CN110627108A - Zinc oxide/reduced graphene oxide composite material and preparation method and application thereof - Google Patents
Zinc oxide/reduced graphene oxide composite material and preparation method and application thereof Download PDFInfo
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- CN110627108A CN110627108A CN201910922111.0A CN201910922111A CN110627108A CN 110627108 A CN110627108 A CN 110627108A CN 201910922111 A CN201910922111 A CN 201910922111A CN 110627108 A CN110627108 A CN 110627108A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/16—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements
- G01K7/18—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements the element being a linear resistance, e.g. platinum resistance thermometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
The invention relates to a zinc oxide/reduced graphene oxide composite material and a preparation method and application thereof. The composite material has good temperature sensitivity. The preparation method is simple and has little pollution.
Description
Technical Field
The invention belongs to the field of temperature-sensitive materials and preparation and application thereof, and particularly relates to a zinc oxide/reduced graphene oxide composite material and a preparation method and application thereof.
Background
It is well known that temperature is an important physical parameter of human health. Usually, a person first measures his body temperature when he is ill. The normal human body temperature is 36-37 ℃, the human body skin surface temperature is about 25-32 ℃, and the temperature of each region of the human body can reflect the health condition. In fields such as intelligence is dressed, medical equipment, more and more people add temperature sensor into it for detect human health.
Zinc oxide is a semiconductor material having excellent electrical properties, and is widely used as a sensor for pressure, humidity, light sensitivity, and the like. In addition, the zinc oxide is easy to dope, and the micro-nano structure is simple to construct and controllable in appearance. Wangzhining et al, the institute of Zongzhi, discovered that zinc oxide can spontaneously polarize to convert thermal energy into electrical energy during temperature changes over time (Yang Y, Guo W, Pradelk C, et al, pyroelectrolytic nanogenerators for harvesing thermal electrochemical generator, Nano Letter,2012,12(6): 2833-2838.). Therefore, the zinc oxide is very suitable to be used as a temperature-sensitive material to be applied to the temperature sensor.
The reduced graphene oxide is prepared by taking graphite oxide as a raw material and performing thermal reduction, chemical reduction and electrochemical reduction. Compared with graphene oxide, the surface of reduced graphene oxide has fewer oxygen-containing functional groups and has good conductivity. Compared with graphene, the graphene oxide is easier to prepare in a large scale, and can meet practical application.
Pure zinc oxide is relatively resistive and nearly non-conductive. By compounding with graphene, a zinc oxide/reduced graphene oxide composite material having good conductivity can be obtained. The zinc oxide/reduced graphene oxide composite material can be prepared by using a simple solvothermal method, and the temperature sensor can be prepared by simply dripping a layer of the zinc oxide/graphene oxide composite material between two conductive electrodes by a dripping method. The existing temperature carry-on sensor material has the problems of large volume, low sensitivity, complex preparation process and the like. The zinc oxide/reduced graphene oxide composite material has good thermolysis performance of zinc oxide and good conductivity of reduced graphene oxide, and is simple to prepare, safe and reliable. Therefore, the zinc oxide/reduced graphene oxide composite material can greatly improve the performance of the temperature carry-on sensor, and is very suitable for practical application.
Disclosure of Invention
The invention aims to solve the technical problem of providing a zinc oxide/reduced graphene oxide composite material, a preparation method and application thereof, and overcomes the defects of large volume, low sensitivity, complex preparation process and the like of the existing temperature portable sensor material.
The zinc oxide/reduced graphene oxide composite material is a reduced graphene oxide coated single crystal zinc oxide nanorod composite material, wherein the mass ratio of zinc oxide to reduced graphene oxide is 4: 1-20.
The preparation method of the zinc oxide/reduced graphene oxide composite material comprises the following steps:
(1) dissolving zinc salt and sodium acetate in a solvent, and performing ultrasonic treatment to obtain a precursor solution;
(2) dissolving polyethylene glycol in graphene oxide aqueous dispersion, and performing ultrasonic treatment to obtain a solution;
(3) and (3) mixing the precursor solution in the step (1) and the solution in the step (2), carrying out hydrothermal reaction, cooling, filtering, cleaning and collecting to obtain the zinc oxide/reduced graphene oxide composite material.
The preferred mode of the above preparation method is as follows:
the zinc salt in the step (1) is zinc nitrate; the solvent is ethylene glycol.
In the step (1), the mass ratio of the zinc salt to the sodium acetate is 1: 1-10; the mass ratio of the zinc salt to the solvent is 1: 10-90, and the ratio of the zinc nitrate to the ethylene glycol is 1: 30-90.
The polyethylene glycol in the step (2) is polyethylene glycol 2000; the mass fraction of the graphene oxide in the graphene oxide aqueous dispersion is 1-10%.
The mass ratio of the polyethylene glycol 2000 to the graphene oxide aqueous dispersion in the step (2) is 1-5: 30.
The hydrothermal reaction temperature in the step (3) is 150-230 ℃, and the hydrothermal reaction time is 4-20 h.
And (4) cooling in the step (3) to be standing for 2-24 h at room temperature.
And (4) ultrasonically dispersing the zinc oxide/reduced graphene oxide composite material obtained in the step (3) into deionized water again to obtain zinc oxide/reduced graphene oxide composite material slurry, wherein the concentration of the slurry is 1 mg/ml-1 g/ml.
The zinc oxide/reduced graphene oxide composite material prepared by the method is provided.
The application of the zinc oxide/reduced graphene oxide composite material provided by the invention comprises a temperature sensor applied to intelligent wearing and medical equipment, and can realize a portable sensor for detecting the temperature of a human body and monitoring the health of the human body.
Advantageous effects
(1) The zinc oxide/reduced graphene oxide composite material is prepared by mixing a zinc oxide precursor solution and a graphene oxide solution and compounding through a hydrothermal reaction; wherein the zinc oxide precursor solution is prepared by dissolving zinc nitrate and sodium acetate in ethylene glycol; the graphene oxide solution is prepared by dissolving polyethylene glycol 2000 in graphene oxide aqueous dispersion;
(2) the structure of the single crystal zinc oxide nano rod wrapped by the reduced graphene oxide has good temperature sensitivity and stability, the resistance change of the composite material can reach about 190 omega/DEG C within a temperature range from 5 ℃ to 40 ℃, the sensitivity of the resistance change can reach 0.67 percent, and the composite material has wide application prospect in intelligent wearable and medical equipment;
(3) the preparation method has the advantages of simplicity, high efficiency, easy commercial production and the like.
Drawings
Fig. 1 is a transmission electron microscope picture of zinc oxide/reduced graphene oxide;
FIG. 2 is a transmission electron microscope photograph of zinc oxide/reduced graphene oxide;
FIG. 3 is an X-ray diffraction pattern of zinc oxide/reduced graphene oxide;
fig. 4 is a graph showing the change of resistance of the zinc oxide/reduced graphene oxide composite material with temperature, wherein the samples 1, 2 and 3 are obtained by three repeated tests;
fig. 5 is a graph of the percentage of resistance of the zinc oxide/reduced graphene oxide composite material as a function of temperature, wherein samples 1, 2, and 3 were obtained from three replicates.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Zinc nitrate, sodium acetate and ethylene glycol are purchased from chemical reagents of national medicine group, Inc., and are analyzed and purified;
graphene oxide was purchased from hexite materials science and technology ltd, model number: SE 2430;
polyethylene glycol 2000 purchased from chemical reagents of national medicine group, chemical purity, product number 30151426
Example 1
(1) A clear solution was obtained by dissolving 1.36g of zinc nitrate and 4.5g of sodium acetate in 45mL of ethylene glycol and sonicating. And obtaining a precursor solution.
(2) 1.397g of polyethylene glycol is dissolved in 15mL of graphene oxide aqueous dispersion (the mass fraction of graphene oxide is 4%), and ultrasonic treatment is carried out on the solution by using ultrasonic waves until a uniform solution is formed.
(3) The two solutions were mixed. The precursor solution was transferred to a stainless steel autoclave lined with teflon, heated to 180 ℃ and held for 12 hours. After the reaction is finished, standing the autoclave at room temperature for 18h, cleaning and collecting, and ultrasonically dispersing again in deionized water at the concentration of 10mg/ml to obtain the zinc oxide/reduced graphene oxide composite material.
A transmission electron microscopy picture of zinc oxide/reduced graphene oxide is shown in fig. 1, indicating: the zinc oxide nano-rod is wrapped by graphene.
A transmission electron microscopy picture of zinc oxide/reduced graphene oxide is shown in fig. 2, indicating that: the interplanar spacing of zinc oxide was 0.26nm, from which it was judged that the crystal form of zinc oxide was hexagonal.
The resistance of the zinc oxide/reduced graphene oxide composite material with respect to temperature is shown in fig. 3, which shows that: the high intensity diffraction peak (2 θ ═ 10.8 °) of the graphene oxide (001) plane was small in the diffraction pattern, while the diffraction peak of the graphene (002) plane was not observed, indicating that the graphene oxide had been highly reduced, and the zinc oxide nanorods contained in the reduced graphene oxide prevented pi-pi stacking between the reduced graphene oxide layers, without forming a graphite-like layered stack structure.
The resistance of the zinc oxide/reduced graphene oxide composite material with respect to temperature is shown in fig. 4, which shows that: the resistance value of the zinc oxide/reduced graphene oxide composite material is 104And the magnitude order shows that the conductivity of the composite material is improved by reducing the graphene oxide. The resistance value of the zinc oxide/reduced graphene oxide composite material is reduced along with the increase of the temperature, and a better linear relation is presented.
The percentage curve of the resistance of the zinc oxide/reduced graphene oxide composite material as a function of temperature is shown in fig. 5, indicating that: the trends of the curves of the resistance variation of the zinc oxide/reduced graphene oxide composite material sample along with the temperature variation almost coincide, which shows that the composite material has stability on temperature sensing, and the sensitivity of the resistance variation is between 0.6% and 0.7%.
Example 2
(1) A clear solution was obtained by dissolving 1.36g of zinc nitrate and 1.36g of sodium acetate in 15mL of ethylene glycol and sonicating. And obtaining a precursor solution.
(2) 1.397g of polyethylene glycol is dissolved in 10mL of reduced graphene oxide aqueous dispersion (the mass fraction of graphene oxide is 4%), and ultrasonic treatment is carried out on the solution by using ultrasonic waves until a uniform solution is formed.
(3) The two solutions were mixed. The precursor solution was transferred to a teflon lined stainless steel autoclave, heated to 160 ℃ and held for 16 hours. After the reaction is finished, standing the autoclave at room temperature for 18h, cleaning and collecting, and ultrasonically dispersing again in deionized water at the concentration of 100mg/ml to obtain the zinc oxide/reduced graphene oxide composite material.
Example 3
(1) A clear solution was obtained by dissolving 1.36g of zinc nitrate and 8.16g of sodium acetate in 80mL of ethylene glycol and sonicating. And obtaining a precursor solution.
(2) 1.397g of polyethylene glycol is dissolved in 27mL of graphene oxide aqueous dispersion (the mass fraction of graphene oxide is 4%), and ultrasonic treatment is carried out on the solution by using ultrasonic waves until a uniform solution is formed.
(3) The two solutions were mixed. The precursor solution was transferred to a teflon lined stainless steel autoclave, heated to 180 ℃ and held for 14 hours. After the reaction is finished, standing the autoclave at room temperature for 18h, cleaning and collecting, and ultrasonically dispersing again in deionized water at the concentration of 10mg/ml to obtain the zinc oxide/reduced graphene oxide composite material.
Example 4
(1) A clear solution was obtained by sonication of 1.36g of zinc nitrate and 2.72g of sodium acetate in 25mL of ethylene glycol. And obtaining a precursor solution.
(2) 1.397g of polyethylene glycol is dissolved in 10mL of graphene oxide aqueous dispersion (the mass fraction of graphene oxide is 4%), and ultrasonic treatment is carried out on the solution by using ultrasonic waves until a uniform solution is formed.
(3) The two solutions were mixed. The precursor solution was transferred to a teflon lined stainless steel autoclave, heated to 170 ℃ and held for 10 hours. After the reaction is finished, the autoclave is naturally cooled to room temperature, cleaned and collected, and ultrasonically dispersed in deionized water again at the concentration of 10mg/ml to obtain the zinc oxide/reduced graphene oxide composite material.
Example 5
(1) A clear solution was obtained by dissolving 1.36g of zinc nitrate and 12.24g of sodium acetate in 120mL of ethylene glycol and sonicating. And obtaining a precursor solution.
(2) 1.397g of polyethylene glycol is dissolved in 40mL of graphene oxide aqueous dispersion (the mass fraction of graphene oxide is 4%), and ultrasonic treatment is carried out on the solution by using ultrasonic waves until a uniform solution is formed.
(3) The two solutions were mixed. The precursor solution was transferred to a teflon lined stainless steel autoclave, heated to 180 ℃ and held for 16 hours. After the reaction is finished, standing the autoclave at room temperature for 18h, cleaning and collecting, and ultrasonically dispersing again in deionized water at the concentration of 10mg/ml to obtain the zinc oxide/reduced graphene oxide composite material.
Comparative example 1
The patent with the application number of 201910293837.2 discloses an ellipsoidal zinc oxide rod/graphene composite material and a preparation method and application thereof, ethanol is added into graphene oxide aqueous dispersion, the hydrothermal temperature is 100-150 ℃, the obtained zinc oxide is ellipsoidal in shape and small in length and diameter, and the zinc oxide graphene composite material is applied to microwave absorption. According to the zinc oxide/reduced graphene oxide composite material prepared by the invention, ethanol is not used as a raw material, ethylene glycol and polyethylene glycol 2000 are used as raw materials, the hydrothermal temperature of the composite material is 150-230 ℃, the obtained zinc oxide micro-nano rod-shaped material has a large major length-diameter ratio, and the zinc oxide/reduced graphene oxide composite material prepared by the invention is applied to the field of temperature sensors.
Claims (10)
1. A zinc oxide/reduced graphene oxide composite material is a reduced graphene oxide coated single crystal zinc oxide nanorod.
2. A preparation method of a zinc oxide/reduced graphene oxide composite material comprises the following steps:
(1) dissolving zinc salt and sodium acetate in a solvent, and performing ultrasonic treatment to obtain a precursor solution;
(2) dissolving polyethylene glycol in graphene oxide aqueous dispersion, and performing ultrasonic treatment to obtain a solution;
(3) and (3) mixing the precursor solution in the step (1) and the solution in the step (2), carrying out hydrothermal reaction, cooling, filtering and cleaning to obtain the zinc oxide/reduced graphene oxide composite material.
3. The preparation method according to claim 2, wherein the zinc salt in the step (1) is zinc nitrate; the solvent is ethylene glycol.
4. The preparation method according to claim 2, wherein in the step (1), the zinc salt and the sodium acetate are mixed in a mass ratio of 1: 1-10; the mass ratio of the zinc salt to the solvent is 1: 10-90.
5. The method according to claim 2, wherein the polyethylene glycol in the step (2) is polyethylene glycol 2000; the mass fraction of the graphene oxide in the graphene oxide aqueous dispersion is 1-10%.
6. The preparation method according to claim 2, wherein the mass ratio of the polyethylene glycol 2000 to the graphene oxide aqueous dispersion in the step (2) is 1-5: 30.
7. The preparation method according to claim 2, wherein the hydrothermal reaction temperature in the step (3) is 150 ℃ to 230 ℃ and the hydrothermal reaction time is 4h to 20 h.
8. The preparation method according to claim 2, wherein the zinc oxide/reduced graphene oxide composite material obtained in the step (3) is re-ultrasonically dispersed in deionized water to obtain zinc oxide/reduced graphene oxide composite material slurry, and the concentration of the slurry is 1 mg/ml-1 g/ml.
9. A zinc oxide/reduced graphene oxide composite material prepared by the method of claim 2.
10. Use of the zinc oxide/reduced graphene oxide composite material according to claim 1.
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