CN102581297A - Method for preparing controllable green synthetic metallic nano-materials based on graphene oxide - Google Patents
Method for preparing controllable green synthetic metallic nano-materials based on graphene oxide Download PDFInfo
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Abstract
A method for preparing controllable green synthetic metallic nano-materials based on graphene oxide includes the steps: firstly, preparing the graphene oxide by using crystalline graphite powder as raw materials, using concentrated sulfuric acid, sodium nitrate and potassium permanganate as oxidizing agents, and using hydrogen peroxide, diluted hydrochloric acid, absolute ethyl alcohol and distilled water for washing to obtain purified graphene oxide; and secondly, dropwise adding silver nitrate solution into graphene oxide solution, sufficiently and uniformly mixing the solution, and standing the solution for a few hours at room temperature to obtain graphene/silver nanoparticle composite materials of various dimensions. The metallic nano-materials prepared by the method are large in specific surface area and adjustable in appearance and size, have a Raman enhancement effect, and have important application value in terms of catalysis, energy storage, friction, medicine carrying, bioassay and the like. Moreover, the method has the advantages of simple process, zero pollution, fewer equipment, low energy consumption, convenience in popularization and the like.
Description
Technical field
The present invention relates to a kind of preparation method of multidimensional micro Nano material, for the raw material one-step method prepares multiple nano material, belong to nano material, functional material technical field of chemistry with the graphene oxide.
Background technology
Nano material is meant the material that in three dimensions, has at least one dimension to be in the nanoscale scope or to be made up of as elementary cell them in broad terms.Mainly comprise zero dimension (0D), refer to its three dimension scale all at nano-scale, like nano particle, elementide, nano aperture etc.; One dimension (1D) refers to that it has one dimension to be in nano-scale, like nanometer rods, nano wire, nanotube etc.; Two dimension (2D) refers to that it has two-dimentional yardstick at nano-scale, like ultrathin membrane, multilayer film, ultra character etc.Because at nano-scale, material has quantum nature, therefore, zero dimension, one dimension, two-dimensional material have the title of quantum dot, quantum wire and SQW again.When the size of particle gets into nanoscale; Will demonstrate traditional physicochemical characteristics that solid material did not have; Like quantum size effect, small-size effect, skin effect and macro quanta tunnel effect; Character such as the unique optics of nano material, electricity, magnetics, thermal conductance, catalysis have been given in the existence of these special effectses, it is had in every field use widely, and bring the influence that can't estimate to the world.
The progress that nano material obtained has proved that it has huge development prospect in synthetic chemistry and material science, and specific physical that especially metal nano material had and chemical property make it all be with a wide range of applications at numerous areas such as optics, electricity, sensing technology and bioassays.The size and the pattern of these performances and nano particle are closely related, therefore, can realize the control to material property through size, dimension, composition and the pattern of regulating nano particle, and the design that finally realizes the functional nano device is with synthetic.Though preparation of nanomaterials is variation day by day, still very limited in the achievement that is obtained aspect the green preparation of the controllability of nano material, thereby obtain the increasing concern of researcher.
Literature search through to prior art is found; One Chinese patent application number: 200980135205.8; Name is called mesopore metal oxide graphene nano composite; This patent provides the method for making these nano composite materials: " at first form the mixture of Graphene, surfactant and metal oxide precursor, said metal oxide precursor of deposition and said surfactant from said mixture and form the mesopore metal oxide.This mesopore metal oxide is deposited on the surface of said Graphene then." the present invention is in order to provide a kind of technology simple, and is pollution-free, the method for the synthetic metal nano material of the green of pattern and controllable size further in the retrieval, is found the technical literature identical or approximate with the present invention as yet.
Summary of the invention
It is simple that the technical problem that the present invention will solve provides a kind of technology, pollution-free, the green method of synthesizing metal nano material of the controllability based on graphene oxide of pattern and controllable size.
The green method of synthesizing metal nano material of a kind of controllability based on graphene oxide provided by the invention is specially:
At first prepare graphene oxide: with the crystalline graphite powder is raw material, uses the concentrated sulfuric acid, sodium nitrate, potassium permanganate to be oxidant, with hydrogen peroxide solution, watery hydrochloric acid, absolute ethyl alcohol and distilled water washing, obtains the graphene oxide that purifying is crossed again;
Get the liquor argenti nitratis ophthalmicus of 0.01-0.1M again, according to 1: 1-1: 10 volume ratios dropwise are added in the graphene oxide solution, fully mixing.Room temperature leaves standstill the Graphene/Nano silver grain composite that promptly obtained various dimensions in several hours.
Said graphene oxide is used for the reducing agent and the template of synthesizing nano-particle.
The reaction time of said silver nitrate and graphene oxide obtained sphere and square Nano silver grain from 1 hour to 48 hours.
The volume ratio of said silver nitrate and graphene oxide obtained silver-colored nanometer rods, nanometer plate and silver-colored nanotrees from 1: 1 to 1: 10.
The concentration of described graphene oxide solution is greater than or equal to 0.5mg/mL.
Said graphene oxide solution pH value is neutrality and purity when high more, the solution good dispersion.
The silver nitrate of the preferred 0.1M of concentration of said liquor argenti nitratis ophthalmicus.
Above-mentioned all synthesis steps of the present invention all carry out at room temperature.
Do not add any reducing agent and surfactant in above-mentioned all building-up processes of the present invention.
The present invention uses the spontaneous reduction silver ion of the groups such as hydroxyl, carbonyl, carboxyl or epoxy radicals on the graphene oxide to obtain the metal nano material of different dimensions, comprising: the nanometer plate of the silver-colored nanometer rods of the silver nano-grain of zero dimension (sphere and square), one dimension, two dimension and three-dimensional nanometer piece and tree-shaped material.
Compared with prior art; Beneficial effect of the present invention: nano material specific area that the inventive method makes is high, nanotopography and size adjustable and have the Raman enhancement effect; There is important use to be worth at aspects such as catalysis, energy storage, friction, medicine carrying and biological detection; And it is simple to have technology, and number of devices is few, and energy consumption is low and be convenient to characteristics such as large-scale production.
Description of drawings
Fig. 1 is the transmission electron microscope picture of the silver nano material of embodiment of the invention preparation;
Fig. 2 is the transmission electron microscope picture of the silver-colored nanotrees of embodiment of the invention preparation;
Fig. 3 is the Raman enhanced spectrum figure of the Nano silver grain of embodiment of the invention preparation.
The specific embodiment
Elaborate in the face of embodiments of the invention down, present embodiment is a prerequisite with technical scheme of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
1) preparation of graphene oxide:
In the beaker of drying, add 230mL, the concentrated sulfuric acid of mass fraction 98% is cooled to 0 ℃ with ice-water bath, adds natural flake graphite (10g), NaNO while stirring
3(5g) and KMnO
4(30g).Control reacting liquid temperature at 10-15 ℃, the stirring reaction certain hour; Then beaker is placed the water bath with thermostatic control about 35 ℃, continue to stir 30min when the question response temperature rises to 35 ℃ of left and right sides; In stirring, add deionized water at last, the control reacting liquid temperature continues to stir 30min in 100 ℃.Add an amount of mass fraction 5%H again after with deionized water reactant liquor being diluted to 1000mL
2O
2, filter while hot, fully washing in filtrating with mass fraction 5%HCl and absolute ethyl alcohol and distilled water does not have SO
4 2-(use BaCl
2Solution detects), promptly obtain the graphene oxide that purifying is crossed.
2) silver nano material is synthetic: the existence of functional groups such as graphene oxide surface carboxyl, hydroxyl more helps silver ion and combines with it, and becomes nuclear reaction.
Concrete steps are following:
(a) get 20mL graphene oxide solution liquid (0.5mg/mL) in clean vial;
(b) liquor argenti nitratis ophthalmicus of absorption 0.01M, each 1mL adds above-mentioned graphene oxide solution, and mixing continues 20 times; Placed room temperature 48 hours;
(c) carry out TEM, performance characterizations such as Raman.
Embodiment 2
1) preparation of graphene oxide:
In the beaker of drying, add 230mL, 98% the concentrated sulfuric acid is cooled to 0 ℃ with ice-water bath, adds natural flake graphite (10g), NaNO while stirring
3(5g) and KMnO
4(30g).Control reacting liquid temperature at 10-15 ℃, the stirring reaction certain hour; Then beaker is placed the water bath with thermostatic control about 35 ℃, continue to stir 30min when the question response temperature rises to 35 ℃ of left and right sides; In stirring, add deionized water at last, the control reacting liquid temperature continues to stir 30min in 100 ℃.Add an amount of 5%H again after with deionized water reactant liquor being diluted to 1000ml
2O
2, filter while hot, fully washing in filtrating with 5%HCl and absolute ethyl alcohol and distilled water does not have SO
4 2-(use BaCl
2Solution detects), promptly obtain the graphene oxide that purifying is crossed.The concentration of graphene oxide solution equals 0.5mg/mL.
2) silver nano material is synthetic: the existence of functional groups such as graphene oxide surface carboxyl, hydroxyl more helps silver ion and combines with it, and becomes nuclear reaction.
Concrete steps are following:
(a) get 100mL graphene oxide solution (0.5mg/mL) in clean vial;
(b) get the liquor argenti nitratis ophthalmicus of 20mL 0.1M, add above-mentioned graphene oxide solution, magnetic stirrer is spent the night;
(c) carry out TEM, performance characterizations such as Raman.
Embodiment 3
1) preparation of graphene oxide:
In the beaker of drying, add 230mL, 98% the concentrated sulfuric acid is cooled to 0 ℃ with ice-water bath, adds natural flake graphite (10g), NaNO while stirring
3(5g) and KMnO
4(30g).Control reacting liquid temperature at 10-15 ℃, the stirring reaction certain hour; Then beaker is placed the water bath with thermostatic control about 35 ℃, continue to stir 30min when the question response temperature rises to 35 ℃ of left and right sides; In stirring, add deionized water at last, the control reacting liquid temperature continues to stir 30min in 100 ℃.Add an amount of 5%H again after with deionized water reactant liquor being diluted to 1000ml
2O
2, filter while hot, fully washing in filtrating with 5%HCl and absolute ethyl alcohol and distilled water does not have SO
4 2-(use BaCl
2Solution detects), promptly obtain the graphene oxide that purifying is crossed.The concentration of graphene oxide solution is greater than 0.5mg/mL.
2) silver nano material is synthetic: the existence of functional groups such as graphene oxide surface carboxyl, hydroxyl more helps silver ion and combines with it, and becomes nuclear reaction.
Concrete steps are following:
(a) get 200mL graphene oxide solution (0.6mg/mL) in clean vial;
(b) get the liquor argenti nitratis ophthalmicus of 20mL 0.06M, add above-mentioned graphene oxide solution, magnetic stirrer placed room temperature 30 hours;
(c) carry out TEM, performance characterizations such as Raman.
As shown in Figure 1, be the transmission electron microscope picture of the silver nano material of embodiment of the invention preparation; Fig. 2 is the transmission electron microscope picture of the silver-colored nanotrees of embodiment of the invention preparation; Fig. 3 is the Raman enhanced spectrum figure of the Nano silver grain of embodiment of the invention preparation, and showing has tangible Raman enhancement effect.
The present invention provides a kind of technology simple; Pollution-free, the method for green synthetic metal nano material, the nano material specific area that makes is high, nanotopography and size adjustable and have the Raman enhancement effect; There is important use to be worth at aspects such as catalysis, energy storage, friction, medicine carrying and biological detection; And it is simple to have technology, and number of devices is few, and energy consumption is low and be convenient to characteristics such as large-scale production.
Should be understood that, more than be the preferred embodiments of the present invention, and the present invention can also have other embodiment, such as the parameter in replacement the foregoing description, perhaps does simple variation etc., and these all are easy to realize for a person skilled in the art.
Although content of the present invention has been done detailed introduction through above-mentioned preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple modification of the present invention with to substitute all will be conspicuous.Therefore, protection scope of the present invention should be limited appended claim.
Claims (6)
1. method based on the green synthetic metal nano material of the controllability of graphene oxide is characterized in that:
At first prepare graphene oxide: with the crystalline graphite powder is raw material, uses the concentrated sulfuric acid, sodium nitrate, potassium permanganate to be oxidant, with hydrogen peroxide solution, watery hydrochloric acid, absolute ethyl alcohol and distilled water washing, obtains the graphene oxide that purifying is crossed again;
Get the 0.01-0.1M liquor argenti nitratis ophthalmicus again; According to 1: 1-1: 10 volume ratios dropwise are added in the graphene oxide solution; The concentration of graphene oxide solution is greater than or equal to 0.5mg/mL, abundant mixing, and room temperature leaves standstill the Graphene/Nano silver grain composite that promptly obtained various dimensions in several hours.
2. the green method of synthesizing metal nano material of the controllability based on graphene oxide according to claim 1, the reaction time that it is characterized in that said silver nitrate and graphene oxide obtained sphere and square Nano silver grain from 1 hour to 48 hours.
3. the green method of synthesizing metal nano material of the controllability based on graphene oxide according to claim 1 and 2 is characterized in that said graphene oxide pH value is neutrality and purity is high more, the solution good dispersion.
4. according to claim 1 or the green method of synthesizing metal nano material of 2 or 3 described controllabilitys based on graphene oxide, the concentration that it is characterized in that said liquor argenti nitratis ophthalmicus is 0.1M.
5. according to the green method of synthesizing metal nano material of each described controllability of claim 1-4, it is characterized in that all synthesis steps all carry out at room temperature based on graphene oxide.
6. according to the green method of synthesizing metal nano material of each described controllability of claim 1-4, it is characterized in that not adding any reducing agent and surfactant in above-mentioned all building-up processes based on graphene oxide.
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| CN103081946A (en) * | 2013-01-18 | 2013-05-08 | 湖南元素密码石墨烯研究院（有限合伙） | Porous graphene loaded cerium nano composite antibacterial agent and preparation method thereof |
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| CN103521780A (en) * | 2013-11-04 | 2014-01-22 | 中国农业科学院农业质量标准与检测技术研究所 | Preparation method and application of oxidized graphene load gold nanoparticle sol with surface-enhanced Raman spectrum activity |
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| CN105529473A (en) * | 2015-12-15 | 2016-04-27 | 中国科学院化学研究所 | Graphene oxide-modified electrode material for energy storage flow battery |
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Application publication date: 20120718 |