CN102160998A - Preparation method of graphene-silver nano particle composite material - Google Patents
Preparation method of graphene-silver nano particle composite material Download PDFInfo
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- CN102160998A CN102160998A CN2011101037813A CN201110103781A CN102160998A CN 102160998 A CN102160998 A CN 102160998A CN 2011101037813 A CN2011101037813 A CN 2011101037813A CN 201110103781 A CN201110103781 A CN 201110103781A CN 102160998 A CN102160998 A CN 102160998A
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Abstract
The invention provides a preparation method of a graphene-silver nano particle composite material. A specific preparation process comprises the following steps of: preparing solution of silver ammonia at certain concentration from the solution of silver nitrate and aqueous solution of dilute ammonia, adding the prepared solution of silver-ammonia into the solution of graphene oxide which is subjected to ultrasonic processing, preheating the solution at a certain temperature for a certain time; adding an appropriate amount of glucose into the mixed solution of graphene oxide and silver ammonia, and reacting the mixed solution at the set temperature for a certain time with stirring; performing suction-filtration on a reaction product by using deionized water for many times, and then drying the product to obtain the graphene-silver nano particle composite material. The method is simple, convenient, easy, environment-friendly and efficient; and silver nano particles in the prepared composite material are distributed narrowly, have a uniform particle size (about 25 nm), can be better inserted into graphene slices and can effectively prevent aggregation of the graphene.
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 (Graphene) is a kind of new carbon of broad research in recent years.Its structure is by the tightly packed bi-dimensional cellular shape lattice structure that becomes of monolayer carbon atom.Because Graphene has the performance of excellent aspects such as electricity, calorifics and mechanics, in a few years of its appearance, just become the material of hot research.Owing to have unique two-dimensional nanostructure, make Graphene become the composite that a very desirable nanometer combination ingredient prepares Graphene.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.At present, the composite of Graphene has shown some superior character and potential application in fields such as energy storage, catalysis, macromolecule, biological medicines.For example, document Kamat P V.Graphene based nanoarchitectures:Anchoring semiconductor and metal nanoparticles on a two-dimensional carbon support.J.Phys.Chem.Lett.[J], 2009,1 (2): 520-527, utilizing Graphene is carrier loaded nano particle, can improve these particles at the application performance in fields such as energy storage, catalysis, sensor, photoelectricity or the like.The research field of grapheme material has also been widened in the preparation of these compounds, makes grapheme material go a step further to the practical application aspect is more advanced in years.
The Ag nano particle is because its special electronic structure and huge specific area make it at the catalysis of chemical reaction, SERS, sensing, biomarker, aspect such as antibiotic important use be arranged.Graphene-the preparation of Nano silver grain compound has caused scientist's concern.As document Ki-Seok Kim, Ick-Jun Kim, Soo-Jin Park.Influence of Ag doped graphene on electrochemical behaviors and specificcapacitance of polypyrrole-based nanocomposites[J] Synthetic Metals, 2010,160, Ki-Seok Kim utilizes hydrazine to prepare the Graphene-Nano silver grain compound of Nano silver grain diameter at 2-5nm as reducing agent in the graphite oxide aqueous solution of stabilizing agent and coupling agent (PVP (polypyrrole alkane ketone) and APTMS (3-aminopropyl trimethoxy siloxane)) existence among the 2355-2360; Jianfeng Shen, Min Shi, Na Li, Bo Yan, Hongwei Ma, Yizhe Hu, and Mingxin Ye.Facile Synthesis and Application of Ag-Chemically ConvertedGrapheneNanocomposite[J].Nano Res, 2010,3, Shen utilizes the mixing reducing agent of sodium borohydride and ethylene glycol to prepare Graphene-Nano silver grain compound among the 339-349; Document Manash R Das, Rupak KSarma, RatulSaikia, Vinayak S Kale, Manjusha V Shelke, Pinaki Sengupta. Synthesis of silver nanoparticles in an aqueous suspension of graphene oxidesheets and its antimic
Although the report about Graphene-Nano silver grain composite has had certain basis, used poisonous strong reductant hydrazine and sodium borohydride but the Graphene of above-mentioned report-Nano silver grain composite material and preparation method thereof has, had plenty of and under the severe corrosive condition, carry out.
Therefore, green, environmental protection, the easy preparation method's research about Graphene-Nano silver grain composite have great importance.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of Graphene-Nano silver grain composite.This method adopts glucose as reducing agent, reduces graphene oxide and silver-colored ammonium ion under the reaction condition of gentleness simultaneously, obtains Graphene-Nano silver grain composite, this preparation method's environmental protection, convenient, efficient.
Technical scheme of the present invention is as follows:
(1) aqueous solution of preparation graphene oxide: the ratio of graphite oxide with 0.5mg/mL～2mg/mL is scattered in the deionized water, and at 50KHz, the 500W power ultrasonic is handled with above-mentioned solution, and the processing time is 30～60min;
(2) utilize liquor argenti nitratis ophthalmicus and dilute ammonia solution to be configured to certain density silver ammino solution, and the silver ammino solution that configures joined in the prepared graphene oxide solution of the ultrasonic step of finishing (1), under 40 ℃～70 ℃ temperature, stir preheating 10min～30min;
(3) an amount of glucose is joined in step (2) prepared solution, under 85 ℃～100 ℃ temperature, react 1h～8h, obtain comprising the solution of reactant;
(4) utilize deionized water that product is repeatedly washed suction filtration after, product vacuum drying 24h is obtained Graphene-Nano silver grain composite.
Wherein in the step (2): the mass fraction of used weak aqua ammonia is 2%～6%; In the mixed solution of graphene oxide and silver-colored ammonia, after the conversion, the mass ratio of silver-colored simple substance and graphite oxide is between 0.5～1.0.
Wherein in the step (3): the used mole of glucose is 2～10 times of silver nitrate mole.
Wherein graphite oxide can any means known in the art be made in the step (1), for example by comprising the chemical oxidizing agent that uses more than one and the intercalator sulfuric acid method of graphite being carried out oxidation for example randomly.The example of oxidant comprises nitric acid, sodium nitrate and potassium nitrate, perchlorate, hydrogen peroxide, sodium permanganate and potassium permanganate, phosphorus pentoxide, acid sulphite etc.Preferred oxidant comprises KClO
4, HNO
3And KClO
3, KMnO
4And/or NaMnO
4, KMnO
4And NaNO
3, K
28
2O
8And P
2O
5And KMnO
4, KMnO
4And HNO
3, and HNO
3Preferred intercalator comprises sulfuric acid.Being equipped with graphite oxide with the Hummers legal system below is example: the natural flake graphite of 5～20g and the sodium nitrate of 0～10g are scattered in the concentrated sulfuric acid of 100～500mL, under the ice bath situation, slowly the potassium permanganate of 10～80g is joined in the reaction solution, in the adition process temperature of reaction solution is controlled at below 20 ℃.Reaction solution is elevated to the reaction solution temperature about 35 ℃ after reacting a period of time at low temperatures, and the deionized water with 300～900mL behind maintenance 20～40min joins in the reaction solution, and the control solution temperature is under 100 ℃ in the process of adding deionized water.Reaction solution is heated to 98 ℃ and keep 20～40min.After reaction finishes with the deionized water of 1000～2000mL and the H of 30～100mL
2O
2Join in the solution.When solution is warm, filter and with 5%HCl and deionized water cyclic washing 4-5 time in filtrate detection less than sulfate ion (checking) with BaNO3, with products therefrom at 60 ℃ of following vacuum drying 24h.
The present invention has environmental protection, convenient, characteristics of high efficiency, in the preparation process of Graphene-Nano silver grain composite, the glucose that utilizes environmental protection is as reducing agent, under the reaction condition of gentleness, prepared composite, and Nano silver grain narrow distribution range, particle size homogeneous (about 25nm) and can be inserted into well in the Graphene lamella in composite.Synthetic Graphene-Nano silver grain the composite of this method has potential using value at aspects such as catalysis and SERSs.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the Graphene-Nano silver grain composite of embodiment 2 preparations;
Fig. 2 is the surface sweeping electron micrograph of the Graphene-Nano silver grain composite of embodiment 2 preparations;
Fig. 3 is the transmission electron microscope photo of the Graphene-Nano silver grain composite of embodiment 2 preparations;
But Fig. 4 is the ultraviolet spectrum of the Graphene-Nano silver grain composite of embodiment 2 preparations.
The specific embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
Embodiment 1
The graphite oxide of 50mg is scattered in the deionized water of 100mL, and at 50KHz, the 500W power ultrasonic is treated to 10min.The silver nitrate of 40mg is dissolved in the deionized water of 5mL, is that 2% weak aqua ammonia dropwise joins in the liquor argenti nitratis ophthalmicus up to the precipitation that generates just till the complete obiteration with mass fraction.The silver ammino solution that configures is joined in the ultrasonic graphene oxide solution that finishes, at 40 ℃ stirred in water bath preheating 10min.With the 50mL aqueous solution that is dissolved with 85mg glucose join preheating graphene oxide and the mixed liquor of silver ammino solution in, at 85 ℃ of following stirring reaction 1h.After reaction is finished, product filtered and repeatedly with deionized water and alcohol flushing.
Embodiment 2
The graphite oxide of 100mg is scattered in the deionized water of 100mL, and at 50KHz, the 500W power ultrasonic is treated to 30min.The silver nitrate of 120mg is dissolved in the deionized water of 5mL, is that 3% weak aqua ammonia dropwise joins in the liquor argenti nitratis ophthalmicus up to the precipitation that generates just till the complete obiteration with mass fraction.The silver ammino solution that configures is joined in the ultrasonic graphene oxide solution that finishes, at 50 ℃ stirred in water bath preheating 20min.With the 50mL aqueous solution that is dissolved with 500mg glucose join preheating graphene oxide and the mixed liquor of silver ammino solution in, at 95 ℃ of following stirring reaction 4h.After reaction is finished, product filtered and repeatedly with deionized water and alcohol flushing.
Embodiment 3
The graphite oxide of 100mg is scattered in the deionized water of 100mL, and at 50KHz, the 500W power ultrasonic is treated to 40min.The silver nitrate of 157mg is dissolved in the deionized water of 10mL, is that 3% weak aqua ammonia dropwise joins in the liquor argenti nitratis ophthalmicus up to the precipitation that generates just till the complete obiteration with mass fraction.The silver ammino solution that configures is joined in the ultrasonic graphene oxide solution that finishes, at 60 ℃ stirred in water bath preheating 30min.With the 100mL aqueous solution that is dissolved with 1330mg glucose join preheating graphene oxide and the mixed liquor of silver ammino solution in, at 95 ℃ of following stirring reaction 8h.After reaction is finished, product filtered and repeatedly with deionized water and alcohol flushing.
Embodiment 4
The graphite oxide of 200mg is scattered in the deionized water of 100mL, and at 50KHz, the 500W power ultrasonic is treated to 1h.The silver nitrate of 236mg is dissolved in the deionized water of 15mL, is that 6% weak aqua ammonia dropwise joins in the liquor argenti nitratis ophthalmicus up to the precipitation that generates just till the complete obiteration with mass fraction.The silver ammino solution that configures is joined in the ultrasonic graphene oxide solution that finishes, at 70 ℃ stirred in water bath preheating 30min.With the 100mL aqueous solution that is dissolved with 2500mg glucose join preheating graphene oxide and the mixed liquor of silver ammino solution in, at 95 ℃ of following stirring reaction 8h.After reaction is finished, product filtered and repeatedly with deionized water and alcohol flushing.
Claims (4)
1. the preparation method of Graphene-Nano silver grain composite is characterized in that concrete steps are as follows:
(1) aqueous solution of preparation graphene oxide: the ratio of graphite oxide with 0.5mg/mL～2mg/mL is scattered in the deionized water, and at 50KHz, the 500W power ultrasonic is handled with above-mentioned solution, and the processing time is 30～60min;
(2) utilize liquor argenti nitratis ophthalmicus and dilute ammonia solution to be configured to certain density silver ammino solution, and the silver ammino solution that configures joined in the prepared graphene oxide solution of the ultrasonic step of finishing (1), under 40 ℃～70 ℃ temperature, stir preheating 10min～30min;
(3) an amount of glucose is joined in step (2) prepared solution, under 85 ℃～100 ℃ temperature, react 1h～8h, obtain comprising the solution of reactant;
(4) utilize deionized water that product is repeatedly washed suction filtration after, product vacuum drying 24h is obtained Graphene-Nano silver grain composite.
2. the preparation method of a kind of Graphene according to claim 1-Nano silver grain composite is characterized in that, wherein in the step (2), the mass fraction of used weak aqua ammonia is 2%～6%; In the mixed solution of graphene oxide and silver-colored ammonia, after the conversion, the mass ratio of silver-colored simple substance and graphite oxide is between 0.5～1.0.
3. the preparation method of a kind of Graphene according to claim 1-Nano silver grain composite is characterized in that, wherein in the step (3), the used mole of glucose is 2～10 times of silver nitrate mole.
4. the preparation method of a kind of Graphene according to claim 1-Nano silver grain composite, it is characterized in that, utilize nontoxic, eco-friendly glucose as reducing agent, thereby reducing graphene oxide and silver-colored ammonium ion original position under the reaction condition of gentleness has simultaneously obtained the Graphene-Nano silver grain composite of Nano silver grain mass fraction between 30%～50% of narrowly distributing, particle size homogeneous (about 25nm).
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