CN102614871B - Method for preparing grapheme/silver nanoparticles composite material by using liquid phase method - Google Patents
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Abstract
The invention discloses a method for preparing a grapheme/silver nanoparticles composite material by using a liquid phase method. N and N-dimethyl formamide (DMF) serve as a reducing agent, grapheme powder with purity as high as 99% serves as a carrier, and silver forms a core and grows on a grapheme layer under a soft reaction condition to obtain the grapheme/silver nanoparticles composite material. The preparation method has the advantages of being simple, convenient, rapid and high-efficient in process, the grapheme/silver nanoparticles composite material prepared by using the method is high in purity and less in impurity content, and silver nanoparticles generated on the surface layer of the grapheme are small in particle size, uniform in distribution and high in bond strength with the grapheme. The silver nanoparticles are closely absorbed on the grapheme layer, aggregation of the grapheme is effectively avoided, and application of the grapheme/silver nanoparticles composite material in the fields of electron, catalysis, antibiosis and the like can be enlarged.
Description
Technical field
The present invention relates to a kind of preparation method of nano composite material, relate in particular to the preparation method of a kind of Graphene-Nano silver grain composite.
Background technology
Graphene is that a kind of carbon atom is distributed in the monoatomic layer crystal on the two-dimentional honeycomb crystal lattice, since the Graphene Graphene is found, because its good physicochemical properties and wide application prospect, the research work relevant with Graphene become the current research focus of related discipline.
Graphene makes Graphene become a very desirable nanoparticulate carriers and prepares graphene-based composite owing to have two unique nanostructureds.Present the characteristic of many excellences and the excellent properties of Graphene inherence is also feasible based on the composite of Graphene, and received great concern.For example, Graphene is added in the SnAgCu solder, can obviously improve the intensity of solder; Utilizing Graphene is carrier loaded nano particle, can improve these particles at the application performance in fields such as energy storage, catalysis, sensor, photoelectricity.
The Ag nano particle makes it at catalysis, SERS, sensing, biomarker, aspect such as antibiotic important use be arranged owing to have special electronic structure and huge specific area ratio.In the prior art, some reports have been arranged about preparation and the application of Graphene-Nano silver grain composite.For example, Germany " little " (Small, 2253 pages of 20 phases in 2009) reported a kind of method of synthetic silver/graphite alkene composite, this method utilizes graphene oxide to reduce silver nitrate under alkali condition, carries out hydrazine then and handles and make Graphene/argentum nano composite material; China " research in nanotechnology " (Nano Research, volume was 339 pages in 2010 the 3rd) reported the preparation method of a kind of Graphene/silver, this method utilizes ethylene glycol and sodium borohydride as mixing reducing agent, reduction silver nitrate and graphene oxide make Graphene-Yin mixture, and have analyzed its application aspect SERS and anti-biotic material; Britain's " chemical communication " (Chemical Communications, 2011 22 phases 6440 pages) has reported and has utilized polyvinylpyrrolidone (PVP) as reducing agent that reduction silver nitrate and graphene oxide prepare Graphene/argentum nano composite material.
Although the preparation method of Graphene/Nano silver grain composite has had some reports, but Graphene in the above-mentioned report/Nano silver grain composite material and preparation method thereof has mostly been used graphene oxide, and graphene oxide is compared with Graphene, contain a lot of oxygen-containing functional groups on the surface of graphene oxide, these oxygen-containing functional groups and carbon atom further reduce in conjunction with process with the form of covalent bond, part functional group still can not eliminate, thereby has had a strong impact on the serviceability of composite.
Therefore, directly generate Nano silver grain on the Graphene surface, thereby preparation Graphene/argentum nano composite material has great importance.
Summary of the invention
At above-mentioned prior art, the invention provides the method that a kind of liquid phase method prepares Graphene/Nano silver grain composite.Adopt N, dinethylformamide (DMF) is as reducing agent, purity up to 99% graphene powder as carrier, under the reaction condition of gentleness, silver on graphene layer forming core, grow up, obtain Graphene/Nano silver grain composite, this preparation method's technology is simple, Graphene/silver composite material purity height of producing, impurity content is few.Graphene-Nano silver grain the composite that is synthesized by preparation method of the present invention has potential extensive use at catalysis, photoelectric field, can enlarge Graphene/argentum nano composite material in the application in electronics, catalysis, field such as antibiotic.
In order to solve the problems of the technologies described above, a kind of liquid phase method of the present invention prepares the technical scheme that Graphene/method of Nano silver grain composite is achieved and is: this preparation method may further comprise the steps:
The N of step 1, preparation Graphene, dinethylformamide solution:
The ratio of Graphene with 0.1mg/mL～0.5mg/mL is scattered in the DMF solution, and adding surfactant lauryl sodium sulfate, its quality is 0.1～0.5 times of Graphene quality, with above-mentioned solution at 40KHz, ultrasonic processing in the ultrasonic cleaner of 100W, the processing time is 60min～180min;
Be to take by weighing silver nitrate in 1: 4～1: 12 according to the mass ratio of Graphene and silver nitrate, the ratio of silver nitrate with 0.01mol/L～0.05mol/L be scattered in the deionized water vigorous stirring 5～10min under magnetic stirring apparatus;
Step 3, will be mixed by two kinds of solution with the step 2 preparation of above-mentioned steps one preparation, ultrasonic concussion 30min～60min, transfer to then in one or three mouthfuls of beakers, the pH value of this mixed solution is adjusted into 6～8, water-bath is heated to 60～70 ℃, and vigorous stirring, reaction 30min～90min;
Step 4, with the static 12h～24h of solution that above-mentioned steps three reaction is finished, obtain Graphene/silver composite precipitation; Precipitated product is filtered, uses ethanol, acetone, washed with de-ionized water then successively, with product in air dry oven under room temperature dry 24h, obtain Graphene-Nano silver grain composite.
Wherein, the Graphene in the step 1 can prepare with physical method, and for example micromechanics is peeled off method, liquid phase or gas phase and directly peeled off method.
Wherein, be to be that 5% ammonia spirit carries out by 0.01mol/L salpeter solution or mass fraction to the adjustment of the pH of mixed solution in the step 3.
In addition, can use condensing unit to prevent the evaporation of solvent in the step 3, its condensing unit is straight shape or spherical condensation tube.
Compared with prior art, the invention has the beneficial effects as follows:
(1) directly generate silver nano-grain at graphene layer, the composite impurity content of preparation is low, applied range;
(2) the silver nano-grain particle diameter that give birth to generate on the Graphene top layer is little, is evenly distributed and the bond strength height of Graphene;
(3) Nano silver grain is adsorbed on the graphene layer closely, has effectively stoped the reunion of Graphene.
The present invention has that technology is simple, convenient, characteristics of high efficiency, and the synthetic Graphene-Nano silver grain composite of this method has potential extensive use at catalysis, photoelectric field.
Description of drawings
Fig. 1 is the Graphene/argentum nano composite material transmission electron microscope picture of embodiment 2 preparations;
Fig. 2 is the Graphene/argentum nano composite material EDX analysis result of embodiment 2 preparations;
Fig. 3 is the Graphene/argentum nano composite material X-ray diffraction analysis figure of embodiment 2 preparations;
Fig. 4 is the Graphene/Nano silver grain composite sem photograph of embodiment 2 preparations.
The specific embodiment
Below embodiments of the invention are elaborated: each embodiment has provided detailed embodiment and process being to implement under the prerequisite with the technical solution of the present invention, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The Graphene of getting 10mg is scattered among the DMF of 30mL, the lauryl sodium sulfate that adds 3mg then, at 40KHz, the 100W power ultrasonic is handled 100min, thereby break the reunion of Graphene, graphene film is dispersed in the DMF solution uniformly, makes the N of Graphene thus, dinethylformamide (DMF) solution; The silver nitrate that takes by weighing 40mg is dissolved in the deionized water of 15mL, and magnetic agitation 5 minutes is fully dissolved it and obtained silver nitrate aqueous solution; N with above-mentioned Graphene, dinethylformamide (DMF) solution and silver nitrate aqueous solution mix, ultrasonic oscillation 30min, transfer to then in one or three mouthfuls of beakers, adjusting the pH value is 7, vigorous stirring reaction 30min in 60 ℃ water-bath, quiescent setting 24h after reaction is finished, to obtain the precipitated product filtration and use ethanol, acetone, washed with de-ionized water successively, drying at room temperature 24h namely obtains product of the present invention in air dry oven: Graphene-Nano silver grain composite.
The Graphene of getting 10mg is scattered among the DMF of 30mL, adds the lauryl sodium sulfate of 3mg then, and at 40KHz, the 100W power ultrasonic is handled 60min, thereby the reunion of breaking Graphene is dispersed in the DMF solution graphene film uniformly; The silver nitrate that takes by weighing 80mg is dissolved in the deionized water of 15mL, and magnetic agitation 7 minutes is fully dissolved it; Above-mentioned two kinds of solution are mixed, ultrasonic oscillation 60min, transfer to then in three mouthfuls of beakers, be that to adjust the pH value be 8 for 5% alkene ammoniacal liquor with mass fraction, vigorous stirring reaction 60min in 65 ℃ water-bath, quiescent setting 20h after reaction is finished also uses ethanol, acetone, washed with de-ionized water successively with the precipitated product filtration, and drying at room temperature 24h obtains Graphene/silver powder and is product of the present invention in air dry oven: Graphene-Nano silver grain composite.
From Fig. 1 we as can be seen, silver nano-grain is adsorbed on the surface of Graphene closely, grain size is little, is evenly distributed.Fig. 2 is the analysis result of EDX, has shown that this composite is made up of Nano Silver and carbon structure.Fig. 3 is that the XRD analysis result shows: 4 diffraction maximums are the characteristic peak of Ag, have 4 crystal faces, and the corresponding indices of crystallographic plane are followed successively by (111) from inside to outside, and (200), (220) and (311) are face-centred cubic structure.Fig. 4 be by sem photograph we as can be seen, the Graphene favorable dispersibility, the silver nano-grain of Graphene top layer absorption has effectively stoped the reunion of Graphene.
Embodiment 3
The Graphene of getting 10mg is scattered among the DMF of 30mL, the lauryl sodium sulfate that adds 3mg then, at 40KHz, the 100W power ultrasonic is handled 120min, thereby break the reunion of Graphene, graphene film is dispersed in the DMF solution uniformly, the silver nitrate that takes by weighing 120mg is dissolved in the deionized water of 15mL, magnetic agitation 10min fully dissolves it, and above-mentioned two kinds of solution are mixed, ultrasonic oscillation 50min, transfer to then in one or three mouthfuls of beakers, with mass fraction be 5% alkene ammoniacal liquor to adjust pH value be 8, vigorous stirring is reacted 80min in 65 ℃ water-bath, quiescent setting 18h after reaction is finished, precipitated product is filtered and uses successively ethanol, acetone, washed with de-ionized water, drying at room temperature 24h in air dry oven, Graphene/silver powder that gained gets is product of the present invention: Graphene-Nano silver grain composite.
Embodiment 4
The Graphene of getting 10mg is scattered among the DMF of 30mL, the lauryl sodium sulfate that adds 3mg then, at 40KHz, the 100W power ultrasonic is handled 180min, thereby break the reunion of Graphene, graphene film is dispersed in the DMF solution uniformly, the silver nitrate that takes by weighing 80mg is dissolved in the deionized water of 15mL, magnetic agitation 10min, it is fully dissolved, above-mentioned two kinds of solution are mixed ultrasonic oscillation 40min, transfer to then in one or three mouthfuls of beakers, adjusting the pH value with the salpeter solution of 0.01mol/L is 6, vigorous stirring reaction 90min in 60 ℃ water-bath, quiescent setting 12h after reaction is finished, precipitated product is filtered and uses successively ethanol, acetone, washed with de-ionized water, drying at room temperature 24h namely gets product of the present invention in air dry oven: Graphene-Nano silver grain composite.
Embodiment 5
The Graphene of getting 10mg is scattered among the DMF of 30mL, the lauryl sodium sulfate that adds 3mg then, at 40KHz, the 100W power ultrasonic is handled 80min, the silver nitrate that takes by weighing 80mg is dissolved in the deionized water of 15mL, magnetic agitation 6min, it is fully dissolved, above-mentioned two kinds of solution are mixed, ultrasonic oscillation 40min, transfer in one or three mouthfuls of beakers, with mass fraction be 5% alkene ammoniacal liquor to adjust pH value be 8, vigorous stirring reaction 40min in 62 ℃ water-bath, react finish after quiescent setting 12h, sediment is used ethanol successively, acetone, washed with de-ionized water, drying at room temperature 24h obtains product of the present invention in drying box: Graphene-Nano silver grain composite.
Although top invention has been described in conjunction with figure; but the present invention is not limited to the above-mentioned specific embodiment; the above-mentioned specific embodiment only is schematic; rather than it is restrictive; those of ordinary skill in the art is under enlightenment of the present invention; under the situation that does not break away from aim of the present invention, can also make a lot of distortion, these all belong within the protection of the present invention.
Claims (4)
1. a liquid phase method prepares the method for Graphene/Nano silver grain composite, it is characterized in that, may further comprise the steps:
The N of step 1, preparation Graphene, dinethylformamide solution:
Graphene is scattered in N with the ratio of 0.1mg/mL～0.5mg/mL, in the dinethylformamide solution, and adding surfactant lauryl sodium sulfate, its quality is 0.1～0.5 times of Graphene quality, with above-mentioned solution at 40KHz, ultrasonic processing in the ultrasonic cleaner of 100W, the processing time is 60min～180min;
Step 2, preparation silver nitrate aqueous solution:
Be to take by weighing silver nitrate in 1: 4～1: 12 according to the mass ratio of Graphene and silver nitrate, the ratio of silver nitrate with 0.01mol/L～0.05mol/L be scattered in the deionized water vigorous stirring 5～10min under magnetic stirring apparatus;
Step 3, will be mixed by two kinds of solution with the step 2 preparation of above-mentioned steps one preparation, ultrasonic concussion 30min～60min, transfer to then in one or three mouthfuls of beakers, the pH value of this mixed solution is adjusted into 6～8, water-bath is heated to 60～70 ℃, and vigorous stirring, reaction 30min～90min;
Step 4, with the static 12h～24h of solution that above-mentioned steps three reaction is finished, obtain Graphene/silver composite precipitation; Precipitated product is filtered, uses ethanol, acetone, washed with de-ionized water then successively, with product in air dry oven under room temperature dry 24h, obtain Graphene-Nano silver grain composite.
2. liquid phase method according to claim 1 prepares the method for Graphene/Nano silver grain composite, and wherein, the Graphene in the step 1 is made by physical method.
3. liquid phase method according to claim 2 prepares the method for Graphene/Nano silver grain composite, and wherein, described Graphene is peeled off method, liquid phase or gas phase by micromechanics and directly peeled off method and make.
4. liquid phase method according to claim 1 prepares the method for Graphene/Nano silver grain composite, wherein, is to be that 5% ammonia spirit carries out by 0.01mol/L salpeter solution or mass fraction to the adjustment of the pH of mixed solution in the step 3.
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