CN105397103A - Nano-silver/graphene composite material and preparation method thereof - Google Patents
Nano-silver/graphene composite material and preparation method thereof Download PDFInfo
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- CN105397103A CN105397103A CN201510737770.9A CN201510737770A CN105397103A CN 105397103 A CN105397103 A CN 105397103A CN 201510737770 A CN201510737770 A CN 201510737770A CN 105397103 A CN105397103 A CN 105397103A
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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Abstract
The invention discloses a nano-silver/graphene composite material and a preparation method thereof. The nano-silver/graphene composite material is synthesized through the supercritical carbon dioxide (ScCO2) assisted chemical deposition method. Firstly, a silver-ammonia solution is added into reductive alcohol, and an appropriate amount of a surfactant and a complexing agent are dissolved in the reductive alcohol; afterwards, graphene oxide powder is added, and homogeneously dispersed suspension liquid is obtained after ultrasonic dispersion; then a reducing agent is added, mixed liquid is quickly transferred into a reaction kettle, CO2 gas is pumped into the reaction kettle, the reaction kettle is heated to reach set pressure and a set temperature, and at the moment, the CO2 is in a supercritical state; and after a mixed solution is stirred and reacted for a period, cooling and pressure relief are carried out, and the nano-silver/graphene composite material is obtained after repeated centrifugal cleaning and drying. The preparation method is environmentally friendly, and the prepared nano-silver/graphene composite material has the characteristics that the phase is singular, the load capacity is controllable, and nano-silver is small in grain size and evenly distributed between graphene nanosheet layers.
Description
Technical field
The invention belongs to new material Inorganic synthese technical field, be specifically related to a kind of silver nanoparticle/graphene composite material and preparation method thereof.
Background technology
Silver Nanoparticles, shows the performance of many uniquenesses due to the reason such as nanometer size effect, skin effect, have broad prospect of application in conduction, catalysis, the field such as antibacterial.Graphene has the two-dimentional honeycomb planar structure being full of pi-electron, by carbon atom with SP
2hydridization is formed by connecting, and it is carbonaceous new material the thinnest in the world, and desirable single-layer graphene thickness only has 0.35nm.Graphene also has many superior physical and chemical performances, is widely used in various fields such as electronics, sensing, energy storage.The nanostructured of Graphene uniqueness and characteristic become the basic composition unit of numerous novel nanocomposite materials.Take Graphene as matrix, plated metal nano particle in its flat sheet structure, can the composite of synthesizing graphite alkene carried metal nano particle.Research shows, this kind of composite not only inherits the excellent properties of metal nanoparticle and Graphene self, but also may show the character surmounting component units, even produces the special character that some are new.
People, for obtaining more high performance material, can utilize various method that component units based on Graphene and nano particle is carried out preparing nano composite usually.Invention CN201110434334.6 discloses a kind of preparation method of Ag/ graphene nanocomposite material, silver nitrate and graphene oxide is dispersed in deionized water and goes back in the dual-solvent system of carbinol, with nanometer WO
3particle makes catalyst, simulated solar irradiation light-catalyzed reaction 1 ~ 5 hour, successfully synthesizes Ag/ graphene composite material.Invention CN201010243147.5 discloses a kind of synthetic method of tin oxide/graphene nanocomposite material, by appropriate graphite oxide and Tin tetrachloride pentahydrate ultrasonic disperse in dimethyl sulfoxide solution, is then transferred in water heating kettle, through 180 by this suspension
oc ~ 190
ounder C, heat treatment is after 12 ~ 24 hours, can obtain composite.A kind of Co disclosed in invention CN201210248034.3
3o
4the synthetic method of/graphene nanocomposite material, is specifically dissolved in deionized water by cobalt salt, polyvinylpyrrolidone, after regulating PH with urea, and 90-95
ounder C, oil bath 3 hours, then adds graphene oxide and reducing agent, is warming up to 100
oc reacts 4 hours.Afterwards, washing and drying collecting precipitation, and successively through tube furnace and muffle furnace calcining, finally obtain Co
3o
4/ graphene nanocomposite material.No matter these methods, be photocatalysis, the reduction of pyrohydrolysis traditional chemical, although the successful synthetic composite material of energy, but be but difficult to ensure the even of nano particle diameter, and it be evenly distributed on graphene sheet layer.So the nano composite material preparing microscopic appearance structure-controllable is still a challenge.For this reason, we introduce supercritical carbon dioxide (ScCO
2) for auxiliary synthesis.ScCO
2density be bordering on liquid, viscosity is bordering on gas, and diffusion coefficient is 100 times of liquid, has surprising solvability.It can overcome to a certain extent, and the dispersive property of routine techniques means is poor, sedimentation rate is low, load capacity is difficult to the defects such as control, is a kind of supplementary means of effective environmental protection.
Summary of the invention
Primary and foremost purpose of the present invention is the controllable synthesis method providing a kind of silver nanoparticle/graphene composite material.The preparation method of described silver nanoparticle/graphene composite material applies supercritical carbon dioxide (ScCO
2) assisted deposition technique.Supercritical carbon dioxide possesses low viscosity, high diffusibility and nearly zero surface tension, easily dispersed encapsulated silver presoma and carried delivery closely surperficial to graphene nano lamella, thus be conducive to Nano Silver reduction after evenly grow up and be deposited on graphene nano lamella surface.Synthesis composite in, Nano Silver is the little (≤10nm of particle diameter not only), and can uniform load graphene layer surface.This synthetic method is simple and convenient, and the composite microstructure prepared is even.
Silver nanoparticle/graphene composite material of the present invention is made up of at the silver nano-grain of graphene nano lamella graphene base body and uniform load.
A preparation method for silver nanoparticle/graphene composite material, comprises following basic step:
(1) under normal temperature, the silver ammino solution of preparation, surfactant and complexing agent are mixed in reproducibility alcohol, after stirring, add graphene oxide, ultrasonic disperse, obtain homodisperse mixed liquor;
(2) reducing agent is joined in above-mentioned mixed liquor and also transfer to rapidly in reactor, obtain mixed solution, then pass into CO
2gas, controls air pressure and temperature makes CO
2reach supercriticality;
(3) mixed solution in step (2) reactor is carried out stirring reaction a period of time, then cool pressure release, centrifugal clean collection solids, obtains silver nanoparticle/graphene composite material after vacuum drying.
Further, described silver ammino solution is prepared by the mixture of the one or more than one in silver-colored precursor compound silver nitrate, silver chlorate and acetylacetone,2,4-pentanedione silver and concentrated ammonia liquor and deionized water;
Preferably, described silver-colored precursor compound is one or more the mixture in silver nitrate, silver chlorate and acetylacetone,2,4-pentanedione silver;
Preferably, the mass percentage of described silver-colored precursor compound in step (1) described mixed liquor is 0.2% ~ 2%;
Preferably, described surfactant is the mixture of the one or more than one in lauryl sodium sulfate (SDS), neopelex and sodium cetanesulfonate;
Further, the concentration of described surfactant in step (1) described mixed liquor is 0.0002 ~ 0.002mol/L;
Preferably, the concentration of described surfactant in step (1) described mixed liquor is 0.0003 ~ 0.001mol/L;
Preferably, described complexing agent is one or more the mixture in sodium acetate, natrium citricum and sodium sulfite;
Further, the concentration of described complexing agent in step (1) described mixed liquor is 0.001-0.004mol/L;
Preferably, the concentration of described complexing agent in step (1) described mixed liquor is 0.001 ~ 0.003mol/L;
Preferably, described reproducibility alcohol is one or both in methyl alcohol and ethanol;
Preferably, in described mixed liquor, the mass ratio of silver nitrate or silver chlorate and graphene oxide is 1:1-6:1;
Preferably, described reducing agent is the one in glucose, gluconic acid sodium salt;
Further, the concentration of described reducing agent in step (2) reactor mixed solution is 0.01-0.1mol/L;
Preferably, the concentration of described reducing agent in step (2) reactor mixed solution is 0.01 ~ 0.04mol/L;
Preferably, the time of step (1) described ultrasonic disperse is 0.5 ~ 2h;
Further, step (2) described air pressure is 8-16MPa, and described temperature is 50-100 DEG C;
Preferably, step (2) described air pressure is 10 ~ 15MPa, and temperature is 60 ~ 90 DEG C;
Further, step (3) described mixing speed is 300-800rpm, and the described reaction time is 0.5-2h;
Preferably, the mixing speed of step (3) described stirring reaction is 500 ~ 600rpm, and the reaction time is 1 ~ 2h;
Further, the described centrifuge washing solvent of step (3) is one or both the mixture in ethanol and deionized water;
Further, the described vacuum drying temperature of step (3) is 40-80 DEG C, and the time is 2-6 hour;
Preferably, the described vacuum drying temperature of step (3) is 40 ~ 60 DEG C, and drying time is 3 ~ 5h.
A kind of silver nanoparticle/graphene composite material is obtained according to above-mentioned preparation method, described silver nanoparticle/graphene composite material is composited by spherical silver nano granule and Graphene, wherein, the diameter of silver nano-grain between 5-10nm, and is evenly distributed on graphene sheet layer surface.
Compared with prior art, the present invention has following advantage and effect:
(1) preparation method's simple and fast of the present invention, the technique used time is short.
(2) compared to general technology, the silver nanoparticle/graphene composite material Argent grain particle diameter that preparation method of the present invention obtains is more tiny, more homogeneous, is more evenly distributed on the surface at graphene sheet layer.
Accompanying drawing explanation
The X ray diffracting spectrum of the silver nanoparticle/graphene composite material (Sc-Ag/GO) that Fig. 1 is graphene oxide (GO), nano-Ag particles (Nano-Ag), conventional method obtain silver nanoparticle/graphene composite material (Ag/GO) and prepared by the embodiment of the present invention 1.
Fig. 2 is the TEM photo of silver nanoparticle/graphene composite material prepared by embodiment 1.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
embodiment 1
A kind of silver nanoparticle/graphene composite material, its preparation method is as follows:
(1) at room temperature, 100mg silver nitrate, 2ml concentrated ammonia liquor are added in 5ml deionized water and prepares silver ammino solution, then join in 50ml absolute ethyl alcohol by silver ammino solution, 5mg lauryl sodium sulfate (SDS), 6mg natrium citricum, ultrasonic agitation 20min forms homogeneous mixture solotion; Then add 100mg graphene oxide, ultrasonic disperse 1 hour, obtains homodisperse suspension;
(2) 100mg glucose is dissolved in 5ml deionized water, and by this solution and above-mentioned mixed liquor Homogeneous phase mixing, then transfers to rapidly in 100 milliliters of stainless steel cauldrons, pump into CO
2gas, is forced into 8MPa, and is heated to 100 DEG C;
(3) by the mixed solution in step (2) reactor under 300rpm rotating speed after stirring reaction 1h, after being cooled to room temperature, pressure release is vented, centrifugal and with ethanol and deionized water cyclic washing three times to sediment, in 40 DEG C of vacuum drying 6h, namely obtain described silver nanoparticle/graphene composite material.
embodiment 2
A kind of silver nanoparticle/graphene composite material, its preparation method is as follows:
(1) at room temperature, 300mg silver nitrate, 2ml concentrated ammonia liquor are added in 5ml deionized water and prepares silver ammino solution, then join in 50ml absolute ethyl alcohol by silver ammino solution, 10mg lauryl sodium sulfate (SDS), 12mg natrium citricum, ultrasonic agitation 15min forms homogeneous solution; Then add 100mg graphene oxide, ultrasonic disperse 1.5 hours, obtains homodisperse mixed liquor;
(2) 200mg glucose is dissolved in 5ml deionized water, and by this solution and above-mentioned mixed liquor Homogeneous phase mixing, then transfers to rapidly in 100 milliliters of stainless steel cauldrons, pump into CO
2gas, is forced into 16MPa, and is heated to 50 DEG C;
(3) by the stirring reaction 2 hours under 550rpm rotating speed of the mixed solution in step (2) reactor, then after being cooled to room temperature, pressure release is vented, centrifugal and with ethanol and deionized water cyclic washing three times to sediment, in 80 DEG C of vacuum drying 2h, namely obtain described silver nanoparticle/graphene composite material.
embodiment 3
A kind of silver nanoparticle/graphene composite material, its preparation method is as follows:
(1) at room temperature, 600mg silver nitrate, 2ml concentrated ammonia liquor are added in 5ml deionized water and prepares silver ammino solution, then join in 50ml absolute ethyl alcohol by silver ammino solution, 15mg lauryl sodium sulfate (SDS), 18mg natrium citricum, ultrasonic agitation 10min forms homogeneous solution; Then add 100mg graphene oxide, ultrasonic disperse 1 hour, obtains homodisperse mixed liquor;
(2) 400mg glucose is dissolved in 5ml deionized water, and by this solution and above-mentioned mixed liquor Homogeneous phase mixing, then transfers to rapidly in 100 milliliters of stainless steel cauldrons, pump into CO
2gas, is forced into 12MPa and is heated to 75 DEG C;
(3) by the stirring reaction 0.5 hour under 800rpm rotating speed of the mixed solution in step (2) reactor, then after being cooled to room temperature, pressure release is vented, centrifugal and with ethanol and deionized water cyclic washing three times to sediment, in 60 DEG C of vacuum drying 4h, namely obtain described silver nanoparticle/graphene composite material.
embodiment 4
A kind of silver nanoparticle/graphene composite material, its preparation method is as follows:
(1) at room temperature, 200mg silver nitrate, 2ml concentrated ammonia liquor added in 5ml deionized water and prepare silver ammino solution, then join in 50ml methyl alcohol by silver ammino solution, 5mg lauryl sodium sulfate, 8.2mg sodium acetate, ultrasonic agitation 10min forms homogeneous solution; Then add 100mg graphene oxide, ultrasonic disperse 2 hours, obtains homodisperse mixed liquor;
(2) 200mg glucose is dissolved in 5ml deionized water, and by this solution and above-mentioned mixed liquor Homogeneous phase mixing, then transfers to rapidly in 100 milliliters of stainless steel cauldrons, pump into CO
2gas, is forced into 15MPa, is heated to 60 DEG C;
(3), by the stirring reaction 1.5h under 550rpm rotating speed of the mixed solution in step (2) reactor, after being then cooled to room temperature, pressure release is vented, centrifugal, by ethanol and deionized water washed product, in 60 DEG C of vacuum drying 4 hours, namely obtain described silver nanoparticle/graphene composite material.
embodiment 5
A kind of silver nanoparticle/graphene composite material, its preparation method is as follows:
(1) at room temperature, 168mg silver chlorate, 3ml concentrated ammonia liquor are added in 5ml deionized water and prepares silver ammino solution, then join in 50ml ethylene glycol by silver ammino solution, 17.5mg neopelex, 25mg sodium sulfite, ultrasonic agitation 20min forms homogeneous solution; Then add 100mg graphene oxide, ultrasonic disperse 1.5 hours, obtains homodisperse mixed liquor;
(2) 250mg glucose is dissolved in 5ml deionized water, and by this solution and above-mentioned mixed liquor Homogeneous phase mixing, then transfers to rapidly in 100 milliliters of stainless steel cauldrons, pump into CO
2gas, is forced into 12MPa, is heated to 75 DEG C;
(3) by the stirring reaction 1.5h under 550rpm rotating speed of the mixed solution in step (2) reactor, then room temperature is cooled to, pressure release is vented, sediment is centrifugal and with ethanol and deionized water cyclic washing three times, in 60 DEG C of vacuum drying 4 hours, namely obtain described silver nanoparticle/graphene composite material.
performance evaluation:
1, get the embodiment of the present invention 1 prepare silver nanoparticle/graphene composite material (Sc-Ag/GO), and contrast graphene oxide (GO) and nano-Ag particles (Nano-Ag) carry out X-ray diffraction analysis, gained XRD figure as shown in Figure 1.
As can be seen from Figure 1, on the collection of illustrative plates of Sc-Ag/GO, the mark peak (001) of Graphene disappears substantially, and (111), (200), (220), (311) and (222) peak of Nano Silver are high-visible.This illustrates, through synthetic reaction, graphene oxide is reduced to Graphene, and silver ion is also reduced into elemental crystal silver simultaneously.
2, the silver nanoparticle/graphene composite material getting the embodiment of the present invention 1 preparation carries out Morphology analysis, and transmission electron microscope picture as shown in Figure 2.As we know from the figure, Nano Silver is that graininess is evenly distributed on graphene sheet layer, and granular size is 5-10nm.
Silver nanoparticle/graphene composite material obtained by all the other embodiments of the present invention carry out the result of Performance Detection and the above results basically identical.
Above-mentioned embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. a preparation method for silver nanoparticle/graphene composite material, is characterized in that, comprises the following steps:
1) silver ammino solution of preparation, surfactant and complexing agent are mixed in reproducibility alcohol, then add graphene oxide, ultrasonic disperse, obtain uniform suspension;
2) reducing agent is joined in above-mentioned suspension and also transfer to rapidly in reactor, obtain mixed solution, then pass into CO
2gas also heating reaches setting pressure and temperature, makes CO
2reach supercriticality;
3) by step 2) mixed solution vigorous stirring reaction in reactor, cooling pressure release, washs pelleting centrifugation, after vacuum drying, obtains silver nanoparticle/graphene composite material powder.
2. the preparation method of a kind of silver nanoparticle/graphene composite material according to claim 1, it is characterized in that, silver ammino solution described in step 1) is prepared by the mixture of the one or more than one in silver-colored precursor compound silver nitrate, silver chlorate and concentrated ammonia liquor and deionized water; In described suspension, the mass percentage of silver-colored precursor compound is 0.2%-2%.
3. the preparation method of a kind of silver nanoparticle/graphene composite material according to claim 1, it is characterized in that, surfactant described in step 1) is the mixture of the one or more than one in lauryl sodium sulfate, neopelex and sodium cetanesulfonate; The concentration of described surfactant in suspension described in step 1) is 0.0002 ~ 0.002mol/L.
4. the preparation method of a kind of silver nanoparticle/graphene composite material according to claim 1, is characterized in that, complexing agent described in step 1) is one or more the mixture in sodium acetate, natrium citricum and sodium sulfite; The concentration of described complexing agent in suspension described in step 1) is 0.001-0.004mol/L.
5. the preparation method of a kind of silver nanoparticle/graphene composite material according to claim 1, is characterized in that, reproducibility alcohol described in step 1) is one or both in methyl alcohol, ethanol.
6. the preparation method of a kind of silver nanoparticle/graphene composite material according to claim 1, is characterized in that, the mass ratio of the silver nitrate in suspension described in step 1) or silver chlorate and graphene oxide is 1:1-6:1.
7. the preparation method of a kind of silver nanoparticle/graphene composite material according to claim 1, is characterized in that, step 2) described reducing agent is gentle glucose or gluconic acid sodium salt; Described reducing agent is in step 2) concentration in reactor mixed solution is 0.01-0.1mol/L.
8. the preparation method of a kind of silver nanoparticle/graphene composite material according to claim 1, is characterized in that, step 2) described CO
2for gas-pressurized, described pressure is 8-16MPa, and described temperature is 50-100 DEG C.
9. the preparation method of a kind of silver nanoparticle/graphene composite material according to claim 1, is characterized in that, mixing speed described in step 3) is 300-800rpm, and the described reaction time is 0.5-2h; Described centrifuge washing solvent is one or both the mixture in ethanol and deionized water; Described vacuum drying temperature is 40-80 DEG C, and the time is 2-6 hour.
10. the silver nanoparticle/graphene composite material obtained by the preparation method of a kind of silver nanoparticle/graphene composite material described in any one of claim 1-9.
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