CN114477152B - Silver nanoparticle/multilayer graphene composite material and preparation method thereof - Google Patents
Silver nanoparticle/multilayer graphene composite material and preparation method thereof Download PDFInfo
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- C01B32/00—Carbon; Compounds thereof
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- 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
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- 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. Wherein, silver nano particles on the surface of the multilayer graphene are uniformly distributed, and the particle size is about 50 nm-100 nm. The invention prepares a silver nanoparticle/multilayer graphene composite material based on molecular force adsorption of silver ammonia complex on the surface 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-time storage without agglomeration). Graphene is a good carrier, has a very stable structure, and has excellent electric transport performance, mechanical performance and surface chemical performance.
At present, raw materials selected from the prepared silver/graphene composite material are generally Graphene Oxide (GO) and silver nitrate (AgNO) 3 ) The active functional groups contained in the graphene oxide are utilized to adsorb silver ions, and a reducing agent is added to prepare the silver nanoparticle/graphene composite material, but the graphene oxide is high in price, so that the material preparation cost is high, and the material is not suitable for large-scale production. Meanwhile, due to the damage of carbon rings, the conductivity of the graphene oxide is greatly reduced. Where high conductivity properties are desired, the properties of such composites employing graphene oxide as a substrate can be affected. The multi-layer graphene is low in price, has excellent electrochemical properties, and can be used as a carrier. However, the surface of the multilayer graphene has no active functional group, so that the nano silver particles are difficult to directly deposit on the surface of the multilayer graphene which is not subjected to oxidation treatment, and no scheme is disclosed at present.
Aiming at the defects existing 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 the 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 molecular force adsorption of silver-ammonia complex based on multilayer graphene and a preparation method thereof. The silver nanoparticle/multilayer graphene composite material prepared by the invention consists 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:
the silver nanoparticle/multilayer graphene composite material consists of a multilayer graphene substrate and nano silver particles uniformly distributed on the surface of the multilayer graphene substrate; wherein, the multilayer graphene is prepared by a mechanical stripping method, the thickness is about 3-6 nm, and the surface has few oxygen-containing functional groups; silver nano-particles 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 molecular force on the surface of the multilayer graphene after forming silver ammonia complex, and silver nano particles generated by reduction of ascorbic acid are uniformly distributed on the surface of the multilayer graphene.
The invention also discloses a preparation method of the silver nanoparticle/multilayer graphene composite material, which comprises the following steps:
step S1, DMF and deionized water with the volume ratio of 8:2 are measured and poured into a small glass bottle, and the mixture is used as a mixed solvent A after uniform mixing;
s2, weighing expanded graphite, adding the expanded graphite into the mixed solvent A, and performing ultrasonic treatment for 4 hours by using an ultrasonic machine to obtain 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;
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 at normal temperature by using a magnetic stirrer, wherein the rotating speed is 300 revolutions per minute; the concentration of the silver nitrate relative to the mixed solvent A is 6-12 mg/mL, and the mass (mg) ratio of the ammonia water volume (mu L) to the silver nitrate is 5:3;
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, wherein the molar ratio of the ascorbic acid to the silver nitrate is 0.4:1, the molar ratio of the anhydrous sodium acetate to the silver nitrate is 6.9:1, stirring the solution C at normal temperature for 10 minutes by using a magnetic stirrer at the rotating speed of 300 r/min, and then placing 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 r/min;
s5, cooling the solution C, and performing centrifugal cleaning, wherein the centrifugal cleaning adopts 3 times of deionized water and 3 times of alcohol centrifugal cleaning; and (3) placing the silver nano particles in an oven to dry for 24 hours at 70 ℃ after cleaning, and drying to obtain the silver nano particles/multi-layer graphene composite material.
As a further improvement scheme, DMF and deionized water with the volume ratio of 8:2 are adopted as solvents, and the multilayer graphene can effectively adsorb silver complexes.
As a further improvement scheme, silver ions are adsorbed by the molecular force on the surface of the multilayer graphene after forming silver ammonia complex, and silver nano particles generated by reduction of ascorbic acid are uniformly distributed on the surface of the multilayer graphene.
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. Wherein the multilayer graphene is prepared by a mechanical stripping method, and the thickness is about 3-6 nm. The silver nano particles on the surface of the multilayer graphene are uniformly distributed, and the particle size is about 50 nm-100 nm.
As a further improvement scheme, the multilayer graphene is used as a substrate, and silver ions form silver ammine complexes, so that the silver ammine complexes are attached to the surface of the multilayer graphene; the particle size of the silver nano particles obtained through reduction of ascorbic acid is 50 nm-100 nm.
In the technical scheme, sodium acetate is used as a dispersing agent, so that silver nano particles 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 silver nano particles can be deposited without activating the surface of the multilayer graphene.
(2) Silver ions form silver ammonia complexes and are adsorbed by the molecular force on the surface of the multilayer graphene, and the generated silver nano particles are uniformly distributed on the surface of the multilayer graphene through reduction of ascorbic acid. The preparation process is simple and the preparation efficiency is high.
(3) Silver nano-particles are all deposited on the surface of the multilayer graphene, and the silver nano-particles 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 step flow chart of a method for preparing nano silver particles uniformly distributed on the multi-layer graphene of embodiment 1 of the present invention;
FIG. 2 is a low-power scanning electron microscope image of a preparation method of silver nanoparticles uniformly distributed on a multilayer graphene of example 1 of the present invention;
FIG. 3 is a high-power scanning electron microscope image of the preparation method of silver nanoparticles uniformly distributed on the multilayer graphene of the embodiment 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, the surface of the multilayer graphene is not provided with oxygen-containing functional groups, and silver ions or silver ammonia ions cannot be adsorbed through active groups on the surface. In order to prepare the silver nanoparticle/multilayer graphene composite material, the following technical scheme is provided.
Referring to fig. 1, a flow chart of a preparation method of the silver nanoparticle/multilayer graphene composite material of the present invention is shown, comprising the steps of:
step S1, DMF and deionized water with the volume ratio of 8:2 are measured and poured into a small glass bottle, and the mixture is used as a mixed solvent A after uniform mixing;
s2, weighing expanded graphite, adding the expanded graphite into the mixed solvent A, and performing ultrasonic treatment for 4 hours by using an ultrasonic machine to obtain 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;
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 at normal temperature by using a magnetic stirrer, wherein the rotating speed is 300 revolutions per minute; the concentration of the silver nitrate relative to the mixed solvent A is 6-12 mg/mL, and the mass (mg) ratio of the ammonia water volume (mu L) to the silver nitrate is 5:3;
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, wherein the molar ratio of the ascorbic acid to the silver nitrate is 0.4:1, the molar ratio of the anhydrous sodium acetate to the silver nitrate is 6.9:1, stirring the solution C at normal temperature for 10 minutes by using a magnetic stirrer at the rotating speed of 300 r/min, and then placing 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 r/min;
s5, cooling the solution C, and performing centrifugal cleaning, wherein the centrifugal cleaning adopts 3 times of deionized water and 3 times of alcohol centrifugal cleaning; and (3) placing the silver nano particles in an oven to dry for 24 hours at 70 ℃ after cleaning, and drying to obtain the silver nano particles/multi-layer graphene composite material.
According to the technical scheme, silver ions form silver ammonia complexes and are adsorbed by the molecular force on the surface of the multilayer graphene, and the generated silver nano particles are uniformly distributed on the surface of the multilayer graphene through reduction of ascorbic acid.
Meanwhile, the multi-layer 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 multi-layer graphene; the particle size of the silver nano particles obtained through reduction of ascorbic acid is 50 nm-100 nm.
As a further improvement scheme, DMF and deionized water with the volume ratio of 8:2 are adopted as solvents, and the multilayer graphene can effectively adsorb silver complexes.
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. Wherein the multilayer graphene is prepared by a mechanical stripping method, and the thickness is about 3-6 nm. The silver nano particles 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 comprises a multilayer graphene substrate and nano silver particles uniformly distributed on the surface of the multilayer graphene substrate; wherein, the multilayer graphene is prepared by a mechanical stripping method, the thickness is about 3-6 nm, and the surface has few oxygen-containing functional groups; silver nano particles 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 described below by combining specific embodiments.
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 uniform multilayer graphene dispersion; subsequently, the multilayered graphene dispersion was poured into a polytetrafluoroethylene tank, 60mg of silver nitrate was weighed, 100 μl of aqueous ammonia was added to the multilayered graphene dispersion, the dispersion was stirred with a magnetic stirrer at room temperature for 10 minutes, then 25mg of ascorbic acid, 200mg of anhydrous sodium acetate was weighed, added to the dispersion, the dispersion was stirred with a magnetic stirrer at room temperature for 10 minutes, and the dispersion was moved to a 50 ℃ water bath pot, and stirred for 2 hours in a water bath at 300 revolutions per minute Zhong Zhuaisu. And (3) carrying out centrifugal cleaning on the reacted product for 3 times with deionized water and 3 times with alcohol, 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.
SEM observation was performed on the composite powder obtained, and fig. 2 and 3 are SEM images at different magnification. The silver nano particles are smaller in size, the diameter is between 50nm and 100nm, and the silver nano particles are uniformly distributed on the surface of the multi-layer graphene. The surface of the multilayer graphene is not subjected to an activation treatment, and silver ions or silver ammonia ions cannot be adsorbed by an activation group. According to the invention, through adopting the mixed solvent of DMF and water, silver ammonia ions can be adsorbed by the molecular force of 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 weak molecular force effect and can only be uniformly adsorbed on the surface of the multilayer graphene. Therefore, after reduction, the nano silver particles have uniform size and are 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 uniform multilayer graphene dispersion; subsequently, the multilayered graphene dispersion was poured into a polytetrafluoroethylene pot, 60mg of silver nitrate was weighed, 100 μl of aqueous ammonia was added to the multilayered graphene dispersion, after stirring the dispersion with a magnetic stirrer at room temperature for 10 minutes, 25mg of ascorbic acid, 200mg of anhydrous sodium acetate were weighed, added to the dispersion, the dispersion was stirred with a magnetic stirrer at room temperature for 10 minutes, and the dispersion was moved to a 50 ℃ water bath pot, and stirred for 1 hour in a water bath at 300 revolutions per minute Zhong Zhuaisu. And (3) carrying out centrifugal cleaning on the reacted product for 3 times with deionized water and 3 times with alcohol, 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 uniform multilayer graphene dispersion; subsequently, the multilayered graphene dispersion was poured into a polytetrafluoroethylene tank, 120mg of silver nitrate was weighed, 200 μl of aqueous ammonia was added to the multilayered graphene dispersion, the dispersion was stirred with a magnetic stirrer at room temperature for 10 minutes, then 50mg of ascorbic acid, 399mg of anhydrous sodium acetate was weighed, added to the dispersion, the dispersion was stirred with a magnetic stirrer at room temperature for 10 minutes, and the dispersion was moved to a 40 ℃ water bath pot, and stirred for 2 hours in a water bath at 300 revolutions per minute Zhong Zhuaisu. And (3) carrying out centrifugal cleaning on the reacted product for 3 times with deionized water and 3 times with alcohol, 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 uniform multilayer graphene dispersion; subsequently, the multilayered graphene dispersion was poured into a polytetrafluoroethylene tank, 80mg of silver nitrate was weighed, 133 μl of aqueous ammonia was added to the multilayered graphene dispersion, the dispersion was stirred with a magnetic stirrer at room temperature for 10 minutes, then 33mg of ascorbic acid, 266mg of anhydrous sodium acetate was weighed, added to the dispersion, the dispersion was stirred with a magnetic stirrer at room temperature for 10 minutes, and the dispersion was moved to a 40 ℃ water bath pot, and stirred in a water bath for 1 hour at 300 revolutions per minute Zhong Zhuaisu. And (3) carrying out centrifugal cleaning on the reacted product for 3 times with deionized water and 3 times with alcohol, 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 for aiding in the understanding of the method of the present invention and its core ideas. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
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 (1)
1. The preparation method of the silver nanoparticle/multilayer graphene composite material is characterized in that the composite material 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, has a thickness of about 3-6 nm, and has a small number of oxygen-containing functional groups on the surface; silver nano particles 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;
silver ions form silver ammonia complexes and then are adsorbed by the molecular force on the surface of the multilayer graphene, and the generated silver nano particles are uniformly distributed on the surface of the multilayer graphene through reduction of ascorbic acid;
the preparation method of the composite material comprises the following steps:
step S1, DMF and deionized water with the volume ratio of 8:2 are measured and poured into a small glass bottle, and the mixture is used as a mixed solvent A after uniform mixing;
s2, weighing expanded graphite, adding the expanded graphite into the mixed solvent A, and performing ultrasonic treatment for 4 hours by using an ultrasonic machine to obtain 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;
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 at normal temperature by using a magnetic stirrer, wherein the rotating speed is 300 revolutions per minute; the concentration of the silver nitrate relative to the mixed solvent A is 6-12 mg/mL, and the mass ratio of the ammonia water volume to the silver nitrate is 5 mu L and is 3 mg;
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, wherein the molar ratio of the ascorbic acid to the silver nitrate is 0.4:1, the molar ratio of the anhydrous sodium acetate to the silver nitrate is 6.9:1, stirring the solution C at normal temperature for 10 minutes by using a magnetic stirrer at the rotating speed of 300 r/min, and then placing 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 r/min;
s5, cooling the solution C, and performing centrifugal cleaning, wherein the centrifugal cleaning adopts 3 times of deionized water and 3 times of alcohol centrifugal cleaning; placing the cleaned silver nano particles in an oven to be dried for 24 hours at 70 ℃ to obtain a silver nano particle/multilayer graphene composite material after drying;
silver ions form silver ammonia complexes and then are adsorbed by the molecular force on the surface of the multilayer graphene, and the generated silver nano particles are uniformly distributed on the surface of the multilayer graphene through reduction of ascorbic acid; because the molecular force effect is weaker, the silver ammonia complex cannot be adsorbed in a large quantity and can only be uniformly adsorbed on the surface of the multilayer graphene; therefore, after reduction, the nano silver particles have uniform size and are uniformly distributed on the surface of the multilayer graphene;
anhydrous sodium acetate is added to prevent the nano silver from growing up, and the diameter of nano silver particles is reduced so as to improve the distribution uniformity of the nano silver particles on the surface of the multilayer graphene;
DMF and deionized water with the volume ratio of 8:2 are used as solvents, and the multilayer graphene can effectively adsorb silver complexes.
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