CN102581267A - Silver-graphene composite material and method for conveniently producing silver-graphene composite material - Google Patents
Silver-graphene composite material and method for conveniently producing silver-graphene composite material Download PDFInfo
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Abstract
The invention relates to a silver-graphene composite material and a method for conveniently producing the silver-graphene composite material. The method comprises the following preparation steps: placing graphite in a ball-milling tank, adding a polar solvent, water and silver nitrate and carrying out ball milling for a certain time; and after finishing ball milling, performing redispersion, filtration, washing and drying on the product to obtain the silver-graphene composite material. The sizes of silver nanoparticles of the composite material prepared by the method is within 50nm, the silver nanoparticles have uniform sizes and dispersion, the thickness of the graphene is between 1-10 carbon atom layers, the silver-graphene composite material has a favorable crystal structure, and the yield of the composite material is 30-50% of the mass of the added graphite. The method has the advantages of being simple in preparation process, and easy in scale enlargement and realization of industrial production.
Description
Technical field
The invention belongs to the Graphene is substrate, and in the technology of preparing of its area load silver nano-grain, belongs to technical field of nano material.
Background technology
Graphene is owing to have unique character such as great specific area, higher electrical conductivity, better physical chemical stability and biocompatibility; Therefore since 2004 find, be the focus that everybody studies as the graphene-based composite of substrate with Graphene always.The nano composite material that with the Graphene is substrate can be widely used in aspects such as catalysis, degraded, energy storage.The preparation of graphene-based composite mainly contains two kinds of methods; The one, prepare composite with graphene oxide as precursor; Owing to contain a large amount of chemical functional group (hydroxyl, carboxyl, epoxy radicals) on the graphene oxide; These groups can make Graphene have bigger load capacity effectively as the binding site of nano-metal particle, and are therefore more extensive what use at present.Yet chemical functional group's existence has destroyed the good sp of Graphene on the graphene film
2Hybrid structure, although most of functional group can remove through electronation, the fault of construction that is caused in the oxidizing process has still influenced the performance of Graphene.And through micromechanics peel off, Graphene that method makes such as liquid phase is ultrasonicly peeled off, wet ball grinding is peeled off is because fault of construction is less; Performance is better in theory, but the binding site on the graphene film that makes through these methods is less, can make the difficulty increase that nano particle and graphene film are compound; Load capacity descends; In addition, the size of the Graphene that makes through these methods is less, productive rate is generally all very low, thereby has influenced its further application.
Silver-graphitic thiazolinyl composite has performances such as excellent antibiotic, catalysis, energy storage.For example Shen etc. has showed excellent antibiotic active (J Shen.et al.Nano Research, 3,339-349 (2010)) through the formed Ag/ graphene composite material of silver ion that reduction is attached on the graphene oxide; The composite that Kima etc. utilize similar method to make is used for the ultracapacitor aspect, shows good energy-storage property, can reach 140F/g (K.S.Kima, et al.Synthetic Metals, 160,2355-2360 (2010)) than electric capacity.But these generally have bigger size through the Ag nano particle that the sedimentation chemistry reducing process makes, thereby influence performance of composites.The silver nano-grain that therefore will have reduced size is carried on the Graphene with better crystalline structure, can be so that performance of composites obtains bigger improvement.
Summary of the invention
The objective of the invention is to overcome the deficiency in the above-mentioned Composite Preparation process, when graphite crystal is thoroughly peeled off, make silver nano-grain be attached to the Graphene surface uniformly, a step makes silver-graphitic alkene composite.The invention enables the preparation process of this composite to simplify greatly, a kind of enlargement of scale that is easy to is provided, realize the preparation method of industrialized silver-graphitic thiazolinyl composite.
The technical solution that realizes the object of the invention is: in organic solvent-aqueous systems, graphite and silver nitrate are carried out ball milling; Wherein, the organic solvent of being selected for use is a polar solvent, and dielectric constant is 15～125.
The method of said production silver-graphitic alkene composite, specifically realize through following process:
One, at first graphite is joined in the ball grinder, add dielectric constant then and be 15～125 polar solvent, water and silver nitrate and ball milling.
Two, after ball milling was accomplished, it was that 15～125 polar solvent disperses again and leaves standstill that mixed liquor is used dielectric constant, after the system of treating is stable, the upper strata part that suspends was poured out, and filtered out deposition, and washing, dry back obtain silver-graphitic alkene composite.
Above-mentioned dielectric constant is that 15～125 polar organic solvent is formic acid, methyl alcohol, ethanol, acetone, cyclohexanone, tetramethylurea, formamide, N-NMF, N-methyl pyrrolidone, N; Dinethylformamide, acetamide, N-methylacetamide, N, one or more mixtures in N-dimethylacetylamide, pyrrolidones, pyrroles, the pyridine etc.
The volume ratio of employed organic solvent and water is 0.1～50: 1 in the above-mentioned mechanical milling process.
The mass ratio of above-mentioned employed graphite and silver nitrate is 1: 0.1～10.
After adopting such scheme, the present invention compared with prior art, advantage is:
1, be raw material with graphite, selecting dielectric constant for use is 15～125 organic polar solvent, can one-step method make silver-graphitic alkene composite, and the preparation process is simple, is easy to enlargement of scale, realizes suitability for industrialized production.The productive rate of composite is add 30%～50% of graphite quality.
2, in the composite, the silver nano-grain size less than 50nm and big or small homogeneous, be dispersed in the Graphene surface, Graphene thickness and has good crystal structure between 1～10 carbon atomic layer.
Description of drawings
Fig. 1 is the XRD figure of embodiment 1 obtained silver-graphitic alkene composite.
Fig. 2 is the transmission electron microscope picture of embodiment 1 obtained silver-graphitic alkene composite.
Fig. 3 is the XRD figure of the composite that makes of ball milling with an organic solvent not.
Fig. 4 is the preparation method's of silver-graphitic alkene composite of the present invention sketch map.
The specific embodiment
Embodiment 1:
Accurately take by weighing graphite 0.5g and drop in the 10mL ball grinder, add 2mLN-methyl pyrrolidone, 2mL deionized water and 0.5g silver nitrate then successively, add the steel abrading-ball at last, ball milling 3h under 30 times/second concussion frequency.Mixed liquor behind the ball milling added pours out the upper strata dispersion liquid after the 20mLN-methyl pyrrolidone disperses to leave standstill 1h, sand core funnel filter remove respectively wash 3 times with 20mL deionized water, ethanol successively behind the organic solvent after sample behind dry 24h under 60 ℃ of conditions of vacuum drying chamber, get silver-graphitic alkene composite.The composite productive rate be about add 50% of graphite quality.Fig. 1,2 shows about nanoparticle size 1～5nm and big or small homogeneous, be dispersed in the Graphene surface, and Graphene thickness and has good crystal structure between 1～3 carbon atomic layer.
Embodiment 2:
Accurately take by weighing graphite 0.5g and drop in the 10mL ball grinder, add 2mLN-methyl pyrrolidone, 0.4mL deionized water and 0.5g silver nitrate then successively, add the steel abrading-ball at last, ball milling 3h under 30 times/second concussion frequency.Mixed liquor behind the ball milling added pours out the upper strata dispersion liquid after the 20mLN-methyl pyrrolidone disperses to leave standstill 1h, sand core funnel filter remove respectively wash 3 times with 20mL deionized water, ethanol successively behind the organic solvent after sample behind dry 24h under 60 ℃ of conditions of vacuum drying chamber, get silver-graphitic alkene composite.The composite productive rate be about add 40% of graphite quality.About nanoparticle size 10～20nm and big or small homogeneous, be dispersed in the Graphene surface, Graphene thickness and has good crystal structure between 4～6 carbon atomic layers.
Embodiment 3:
Accurately take by weighing graphite 0.5g and drop in the 10mL ball grinder, add 0.3mLN-methyl pyrrolidone, 2mL deionized water and 0.5g silver nitrate then successively, add the steel abrading-ball at last, ball milling 3h under 30 times/second concussion frequency.Mixed liquor behind the ball milling added pours out the upper strata dispersion liquid after the 20mLN-methyl pyrrolidone disperses to leave standstill 1h, sand core funnel filter remove respectively wash 3 times with 20mL deionized water, ethanol successively behind the organic solvent after sample behind dry 24h under 60 ℃ of conditions of vacuum drying chamber, get silver-graphitic alkene composite.The composite productive rate be about add 42% of graphite quality.About nanoparticle size 10～15nm and big or small homogeneous, be dispersed in the Graphene surface, Graphene thickness and has good crystal structure between 8～10 carbon atomic layers.
Embodiment 4:
Accurately take by weighing graphite 0.5g and drop in the 10mL ball grinder, add 2mLN-methyl pyrrolidone, 2mL deionized water and 0.05g silver nitrate then successively, add the steel abrading-ball at last, ball milling 3h under 30 times/second concussion frequency.Mixed liquor behind the ball milling added pours out the upper strata dispersion liquid after the 10mLN-methyl pyrrolidone disperses to leave standstill 1h, sand core funnel filter remove respectively wash 3 times with 20mL deionized water, ethanol successively behind the organic solvent after sample behind dry 24h under 60 ℃ of conditions of vacuum drying chamber, get silver-graphitic alkene composite.The composite productive rate be about add 35% of graphite quality.About nanoparticle size 1～5nm and big or small homogeneous, be dispersed in the Graphene surface, Graphene thickness and has good crystal structure between 4～6 carbon atomic layers.
Embodiment 5:
Accurately take by weighing graphite 0.5g and drop in the 10mL ball grinder, add 2mLN-methyl pyrrolidone, 0.4mL deionized water and 4.0g silver nitrate then successively, add the steel abrading-ball at last, ball milling 3h under 30 times/second concussion frequency.Mixed liquor behind the ball milling added pours out the upper strata dispersion liquid after the 10mLN-methyl pyrrolidone disperses to leave standstill 1h, sand core funnel filter remove respectively wash 3 times with 20mL deionized water, ethanol successively behind the organic solvent after sample behind dry 24h under 60 ℃ of conditions of vacuum drying chamber, get silver-graphitic alkene composite.The composite productive rate be about add 48% of graphite quality.About nanoparticle size 30～50nm and big or small homogeneous, be dispersed in the Graphene surface, Graphene thickness and has good crystal structure between 3～6 carbon atomic layers.
Embodiment 6:
Accurately take by weighing graphite 0.5g and drop in the 10mL ball grinder, add 2mL N then successively, dinethylformamide, 0.4mL deionized water and 0.5g silver nitrate add the steel abrading-ball at last, ball milling 3h under 30 times/second concussion frequency.Mixed liquor behind the ball milling is added 20mL N; Dinethylformamide is poured out the upper strata dispersion liquid after disperseing to leave standstill 1h, sand core funnel filter remove respectively wash 3 times with 20mL deionized water, ethanol successively behind the organic solvent after sample must silver-graphitic alkene composite behind dry 24h under 60 ℃ of conditions of vacuum drying chamber.The composite productive rate be about add 39% of graphite quality.About nanoparticle size 10～20nm and big or small homogeneous, be dispersed in the Graphene surface, Graphene thickness and has good crystal structure between 4～8 carbon atomic layers.
Embodiment 7:
Accurately take by weighing graphite 0.5g and drop in the 10mL ball grinder, add 0.3mL N then successively, dinethylformamide, 2mL deionized water and 0.5g silver nitrate add the steel abrading-ball at last, ball milling 3h under 30 times/second concussion frequency.Mixed liquor behind the ball milling is added 20mL N; Dinethylformamide is poured out the upper strata dispersion liquid after disperseing to leave standstill 1h, sand core funnel filter remove respectively wash 3 times with 20mL deionized water, ethanol successively behind the organic solvent after sample must silver-graphitic alkene composite behind dry 24h under 60 ℃ of conditions of vacuum drying chamber.The composite productive rate be about add 42% of graphite quality.About nanoparticle size 8～15nm and big or small homogeneous, be dispersed in the Graphene surface, Graphene thickness and has good crystal structure between 8～10 carbon atomic layers.
Embodiment 8:
Accurately take by weighing graphite 0.5g and drop in the 10mL ball grinder, add 1mL N then successively, dinethylformamide, 1mL N-methyl pyrrolidone, 2mL deionized water and 0.5g silver nitrate add the steel abrading-ball at last, ball milling 3h under 30 times/second concussion frequency.Mixed liquor behind the ball milling is added 20mL N; Dinethylformamide is poured out the upper strata dispersion liquid after disperseing to leave standstill 1h, sand core funnel filter remove respectively wash 3 times with 20mL deionized water, ethanol successively behind the organic solvent after sample must silver-graphitic alkene composite behind dry 24h under 60 ℃ of conditions of vacuum drying chamber.The composite productive rate be about add 45% of graphite quality.About nanoparticle size 4～8nm and big or small homogeneous, be dispersed in the Graphene surface, Graphene thickness and has good crystal structure between 5～7 carbon atomic layers.
Embodiment 9:
Accurately take by weighing graphite 0.5g and drop in the 10mL ball grinder, add 2mL pyridine, 2mL deionized water and 0.5g silver nitrate then successively, add the steel abrading-ball at last, ball milling 3h under 30 times/second concussion frequency.Mixed liquor behind the ball milling added pours out the upper strata dispersion liquid after the 20mL pyridine disperses to leave standstill 1h, sand core funnel filter remove respectively wash 3 times with 20mL deionized water, ethanol successively behind the organic solvent after sample behind dry 24h under 60 ℃ of conditions of vacuum drying chamber, get silver-graphitic alkene composite.The composite productive rate be about add 38% of graphite quality.About nanoparticle size 10～20nm and big or small homogeneous, be dispersed in the Graphene surface, Graphene thickness and has good crystal structure between 4～8 carbon atomic layers.
Comparative Examples 1:
Accurately take by weighing graphite 0.5g and drop in the 10mL ball grinder, add 4mL deionized water and 0.5g silver nitrate then successively, add the steel abrading-ball at last, ball milling 3h under 30 times/second concussion frequency.Mixed liquor behind the ball milling added pours out the upper strata dispersion liquid after 20mL N-methyl pyrrolidone disperses to leave standstill 1h, sand core funnel filter remove respectively wash 3 times with 20mL deionized water, ethanol successively behind the organic solvent after sample behind dry 24h under 60 ℃ of conditions of vacuum drying chamber, get the silver-graphitic composite.The composite productive rate be about add 5% of graphite quality.Fig. 3 is illustrated in ball milling under the condition that does not add organic solvent, and graphite can not effectively be peeled off, and silver has lower content in the composite.
Comparative Examples 2:
Accurately take by weighing graphite 0.5g and drop in the 10mL ball grinder, add 2mL deionized water, 2mL chloroform and 0.5g silver nitrate then successively, add the steel abrading-ball at last, ball milling 3h under 30 times/second concussion frequency.Mixed liquor behind the ball milling added pours out the upper strata dispersion liquid after the 20mL chloroform disperses to leave standstill 1h, sand core funnel filter remove respectively wash 3 times with 20mL deionized water, ethanol successively behind the organic solvent after sample behind dry 24h under 60 ℃ of conditions of vacuum drying chamber, get the silver-graphitic composite.The composite productive rate be about add 8% of graphite quality.Adding ball milling under organic non-polar solven-water condition, graphite can not effectively be peeled off, and silver has lower content in the composite.
Comparative Examples 3:
Accurately take by weighing graphite 0.5g and drop in the 10mL ball grinder, add 4mL N then successively, dinethylformamide 0.5g silver nitrate adds the steel abrading-ball at last, ball milling 3h under 30 times/second concussion frequency.Mixed liquor behind the ball milling is added 20mL N; Dinethylformamide is poured out the upper strata dispersion liquid after disperseing to leave standstill 1h, sand core funnel filter remove respectively wash 3 times with 20mL deionized water, ethanol successively behind the organic solvent after sample must the silver-graphitic composite behind dry 24h under 60 ℃ of conditions of vacuum drying chamber.The composite productive rate be about add 0% of graphite quality.Do not adding ball milling under the condition that water only adds organic solvent, silver nitrate can not hydrolysis.
With above-mentioned foundation desirable embodiment of the present invention is enlightenment, and through above-mentioned description, the related work personnel can carry out various change and modification fully in the scope that does not depart from this invention technological thought.The technical scope of this invention is not limited to the content on the specification, must confirm its technical scope according to the claim scope.
Claims (6)
1. silver-graphitic alkene composite is characterized in that: nano silver particles size homogeneous, and particle diameter is scattered in the Graphene surface uniformly less than 50nm, and Graphene thickness is between 1～10 carbon atomic layer.
2. the method for a convenient production silver-graphitic alkene composite is characterized in that: in organic solvent-aqueous systems, graphite and silver nitrate are carried out ball milling; Wherein, the organic solvent of being selected for use is a polar solvent, and dielectric constant is 15～125.
3. according to the method for right 2 described a kind of convenient production silver-graphitic alkene composites, it is characterized in that: specifically realize through following steps:
One, at first graphite is joined in the ball grinder, add dielectric constant then and be 15～125 polar solvent, water and silver nitrate and ball milling.
Two, after ball milling was accomplished, it was that 15～125 polar solvent disperses again and leaves standstill that mixed liquor is used dielectric constant, after the system of treating is stable, the upper strata part that suspends was poured out, and filtered out deposition, and washing, dry back obtain silver-graphitic alkene composite.
4. the method for a kind of convenient production silver-graphitic alkene according to claim 2; It is characterized in that: above-mentioned dielectric constant is that 15～125 polar organic solvent is formic acid, methyl alcohol, ethanol, acetone, cyclohexanone, tetramethylurea, formamide, N-NMF, N-methyl pyrrolidone, N; Dinethylformamide, acetamide, N-methylacetamide, N, one or more mixtures in N-dimethylacetylamide, pyrrolidones, pyrroles, the pyridine etc.
5. the method for a kind of convenient production silver-graphitic alkene according to claim 2 is characterized in that: the volume ratio of employed organic solvent and water is 0.1～50: 1 in the above-mentioned mechanical milling process.
6. the method for a kind of convenient production silver-graphitic alkene according to claim 2 is characterized in that: the mass ratio of above-mentioned employed graphite and silver nitrate is 1: 0.1～10.
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| CN108788133A (en) * | 2018-07-24 | 2018-11-13 | 深圳市中科睿金贵材科技有限公司 | Test silver-graphene synthetic method |
| CN108751175A (en) * | 2018-08-15 | 2018-11-06 | 辽宁科技大学 | A kind of graphene/carbon SiClx composite material and preparation method |
| CN110373056A (en) * | 2019-07-03 | 2019-10-25 | 江苏华夏制漆科技有限公司 | A kind of ocean protective coating Antimicrobial preservative filler and its preparation method and application |
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Address after: 215500 5th floor, building 4, 68 Lianfeng Road, Changfu street, Changshu City, Suzhou City, Jiangsu Province Patentee after: Changshu intellectual property operation center Co.,Ltd. Address before: No.13 caodang Road, Changshu City, Suzhou City, Jiangsu Province Patentee before: Changshu intellectual property operation center Co.,Ltd. |
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