CN105618779A - Preparation method of silver/reduced grapheme nanocomposite - Google Patents
Preparation method of silver/reduced grapheme nanocomposite Download PDFInfo
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- CN105618779A CN105618779A CN201410626243.6A CN201410626243A CN105618779A CN 105618779 A CN105618779 A CN 105618779A CN 201410626243 A CN201410626243 A CN 201410626243A CN 105618779 A CN105618779 A CN 105618779A
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Abstract
The invention discloses a preparation method of a silver/reduced grapheme nanocomposite. The preparation method comprises the following steps: graphite oxide and silver nitrate are used as precursor solutions, sodium hydroxide is used as a reactant, and the silver/reduced grapheme nanocomposite is prepared by a hydrothermal method. Graphite oxide and silver nitrate are reduced synchronously in a hydrothermal reaction system, and silver nanoparticles are uniformly dispersed on the surface of a reduced grapheme sheet layer. The preparation method is simple in preparation process, low in cost and reagent toxicity, and mild in reaction condition, has no introduce of a reducing agent, and is an efficient environment-friendly preparation technology. The silver/reduced grapheme nanocomposite has a high potential application value in the fields, such as the bio-antimicrobial field, the electrode material field and the detection material field.
Description
Technical field
The invention belongs to new material and preparing technical field thereof, the preparation method being specifically related to a kind of silver/reduced graphene nano composite material.
Background technology
Nano material is the research boom of recent decades, and precious metal material (Au and Ag etc.) is because of its premium properties unique in sound, optical, electrical and catalysis, and becomes the study hotspot of every field. Wherein silver nano material, by excellent features such as its good electric conductivity, chemical stability, high-ductility and non-oxidizabilitys, has wide application in chemical catalysis, the energy, electronics, biological antibiotic etc. Graphene carbon material, due to its bigger specific surface area, excellent mechanical performance and electronic conduction ability free from worldly cares, has huge application prospect in battery electrode, photocatalysis, sensor and biochemistry. By noble metal nanometer material load on Graphene, it is possible to be effectively improved chemical stability and the catalytic performance of material. In recent years, silver also becomes a focus with the research of graphene composite material.
Document 1 (Shen.Jetal.JournalofMaterialsChemistry., 2011,21,7795) silver nitrate is dissolved in the mixed solution of 1-butyl-3-Methylimidazole. hexafluorophosphoric acid ionic liquid and water, graphite oxide solution adds ascorbic acid and ammonia, it is vigorously agitated again 1h after supersound process graphite solution 0.5h, after two kinds of solution mixing, utilizes one step hydro thermal method to react the composite obtaining nanometer silver and Graphene for 4 hours at 160 DEG C. Reaction temperature used by experimental technique described in the document is higher, and energy consumption is relatively big, has used organic ion liquid simultaneously, can produce certain impact for environment.
Silver ammino solution and graphite oxide solution are mixed by document 2 (Lu.Letal.AdvancedMaterials., 2013,25,1270-1274), utilize hydrazine hydrate first to reduce prepared silver nano-grain. Improving system temperature to 95 DEG C to react a night, reduction obtains reduced graphene. Experimental technique described in the document adopts strong reductant hydrazine hydrate that silver nano-grain and graphite oxide substep are reduced, and reagent toxicity is relatively big, and the response time is long, is unfavorable for again the control of Argent grain pattern.
Document 3 (R.Pasrichaetal.Small., 2009,20,5,2253-2259) mix with by silver sulfate solution and graphite oxide, utilize potassium hydroxide to process 24h followed by hydrazine hydrate after providing alkali condition, reaction to terminate and obtain silver/reduction graphite composite material. It is poor that this method obtains Graphene reduction degree, it is necessary to reacts through secondary reduction, adds the time of reaction and the difficulty of reaction. The Argent grain load on reduced graphene surface simultaneously is uneven, and load capacity is less, so can reduce the using value of material.
Summary of the invention
It is an object of the invention to, for the deficiencies in the prior art, it is provided that the preparation method of a kind of silver/reduced graphene nano composite material, described method is simple, and mild condition goes back original reagent without any, is a kind of green environment friendly technology.
Realization the technical scheme is that
The preparation method of the silver of the present invention/reduced graphene nano composite material comprises the following steps:
1) configuration graphite oxide suspension: by graphite oxide ultrasonic disperse in deionized water/dehydrated alcohol mixed solution;
2) configuration mixed solution: drip ammonia in graphite oxide suspension, by a certain amount of solid nitric acid silver solution ultrasonic disperse in graphite oxide suspension, drips the sodium hydroxide solution configured, ultrasonic disperse wherein.
3) hydro-thermal reaction is obtained by reacting silver/reduced graphene nano composite material;
Step 1) in described graphite oxide mixed solution graphite oxide be 1:(1228��1283 with the mass ratio of solution), described mixed liquor deionized water and dehydrated alcohol volume ratio are 1:(2��4);
Step 2) described in ammonia concn be 25%, consumption is 0.05��0.1mL;
Step 2) described in the mass ratio of graphite oxide and silver nitrate be 1:(4.225��16.900);
Step 2) concentration of described sodium hydroxide solution is 1��2mol/L, consumption is 10��20mL, and the time of ultrasonic disperse is 0.5h;
Step 3) solvent thermal reaction temperature is 100��120 DEG C, the response time is 6��10h.
Compared with prior art, the major advantage of the technology of the present invention is embodied in:
1, take a simple step solvent thermal reaction method and prepare compound particle, do not use and go back original reagent, without any surfactant, be a kind of green friendly method.
2, graphite oxide and silver nitrate are reduced in system simultaneously, and the Argent grain size obtained, within the scope of 10��50nm, is evenly distributed in graphenic surface.
3, the flow process of experiment is simple, and the response time is short. Using reduced graphene as backing material, utilize the specific surface area that it is bigger, enhance the chemical stability of Nano silver grain.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of the silver prepared by the embodiment of the present invention 1/reduced graphene composite.
Fig. 2 is the XRD figure of the silver prepared by the embodiment of the present invention 1/reduced graphene composite.
Fig. 3 is the Raman scattering figure of the silver prepared by the embodiment of the present invention 1/reduced graphene composite.
Fig. 4 is the XPS figure of the silver prepared by the embodiment of the present invention 1/reduced graphene composite.
Specific embodiment
In order to be more fully understood that the present invention, illustrate technical scheme below by specific embodiment.
Embodiment 1
(1) weigh 0.02g graphite oxide, be dissolved in the mixed solution of 10mL deionized water and 20mL dehydrated alcohol composition, ultrasonic disperse 30min, form graphite oxide suspension.
(2) drip in suspension 0.05mL 25% ammonia, 0.169g solid nitric acid silver is added in graphite oxide solution, supersound process 10min. The sodium hydroxide solution of the 2mol/L of 10mL is dripped wherein under magnetic agitation. Ultrasonic disperse 30min.
(3) reaction system being transferred in the hydrothermal reaction kettle that politef is liner, 120 DEG C are reacted 6 hours. The solution obtained uses high speed centrifuge 10000r/min centrifugation, washes respectively three times with ethanol and washing, and then vacuum drying 3h at 40 DEG C, obtains product.
Fig. 1 is the TEM figure of embodiment 1, and silver nano-grain is carried on reduced graphene surface equably as seen from Figure 1.
Fig. 2 is the XRD figure of embodiment 1, and graphite oxide is reduced to reduced graphene as seen from the figure, and reduction degree is better. The characteristic peak of Emission in Cubic silver proves that Argent grain is present in complex.
Fig. 3 is the Raman figure of embodiment 1, and graphite oxide is reduced as seen from the figure.
Fig. 4 is the XPS figure of embodiment 1, the characteristic peak of C, O, Ag as seen from the figure, the minimizing of O constituent content, it was demonstrated that the reduction of graphite oxide.
Embodiment 2
(1) weigh in the mixed solution that 0.02g graphite oxide is dissolved in 5mL deionized water and 25mL dehydrated alcohol composition, ultrasonic disperse 30min, form graphite oxide suspension.
(2) drip in suspension 0.05mL 25% ammonia, 0.0845g solid nitric acid silver is added in graphite oxide solution, supersound process 10min. To the sodium hydroxide solution of the 1mol/L of mixed solution and dripping 15mL under magnetic agitation, ultrasonic disperse 30min.
(3) reaction system being transferred in the hydrothermal reaction kettle that politef is liner, 120 DEG C are reacted 10 hours. The solution obtained uses high speed centrifuge 10000r/min centrifugation, washes respectively three times with ethanol and washing, and then vacuum drying 3h at 40 DEG C, obtains product.
Embodiment 3
(1) weighing in the mixed solution that 0.02g graphite oxide is dissolved in 10mL deionized water and 20mL dehydrated alcohol composition, ultrasonic 30min forms graphite oxide suspension.
(2) drip in suspension 0.01mL 25% ammonia, 0.338g solid nitric acid silver is added in graphite oxide solution, supersound process 10min. To the sodium hydroxide solution of the 2mol/L of mixed solution and dripping 20mL under magnetic agitation, ultrasonic disperse 30min.
(3) reaction system being transferred in the hydrothermal reaction kettle that politef is liner, 100 DEG C are reacted 8 hours. The solution obtained uses high speed centrifuge 10000r/min centrifugation, washes respectively three times with ethanol and washing, and then vacuum drying 3h at 40 DEG C, obtains product.
Above-described embodiment does not limit the present invention in any way, and the technical scheme that every employing is equal to replacement or the mode of equivalent transformation obtains all falls within protection scope of the present invention.
Claims (6)
1. the preparation method of silver/reduced graphene nano composite material, it is characterised in that described method is not introduce to go back original reagent, in the basic conditions reduction silver nitrate and graphite oxide simultaneously, obtain silver/reduced graphene nano composite material; Specifically include following steps:
(1) prepare graphite oxide mixing suspension: by graphite oxide powder ultrasonic disperse in the mixed solution of deionized water/dehydrated alcohol, form suspension;
(2) silver nitrate/graphite oxide mixed solution is prepared: in oxidized graphite mixed liquor, drip ammonia, solid nitric acid silver is dissolved in mixed solution, ultrasonic disperse, configuration sodium hydroxide solution, sodium hydroxide solution is added drop-wise in silver nitrate/graphite oxide mixed solution, forms mixed solution.
(3) hydro-thermal method prepares silver/reduced graphene nano composite material: mixed solution is transferred in hydrothermal reaction kettle, generates silver/reduced graphene nano composite material through hydro-thermal reaction.
2. the preparation method of silver according to claim 1/reduced graphene nano composite material, it is characterized in that, in the described graphite oxide mixed solution of step (1), graphite oxide is 1:(1228��1283 with the mass ratio of solution), described mixed liquor deionized water and dehydrated alcohol volume ratio are 1:(2��4).
3. the preparation method of silver according to claim 1/reduced graphene nano composite material, it is characterised in that the ammonia concn described in step (2) is 25%, consumption is 0.05��0.1mL.
4. the preparation method of silver according to claim 1/reduced graphene nano composite material, it is characterised in that the mass ratio of the graphite oxide described in step (2) and silver nitrate is 1:(4.225��16.900).
5. the preparation method of silver according to claim 1/reduced graphene nano composite material, it is characterised in that the concentration of step (2) described sodium hydroxide solution is 1��2mol/L, consumption is 10��20mL, and the time of ultrasonic disperse is 0.5h.
6. the preparation method of silver according to claim 1/reduced graphene nano composite material, it is characterised in that step (3) solvent thermal reaction temperature is 100��120 DEG C, the response time is 6��10h.
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| CN112048817A (en) * | 2020-09-04 | 2020-12-08 | 润克(集团)股份有限公司 | Warm-keeping and antibacterial school uniform fabric and preparation method thereof |
| CN114523119A (en) * | 2021-12-31 | 2022-05-24 | 嘉兴辰昊新材料科技有限公司 | Preparation method of graphene silver powder and graphene silver powder |
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| CN114523119B (en) * | 2021-12-31 | 2024-01-09 | 嘉兴辰昊新材料科技有限公司 | Preparation method of graphene silver powder and graphene silver powder |
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