CN114853017A - Silver-carbon composite temperature-sensitive material and preparation method and application thereof - Google Patents
Silver-carbon composite temperature-sensitive material and preparation method and application thereof Download PDFInfo
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- CN114853017A CN114853017A CN202210354460.9A CN202210354460A CN114853017A CN 114853017 A CN114853017 A CN 114853017A CN 202210354460 A CN202210354460 A CN 202210354460A CN 114853017 A CN114853017 A CN 114853017A
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Abstract
The invention belongs to the technical field of nano temperature-sensitive composite materials, and relates to a silver-carbon composite temperature-sensitive material capable of responding to temperature, and a preparation method and application thereof. The invention adopts a supermolecule self-assembly approach to synthesize a melamine-silver nano composite material, and then the melamine-silver nano composite material is subjected to high-temperature calcination and hydrothermal treatment to prepare a temperature-sensitive silver carbide nano material, the temperature-sensitive silver carbide nano material is mixed with epoxy resin, coupled and cured into a sheet, and two ends of the temperature-sensitive silver carbide nano material are connected and fixed by conductive silver adhesive to prepare a temperature sensor which is used for responding to a test temperature (body temperature) and investigating the temperature response performance of silver carbide, including temperature response time and temperature-sensitive stability of the material. The result shows that the silver carbide nano composite material with excellent temperature response performance can be prepared by optimizing the conditions of the molar ratio of melamine-silver ions, the calcining temperature, the calcining time and the like, and can be successfully used for high-sensitivity sensing detection of temperature.
Description
Technical Field
The invention belongs to the technical field of nano temperature-sensitive composite materials, and relates to a silver-carbon composite temperature-sensitive material capable of responding to temperature, and a preparation method and application thereof.
Background
The temperature sensor is a sensor which can sense temperature and convert the temperature into a readable digital output signal, is a common sensor, and plays an important role in the fields of environmental temperature detection, human body temperature monitoring, medical health and the like. The sensor can be classified into a thermocouple and a thermal resistor according to the characteristics of the sensor electronic component and the nanomaterial used. The thermal resistance sensor is widely applied due to flexible use, stable performance, small volume, high reliability, convenience for mass production and the like, and mainly utilizes a temperature-sensitive material to realize temperature measurement. The traditional temperature-sensitive material mainly comprises various metals such as gold platinum, nickel chromium, copper silver and the like, has the defects of high cost, low sensitivity, unstable sensing performance and the like, and is difficult to meet the actual application requirement. Therefore, researchers have continually explored the feasibility of different other new materials for temperature sensing.
The carbon nano material has the characteristics of low price, good electric and heat conduction capability, high stability, stable chemical property and the like, thereby arousing great research interest of people and rapidly becoming a hotspot for the development of novel temperature sensor materials. It has been found that the content of multi-walled carbon nanotubes in a multi-walled carbon nanotube based temperature sensor directly affects the temperature coefficient of resistance of the temperature sensor. Carbon materials such as graphene have been developed for the construction of temperature sensors. In view of the importance and wide application of temperature sensors, the current achievements are difficult to meet the increasing demands, so the development of new composite nanomaterial-based temperature sensors remains at random.
Disclosure of Invention
The invention provides a silver-carbon composite temperature-sensitive material aiming at the defects of the existing temperature-sensitive material and the related temperature sensing technology thereof.
The invention also provides a preparation method of the silver-carbon composite temperature-sensitive material, which adopts a supermolecule self-assembly approach to synthesize the melamine-silver nano composite material, and the melamine-silver nano composite material is calcined at high temperature and treated by hydrothermal treatment to prepare the temperature-sensitive silver carbide nano material.
The invention also provides an application of the silver-carbon composite temperature-sensitive material in preparing a temperature sensor, wherein silver carbide and epoxy resin are mixed, coupled and cured into a sheet, and then two ends of the sheet are connected and fixed by conductive silver paste to prepare the temperature sensor for responding to the test temperature (body temperature). The temperature sensor has the characteristics of low preparation cost, high sensitivity and quick response, and overcomes the defects of the prior art in the aspect of temperature detection.
In order to achieve the purpose, the invention adopts the following specific scheme:
the invention provides a preparation method of a silver-carbon composite temperature-sensitive material, which comprises the following steps: :
(1) preparation of melamine-silver nano material
Preparing a melamine aqueous solution, adding a silver nitrate aqueous solution under the stirring condition, standing, centrifuging, washing and vacuum-drying the mixture to obtain a melamine-silver nano composite material;
(2) preparation of melamine-silver based silver carbide nano material
Placing a certain amount of melamine-silver nano material in a muffle furnace to carry out high-temperature calcination treatment in a nitrogen atmosphere; subsequently, the obtained mass was ground to a powder g-C3N 4; and then weighing powdery g-C3N4, ultrasonically dispersing in ethanol to obtain g-C3N 4-ethanol dispersion liquid, uniformly dispersing the g-C3N 4-ethanol dispersion liquid, then placing the dispersion liquid in a stainless steel autoclave with a polytetrafluoroethylene lining, heating for reaction, after the reaction is finished, centrifugally separating, then washing for a plurality of times by using ethanol, and drying to obtain the silver carbide nano composite material.
Further, in the step (1), the concentration of the melamine aqueous solution is 10 mM; the concentration of the silver nitrate aqueous solution is 2-50 mM.
The volume ratio of the melamine aqueous solution to the silver nitrate aqueous solution is 1: 1; the standing time is 1-2 h.
Further, in the step (2), the temperature of the high-temperature calcination treatment is 500-1000 ℃, and the calcination time is 2-7 h.
Further, in the step (2), the concentration of the g-C3N 4-ethanol dispersion liquid is 0.0025 g/mL.
Further, in the step (2), the heating reaction is to keep heating at 180 ℃ for 6 h; the drying is drying at 60 ℃ for 24 h.
The invention also provides the silver-carbon composite temperature-sensitive material prepared by the preparation method.
The invention also provides an application of the silver-carbon composite temperature-sensitive material in preparing a temperature sensor.
The temperature sensor provided by the invention is prepared by the following steps: adding 0.25 g of silver carbide into 40 mL of ethanol solution, and then stirring for 1 h by using ultrasonic waves to obtain a silver carbide dispersion liquid; dissolving 0.12 g of epoxy resin in an acetone solution; pouring the silver carbide dispersion liquid into the epoxy resin solution, fully mixing, and ultrasonically stirring for 1 h; then adding 0.011 g of silane coupling agent into the mixed solution, and placing the mixed solution in a forced air drying oven for drying for 10 hours to fully volatilize the solvent; adding a curing agent, pouring the mixture into a silicon rubber mold, putting the silicon rubber mold into a drying oven for step curing, namely, heating the silicon rubber mold to 70 ℃ along with a furnace, keeping the silicon rubber mold for 1 hour, then heating the silicon rubber mold to 110 ℃, keeping the silicon rubber mold for 2.5 hours, and obtaining a silver carbide-epoxy resin composite material sheet after curing is finished; and uniformly coating conductive silver adhesive at two ends of the thin sheet to be used as electrodes to prepare the temperature sensor.
The thickness of the silver carbide-epoxy resin composite material sheet is 1 mm.
The invention has the beneficial effects that:
(1) after the temperature-sensitive material prepared by the invention is applied to a temperature sensor, the resistance values of silver carbide prepared by different molar ratios of melamine to silver ions are all reduced along with the rise of temperature, wherein the molar ratio of the melamine to the silver ions is 1: the resistance value of the silver carbide prepared at 3 is most reduced.
(2) The silver-carbon composite temperature-sensitive material prepared by the invention has the advantages that the resistance value of the silver carbide is gradually reduced along with the increase of the calcining temperature and the calcining time, and the controllable resistance of the temperature-sensitive material is realized.
(3) The response time of the temperature sensor prepared by the invention is about 6 s, and the temperature sensor has a faster temperature response performance; the maximum resistance variation of the temperature sensor is 0.21 omega at 30 ℃, the relative change rate is 2.97%, the maximum resistance variation of the sensor is 0.084 omega at 70 ℃, the relative change rate is 1.68%, the maximum resistance variation of the sensor is 0.043 omega at 110 ℃, the relative change rate is 0.96%, and the temperature sensor has good stability.
Drawings
FIG. 1 is a scanning electron microscope image of a melamine-silver based silver carbide nano material.
Fig. 2 temperature sensor film.
FIG. 3 shows the resistance-temperature relationship of silver carbide synthesized by different molar ratios of melamine to silver ions.
FIG. 4 shows the resistance-temperature relationship of silver carbide synthesized at different calcination temperatures.
FIG. 5 resistance versus temperature for silver carbide synthesized at different calcination times.
The response time of the sensor of fig. 6 from room temperature to 140 c was tested.
Figure 7 testing of the stability of the sensor at different temperatures.
Detailed Description
By describing the present invention in conjunction with the specific embodiments, various substitutions or alterations made on the basis of the knowledge and the conventional means of the ordinary skill in the art without departing from the technical idea of the present invention as described above are included in the scope of the present invention.
Example 1: preparation of melamine-silver nano material and silver carbide nano material
Preparing 10 mL of 10 mM melamine aqueous solution, adding 10 mL of 2-50 mM silver nitrate aqueous solution with different concentrations under the stirring condition, standing for 1-2 h, centrifuging, washing, and drying in vacuum to obtain the melamine-silver nanocomposite.
Placing a certain amount of melamine-silver nano material in a crucible, placing the crucible in a muffle furnace, and performing high-temperature calcination treatment at different temperatures (500-1000 ℃); subsequently, the obtained block was pulverized into a powder (g-C3N 4) with an agate mortar. Then 0.10 g of powdered g-C3N4 is weighed and ultrasonically dispersed in 40 mL of ethanol, and after uniform dispersion, the powder is placed in a 70 mL stainless steel autoclave with a polytetrafluoroethylene lining and heated for 6h at 180 ℃. After the reaction is finished, washing the reaction product for a plurality of times by using ethanol after centrifugal separation, and drying the reaction product for 24 hours at the temperature of 60 ℃ to obtain the silver carbide nano composite material, wherein an SEM electron microscope picture is shown in figure 1.
Specific parameter settings are shown in table 1.
TABLE 1
Example 2: preparation of silver carbide-epoxy resin film temperature sensor
Mixing, coupling and curing the silver carbide and the epoxy resin into a sheet, connecting and fixing two ends of the sheet by conductive silver adhesive to prepare the temperature sensor, and systematically testing the temperature response performance of the temperature sensor. The method comprises the following specific steps: adding silver carbide with specified mass into ethanol solution with proper volume, and then stirring for 1 h by using ultrasonic to obtain silver carbide dispersion liquid; dissolving a proper amount of epoxy resin in an acetone solution; pouring the silver carbide dispersion liquid into the epoxy resin solution, fully mixing, and ultrasonically stirring for 1 h; then adding a silane coupling agent into the mixed solution, and placing the mixed solution in a forced air drying oven for drying for 10 hours to fully volatilize the solvent; adding a curing agent, pouring the mixture into a silicon rubber mold, putting the silicon rubber mold into a drying oven for step curing, namely heating the silicon rubber mold to 70 ℃ along with a furnace, keeping the silicon rubber mold for 1 hour, then heating the silicon rubber mold to 110 ℃, keeping the silicon rubber mold for 2.5 hours, and obtaining a silver carbide-epoxy resin composite material sheet (thickness: 1 mm) after curing is finished; the two ends of the thin sheet are uniformly coated with conductive silver adhesive to be used as electrodes, and the temperature sensor (figure 2) is manufactured.
Effect examples-temperature response test
Putting the silver carbide-epoxy resin film temperature sensor to be tested into a temperature control box and connecting the temperature control box with a resistance tester, wherein the temperature control box takes 30 ℃ as an initial temperature, heating the silver carbide-epoxy resin film temperature sensor to 140 ℃, and the heating rate is 10 ℃/min. Every 10 ℃ was used as a temperature measurement point. In order to ensure that the interior of the temperature control box completely reaches the temperature to be measured, when the temperature control box reaches the temperature to be measured, the temperature is kept for 5 min, then a digital multimeter (Agilent 34401A) is used for testing the resistance value of the temperature control box, the operation is repeated, and finally the resistance-temperature relation of the silver carbide-epoxy resin film temperature sensor is obtained, and the temperature response performance of the temperature control box is measured through the resistance change of the silver carbide-epoxy resin film temperature sensor. The different conditions tested included: the influence of different molar ratios of silver ions to melamine, different calcination temperatures (500-.
Results and discussion:
(1) resistance-temperature relationship for silver carbide prepared with different silver ion and melamine molar ratios:
and (3) placing the silver carbide-epoxy resin film temperature sensor in a temperature control box with gradually increased temperature, and inspecting the resistance-temperature relationship of the silver carbide prepared by different molar ratios of melamine and silver ions. As can be seen from fig. 3, the resistance values of the silver carbide prepared by different molar ratios of melamine to silver ions, namely 1: the resistance value of the silver carbide prepared at 3 is most reduced.
(2) Resistance-temperature relationship for silver carbide prepared at different calcination temperatures:
fig. 4 is a resistance-temperature relationship curve for silver carbide prepared under different calcination temperature conditions. It can be seen from the graph that the resistance value of the silver carbide gradually decreases with the increase of the calcination temperature, the resistance at 900 ℃ is significantly lower than that at 700 ℃, the resistance above 900 ℃ has lower resistance and the decrease trend tends to be gentle, which is mainly due to the increase of the number of conductive ions and the graphitization of the microcrystalline structure.
(3) Resistance versus temperature relationship for silver carbide prepared at different calcination times:
fig. 5 is a graph of resistance versus temperature for silver carbide prepared at different calcination times. It can be seen from the figure that the resistance value of the silver carbide gradually decreases with the increase of the calcination time, the resistance value reaches the minimum when the calcination time is 5h, and the resistance value increases when the calcination is continued, which is mainly because the calcination for too long time destroys the structure of the silver carbide material and is not beneficial to electron transfer.
) Temperature response time study
The response time more accurately represents the speed of change of the output information of the temperature response material when the environmental temperature changes. And (3) heating the temperature control box to 140 ℃, putting the silver carbide-epoxy resin film temperature sensor into the temperature control box from a room temperature environment, and analyzing the response curve of the resistor along with time. As can be seen from fig. 6, when the ambient temperature is from room temperature to 140 ℃, the response time of the sensor is about 6 s, and the sensor has a faster temperature response performance.
(5) Temperature sensitive material stability study
In order to test the temperature-sensitive stability of the silver carbide-epoxy resin film temperature sensor, the silver carbide-epoxy resin film is placed into a test system, the temperature is respectively set to be 30 ℃, 70 ℃ and 110 ℃, the resistance value change of the silver carbide-epoxy resin film along with the time change is tested, and the test is continued for 20 hours. As shown in fig. 7, the maximum change amount of the resistance of the sensor at 30 ℃ was 0.21 Ω and the relative change rate was 2.97%, the maximum change amount of the resistance of the sensor at 70 ℃ was 0.084 Ω and the relative change rate was 1.68%, and the maximum change amount of the resistance of the sensor at 110 ℃ was 0.043 Ω and the relative change rate was 0.96%, indicating that silver carbide has good stability.
Claims (10)
1. The preparation method of the silver-carbon composite temperature-sensitive material is characterized by comprising the following steps of: :
(1) preparation of melamine-silver nano material
Preparing a melamine aqueous solution, adding a silver nitrate aqueous solution under the stirring condition, standing, centrifuging, washing and drying in vacuum to obtain a melamine-silver nano composite material;
(2) preparation of melamine-silver based silver carbide nano material
Placing a certain amount of melamine-silver nano material in a muffle furnace to carry out high-temperature calcination treatment in a nitrogen atmosphere; subsequently, the obtained mass was ground to a powder g-C3N 4; and then weighing powdery g-C3N4, ultrasonically dispersing in ethanol to obtain g-C3N 4-ethanol dispersion liquid, uniformly dispersing the g-C3N 4-ethanol dispersion liquid, then placing the dispersion liquid in a stainless steel autoclave with a polytetrafluoroethylene lining, heating for reaction, after the reaction is finished, centrifugally separating, then washing for a plurality of times by using ethanol, and drying to obtain the silver carbide nano composite material.
2. The method according to claim 1, wherein in the step (1), the concentration of the melamine aqueous solution is 10 mM; the concentration of the silver nitrate aqueous solution is 2-50 mM.
3. The method according to claim 1 or 2, wherein in step (1), the volume ratio of the aqueous melamine solution to the aqueous silver nitrate solution is 1: 1; the standing time is 1-2 h.
4. The method according to any one of claims 1 to 3, wherein in the step (2), the temperature of the high-temperature calcination treatment is 500-1000 ℃, and the calcination time is 2-7 h.
5. The method according to claim 1, wherein the g-C3N 4-ethanol dispersion in step (2) has a concentration of 0.0025 g/mL.
6. The process according to claim 1 or 5, wherein in the step (2), the heating reaction is carried out by keeping 180 ℃ for 6 hours; the drying is carried out at 60 ℃ for 24 h.
7. A silver-carbon composite temperature-sensitive material prepared by the preparation method according to any one of claims 1 to 6.
8. Use of the silver-carbon composite temperature-sensitive material according to claim 7 in the preparation of a temperature sensor.
9. The use according to claim 8, wherein the temperature sensor is prepared by: adding 0.25 g of silver carbide into 40 mL of ethanol solution, and then stirring for 1 h by using ultrasonic waves to obtain a silver carbide dispersion liquid; dissolving 0.12 g of epoxy resin in an acetone solution; pouring the silver carbide dispersion liquid into the epoxy resin solution, fully mixing, and ultrasonically stirring for 1 h; then adding 0.011 g of silane coupling agent into the mixed solution, and placing the mixed solution in a forced air drying oven for drying for 10 hours to fully volatilize the solvent; adding a curing agent, pouring the mixture into a silicon rubber mold, putting the silicon rubber mold into a drying oven for step curing, namely, heating the silicon rubber mold to 70 ℃ along with a furnace, keeping the silicon rubber mold for 1 hour, then heating the silicon rubber mold to 110 ℃, keeping the silicon rubber mold for 2.5 hours, and obtaining a silver carbide-epoxy resin composite material sheet after curing is finished; and uniformly coating conductive silver adhesive at two ends of the thin sheet to be used as electrodes to prepare the temperature sensor.
10. Use according to claim 9, wherein the silver carbide-epoxy composite sheet has a thickness of 1 mm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117091727A (en) * | 2023-08-24 | 2023-11-21 | 哈尔滨理工大学 | PEO-based implantable battery temperature sensor and preparation method and application thereof |
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| EP0810681A1 (en) * | 1996-05-31 | 1997-12-03 | Matsushita Electric Industrial Co., Ltd. | Nonaqueous electrolyte secondary battery |
| CN101419394A (en) * | 2007-10-22 | 2009-04-29 | 中国科学院理化技术研究所 | High-sensitivity light-sensitive thermal imaging material emulsion, reparation method and application thereof |
| CN110339854A (en) * | 2019-08-23 | 2019-10-18 | 南京邮电大学 | A kind of p-n homojunction carbonitride@cube argentum nano composite material and preparation method thereof of cyano modulation |
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Patent Citations (3)
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| EP0810681A1 (en) * | 1996-05-31 | 1997-12-03 | Matsushita Electric Industrial Co., Ltd. | Nonaqueous electrolyte secondary battery |
| CN101419394A (en) * | 2007-10-22 | 2009-04-29 | 中国科学院理化技术研究所 | High-sensitivity light-sensitive thermal imaging material emulsion, reparation method and application thereof |
| CN110339854A (en) * | 2019-08-23 | 2019-10-18 | 南京邮电大学 | A kind of p-n homojunction carbonitride@cube argentum nano composite material and preparation method thereof of cyano modulation |
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| 崔玉民等: "氮化碳光催化材料合成及应用", 中国书籍出版社, pages: 232 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117091727A (en) * | 2023-08-24 | 2023-11-21 | 哈尔滨理工大学 | PEO-based implantable battery temperature sensor and preparation method and application thereof |
| CN117091727B (en) * | 2023-08-24 | 2024-04-23 | 哈尔滨理工大学 | PEO-based implantable battery temperature sensor and preparation method and application thereof |
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