CN111100598A - Zinc oxide/silver/graphene nanocomposite and preparation method and application thereof - Google Patents
Zinc oxide/silver/graphene nanocomposite and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a zinc oxide/silver/graphene nano composite material and a preparation method and application thereof. A preparation method of a zinc oxide/silver/graphene nanocomposite material comprises the following sequential steps: firstly preparing graphene oxide modified with nano-silver particles, and then preparing a zinc oxide/silver/graphene nano composite material. After the zinc oxide/silver/graphene nano composite material prepared by the invention is compounded with polyurethane to form a coating, when the content of the composite material is 10%, the composite material has an obvious ultraviolet absorption function and an electromagnetic shielding effect.
Description
Technical Field
The invention belongs to the field of preparation of polymer-based composite membrane materials, and particularly relates to a zinc oxide/silver/graphene nano composite material as well as a preparation method and application thereof.
Background
The wide use of high-performance communication equipment, computers, smart phones and other terminal products has driven the rapid expansion of electromagnetic shielding and related industrial applications. Among them, silver, which is a metal-based material, has excellent light transmittance and flexibility resistance in addition to a nano-scale dimensional effect, and is an ideal material for electromagnetic shielding materials. The zinc oxide belongs to an N-type semiconductor, and can absorb ultraviolet rays due to the transition of energy in the ultraviolet rays which can be accepted by electrons on a valence band, and the nano zinc oxide can provide broad-spectrum ultraviolet protection and has the functions of antibiosis and anti-inflammation, so the zinc oxide can be used as a material for preventing ultraviolet radiation. The graphene is a novel material with excellent performance, and has good electromagnetic shielding performance and mechanical performance. The organic combination of the nano silver, the zinc oxide and the graphene is an effective way for preparing the ultraviolet-resistant electromagnetic shielding material. Polyurethane is a new organic polymer material, and is widely applied to various fields of national economy such as light industry, chemical industry, electronics, textile, medical treatment, building and the like due to the excellent performance of the polyurethane.
At present, the preparation of the zinc oxide @ silver @ graphene ternary composite nano material is not reported in a public way.
Disclosure of Invention
The invention provides a zinc oxide/silver/graphene nanocomposite material and a preparation method and application thereof.
The invention is realized by adopting the following technical scheme:
a preparation method of a zinc oxide/silver/graphene nanocomposite material comprises the following sequential steps:
1) adding graphene oxide into an ethanol-water mixed solution, and then carrying out ultrasonic treatment for 5-60 minutes to prepare a graphene oxide solution with the concentration of 1-20 mg/mL; the volume ratio of ethanol to water in the ethanol-water mixed solution is 1-10: 1;
2) dropwise adding 3-aminopropyltriethoxysilane into the graphene oxide solution prepared in the step 1), and continuously stirring for 0.5-3.0 hours at room temperature after stirring stably; the volume ratio of the 3-aminopropyltriethoxysilane to the graphene oxide solution prepared in the step 1) is 1: 28-52;
3) dripping a silver nitrate aqueous solution into the solution obtained in the step 2), putting the solution into a reaction kettle after finishing dripping, reacting for 2-24 hours at the temperature of 100-160 ℃, cooling to room temperature to obtain graphene oxide modified with nano-silver particles, washing with ethanol for more than two times, centrifuging, and dissolving the centrifuged graphene oxide modified with nano-silver particles into ethanol for storage; the concentration of silver nitrate in the silver nitrate water solution is 0.01-0.7 mol/L; the volume ratio of the silver nitrate aqueous solution to the solution prepared in the step 2) is 5: 28-52;
4) dissolving zinc acetate dihydrate in dimethyl sulfoxide to obtain a zinc acetate dihydrate dimethyl sulfoxide solution, and then dropwise adding the zinc acetate dihydrate dimethyl sulfoxide solution into the solution prepared in the step 3) in stirring, wherein the dropwise adding speed is 1-2.5 mL/min; the stirring speed is 700-900 rpm; the concentration of zinc acetate dihydrate in the zinc acetate dihydrate dimethyl sulfoxide solution is 1-100mg/1-200 mL; the volume ratio of the zinc acetate dihydrate dimethyl sulfoxide solution to the solution prepared in the step 3) is 20: 16-30;
5) dissolving sodium hydroxide in ethanol to obtain a sodium hydroxide ethanol solution, dropwise adding the sodium hydroxide ethanol solution into the solution obtained in the step 4), and stirring for 2-4 hours after dropwise adding to obtain a zinc oxide/silver/graphene nanocomposite material; the concentration of sodium hydroxide in the sodium hydroxide ethanol solution is 1-50mg/10-200 mL; the volume ratio of the sodium hydroxide ethanol solution to the solution obtained in the step 4) is 40: 30-56.
A zinc oxide/silver/graphene nano composite material is prepared by the method.
The application of the zinc oxide/silver/graphene nano composite material prepared by the method in preparing an electromagnetic shielding uvioresistant multifunctional coating.
The multifunctional electromagnetic shielding and ultraviolet resisting coating is prepared by adding the prepared zinc oxide/silver/graphene nano composite material into waterborne polyurethane, uniformly stirring, coating on a base material, and drying at 80-120 ℃ for 1-10 hours to form the multifunctional electromagnetic shielding and ultraviolet resisting coating, wherein the mass ratio of the zinc oxide/silver/graphene nano composite material to the waterborne polyurethane is 0.1-10: 100.
The principle of the invention is as follows: the electromagnetic shielding and ultraviolet resistant multifunctional coating is mainly prepared from an electromagnetic shielding and ultraviolet resistant multifunctional nano modifier (zinc oxide @ silver @ graphene), namely silver is firstly modified on the graphene, and then the zinc oxide is modified on the graphene. And then compounding the zinc oxide @ silver @ graphene with polyurethane to obtain the coating.
Compared with the prior art, the invention has the following beneficial effects: after the zinc oxide/silver/graphene nanocomposite material prepared by the invention is compounded with polyurethane into a coating, when the content of the composite material is 10%, the zinc oxide/silver/graphene nanocomposite material has an obvious ultraviolet absorption function and an electromagnetic shielding effect.
Drawings
FIG. 1 is a scanning electron micrograph of a zinc oxide @ silver @ graphene ternary composite nanomaterial prepared in an example;
FIG. 2 is an ultraviolet absorption performance of the electromagnetic shielding ultraviolet resistant multifunctional coating of the embodiment;
fig. 3 electromagnetic shielding performance of the electromagnetic shielding ultraviolet resistant multifunctional coating.
Detailed Description
Example 1
A preparation method of a zinc oxide/silver/graphene nanocomposite material comprises the following sequential steps:
1) adding 1mg of graphene oxide into 1mL of ethanol-water mixed solution, and then carrying out ultrasonic treatment for 5 minutes to prepare a graphene oxide solution with the concentration of 1 mg/mL; the volume ratio of ethanol to water in the ethanol-water mixed solution is 1: 1;
2) dropwise adding 3-aminopropyltriethoxysilane into the graphene oxide solution prepared in the step 1), and continuously stirring for 0.5 hour at room temperature after stirring stably; the volume ratio of the 3-aminopropyltriethoxysilane to the graphene oxide solution prepared in the step 1) is 1: 28;
3) dripping a silver nitrate aqueous solution into the solution obtained in the step 2), putting the solution into a reaction kettle after the dripping is finished, reacting for 2 hours at the temperature of 100 ℃, cooling to room temperature to obtain graphene oxide modified with nano-silver particles, washing with ethanol for more than two times, centrifuging, and dissolving the centrifuged graphene oxide modified with nano-silver particles into ethanol for storage; the volume ratio of the silver nitrate aqueous solution to the solution prepared in the step 2) is 5: 28; the concentration of silver nitrate in the silver nitrate water solution is 0.01 mol/L;
4) dissolving zinc acetate dihydrate in dimethyl sulfoxide to obtain a zinc acetate dihydrate dimethyl sulfoxide solution, and then dropwise adding the zinc acetate dihydrate dimethyl sulfoxide solution into the solution prepared in the step 3) in stirring, wherein the dropwise adding speed is 1 mL/min; the stirring speed is 700 r/min; the concentration of zinc acetate dihydrate in the zinc acetate dihydrate dimethyl sulfoxide solution is 1mg/1 mL; the volume ratio of the zinc acetate dihydrate dimethyl sulfoxide solution to the solution prepared in the step 3) is 20: 16;
5) dissolving sodium hydroxide in ethanol to obtain a sodium hydroxide ethanol solution, dropwise adding the sodium hydroxide ethanol solution into the solution obtained in the step 4), and stirring for 2 hours after dropwise adding to obtain a zinc oxide/silver/graphene nanocomposite material; the concentration of sodium hydroxide in the sodium hydroxide ethanol solution is 1mg/10 mL; the volume ratio of the sodium hydroxide ethanol solution to the solution obtained in the step 4) is 40: 30.
A zinc oxide/silver/graphene nano composite material is prepared by the method.
The electromagnetic shielding and ultraviolet resisting multifunctional coating is prepared by adding the zinc oxide/silver/graphene nano composite material into waterborne polyurethane, uniformly stirring, coating on a substrate, and drying at 80 ℃ for 10 hours. Wherein the mass ratio of the zinc oxide/silver/graphene nano composite material to the waterborne polyurethane is 0.1: 100.
Example 2
A preparation method of a zinc oxide/silver/graphene nanocomposite material comprises the following sequential steps:
1) adding 20mg of graphene oxide into 1mL of ethanol-water mixed solution, and then carrying out ultrasonic treatment for 60 minutes to prepare a graphene oxide solution with the concentration of 20 mg/mL; the volume ratio of ethanol to water in the ethanol-water mixed solution is 10: 1;
2) dropwise adding 3-aminopropyltriethoxysilane into the graphene oxide solution prepared in the step 1), and stirring for 3.0 hours at room temperature after stirring stably; the volume ratio of the 3-aminopropyltriethoxysilane to the graphene oxide solution prepared in the step 1) is 1: 52;
3) dripping a silver nitrate aqueous solution into the solution obtained in the step 2), putting the solution into a reaction kettle after finishing dripping, reacting for 2 hours at 160 ℃, cooling to room temperature to obtain graphene oxide modified with nano-silver particles, washing with ethanol for more than two times, centrifuging, and dissolving the centrifuged graphene oxide modified with nano-silver particles into ethanol for storage; the volume ratio of the silver nitrate aqueous solution to the solution prepared in the step 2) is 5: 52; the concentration of silver nitrate in the silver nitrate aqueous solution is 0.5 mol/L;
4) dissolving zinc acetate dihydrate in dimethyl sulfoxide to obtain a zinc acetate dihydrate dimethyl sulfoxide solution, and then dropwise adding the zinc acetate dihydrate dimethyl sulfoxide solution into the solution prepared in the step 3) in stirring, wherein the dropwise adding speed is 1-2.5 mL/min; the stirring speed is 900 revolutions per minute; the concentration of zinc acetate dihydrate in the zinc acetate dihydrate dimethyl sulfoxide solution is 1mg/2 mL; the volume ratio of the zinc acetate dihydrate dimethyl sulfoxide solution to the solution prepared in the step 3) is 20: 30;
5) dissolving sodium hydroxide in ethanol to obtain a sodium hydroxide ethanol solution, dropwise adding the sodium hydroxide ethanol solution into the solution obtained in the step 4), and stirring for 2 hours after dropwise adding to obtain a zinc oxide/silver/graphene nanocomposite material; the concentration of sodium hydroxide in the sodium hydroxide ethanol solution is 50mg/200 mL; the volume ratio of the sodium hydroxide ethanol solution to the solution obtained in the step 4) is 40: 56.
A zinc oxide/silver/graphene nano composite material is prepared by the method.
The electromagnetic shielding and ultraviolet resisting multifunctional coating is prepared by adding the zinc oxide/silver/graphene nano composite material into waterborne polyurethane, uniformly stirring, coating on a substrate, and drying at 120 ℃ for 1 hour. Wherein the mass ratio of the zinc oxide/silver/graphene nano composite material to the waterborne polyurethane is 10: 100.
Example 3
A preparation method of a zinc oxide/silver/graphene nanocomposite material comprises the following sequential steps:
1) adding 10mg of graphene oxide into 1mL of ethanol-water mixed solution, and then carrying out ultrasonic treatment for 30 minutes to prepare a graphene oxide solution with the concentration of 10 mg/mL; the volume ratio of ethanol to water in the ethanol-water mixed solution is 51;
2) dropwise adding 3-aminopropyltriethoxysilane into the graphene oxide solution prepared in the step 1), and stirring for 2.0 hours at room temperature after stirring stably; the volume ratio of the 3-aminopropyltriethoxysilane to the graphene oxide solution prepared in the step 1) is 1: 40;
3) dripping a silver nitrate aqueous solution into the solution obtained in the step 2), putting the solution into a reaction kettle after finishing dripping, reacting for 10 hours at 140 ℃, cooling to room temperature to obtain graphene oxide modified with nano-silver particles, washing with ethanol for more than two times, centrifuging, and dissolving the centrifuged graphene oxide modified with nano-silver particles into ethanol for storage; the volume ratio of the silver nitrate aqueous solution to the solution prepared in the step 2) is 5: 41; the concentration of silver nitrate in the silver nitrate aqueous solution is 0.2 mol/L;
4) dissolving zinc acetate dihydrate in dimethyl sulfoxide to obtain a zinc acetate dihydrate dimethyl sulfoxide solution, and then dropwise adding the zinc acetate dihydrate dimethyl sulfoxide solution into the solution prepared in the step 3) in stirring, wherein the dropwise adding speed is 1.5 mL/min; the stirring speed is 800 r/min; the concentration of zinc acetate dihydrate in the zinc acetate dihydrate dimethyl sulfoxide solution is 100mg/1 mL; the volume ratio of the zinc acetate dihydrate dimethyl sulfoxide solution to the solution prepared in the step 3) is 20: 24;
5) dissolving sodium hydroxide in ethanol to obtain a sodium hydroxide ethanol solution, dropwise adding the sodium hydroxide ethanol solution into the solution obtained in the step 4), and stirring for 2 hours after dropwise adding to obtain a zinc oxide/silver/graphene nanocomposite material; the concentration of sodium hydroxide in the sodium hydroxide ethanol solution is 50mg/10 mL; the volume ratio of the sodium hydroxide ethanol solution to the solution obtained in the step 4) is 40: 43.
A zinc oxide/silver/graphene nano composite material is prepared by the method.
The electromagnetic shielding and ultraviolet resisting multifunctional coating is prepared by adding the zinc oxide/silver/graphene nano composite material into waterborne polyurethane, uniformly stirring, coating on a base material, and drying at 100 ℃ for 5 hours to form the electromagnetic shielding and ultraviolet resisting multifunctional coating. Wherein the mass ratio of the zinc oxide/silver/graphene nano composite material to the waterborne polyurethane is 5: 100.
according to the surfaces of fig. 2 and 3, when the content of zinc oxide @ silver @ graphene is 0, the coating has no electromagnetic shielding effect. When the content of zinc oxide @ silver @ graphene is 10%, the coating has an obvious electromagnetic shielding effect. When the polyurethane coating containing 10% of zinc oxide @ silver @ graphene has an obvious ultraviolet absorption function, the pure polyurethane coating (0% of zinc oxide @ silver @ graphene) does not have the ultraviolet absorption function.
Claims (4)
1. A preparation method of a zinc oxide/silver/graphene nanocomposite material is characterized by comprising the following steps in sequence:
1) adding graphene oxide into an ethanol-water mixed solution, and then carrying out ultrasonic treatment for 5-60 minutes to prepare a graphene oxide solution with the concentration of 1-20 mg/mL; the volume ratio of ethanol to water in the ethanol-water mixed solution is 1-10: 1;
2) dropwise adding 3-aminopropyltriethoxysilane into the graphene oxide solution prepared in the step 1), and continuously stirring for 0.5-3.0 hours at room temperature after stirring stably; the volume ratio of the 3-aminopropyltriethoxysilane to the graphene oxide solution prepared in the step 1) is 1: 28-52;
3) dripping a silver nitrate aqueous solution into the solution obtained in the step 2), putting the solution into a reaction kettle after finishing dripping, reacting for 2-24 hours at the temperature of 100-160 ℃, cooling to room temperature to obtain graphene oxide modified with nano-silver particles, washing with ethanol for more than two times, centrifuging, and dissolving the centrifuged graphene oxide modified with nano-silver particles into ethanol for storage; the concentration of silver nitrate in the silver nitrate water solution is 0.01-0.7 mol/L; the volume ratio of the silver nitrate aqueous solution to the solution prepared in the step 2) is 5: 28-52;
4) dissolving zinc acetate dihydrate in dimethyl sulfoxide to obtain a zinc acetate dihydrate dimethyl sulfoxide solution, and then dropwise adding the zinc acetate dihydrate dimethyl sulfoxide solution into the solution prepared in the step 3) in stirring, wherein the dropwise adding speed is 1-2.5 mL/min; the stirring speed is 700-900 rpm; the concentration of zinc acetate dihydrate in the zinc acetate dihydrate dimethyl sulfoxide solution is 1-100mg/1-200 mL; the volume ratio of the zinc acetate dihydrate dimethyl sulfoxide solution to the solution prepared in the step 3) is 20: 16-30;
5) dissolving sodium hydroxide in ethanol to obtain a sodium hydroxide ethanol solution, dropwise adding the sodium hydroxide ethanol solution into the solution obtained in the step 4), and stirring for 2-4 hours after dropwise adding to obtain a zinc oxide/silver/graphene nanocomposite material; the concentration of sodium hydroxide in the sodium hydroxide ethanol solution is 1-50mg/10-200 mL; the volume ratio of the sodium hydroxide ethanol solution to the solution obtained in the step 4) is 40: 30-56.
2. A zinc oxide/silver/graphene nanocomposite material is characterized in that: prepared by the method of claim 1.
3. Use of the zinc oxide/silver/graphene nanocomposite prepared by the method of claim 1 in the preparation of electromagnetic shielding uvioresistant multifunctional coatings.
4. An electromagnetic shielding uvioresistant multifunctional coating is characterized in that: adding the zinc oxide/silver/graphene nanocomposite material prepared according to claim 1 into waterborne polyurethane, uniformly stirring, coating on a base material, and drying at 80-120 ℃ for 1-10 hours to form an electromagnetic shielding and ultraviolet resistant multifunctional coating, wherein the mass ratio of the zinc oxide/silver/graphene nanocomposite material to the waterborne polyurethane is 0.1-10: 100.
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