amount of the modified graphene oxide is 0.8-1.2 wt% of the epoxy resin; the mass ratio of the curing agent to the epoxy resin is 1: 3 to 3.5.
10. The method for manufacturing a temperature sensor according to claim 8, wherein: in the preparation process, 4- [2- (2-methoxy-5-chlorobenzoylamino) ethyl ] benzenesulfonamide is added, and the addition amount is 1.2-2.5 wt% of the epoxy resin.
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| EP4296226A1 (en) | 2022-06-24 | 2023-12-27 | Espio, s.r.o. | The method of preparing functionalized reduced graphene oxide layer and the temperature sensor comprising such a layer |
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