CN104148663A - Method for efficiently preparing silver nano particle-graphene three-dimensional composite structure - Google Patents
Method for efficiently preparing silver nano particle-graphene three-dimensional composite structure Download PDFInfo
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Abstract
The invention provides a method for efficiently preparing a silver nano particle-graphene three-dimensional composite structure. The method includes the steps of firstly, reducing silver nitrate through glucose under a condition of adding ammonia water to obtain silver nano particles, and allowing the silver nano particles to be deposited on a graphene oxide sheet layer by the aid of ; secondly, reducing to remove the oxygen-containing functional group on the surface of the graphene oxide through a hydrothermal method in a reaction kettle to obtain silver nano particle-graphene three-dimensional composite structure hydrogel; thirdly, refrigerating and drying the obtained three-dimensional composite structure hydrogel to remove moisture and obtain the silver nano particle-graphene three-dimensional composite structure which is high in strength, good in conductivity, pollution-free, even in composition, antibacterial, lightweight, oleophylic, hydrophobic, promising in application prospects in aspects of catalysis, sensing, environmental protection and super-capacitors, and the like.
Description
Technical field
The present invention relates to the preparation method of Nano silver grain, three-dimensional grapheme and composite construction thereof, belong to materials chemistry preparing technical field.
Background technology
Ag nano particle is because its special electronic structure and huge specific area make its catalysis at chemical reaction, SERS, sensing, biomarker, there is important application the aspect such as antibacterial, SERS technology can make the scattered signal of the molecular layer being directly connected with metal (gold, silver nano particle etc.) strengthen, and this discovery makes laser Raman spectroscopy become the important detection means in the fields such as research surface chemistry, surface catalysis and glucose biological sensor.Utilize the Resonance Rayleigh Scattering mensuration trace inorganic ions of ionic associate also to obtain good effect.Recently, nano particle can reduce in nanoparticle surface by catalytic metal ion, makes this characteristic that nano particle is grown up be used to prepare various biology sensors.
The bi-dimensional cellular shape crystal that Graphene is made up of hexagonal primitive unit cell carbon atom is the elementary cell that builds other dimension carbonaceous materials.Due to its unique two-dimensional structure and excellent crystallography quality, Graphene has the special performance of many excellences, for example high electron mobility, high transparent, high heat conductivity etc., make it at transparent conductive film, semiconductor devices, composite, in sensor various fields, have broad application prospects, 2004, a kind of methods of quite simply peeling off of use such as the physics professor Geim of Univ Manchester UK observed the Graphene of individual layer, and its discovery becomes rapidly many multi-disciplinary study hotspots.Graphene is expected to be widely used in the fields such as electron trade, sensor, brake, catalyst and bioenergy.Than two-dimentional Graphene (Graphene, Gr), three-dimensional grapheme has higher specific area and unique tridimensional network.Compound by Ag nano particle and three-dimensional grapheme; be expected to the cooperative effect by Aag nano particle and Graphene; make material there is more excellent electric conductivity and surface-active, be with a wide range of applications at aspects such as catalysis, sensing, environmental protection and capacitors.
Summary of the invention
Technical problem: the present invention is combined three-dimensional grapheme with Nano silver grain, by hyperbaric environment reduction-oxidation graphite, utilizes glucose to obtain Nano silver grain as reducing agent.Obtain Nano silver grain-Graphene three dimensional composite structure at Graphene superficial growth Nano silver grain with this, a kind of method of efficiently preparing Nano silver grain-Graphene three dimensional composite structure is provided.This method cost is low, simple to operate, efficiency is high, environmental protection, can prepare in a large number.
Technical scheme: the present invention utilizes green reducing agent glucose to prepare Nano silver grain, reduction-oxidation graphite under the condition of high pressure, and Nano silver grain is attached in Graphene three-dimensional net structure.The described method of efficiently preparing Nano silver grain-Graphene three dimensional composite structure comprises following two parts:
The preparation of A graphene oxide: utilize improved Hummers legal system for graphite oxide, obtain graphite oxide gel, obtain graphene oxide, put into baking oven dry for standby for ultrasonic 0.5-1 hour;
The preparation of B Nano silver grain/Graphene three dimensional composite structure:
1) the graphite oxide aqueous solution of preparation 1-4mg/ml, by being 1:14-1:16 with graphite oxide aqueous solution weight ratio, glucose joins in above-mentioned solution, stirs 0.5-1 hour, obtains mixed solution;
2) AgNO3 that is 0.10-0.20% by percentage by weight is dissolved in deionized water, stirs 10-20mins, then adds the ammoniacal liquor of 0.1-0.8mol/L, disappears completely to white precipitate, obtains reaction solution;
3) by step 2) reaction solution of gained joins step 1) in the mixed solution of gained, and stir 5-15mins, place room temperature for subsequent use;
4) by step 3) the mixed solution of gained packs in reactor, be warming up to 80-100 DEG C, insulation 30-50mins, then be warming up to 150-180 DEG C, insulation 12-24 hour, cooling rear taking-up Nano silver grain-Graphene three dimensional composite structure hydrogel, uses deionized water repeated washing 3-9 time;
5) by three dimensional composite structure hydrogel at-45 to-55 DEG C freezing 1-5 hour, after taking-up, put into freeze drying box and vacuumize 18-26 hour.
Wherein, the described improved Hummers legal system of utilizing for graphite oxide concrete steps is:
A. the low-temp reaction stage:
A1. under the condition of ice-water bath, get mass fraction and be 98% concentrated sulfuric acid 20-23ml in there-necked flask, stir 5-10mins, the graphite powder that to add subsequently with described concentrated sulfuric acid solution weight ratio be 4.35-4.55%, particle diameter≤30um, stir 15-30mins, obtain the concentrated sulfuric acid and graphite powder mixed solution
A2. the sodium nitrate that to take with the above-mentioned concentrated sulfuric acid and graphite powder mixed liquor weight ratio be 2.50-3.60% joins in the concentrated sulfuric acid and graphite powder mixed solution, stirs 10-15mins,
A3. finally by with the mixed solution weight ratio of steps A 2 gained be 66.67-100% potassium permanganate pulverize, slowly add, prevent that temperature from raising suddenly, stir 80-100mins;
B. the warm stage of reaction in: bath temperature is adjusted to 35 ± 1 DEG C, the mixed solution reaction 30-120mins that steps A is finally obtained;
C. the pyroreaction stage: add 40-50ml deionized water in the mixed solution finally obtaining in steps A, dropwise add, be then warmed up to 90-100 DEG C, stir 30-40mins; By being 25-30% with deionized water volume ratio, hydrogen peroxide dropwise adds again, stirs 10-20mins, treats that solution is cooling after reaction, adds deionized water, leaves standstill, and removes supernatant liquor, obtains graphite oxide.
Beneficial effect: the present invention obtains Nano silver grain with Reduction of Glucose silver nitrate, make on its oxygen-containing functional group that deposits to graphene oxide by charge effect, then obtain by high pressure redox graphene and freeze drying Nano silver grain-Graphene three dimensional composite structure that intensity is high, compound evenly, conduct electricity.Adopt the inventive method, can be efficiently, stablize, high-qualityly prepare shape, size is controlled, and conduction, hydrophobic, Nano silver grain/Graphene three dimensional composite structure of oleophylic.
Brief description of the drawings
Fig. 1 is the color contrast figure of graphene oxide and graphene oxide/Nano silver solution in embodiment of the present invention 1-3 process.
The sample graphene oxide (1) that Fig. 2 is embodiment of the present invention 1-3 and the X ray diffracting spectrum of graphene/nano silver (2).
Detailed description of the invention
The preparation of A graphene oxide: utilize improved Hummers legal system for graphite oxide, obtain graphite oxide gel, obtain graphene oxide, put into baking oven dry for standby for ultrasonic 0.5-1 hour;
The described improved Hummers legal system of utilizing for graphite oxide concrete steps is:
A. the low-temp reaction stage:
A1. under the condition of ice-water bath, get mass fraction and be 98% concentrated sulfuric acid 20-23ml in there-necked flask, stir 5-10mins, the graphite powder that to add subsequently with described concentrated sulfuric acid solution weight ratio be 4.35-4.55%, particle diameter≤30um, stir 15-30mins, obtain the concentrated sulfuric acid and graphite powder mixed solution
A2. the sodium nitrate that to take with the above-mentioned concentrated sulfuric acid and graphite powder mixed liquor weight ratio be 2.50-3.60% joins in the concentrated sulfuric acid and graphite powder mixed solution, stirs 10-15mins,
A3. finally by with the mixed solution weight ratio of steps A 2 gained be 66.67-100% potassium permanganate pulverize, slowly add, prevent that temperature from raising suddenly, stir 80-100mins;
B. the warm stage of reaction in: bath temperature is adjusted to 35 ± 1 DEG C, the mixed solution reaction 30-120mins that steps A is finally obtained;
C. the pyroreaction stage: add 40-50ml deionized water in the mixed solution finally obtaining in steps A, dropwise add, be then warmed up to 90-100 DEG C, stir 30-40mins; By being 25-30% with deionized water volume ratio, hydrogen peroxide dropwise adds again, stirs 10-20mins, treats that solution is cooling after reaction, adds deionized water, leaves standstill, and removes supernatant liquor, obtains graphite oxide.
The preparation of B Nano silver grain/Graphene three dimensional composite structure:
1) the graphite oxide aqueous solution of preparation 1-4mg/ml, by being 1:14-1:16 with graphite oxide aqueous solution weight ratio, glucose joins in above-mentioned solution, stirs 0.5-1 hour, obtains mixed solution;
2) AgNO3 that is 0.10-0.20% by percentage by weight is dissolved in deionized water, stirs 10-20mins, then adds the ammoniacal liquor of 0.1-0.8mol/L, disappears completely to white precipitate, obtains reaction solution;
3) by step 2) reaction solution of gained joins step 1) in the mixed solution of gained, and stir 5-15mins, place room temperature for subsequent use;
4) by step 3) the mixed solution of gained packs in reactor, be warming up to 80-100 DEG C, insulation 30-50mins, then be warming up to 150-180 DEG C, insulation 12-24 hour, cooling rear taking-up Nano silver grain-Graphene three dimensional composite structure hydrogel, uses deionized water repeated washing 3-9 time;
5) by three dimensional composite structure hydrogel at-45 to-55 DEG C freezing 1-5 hour, after taking-up, put into freeze drying box and vacuumize 18-26 hour.
Below reference example of the present invention is described in detail, it should be noted that, the following example is only for the present invention is described, but is not used for limiting practical range of the present invention.
Embodiment 1:
1, low-temp reaction: the concentrated sulfuric acid (98%) 20-23ml, in ice-water bath, stir 5-8mins, add 1000mg graphite powder, reaction 15-20mins, adds 0.5-0.9g sodium nitrate, hybrid reaction 10-15mins, 3000mg potassium permanganate slowly adds, prevent that temperature from raising suddenly, stir 80-100mins, the equal ice-water bath of above step.
2, middle temperature reaction: heat up, bath temperature 35-36 DEG C left and right, reaction 30-50mins
3, pyroreaction: add 40-50ml deionized water, dropwise add, be then warmed up to 90-100 DEG C, stir 30-40mins, 10-15ml hydrogen peroxide is dropwise added, stir 10-20mins, treat after reaction that solution is cooling, add deionized water, leave standstill, remove supernatant liquor
4, repeated centrifugation 5-6 time, rotating speed is 13000-15000rpm, each centrifugal time is 10-15mins, gets supernatant liquor after each centrifugal, detects and there is no white precipitate with barium hydroxide
5, peeled off ultrasonic the graphite oxide of acquisition half an hour, obtain graphene oxide, be placed in baking oven and dry, for subsequent use.
6, the graphite oxide aqueous solution 20ml of preparation 2mg/ml, joins 2g glucose in above-mentioned solution, stirs half an hour.
7,100mgAgNO3 is dissolved in the deionized water of 11ml, stirs 10-12mins, then add 3-4 to drip the ammoniacal liquor of 0.55mol/L, disappear completely to white precipitate.
8, the solution in step 7 is joined in step 6, and stir 5-10mins, placement room temperature is for subsequent use.
9, the material of step 8 is packed in the reactor of 50ml, be warming up to 100 DEG C, insulation 30-50mins, is then warming up to 180 DEG C, is incubated 24 hours, and cooling rear taking-up Nano silver grain/Graphene three dimensional composite structure hydrogel is used deionized water repeated washing 3-4 time.
10, three dimensional composite structure hydrogel is put into refrigerator, freezing 2 hours, puts into freeze drying box and vacuumize 20-24 hour after taking-up at-45 to-55 DEG C of temperature.
Accompanying drawing 1 is the circulation absorption test of the embodiment of the present invention 1 gained sample to acetone, and as we can see from the figure, three dimensional composite structure has good absorption property to organic matter, can reuse.
Embodiment 2:
Present embodiment is prepared the graphite oxide aqueous solution of 3mg/ml as different from Example 1 in step 7, and other are identical with embodiment 1.
Embodiment 3:
Present embodiment is warming up to 160 DEG C in step 9 as different from Example 1, is incubated 16 hours, and other are identical with embodiment 1.
Fig. 2 is the X ray diffracting spectrum of embodiment of the present invention 1-3 gained sample graphene oxide and graphene/nano silver.The collection of illustrative plates that curve 1 is graphene oxide, the peak of graphene oxide is 11 ° of left and right, diffraction maximum at 30 ° of corresponding carbon at (002) crystal face, the collection of illustrative plates that curve 2 is graphene/nano silver, the peak of Graphene is covered by the peak of Nano Silver, the diffraction maximum at 38 ° of corresponding Nano silver grains at (111) crystal face.
Claims (2)
1. efficiently prepare a method for Nano silver grain-Graphene three dimensional composite structure, it is characterized in that the method comprises following two parts:
The preparation of A graphene oxide: utilize improved Hummers legal system for graphite oxide, obtain graphite oxide gel, obtain graphene oxide, put into baking oven dry for standby for ultrasonic 0.5-1 hour;
The preparation of B Nano silver grain/Graphene three dimensional composite structure:
1) the graphite oxide aqueous solution of preparation 1-4mg/ml, by being 1:14-1:16 with graphite oxide aqueous solution weight ratio, glucose joins in above-mentioned solution, stirs 0.5-1 hour, obtains mixed solution;
2) AgNO3 that is 0.10-0.20% by percentage by weight is dissolved in deionized water, stirs 10-20mins, then adds the ammoniacal liquor of 0.1-0.8mol/L, disappears completely to white precipitate, obtains reaction solution;
3) by step 2) reaction solution of gained joins step 1) in the mixed solution of gained, and stir 5-15mins, place room temperature for subsequent use;
4) by step 3) the mixed solution of gained packs in reactor, be warming up to 80-100 DEG C, insulation 30-50mins, then be warming up to 150-180 DEG C, insulation 12-24 hour, cooling rear taking-up Nano silver grain-Graphene three dimensional composite structure hydrogel, uses deionized water repeated washing 3-9 time;
5) by three dimensional composite structure hydrogel at-45 to-55 DEG C freezing 1-5 hour, after taking-up, put into freeze drying box and vacuumize 18-26 hour.
2. the method for efficiently preparing Nano silver grain-Graphene three dimensional composite structure according to claim 1, is characterized in that the described improved Hummers legal system of utilizing for graphite oxide concrete steps is:
A. the low-temp reaction stage:
A1. under the condition of ice-water bath, get mass fraction and be 98% the concentrated sulfuric acid in there-necked flask, stir 5-10mins, the graphite powder that to add subsequently with described concentrated sulfuric acid solution weight ratio be 4.35-4.55%, particle diameter≤30um, stirs 15-30mins, obtain the concentrated sulfuric acid and graphite powder mixed solution
A2. the sodium nitrate that to take with the above-mentioned concentrated sulfuric acid and graphite powder mixed liquor weight ratio be 2.50-3.60% joins in the concentrated sulfuric acid and graphite powder mixed solution, stirs 10-15mins,
A3. finally by with the mixed solution weight ratio of steps A 2 gained be 66.67-100% potassium permanganate pulverize, slowly add, prevent that temperature from raising suddenly, stir 80-100mins;
B. the warm stage of reaction in: bath temperature is adjusted to 35 ± 1 DEG C, the mixed solution reaction 30-120mins that steps A is finally obtained;
C. the pyroreaction stage: add 40-50ml deionized water in the mixed solution finally obtaining in steps A, dropwise add, be then warmed up to 90-100 DEG C, stir 30-40mins; By being 25-30% with deionized water volume ratio, hydrogen peroxide dropwise adds again, stirs 10-20mins, treats that solution is cooling after reaction, adds deionized water, leaves standstill, and removes supernatant liquor, obtains graphite oxide.
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| CN112151285A (en) * | 2020-09-04 | 2020-12-29 | 安徽壹石通材料科技股份有限公司 | Two-dimensional lamellar phase enhanced silver-based electric contact material and preparation method thereof |
| CN112151285B (en) * | 2020-09-04 | 2023-06-20 | 安徽壹石通材料科技股份有限公司 | Silver-based electric contact material with two-dimensional lamellar phase enhancement and preparation method thereof |
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