CN104148663B - The method efficiently preparing Nano silver grain-Graphene three dimensional composite structure - Google Patents
The method efficiently preparing Nano silver grain-Graphene three dimensional composite structure Download PDFInfo
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- CN104148663B CN104148663B CN201410337717.5A CN201410337717A CN104148663B CN 104148663 B CN104148663 B CN 104148663B CN 201410337717 A CN201410337717 A CN 201410337717A CN 104148663 B CN104148663 B CN 104148663B
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Abstract
The present invention provides a kind of method efficiently preparing Nano silver grain Graphene three dimensional composite structure, the method comprises the following steps: 1. obtain Nano silver grain by glucose reduction silver nitrate under conditions of adding ammonia, make it be deposited on graphene oxide lamella by charge effect；2. in autoclave, removed the oxygen-containing functional group of surface of graphene oxide by hydro-thermal method reduction, it is thus achieved that Nano silver grain Graphene three dimensional composite structure hydrogel；3. obtained three dimensional composite structure hydrogel is carried out lyophilization, remove moisture removal, it is thus achieved that intensity height, well conducting, compound uniform Nano silver grain Graphene three dimensional composite structure.The method technique is simple, low cost, and efficiency is high, green non-pollution, compound uniform.Prepared Nano silver grain/Graphene three dimensional composite structure has that conduction, intensity is high, antibacterial, light weight, oleophylic and the characteristic such as hydrophobic.It is with a wide range of applications at aspects such as catalysis, sensing, environmental conservation and ultracapacitors.
Description
Technical field
The present invention relates to the preparation method of Nano silver grain, three-dimensional grapheme and composite construction thereof, belong to materialized
Learn preparing technical field.
Background technology
Ag nanoparticle due to its special electronic structure and huge specific surface area make it in the catalysis of chemical reaction,
The aspects such as surface enhanced raman spectroscopy, senses, biomarker, antibacterial have important application, surface-enhanced Raman
Scattering technology can make the scattered signal of the molecular layer being joined directly together with metal (gold, silver nanoparticle etc.) strengthen, this
One finds to make laser Raman spectroscopy become the fields such as research surface chemistry, surface catalysis and glucose biological sensor
Important detection means.The Resonance Rayleigh Scattering utilizing ionic associate measures trace inorganic ion and also obtains good effect
Really.Recently, nanoparticle can reduce in nanoparticle surface with catalytic metal ion, makes nanoparticle grows up this
One characteristic is used for preparing various biosensor.
The bi-dimensional cellular shape crystal that Graphene is made up of hexagonal primitive unit cell carbon atom, is to build other dimension carbonaceous materials
Elementary cell.Due to two-dimensional structure and the excellent crystallography quality of its uniqueness, Graphene has many excellences
Special performance, such as high electron mobility, high transparent, high heat conductivity etc. so that it is at transparent conductive film,
Semiconductor device, composite, the various fields such as sensor has broad application prospects, 2004, Britain
The physics of University of Manchester teaches Geim etc. and has observed the stone of monolayer by a kind of method of fairly simple stripping
Ink alkene, its discovery rapidly becomes many multi-disciplinary study hotspots.Graphene is expected to be widely used in electron trade,
Sensor, brake, the field such as catalyst and bioenergy.Compared to two-dimensional graphene (Graphene, Gr),
Three-dimensional grapheme has higher specific surface area and unique tridimensional network.By Ag nanoparticle and three
Being combined of dimension Graphene, is expected to the cooperative effect by Ag nanoparticle Yu Graphene, makes material have more
Excellent electric conductivity and surface activity, have extensively at aspects such as catalysis, sensing, environmental conservation and capacitors
Application prospect.
Summary of the invention
Technical problem: three-dimensional grapheme is combined by the present invention with Nano silver grain, by environment under high pressure reduction-oxidation
Graphite, uses glucose as reducing agent and obtains Nano silver grain.Graphenic surface growth Nano silver grain with
This obtains Nano silver grain-Graphene three dimensional composite structure, it is provided that one efficiently prepares Nano silver grain-graphite
The method of alkene three dimensional composite structure.This method low cost, simple to operate, efficiency is high, environmental protection, Ke Yi great
Amount preparation.
Technical scheme: the present invention utilizes green reducing agent glucose to prepare Nano silver grain, under conditions of high pressure
Reduction-oxidation graphite, and Nano silver grain is attached in Graphene three-dimensional net structure.Described efficient preparation
The method of Nano silver grain-Graphene three dimensional composite structure includes following two parts:
The preparation of A graphene oxide: utilize the Hummers method improved to prepare graphite oxide, it is thus achieved that graphite oxide
Gel, obtains graphene oxide, puts into dry for standby in baking oven for ultrasonic 0.5-1 hour；
The preparation of B Nano silver grain-Graphene three dimensional composite structure:
1) prepare graphene oxide water solution 20ml of 2mg/ml, 2g glucose is joined above-mentioned solution
In, stir 0.5-1 hour, obtain mixed solution；
2) by 100mgAgNO3It is dissolved in the deionized water of 11mL, stirs 10-20min, then add
Enter the ammonia of 0.1-0.8mol/L, be wholly absent to white precipitate, obtain reaction solution；
3) by step 2) reaction solution of gained joins step 1) in the mixed solution of gained, and stir
Mix 5-15min, place room temperature standby；
4) by step 3) the mixed solution of gained loads in reactor, is warming up to 80-100 DEG C, protects
Temperature 30-50min, then heats to 150-180 DEG C, is incubated 12-24 hour, takes out nano grain of silver after cooling
Son-Graphene three dimensional composite structure hydrogel, with deionized water repeated washing 3-9 time；
5) by three dimensional composite structure hydrogel individual hour of freezing 1-5 at-45 to-55 DEG C, put into after taking-up
Evacuation 18-26 hour in freeze drying box；
Wherein, the described Hummers method utilizing improvement is prepared graphite oxide and is concretely comprised the following steps:
The 2A. low-temp reaction stage:
2A1., under conditions of ice-water bath, takes concentrated sulphuric acid 20-23mL that mass fraction is 98% in there-necked flask
In, stir 5-10min, be subsequently added 1000mg graphite powder, particle diameter≤30 μm, stir 15-30min,
To concentrated sulphuric acid and graphite powder mixed solution,
2A2. weighs 0.5-0.9g sodium nitrate and joins in concentrated sulphuric acid and graphite powder mixed solution, stirs 10-15min,
3000mg potassium permanganate is finally ground into powder by 2A3., is slowly added to, and prevents temperature from suddenly raising, stirs
Mix 80-100min；
The 2B. middle temperature stage of reaction: bath temperature is adjusted to 35 ± 1 DEG C, makes the mixed solution that step 2A finally obtains
Reaction 30-120min；
The 2C. pyroreaction stage: add 40-50mL deionized water in the mixed solution that step 2B finally obtains,
It is added dropwise over, is then warmed up to 90-100 DEG C, stir 30-40min；To be with deionized water volume ratio again
The hydrogen peroxide of 25-30% is added dropwise over, and stirs 10-20min, treats that solution cools down, and adds deionized water after reaction,
Stand, go the supernatant, obtain graphite oxide.
Beneficial effect: the present invention obtains Nano silver grain with glucose reduction silver nitrate, is made by charge effect
It deposits on the oxygen-containing functional group of graphene oxide, then is obtained by high pressure redox graphene and lyophilization
Obtain Nano silver grain-Graphene three dimensional composite structure that intensity is high, compound uniformly, conduct electricity.Use side of the present invention
Method, can efficiently, shape, the size prepared stable, high-quality controlled, and conduct electricity, hydrophobic, oleophylic
Nano silver grain/Graphene three dimensional composite structure.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention 1 gained sample circulation absorption test result to acetone: three dimensional composite structure
Organic substance is had good absorption property, can reuse.
Fig. 2 is embodiment of the present invention 1-3 gained sample oxidation Graphene (1) and graphene/nano silver (2)
X ray diffracting spectrum.
Detailed description of the invention
The preparation of A graphene oxide: utilize the Hummers method improved to prepare graphite oxide, it is thus achieved that graphite oxide
Gel, obtains graphene oxide, puts into dry for standby in baking oven for ultrasonic 0.5-1 hour；
The described Hummers method utilizing improvement is prepared graphite oxide and is concretely comprised the following steps:
The 1A. low-temp reaction stage:
1A1., under conditions of ice-water bath, takes concentrated sulphuric acid 20-23ml that mass fraction is 98% in there-necked flask,
Stirring 5-10mins, being subsequently added with described concentrated sulfuric acid solution weight ratio is the graphite powder of 4.35-4.55%, particle diameter
≤ 30um, stirs 15-30mins, obtains concentrated sulphuric acid and graphite powder mixed solution,
The sodium nitrate that 1A2. weighs with above-mentioned concentrated sulphuric acid and graphite powder mixed liquor weight ratio are 2.50-3.60% adds
To concentrated sulphuric acid with graphite powder mixed solution, stir 10-15mins,
Mixed solution weight ratio with step 1A2 gained is finally that 66.67-100% potassium permanganate is ground into by 1A3.
Powder, is slowly added to, and prevents temperature from suddenly raising, and stirs 80-100mins；
The 1B. middle temperature stage of reaction: bath temperature is adjusted to 35 ± 1 DEG C, makes the mixed solution that step 1A finally obtains
Reaction 30-120mins；
The 1C. pyroreaction stage: add 40-50ml deionized water in the mixed solution that step 1A finally obtains,
It is added dropwise over, is then warmed up to 90-100 DEG C, stir 30-40mins；To be with deionized water volume ratio again
The hydrogen peroxide of 25-30% is added dropwise over, and stirs 10-20mins, treats that solution cools down, and adds deionized water after reaction,
Stand, go the supernatant, obtain graphite oxide.
The preparation of B Nano silver grain/Graphene three dimensional composite structure:
1) graphene oxide water solution of 1-4mg/ml is prepared, will be with graphene oxide water solution weight ratio
Glucose for 1:14-1:16 joins in above-mentioned solution, stirs 0.5-1 hour, obtains mixed solution；
2) AgNO3 that percentage by weight is 0.10-0.20% is dissolved in deionized water, stirring
10-20mins, is subsequently adding the ammonia of 0.1-0.8mol/L, is wholly absent to white precipitate, reacted
Solution；
3) by step 2) reaction solution of gained joins step 1) in the mixed solution of gained, and stir
Mix 5-15mins, place room temperature standby；
4) by step 3) the mixed solution of gained loads in reactor, is warming up to 80-100 DEG C, protects
Temperature 30-50mins, then heats to 150-180 DEG C, is incubated 12-24 hour, takes out silver nanoparticle after cooling
Particle-Graphene three dimensional composite structure hydrogel, with deionized water repeated washing 3-9 time；
5) by three dimensional composite structure hydrogel individual hour of freezing 1-5 at-45 to-55 DEG C, put into after taking-up
Evacuation 18-26 hour in freeze drying box.
Below the reference example of the present invention is described in detail, it should be noted that the following example is only used for
The present invention is described, but is not used to limit the practical range of the present invention.
Embodiment 1:
1, low-temp reaction: concentrated sulphuric acid (98%) 20-23ml, stirs 5-8mins in ice-water bath, adds 1000mg
Graphite powder, reacts 15-20mins, adds 0.5-0.9g sodium nitrate, hybrid reaction 10-15mins, and 3000mg is high
Potassium manganate is slowly added to, and prevents temperature from suddenly raising, and stirs 80-100mins, the equal ice-water bath of above step.
2, middle temperature reaction: heat up, bath temperature about 35-36 DEG C, reacts 30-50mins
3, pyroreaction: add 40-50ml deionized water, be added dropwise over, be then warmed up to 90-100 DEG C, stirring
30-40mins, is added dropwise over 10-15ml hydrogen peroxide, stirs 10-20mins, treats that solution cools down after reaction,
Add deionized water, stand, go the supernatant.
4, repeated centrifugation 5-6 time, rotating speed is 13000-15000rpm, and the most centrifugal time is 10-15mins, often
Secondary centrifugal after take the supernatant, there is no white precipitate with barium hydroxide detection
5, ultrasonic for the graphite oxide of acquisition half an hour is peeled off, it is thus achieved that graphene oxide, puts and dry in an oven,
Standby.
6, prepare graphene oxide water solution 20ml of 2mg/ml, 2g glucose joined in above-mentioned solution,
Stir half an hour.
7,100mgAgNO3 is dissolved in the deionized water of 11ml, stirs 10-12mins, be subsequently adding 3-4
Drip the ammonia of 0.55mol/L, be wholly absent to white precipitate.
8, the solution in step 7 is joined in step 6, and stir 5-10mins, place room temperature standby.
9, the material of step 8 is loaded in the reactor of 50ml, be warming up to 100 DEG C, be incubated 30-50mins, so
After be warming up to 180 DEG C, be incubated 24 hours, after cooling take out Nano silver grain/Graphene three dimensional composite structure water
Gel, with deionized water repeated washing 3-4 time.
10, refrigerator put into by three dimensional composite structure hydrogel, freezing 2 hours, puts in freeze drying box after taking-up
Evacuation 20-24 hour at a temperature of-45 to-55 DEG C.
Accompanying drawing 1 is that the circulation absorption of acetone is tested by the embodiment of the present invention 1 gained sample, from the figure, it can be seen that
Three dimensional composite structure has good absorption property to Organic substance, can reuse.
Embodiment 2:
Present embodiment step 7 as different from Example 1 is prepared the graphene oxide water solution of 3mg/ml,
Other are same as in Example 1.
Embodiment 3:
Present embodiment step 9 as different from Example 1 is warming up to 160 DEG C, is incubated 16 hours, its
He is same as in Example 1.
Fig. 2 is that the X-ray of embodiment of the present invention 1-3 gained sample oxidation Graphene and graphene/nano silver is spread out
Penetrate collection of illustrative plates.Curve 1 is the collection of illustrative plates of graphene oxide, and the peak of graphene oxide is at about 11 °, right at 30 °
Answering carbon is the collection of illustrative plates of graphene/nano silver at the diffraction maximum of (002) crystal face, curve 2, and the peak of Graphene is received
The peak of meter Yin is covered, at 38 ° of corresponding Nano silver grains in the diffraction maximum of (111) crystal face.
Claims (1)
1. the method efficiently preparing Nano silver grain-Graphene three dimensional composite structure, it is characterised in that the party
Method includes following two parts:
The preparation of A graphene oxide: utilize the Hummers method improved to prepare graphite oxide, it is thus achieved that graphite oxide
Gel, obtains graphene oxide, puts into dry for standby in baking oven for ultrasonic 0.5-1 hour；
The preparation of B Nano silver grain-Graphene three dimensional composite structure:
1) prepare graphene oxide water solution 20ml of 2mg/ml, 2g glucose is joined above-mentioned solution
In, stir 0.5-1 hour, obtain mixed solution；
2) by 100mgAgNO3It is dissolved in the deionized water of 11mL, stirs 10-20min, then add
Enter the ammonia of 0.1-0.8mol/L, be wholly absent to white precipitate, obtain reaction solution；
3) by step 2) reaction solution of gained joins step 1) in the mixed solution of gained, and stir
Mix 5-15min, place room temperature standby；
4) by step 3) the mixed solution of gained loads in reactor, is warming up to 80-100 DEG C, protects
Temperature 30-50min, then heats to 150-180 DEG C, is incubated 12-24 hour, takes out nano grain of silver after cooling
Son-Graphene three dimensional composite structure hydrogel, with deionized water repeated washing 3-9 time；
5) by three dimensional composite structure hydrogel individual hour of freezing 1-5 at-45 to-55 DEG C, put into after taking-up
Evacuation 18-26 hour in freeze drying box；
Wherein, the described Hummers method utilizing improvement is prepared graphite oxide and is concretely comprised the following steps:
The 2A. low-temp reaction stage:
2A1., under conditions of ice-water bath, takes concentrated sulphuric acid 20-23mL that mass fraction is 98% in there-necked flask
In, stir 5-10min, be subsequently added 1000mg graphite powder, particle diameter≤30 μm, stir 15-30min,
To concentrated sulphuric acid and graphite powder mixed solution,
2A2. weighs 0.5-0.9g sodium nitrate and joins in concentrated sulphuric acid and graphite powder mixed solution, stirs 10-15min,
3000mg potassium permanganate is finally ground into powder by 2A3., is slowly added to, and prevents temperature from suddenly raising, stirs
Mix 80-100min；
The 2B. middle temperature stage of reaction: bath temperature is adjusted to 35 ± 1 DEG C, makes the mixed solution that step 2A finally obtains
Reaction 30-120min；
The 2C. pyroreaction stage: add 40-50mL deionized water in the mixed solution that step 2B finally obtains,
It is added dropwise over, is then warmed up to 90-100 DEG C, stir 30-40min；To be with deionized water volume ratio again
The hydrogen peroxide of 25-30% is added dropwise over, and stirs 10-20min, treats that solution cools down, and adds deionized water after reaction,
Stand, go the supernatant, obtain graphite oxide.
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| CN103433037A (en) * | 2013-09-09 | 2013-12-11 | 东南大学 | Preparation method of graphene foam and precious metal nano-particle composite material |
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