CN114477152A - Silver nanoparticle/multilayer graphene composite material and preparation method thereof - Google Patents
Silver nanoparticle/multilayer graphene composite material and preparation method thereof Download PDFInfo
- Publication number
- CN114477152A CN114477152A CN202111680720.3A CN202111680720A CN114477152A CN 114477152 A CN114477152 A CN 114477152A CN 202111680720 A CN202111680720 A CN 202111680720A CN 114477152 A CN114477152 A CN 114477152A
- Authority
- CN
- China
- Prior art keywords
- multilayer graphene
- silver
- composite material
- solution
- dispersion liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- 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
- C01B32/19—Preparation by exfoliation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C01B32/194—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
- C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
Abstract
The invention discloses a silver nanoparticle/multilayer graphene composite material and a preparation method thereof. The silver nanoparticles on the surface of the multilayer graphene are uniformly distributed, and the particle size is about 50 nm-100 nm. The invention discloses a method for preparing a silver nanoparticle/multilayer graphene composite material by adsorbing a silver-ammonia complex on the basis of the surface molecular force of multilayer graphene. The composite material has potential application in the fields of conductive adhesive, conductive films, flexible transmission, electrostatic shielding, pressure sensors, catalysts, antibacterial property, photoelectric materials and the like.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of a silver nanoparticle/multilayer graphene composite material.
Background
The nano Ag particles have wide application in the aspects of catalysts, antibacterial materials, photoelectric materials, flexible pressure sensors and the like. The preparation method of the nano silver can meet the application requirements of different fields (uniform particle size, good particle dispersibility, consistent surface structure and long-term storage without agglomeration). Graphene is a good carrier, and has a very stable structure, excellent electric transport properties, mechanical properties and surface chemical properties.
At present, raw materials selected by the prepared silver/graphene composite material are generally Graphene Oxide (GO) and silver nitrate (AgNO)3) The silver nanoparticle/graphene composite material is prepared by adsorbing silver ions by using active functional groups contained in graphene oxide and adding a reducing agent, but the material preparation cost is high due to the high price of the graphene oxide, and the material is not suitable for large-scale production. Meanwhile, the conductivity of the graphene oxide is greatly reduced due to the damage of the carbon ring. Where high conductivity is required, the performance of such composites using graphene oxide as a substrate can be affected. The multilayer graphene is low in price, has excellent electrochemical performance, and can be used as a carrier. However, the surface of the multilayer graphene has no active functional group, so that it is difficult to directly deposit nano silver particles on the surface of the multilayer graphene without oxidation treatment, and a scheme which is not disclosed at present is not provided.
Aiming at the defects in the prior art, the invention provides a technical scheme to solve the technical problem that uniform nano silver particles cannot be deposited on the surface of multi-layer graphene without activation in the prior art.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a silver nanoparticle/multilayer graphene composite material prepared by adsorbing a silver-ammonia complex through molecular force based on multilayer graphene and a preparation method thereof. The silver nanoparticle/multilayer graphene composite material prepared by the invention is composed of a multilayer graphene substrate and nano silver particles uniformly distributed on the surface of the multilayer graphene substrate.
In order to solve the technical problems in the prior art, the technical scheme of the invention is as follows:
a silver nanoparticle/multilayer graphene composite material is composed of a multilayer graphene substrate and nano silver particles uniformly distributed on the surface of the multilayer graphene substrate; the multilayer graphene is prepared by a mechanical stripping method, the thickness is about 3-6 nm, and oxygen-containing functional groups on the surface are few; the silver nanoparticles on the surface of the multilayer graphene are prepared by an in-situ chemical method, are uniformly distributed on the surface of the multilayer graphene, and have the particle size of about 50 nm-100 nm.
As a further improvement scheme, silver ions are adsorbed by the surface molecular force of the multilayer graphene after forming a silver-ammonia complex, and generated silver nanoparticles are uniformly distributed on the surface of the multilayer graphene through the reduction of ascorbic acid.
The invention also discloses a preparation method of the silver nanoparticle/multilayer graphene composite material, which comprises the following steps:
step S1, weighing DMF and deionized water in a volume ratio of 8:2, pouring the DMF and the deionized water into a small glass bottle, and uniformly mixing the DMF and the deionized water to obtain a mixed solvent A;
step S2, weighing expanded graphite, adding the weighed expanded graphite into the mixed solvent A, and performing ultrasonic treatment for 4 hours by using an ultrasonic machine to obtain a uniform dispersion liquid, wherein the dispersion liquid is a multilayer graphene dispersion liquid C, and the concentration of the expanded graphite relative to the mixed solvent A is 0.5-2 mg/mL;
step S3, pouring the solution C into a polytetrafluoroethylene tank, weighing silver nitrate and ammonia water, and adding the silver nitrate and the ammonia water into the solution C; stirring the solution C for 10 minutes by using a magnetic stirrer at normal temperature, wherein the rotating speed is 300 revolutions per minute; the concentration of silver nitrate relative to the mixed solvent A is 6-12 mg/mL, and the ratio of the volume (mu L) of ammonia water to the mass (mg) of silver nitrate is 5: 3;
step S4, taking out the solution C, weighing ascorbic acid and anhydrous sodium acetate, adding the ascorbic acid and the anhydrous sodium acetate into the solution C, stirring the solution C for 10 minutes at normal temperature by using a magnetic stirrer at the rotating speed of 300 revolutions per minute, and then putting the solution C into a water bath at the temperature of 40-50 ℃ for magnetic stirring reaction for 1-2 hours at the rotating speed of 300 revolutions per minute, wherein the molar ratio of the ascorbic acid to the silver nitrate is 0.4:1, and the molar ratio of the anhydrous sodium acetate to the silver nitrate is 6.9: 1;
step S5, cooling the solution C, and then carrying out centrifugal cleaning, wherein the centrifugal cleaning adopts 3 times of deionized water and 3 times of alcohol centrifugal cleaning; and (3) after cleaning, placing the obtained product in an oven to dry for 24 hours at 70 ℃, and drying to obtain the silver nanoparticle/multilayer graphene composite material.
As a further improvement scheme, DMF and deionized water in a volume ratio of 8:2 are used as solvents, and the multilayer graphene can effectively adsorb the silver complex.
As a further improvement scheme, silver ions are adsorbed by the surface molecular force of the multilayer graphene after forming a silver-ammonia complex, and generated silver nanoparticles are uniformly distributed on the surface of the multilayer graphene through the reduction of ascorbic acid.
As a further improvement scheme, the diameter of the nano-silver particles can be reduced by adding anhydrous sodium acetate, and the distribution uniformity of the nano-silver particles on the surface of the multilayer graphene is improved. The multilayer graphene is prepared by a mechanical stripping method, and the thickness of the multilayer graphene is about 3-6 nm. The silver nanoparticles on the surface of the multilayer graphene are uniformly distributed, and the particle size is about 50 nm-100 nm.
As a further improvement, the multilayer graphene is used as a substrate, and silver ions form a silver-ammonia complex, so that the silver-ammonia complex is attached to the surface of the multilayer graphene; the silver nano-particles obtained by the reduction of ascorbic acid have the particle size of 50 nm-100 nm.
In the technical scheme, sodium acetate is used as a dispersing agent, so that the silver nanoparticles are distributed more uniformly.
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation of the substrate multilayer graphene is simple, the cost is low, and the silver nanoparticles can be deposited without activating the surface of the multilayer graphene.
(2) After silver ions form a silver-ammonia complex, the silver ions are adsorbed by the surface molecular force of the multilayer graphene, and the generated silver nanoparticles are uniformly distributed on the surface of the multilayer graphene through the reduction of ascorbic acid. The preparation process is simple and the preparation efficiency is high.
(3) The silver nanoparticles are completely deposited on the surface of the multilayer graphene, and the silver nanoparticles are uniformly distributed on the surface of the multilayer graphene.
(4) The material has potential application in the fields of flexible pressure sensors, conductive coatings, catalysts, antibiosis and the like.
Drawings
Fig. 1 is a flowchart illustrating steps of a method for preparing nano silver particles uniformly distributed on multi-layered graphene according to example 1 of the present invention;
fig. 2 is a low-power scanning electron microscope image of the method for preparing silver nanoparticles uniformly distributed on multilayer graphene according to example 1 of the present invention;
fig. 3 is a high-power scanning electron microscope image of the method for preparing silver nanoparticles uniformly distributed on multilayer graphene according to example 1 of the present invention;
Detailed Description
Preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
The preparation of the multilayer graphene is simple, but the multilayer graphene is not subjected to activation treatment, and the surface of the multilayer graphene does not contain an oxygen-containing functional group, so that silver ions or silver ammonia ions cannot be adsorbed by active groups on the surface. In order to prepare the silver nanoparticle/multilayer graphene composite material, the invention provides the following technical scheme.
Referring to fig. 1, a flow chart of a method for preparing a silver nanoparticle/multilayer graphene composite material according to the present invention is shown, and includes the following steps:
step S1, weighing DMF and deionized water in a volume ratio of 8:2, pouring the DMF and the deionized water into a small glass bottle, and uniformly mixing the DMF and the deionized water to obtain a mixed solvent A;
step S2, weighing expanded graphite, adding the weighed expanded graphite into the mixed solvent A, and performing ultrasonic treatment for 4 hours by using an ultrasonic machine to obtain a uniform dispersion liquid, wherein the dispersion liquid is a multilayer graphene dispersion liquid C, and the concentration of the expanded graphite relative to the mixed solvent A is 0.5-2 mg/mL;
step S3, pouring the solution C into a polytetrafluoroethylene tank, weighing silver nitrate and ammonia water, and adding the silver nitrate and the ammonia water into the solution C; stirring the solution C for 10 minutes by using a magnetic stirrer at normal temperature, wherein the rotating speed is 300 revolutions per minute; the concentration of silver nitrate relative to the mixed solvent A is 6-12 mg/mL, and the ratio of the volume (mu L) of ammonia water to the mass (mg) of silver nitrate is 5: 3;
step S4, taking out the solution C, weighing ascorbic acid and anhydrous sodium acetate, adding the ascorbic acid and the anhydrous sodium acetate into the solution C, stirring the solution C for 10 minutes at normal temperature by using a magnetic stirrer at the rotating speed of 300 revolutions per minute, and then putting the solution C into a water bath at the temperature of 40-50 ℃ for magnetic stirring reaction for 1-2 hours at the rotating speed of 300 revolutions per minute, wherein the molar ratio of the ascorbic acid to the silver nitrate is 0.4:1, and the molar ratio of the anhydrous sodium acetate to the silver nitrate is 6.9: 1;
step S5, cooling the solution C, and then carrying out centrifugal cleaning, wherein the centrifugal cleaning adopts 3 times of deionized water and 3 times of alcohol centrifugal cleaning; and (3) after cleaning, placing the obtained product in an oven to dry for 24 hours at 70 ℃, and drying to obtain the silver nanoparticle/multilayer graphene composite material.
In the technical scheme, silver ions form a silver-ammonia complex, the silver-ammonia complex is adsorbed by the surface molecular force of the multilayer graphene, and the generated silver nanoparticles are uniformly distributed on the surface of the multilayer graphene through the reduction of ascorbic acid.
Meanwhile, the multilayer graphene is used as a substrate, and the silver ammonia solution is used as a silver source, so that silver nitrate is attached to the surface of the multilayer graphene; the silver nano-particles obtained by the reduction of ascorbic acid have the particle size of 50 nm-100 nm.
As a further improvement scheme, DMF and deionized water in a volume ratio of 8:2 are used as solvents, and the multilayer graphene can effectively adsorb the silver complex.
As a further improvement scheme, the diameter of the nano-silver particles can be reduced by adding anhydrous sodium acetate, and the distribution uniformity of the nano-silver particles on the surface of the multilayer graphene is improved. The multilayer graphene is prepared by a mechanical stripping method, and the thickness of the multilayer graphene is about 3-6 nm. The silver nanoparticles on the surface of the multilayer graphene are uniformly distributed, and the particle size is about 50 nm-100 nm.
The silver nanoparticle/multilayer graphene composite material prepared by the method consists of a multilayer graphene substrate and nano silver particles uniformly distributed on the surface of the multilayer graphene substrate; the multilayer graphene is prepared by a mechanical stripping method, the thickness is about 3-6 nm, and oxygen-containing functional groups on the surface are few; the silver nanoparticles on the surface of the multilayer graphene are grown in situ by a chemical method, are uniformly distributed, and have the particle size of about 50 nm-100 nm.
The technical scheme of the invention is further explained by combining specific examples.
EXAMPLE 1
Weighing 8mL of DMF and 2mL of deionized water, pouring into a small glass bottle, and uniformly mixing to obtain a mixed solvent; weighing 20mg of expanded graphite, adding the expanded graphite into a mixed solvent, and performing ultrasonic treatment for 4 hours by using an ultrasonic machine to obtain a uniform multilayer graphene dispersion liquid; and then pouring the multilayer graphene dispersion liquid into a polytetrafluoroethylene tank, weighing 60mg of silver nitrate and 100 mu L of ammonia water, adding the silver nitrate and the ammonia water into the multilayer graphene dispersion liquid, stirring the dispersion liquid for 10 minutes by using a magnetic stirrer at normal temperature, then weighing 25mg of ascorbic acid and 200mg of anhydrous sodium acetate, adding the ascorbic acid and the anhydrous sodium acetate into the dispersion liquid, stirring the dispersion liquid for 10 minutes by using the magnetic stirrer at normal temperature, transferring the dispersion liquid into a 50 ℃ water bath kettle, and stirring the dispersion liquid in the water bath at the rotating speed of 300 revolutions per minute for 2 hours. And (3) carrying out deionized water and alcohol centrifugal cleaning on the reacted product for 3 times, and placing the cleaned product in an oven to dry for 24 hours at 70 ℃ to obtain dry silver nanoparticle/multilayer graphene composite material powder.
The composite material powder obtained by the preparation was subjected to SEM observation, and fig. 2 and 3 are SEM images at different magnifications. From the figure, the silver nanoparticles are small in size, the diameter is between 50nm and 100nm, and the silver nanoparticles are uniformly distributed on the surface of the multilayer graphene. The surface of the multilayer graphene is not subjected to activation treatment, and silver ions or silver ammonia ions cannot be adsorbed by an activated group. According to the invention, the mixed solvent of DMF and water is adopted, so that silver ammonia ions can be adsorbed by the molecular force on the surface of the multilayer graphene in the mixed solvent of DMF and water, and the silver ammonia complex cannot be adsorbed in a large amount due to weaker molecular force, and can only be adsorbed on the surface of the multilayer graphene uniformly. Therefore, after reduction, the nano-silver particles are uniform in size and are also uniformly distributed on the surface of the multilayer graphene.
Instantiation 2
Weighing 8mL of DMF and 2mL of deionized water, pouring into a small glass bottle, and uniformly mixing to obtain a mixed solvent; weighing 20mg of expanded graphite, adding the expanded graphite into a mixed solvent, and performing ultrasonic treatment for 4 hours by using an ultrasonic machine to obtain a uniform multilayer graphene dispersion liquid; and then pouring the multilayer graphene dispersion liquid into a polytetrafluoroethylene tank, weighing 60mg of silver nitrate and 100 mu L of ammonia water, adding the silver nitrate and the ammonia water into the multilayer graphene dispersion liquid, stirring the dispersion liquid for 10 minutes by using a magnetic stirrer at normal temperature, weighing 25mg of ascorbic acid and 200mg of anhydrous sodium acetate, adding the ascorbic acid and the anhydrous sodium acetate into the dispersion liquid, stirring the dispersion liquid for 10 minutes by using the magnetic stirrer at normal temperature, transferring the dispersion liquid into a water bath kettle at 50 ℃, and stirring the dispersion liquid in a water bath at the rotating speed of 300 revolutions per minute for 1 hour. And (3) carrying out deionized water and alcohol centrifugal cleaning on the reacted product for 3 times, and placing the cleaned product in an oven to dry for 24 hours at 70 ℃ to obtain dry silver nanoparticle/multilayer graphene composite material powder.
Instantiation 3
Weighing 8mL of DMF and 2mL of deionized water, pouring into a small glass bottle, and uniformly mixing to obtain a mixed solvent; weighing 20mg of expanded graphite, adding the expanded graphite into a mixed solvent, and performing ultrasonic treatment for 4 hours by using an ultrasonic machine to obtain a uniform multilayer graphene dispersion liquid; and then pouring the multilayer graphene dispersion liquid into a polytetrafluoroethylene tank, weighing 120mg of silver nitrate and 200 mu L of ammonia water, adding the silver nitrate and the ammonia water into the multilayer graphene dispersion liquid, stirring the dispersion liquid for 10 minutes by using a magnetic stirrer at normal temperature, then weighing 50mg of ascorbic acid and 399mg of anhydrous sodium acetate, adding the ascorbic acid and the anhydrous sodium acetate into the dispersion liquid, stirring the dispersion liquid for 10 minutes by using the magnetic stirrer at normal temperature, transferring the dispersion liquid into a water bath kettle at 40 ℃, and stirring the dispersion liquid in the water bath at the rotating speed of 300 revolutions per minute for 2 hours. And (3) carrying out deionized water and alcohol centrifugal cleaning on the reacted product for 3 times, and placing the cleaned product in an oven to dry for 24 hours at 70 ℃ to obtain dry silver nanoparticle/multilayer graphene composite material powder.
Instantiation 4
Weighing 8mL of DMF and 2mL of deionized water, pouring into a small glass bottle, and uniformly mixing to obtain a mixed solvent; weighing 5mg of expanded graphite, adding the expanded graphite into a mixed solvent, and performing ultrasonic treatment for 4 hours by using an ultrasonic machine to obtain a uniform multilayer graphene dispersion liquid; and then pouring the multilayer graphene dispersion liquid into a polytetrafluoroethylene tank, weighing 80mg of silver nitrate and 133 mu L of ammonia water, adding the silver nitrate and the 133 mu L of ammonia water into the multilayer graphene dispersion liquid, stirring the dispersion liquid for 10 minutes by using a magnetic stirrer at normal temperature, then weighing 33mg of ascorbic acid and 266mg of anhydrous sodium acetate, adding the ascorbic acid and the 266mg of anhydrous sodium acetate into the dispersion liquid, stirring the dispersion liquid for 10 minutes by using the magnetic stirrer at normal temperature, transferring the dispersion liquid into a water bath kettle at 40 ℃, and stirring the dispersion liquid in a water bath at the rotating speed of 300 revolutions per minute for 1 hour. And (3) carrying out deionized water and alcohol centrifugal cleaning on the reacted product for 3 times, and placing the cleaned product in an oven to dry for 24 hours at 70 ℃ to obtain dry silver nanoparticle/multilayer graphene composite material powder.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. The silver nanoparticle/multilayer graphene composite material is characterized by comprising a multilayer graphene substrate and nano silver particles uniformly distributed on the surface of the multilayer graphene substrate; the multilayer graphene is prepared by a mechanical stripping method, the thickness is about 3-6 nm, and oxygen-containing functional groups on the surface are few; the silver nanoparticles on the surface of the multilayer graphene are prepared by an in-situ chemical method, are uniformly distributed on the surface of the multilayer graphene, and have the particle size of about 50 nm-100 nm.
2. The silver nanoparticle/multilayer graphene composite material of claim 1, wherein silver ions are adsorbed by the surface molecular force of the multilayer graphene after forming a silver-ammonia complex, and the generated silver nanoparticles are uniformly distributed on the surface of the multilayer graphene through the reduction of ascorbic acid.
3. A preparation method of a silver nanoparticle/multilayer graphene composite material is characterized by comprising the following steps:
step S1, weighing DMF and deionized water in a volume ratio of 8:2, pouring the DMF and the deionized water into a small glass bottle, and uniformly mixing the DMF and the deionized water to obtain a mixed solvent A;
step S2, weighing expanded graphite, adding the weighed expanded graphite into the mixed solvent A, and performing ultrasonic treatment for 4 hours by using an ultrasonic machine to obtain a uniform dispersion liquid, wherein the dispersion liquid is a multilayer graphene dispersion liquid C, and the concentration of the expanded graphite relative to the mixed solvent A is 0.5-2 mg/mL;
step S3, pouring the solution C into a polytetrafluoroethylene tank, weighing silver nitrate and ammonia water, and adding the silver nitrate and the ammonia water into the solution C; stirring the solution C for 10 minutes by using a magnetic stirrer at normal temperature, wherein the rotating speed is 300 revolutions per minute; the concentration of silver nitrate relative to the mixed solvent A is 6-12 mg/mL, and the ratio of the volume (mu L) of ammonia water to the mass (mg) of silver nitrate is 5: 3;
step S4, taking out the solution C, weighing ascorbic acid and anhydrous sodium acetate, adding the ascorbic acid and the anhydrous sodium acetate into the solution C, stirring the solution C for 10 minutes at normal temperature by using a magnetic stirrer at the rotating speed of 300 revolutions per minute, and then putting the solution C into a water bath at the temperature of 40-50 ℃ for magnetic stirring reaction for 1-2 hours at the rotating speed of 300 revolutions per minute, wherein the molar ratio of the ascorbic acid to the silver nitrate is 0.4:1, and the molar ratio of the anhydrous sodium acetate to the silver nitrate is 6.9: 1;
step S5, cooling the solution C, and then carrying out centrifugal cleaning, wherein the centrifugal cleaning adopts 3 times of deionized water and 3 times of alcohol centrifugal cleaning; and (3) after cleaning, placing the obtained product in an oven to dry for 24 hours at 70 ℃, and drying to obtain the silver nanoparticle/multilayer graphene composite material.
4. The method for preparing the silver nanoparticle/multilayer graphene composite material of claim 3, wherein the multilayer graphene can effectively adsorb a silver complex by using DMF and deionized water in a volume ratio of 8:2 as solvents.
5. The method for preparing the silver nanoparticle/multilayer graphene composite material according to claim 3, wherein silver ions are adsorbed by the surface molecular force of the multilayer graphene after forming a silver-ammonia complex, and the generated silver nanoparticles are uniformly distributed on the surface of the multilayer graphene through the reduction of ascorbic acid. Due to the weak molecular force, the silver-ammonia complex cannot be adsorbed in a large amount and can only be uniformly adsorbed on the surface of the multilayer graphene. Therefore, after reduction, the nano-silver particles are uniform in size and are also uniformly distributed on the surface of the multilayer graphene.
6. The method for preparing the silver nanoparticle/multilayer graphene composite material of claim 3, wherein the addition of anhydrous sodium acetate can prevent the growth of the nano silver, reduce the diameter of the nano silver particles, and improve the distribution uniformity of the nano silver particles on the surface of the multilayer graphene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111680720.3A CN114477152B (en) | 2021-12-30 | 2021-12-30 | Silver nanoparticle/multilayer graphene composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111680720.3A CN114477152B (en) | 2021-12-30 | 2021-12-30 | Silver nanoparticle/multilayer graphene composite material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114477152A true CN114477152A (en) | 2022-05-13 |
| CN114477152B CN114477152B (en) | 2023-08-15 |
Family
ID=81510072
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111680720.3A Active CN114477152B (en) | 2021-12-30 | 2021-12-30 | Silver nanoparticle/multilayer graphene composite material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114477152B (en) |
Citations (34)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101740785A (en) * | 2009-12-14 | 2010-06-16 | 浙江大学 | Palladium/graphene nano electro-catalyst and preparation method thereof |
| CN102614871A (en) * | 2012-03-05 | 2012-08-01 | 天津大学 | Method for preparing grapheme/silver nanoparticles composite material by using liquid phase method |
| WO2013137654A1 (en) * | 2012-03-15 | 2013-09-19 | 주식회사 동진쎄미켐 | Metal-plate graphene powder, and electromagnetic interference shielding coating composition containing same |
| KR20140014700A (en) * | 2012-07-25 | 2014-02-06 | 서울대학교산학협력단 | Synthesis method of urchin-like copper oxide nanostructures decorated graphene nanosheet |
| US20140121425A1 (en) * | 2012-07-27 | 2014-05-01 | Lawrence Livermore National Security, Llc | High surface area graphene-supported metal chalcogenide assembly |
| US20140161972A1 (en) * | 2012-12-09 | 2014-06-12 | National Sun Yat-Sen University | Method for forming conductive film at room temperature |
| CN104148666A (en) * | 2014-07-26 | 2014-11-19 | 哈尔滨工业大学 | Method for modifying graphene through nano-sliver |
| CN104591174A (en) * | 2015-01-23 | 2015-05-06 | 西安理工大学 | Preparation method of silver nanocrystal-multilayer graphene composite material |
| WO2015142159A1 (en) * | 2014-03-17 | 2015-09-24 | Universiti Kebangsaan Malaysia | A method for preparing a cellulose based material |
| CN105237847A (en) * | 2015-08-27 | 2016-01-13 | 常州大学 | Preparation method of silver-plated graphene, and application of the silver-plated graphene in electric-conductive flame-retarding high-density polyethylene explosion-inhibiting material |
| CN105329851A (en) * | 2015-11-02 | 2016-02-17 | 杭州电子科技大学 | Preparation method of nano iron oxide-multilayered graphene composite material |
| CN105562707A (en) * | 2015-12-23 | 2016-05-11 | 陈添乾 | Preparation method for silver-graphene composite and application method of silver-graphene composite to preparing silver-graphene alloy wire |
| WO2016145985A1 (en) * | 2015-03-18 | 2016-09-22 | 上海和伍复合材料有限公司 | Graphene/silver composite material and preparation method thereof |
| WO2016172755A1 (en) * | 2015-04-28 | 2016-11-03 | Monash University | Non-covalent magnetic graphene oxide composite material and method of production thereof |
| CN106935826A (en) * | 2017-03-23 | 2017-07-07 | 江西理工大学 | The lithium ion battery preparation method of nano cupric oxide graphene composite material |
| CN107096529A (en) * | 2017-04-12 | 2017-08-29 | 浙江大学 | A kind of graphene aerogel of minimum particle size of nanometer silver load and its preparation method and application |
| US20170341939A1 (en) * | 2016-05-31 | 2017-11-30 | Gachon University Of Industry-Academic Cooperation Foundation | Graphene metal nanoparticle-composite |
| CN107417962A (en) * | 2017-07-28 | 2017-12-01 | 合肥泓定科技有限公司 | A kind of purification of air graphene sponge and preparation method thereof |
| CN107502138A (en) * | 2017-08-29 | 2017-12-22 | 国家电网公司 | A kind of water-based highly conductive coating of silvering graphite alkene and preparation method thereof |
| CN109103467A (en) * | 2018-08-17 | 2018-12-28 | 北京师范大学 | A kind of preparation method and application of the graphene-based metallic catalyst of electrochemical stripping |
| CN109216670A (en) * | 2018-08-06 | 2019-01-15 | 杭州电子科技大学 | A kind of nano SnO2Particle/multi-layer graphene composite material and preparation method |
| CN109243832A (en) * | 2018-08-06 | 2019-01-18 | 杭州电子科技大学 | A kind of α type Fe2O3Nano particle/multi-layer graphene composite material preparation method |
| CN109231281A (en) * | 2018-08-06 | 2019-01-18 | 杭州电子科技大学 | Fe3O4Preparation method of quasi-cubic particle/multilayer graphene composite material |
| CN109329304A (en) * | 2018-11-27 | 2019-02-15 | 辽宁大学 | Mesoporous graphene-supported silver nano particle composite material of one kind and its preparation method and application |
| CN109368623A (en) * | 2018-09-20 | 2019-02-22 | 苏州博努奇纺织有限公司 | A kind of nano metal intercalated graphite alkene preparation method |
| CN110004713A (en) * | 2019-04-25 | 2019-07-12 | 北京洁尔爽高科技有限公司 | Graphene slurry of argentiferous and preparation method thereof and prepared product |
| CN110201658A (en) * | 2019-04-22 | 2019-09-06 | 杭州电子科技大学 | A kind of preparation method of Titanium dioxide nanoparticle/multi-layer graphene composite material |
| EP3636804A1 (en) * | 2018-10-11 | 2020-04-15 | ABB Schweiz AG | Silver-graphene composite coating for sliding contact and electroplating method thereof |
| CN111348689A (en) * | 2020-02-12 | 2020-06-30 | 杭州电子科技大学 | A kind of Ni (OH)2Graphene composite material and preparation method thereof |
| CN111715889A (en) * | 2020-06-22 | 2020-09-29 | 大连理工大学 | Method for preparing defect-free graphene/silver nanoparticle composite material by one-step method and application of defect-free graphene/silver nanoparticle composite material |
| CN112071507A (en) * | 2020-09-08 | 2020-12-11 | 杭州梵云新材料科技有限公司 | Copper-coated multilayer graphene composite material and preparation method thereof |
| CN113060723A (en) * | 2021-03-18 | 2021-07-02 | 上海健康医学院 | Nano-silver amino modified reduced graphene oxide framework material and preparation method thereof |
| WO2021232597A1 (en) * | 2020-05-21 | 2021-11-25 | 电子科技大学中山学院 | Near-infrared thermal repair flexible conductive film and preparation method therefor |
| CN113772661A (en) * | 2021-10-29 | 2021-12-10 | 浙江理工大学 | Preparation method of reduced graphene oxide/nano-silver composite film |
-
2021
- 2021-12-30 CN CN202111680720.3A patent/CN114477152B/en active Active
Patent Citations (34)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101740785A (en) * | 2009-12-14 | 2010-06-16 | 浙江大学 | Palladium/graphene nano electro-catalyst and preparation method thereof |
| CN102614871A (en) * | 2012-03-05 | 2012-08-01 | 天津大学 | Method for preparing grapheme/silver nanoparticles composite material by using liquid phase method |
| WO2013137654A1 (en) * | 2012-03-15 | 2013-09-19 | 주식회사 동진쎄미켐 | Metal-plate graphene powder, and electromagnetic interference shielding coating composition containing same |
| KR20140014700A (en) * | 2012-07-25 | 2014-02-06 | 서울대학교산학협력단 | Synthesis method of urchin-like copper oxide nanostructures decorated graphene nanosheet |
| US20140121425A1 (en) * | 2012-07-27 | 2014-05-01 | Lawrence Livermore National Security, Llc | High surface area graphene-supported metal chalcogenide assembly |
| US20140161972A1 (en) * | 2012-12-09 | 2014-06-12 | National Sun Yat-Sen University | Method for forming conductive film at room temperature |
| WO2015142159A1 (en) * | 2014-03-17 | 2015-09-24 | Universiti Kebangsaan Malaysia | A method for preparing a cellulose based material |
| CN104148666A (en) * | 2014-07-26 | 2014-11-19 | 哈尔滨工业大学 | Method for modifying graphene through nano-sliver |
| CN104591174A (en) * | 2015-01-23 | 2015-05-06 | 西安理工大学 | Preparation method of silver nanocrystal-multilayer graphene composite material |
| WO2016145985A1 (en) * | 2015-03-18 | 2016-09-22 | 上海和伍复合材料有限公司 | Graphene/silver composite material and preparation method thereof |
| WO2016172755A1 (en) * | 2015-04-28 | 2016-11-03 | Monash University | Non-covalent magnetic graphene oxide composite material and method of production thereof |
| CN105237847A (en) * | 2015-08-27 | 2016-01-13 | 常州大学 | Preparation method of silver-plated graphene, and application of the silver-plated graphene in electric-conductive flame-retarding high-density polyethylene explosion-inhibiting material |
| CN105329851A (en) * | 2015-11-02 | 2016-02-17 | 杭州电子科技大学 | Preparation method of nano iron oxide-multilayered graphene composite material |
| CN105562707A (en) * | 2015-12-23 | 2016-05-11 | 陈添乾 | Preparation method for silver-graphene composite and application method of silver-graphene composite to preparing silver-graphene alloy wire |
| US20170341939A1 (en) * | 2016-05-31 | 2017-11-30 | Gachon University Of Industry-Academic Cooperation Foundation | Graphene metal nanoparticle-composite |
| CN106935826A (en) * | 2017-03-23 | 2017-07-07 | 江西理工大学 | The lithium ion battery preparation method of nano cupric oxide graphene composite material |
| CN107096529A (en) * | 2017-04-12 | 2017-08-29 | 浙江大学 | A kind of graphene aerogel of minimum particle size of nanometer silver load and its preparation method and application |
| CN107417962A (en) * | 2017-07-28 | 2017-12-01 | 合肥泓定科技有限公司 | A kind of purification of air graphene sponge and preparation method thereof |
| CN107502138A (en) * | 2017-08-29 | 2017-12-22 | 国家电网公司 | A kind of water-based highly conductive coating of silvering graphite alkene and preparation method thereof |
| CN109216670A (en) * | 2018-08-06 | 2019-01-15 | 杭州电子科技大学 | A kind of nano SnO2Particle/multi-layer graphene composite material and preparation method |
| CN109243832A (en) * | 2018-08-06 | 2019-01-18 | 杭州电子科技大学 | A kind of α type Fe2O3Nano particle/multi-layer graphene composite material preparation method |
| CN109231281A (en) * | 2018-08-06 | 2019-01-18 | 杭州电子科技大学 | Fe3O4Preparation method of quasi-cubic particle/multilayer graphene composite material |
| CN109103467A (en) * | 2018-08-17 | 2018-12-28 | 北京师范大学 | A kind of preparation method and application of the graphene-based metallic catalyst of electrochemical stripping |
| CN109368623A (en) * | 2018-09-20 | 2019-02-22 | 苏州博努奇纺织有限公司 | A kind of nano metal intercalated graphite alkene preparation method |
| EP3636804A1 (en) * | 2018-10-11 | 2020-04-15 | ABB Schweiz AG | Silver-graphene composite coating for sliding contact and electroplating method thereof |
| CN109329304A (en) * | 2018-11-27 | 2019-02-15 | 辽宁大学 | Mesoporous graphene-supported silver nano particle composite material of one kind and its preparation method and application |
| CN110201658A (en) * | 2019-04-22 | 2019-09-06 | 杭州电子科技大学 | A kind of preparation method of Titanium dioxide nanoparticle/multi-layer graphene composite material |
| CN110004713A (en) * | 2019-04-25 | 2019-07-12 | 北京洁尔爽高科技有限公司 | Graphene slurry of argentiferous and preparation method thereof and prepared product |
| CN111348689A (en) * | 2020-02-12 | 2020-06-30 | 杭州电子科技大学 | A kind of Ni (OH)2Graphene composite material and preparation method thereof |
| WO2021232597A1 (en) * | 2020-05-21 | 2021-11-25 | 电子科技大学中山学院 | Near-infrared thermal repair flexible conductive film and preparation method therefor |
| CN111715889A (en) * | 2020-06-22 | 2020-09-29 | 大连理工大学 | Method for preparing defect-free graphene/silver nanoparticle composite material by one-step method and application of defect-free graphene/silver nanoparticle composite material |
| CN112071507A (en) * | 2020-09-08 | 2020-12-11 | 杭州梵云新材料科技有限公司 | Copper-coated multilayer graphene composite material and preparation method thereof |
| CN113060723A (en) * | 2021-03-18 | 2021-07-02 | 上海健康医学院 | Nano-silver amino modified reduced graphene oxide framework material and preparation method thereof |
| CN113772661A (en) * | 2021-10-29 | 2021-12-10 | 浙江理工大学 | Preparation method of reduced graphene oxide/nano-silver composite film |
Non-Patent Citations (10)
| Title |
|---|
| JUN BIAN，等: "Highly effective synthesis of dimethyl carbonate from methanol and carbon dioxide using a novel copper–nickel/graphite bimetallic nanocomposite catalyst", CHEMICAL ENGINEERING JOURNAL * |
| LI ZHOU,等: "The Roles of Graphene and Ag in the Hybrid Ag@Ag2O-Graphene for Sulfamethoxazole Degradation", CATALYSTS * |
| ROZALINA ZAKARIA，等: "Investigation on the Effects of the Formation of a Silver "Flower-Like Structure" on Graphene", NANO EXPRESS * |
| SUMIT RANJAN SAHU，等: "Optical Property Characterization of Novel Graphene-X (X=Ag, Au and Cu) Nanoparticle Hybrids", JOURNAL OF NANOMATERIALS * |
| 于美，等: "石墨烯−银纳米粒子复合材料的制备及表征", 《无机材料学报》 * |
| 于美，等: "石墨烯−银纳米粒子复合材料的制备及表征", 《无机材料学报》, 31 January 2012 (2012-01-31), pages 89 - 94 * |
| 刘冉彤;于浩;宋诗稳;杨力;万向权;马壮;: "纳米银/石墨烯电化学传感器的制备及应用研究", 传感器与微***, no. 07 * |
| 柏嵩;沈小平;: "石墨烯基无机纳米复合材料", 化学进展, no. 11 * |
| 简明化学试剂手册编写组: "《简明化学试剂手册》", 31 January 1991, pages: 20 * |
| 郜思衡;杨宇;毋金玲;秦利霞;康诗钊;李向清;: "氧化石墨烯/超细银粒子复合物的制备及其光电性能", 应用化学, no. 08 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114477152B (en) | 2023-08-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101789213B1 (en) | Method of Manufacturing Silver-Coated Copper Nano Wire Having Core-Shell Structure by Chemical Reduction Method | |
| CN106011809B (en) | A method of preparing the composite material of coated with silver on surface by catechol-polyamines | |
| Ma et al. | Preparation and characterization of monodispersed PS/Ag composite microspheres through modified electroless plating | |
| JP4378513B2 (en) | Metal nanoparticles with support, metal nanoparticle continuum and methods for producing them | |
| CN108249482B (en) | Magnetic Fe2O3Preparation method of nano particles and method for compounding nano particles with nano carbon material | |
| CN111515385B (en) | Copper-nickel core-shell type nano powder and conductive film, and preparation method and application thereof | |
| CN110201658B (en) | Preparation method of titanium oxide nanoparticle/multilayer graphene composite material | |
| KR101313149B1 (en) | Fabrication Method of CNT-Metal Composite and Fabrication Method of Conductive Paste Using Thereof | |
| KR20100046459A (en) | Method for making copper-silver shell nanopowders | |
| Dai et al. | Synthesis of silver nanoparticles on functional multi-walled carbon nanotubes | |
| CN114477152B (en) | Silver nanoparticle/multilayer graphene composite material and preparation method thereof | |
| CN111243939A (en) | Method for preparing semiconductor oxide film based on metal powder | |
| CN113649558B (en) | Nano silver wire and preparation method thereof | |
| CN115246949B (en) | Reduced graphene oxide flexible conductive film and three-step moderate reduction preparation process thereof | |
| CN116417198A (en) | Method for directly depositing silver particles on surface of non-activated carbon material multilayer graphene | |
| TW201223876A (en) | High concentration nano-silver colloid and preparation method for nano-silver colloid precursor | |
| CN114464782B (en) | Amorphous ferric oxide nanoparticle/multilayer graphene composite material and preparation method thereof | |
| CN105251996A (en) | Core-shell structure copper-coated iron nanometer composite powder and preparation method and application thereof | |
| TW201430923A (en) | Metal nanoparticles with enhanced stability of oxidation and method of preparing the same | |
| CN116005145B (en) | Preparation method of environment-friendly pollution-free nano-silver modified carbon nanotube | |
| CN115740436B (en) | One-dimensional core-shell structure carbon-coated ferromagnetic nanowire, preparation method and application thereof | |
| Yang et al. | One-step synthesis of ultrathin Ag nanowires with high aspect ratio and their application in transparent conductive films | |
| CN114734036B (en) | Powder for coating silver layer of silver-plated activated substrate of core-shell structure, preparation method and application | |
| CN112063380B (en) | Composite material with metal nanowires wrapped by organic luminescent material and preparation method thereof | |
| CN115644174B (en) | Silver/graphite alkyne composite material and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |