CN103771406A - Graphene/manganese tetraoxide nanocomposite and preparation method thereof - Google Patents
Graphene/manganese tetraoxide nanocomposite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a graphene/manganese tetraoxide nanocomposite and a preparation method thereof. The method comprises the following steps of firstly, diluting graphite oxide concentrated solution to be 0.1-5mg/mL with deionized water, stirring uniformly, after water bath ultrasonic at room temperature, putting a beaker into ice-water bath, and carrying out ultrasonic treatment by a probe ultrasonic processor to obtain graphene oxide solution; secondly, adding permanganate into the graphene oxide solution, stirring till the permanganate is dissolved completely, adding a reducing agent, and stirring uniformly; thirdly, reacting the solution obtained in step two at 80-120 DEG C, after reacting, cooling, centrifuging and washing, and vacuum-drying, so as to obtain the graphene/manganese tetraoxide nanocomposite. The graphene/manganese tetraoxide nanocomposite is prepared by one-step hydrothermal method, the reducing agent simultaneously reduces the two raw materials, and the method is simple and easy to operate.
Description
Technical field
The invention belongs to field of inorganic nano-material preparation, be specifically related to a kind of preparation method of Graphene/trimanganese tetroxide nano matrix material.
Background technology
Nano material claims again nano structural material, refers to that three-dimensional space has one dimension at least in nanoscale scope (1-100nm) or the material that is made up of as elementary cell them.The size of nano material is in the transitional region of atom and macroscopic material, such system is also atypical microsystem of atypical meta system both, but a kind of Jie's sight system, therefore there is the special effectses such as small-size effect, surface effects, quantum size effect, macro quanta tunnel effect, simultaneously also given the specific physical chemical property that it had not only been different from individual molecule but also had been different from body phase material.Because different nano materials has different physicochemical property, in actual applications, sometimes need two kinds or more of nano materials to combine, be prepared into matrix material, differing materials can be learnt from other's strong points to offset one's weaknesses, performance synergistic effect, thus make nano material produce better properties.
Graphene is the monolayer carbon atomic structure material of a kind of two dimension of discovered in recent years, the monoatomic layer structure of its uniqueness makes it have the physicochemical property of many excellences, as high mechanical property, thermal conductivity, charge mobility, the quantum hall effects of large specific surface area and uniqueness etc., are therefore widely used in multiple fields such as field-effect transistor, liquid crystal apparatus and stored energy.But owing to existing Van der Waals force to interact between graphene sheet layer, reuniting very easily appears in graphene sheet layer, this has not only reduced the specific surface area of Graphene greatly, and directly has influence on its excellent physical and chemical performance.So far, solving the most effective means of Graphene agglomeration traits is inorganic nano-particle to be distributed to graphene nano lamella surface make Graphene/inorganic nano composite material.The existence of inorganic nano-particle can make graphene film interlamellar spacing be increased to the even hundreds of nanometers of several nanometers, thereby greatly reduces the interaction between graphene sheet layer, and the peculiar property of single-layer graphene is retained.In addition, prepared Graphene/inorganic nano composite material not only can keep the natural characteristics of Graphene and inorganic nano-particle simultaneously, and can produce novel synergistic effect, is with a wide range of applications.Graphene/inorganic nano composite material is take the compound various inorganic nanometer oxides of Graphene as main, as Graphene/zinc oxide, Graphene/Mn oxide, Graphene/bismuth oxide compound, Graphene/titanium oxide etc. at present.Wherein, because of multiple advantages such as manganese element reserves are abundant, cheap, clean nontoxicitys, the research of Graphene/Mn oxide nano composite material receives much concern in new energy materials field.Trimanganese tetroxide is the Mn oxide that chemical property is the most stable, be added on the stability that discharges and recharges that can effectively improve battery in electrode materials, extend the work-ing life of battery, be therefore used as gradually in recent years the electrode materials of lithium ion battery and ultracapacitor.
Graphene and manganic manganous oxide nano-material are carried out compound, not only combine the light and high advantage of Mn oxide specific energy of carbon material good stability, quality, and can prevent the reunion of Graphene, increase the specific surface area of matrix material.Meanwhile, Graphene, as the propping material of trimanganese tetroxide nano particle, can play the effect of electronics transmission channels, thereby has effectively improved the conductivity of manganic manganous oxide nano-material.In addition, due to trimanganese tetroxide nano uniform particles load on graphene sheet layer, make this matrix material there is open cavernous structure, be conducive to the migration of electrolyte ion, this is also very helpful to improving performance of device.But, less about the report of the preparation of Graphene/trimanganese tetroxide nano matrix material, and the general more complicated of synthesis technique.Therefore the preparation method who, develops a kind of easy Graphene/trimanganese tetroxide nano matrix material is for the exploitation of the new energy materials outbalance that seems.
Summary of the invention
The object of this invention is to provide a kind of technique simple, the preparation method of stable and the Graphene/trimanganese tetroxide nano matrix material that can suitability for industrialized production of with low cost, product property.
In order to reach above-mentioned technique effect, the present invention takes following technical scheme:
A preparation method for Graphene/trimanganese tetroxide nano matrix material, comprises the following steps:
Step 1: with deionized water dilution graphite oxide concentrated solution to 0.1～5mg/mL, stir, after room-temperature water bath is ultrasonic, beaker is placed in to ice-water bath, and ultrasonic under probe processor for ultrasonic wave, products therefrom is graphene oxide solution;
Step 2: add permanganate in graphene oxide solution, be stirred to permanganate and dissolve completely, add reductive agent, stir;
Step 3: the solution that step 2 is obtained reacts at 80～120 ℃, reaction finishes rear cooling, and centrifuge washing, vacuum-drying, can obtain Graphene/trimanganese tetroxide nano matrix material.
Further technical scheme is: the ultrasonic time of water-bath is 10～50min; Under probe processor for ultrasonic wave, the ultrasonic time is 30～120min.
Further technical scheme is: described permanganate is one or more in high manganese lithium, sodium permanganate, potassium permanganate, ammonium permanganate, calcium permanganate, barium permanganate, magnesium permanganate, permanganic acid mercury, cadmium permanganate, permanganic acid rubidium, preferably potassium permanganate.
Further technical scheme is: described reductive agent is one or more in hydrazine hydrate, quadrol, xitix, Trisodium Citrate, Cys, ammoniacal liquor, hydroiodic acid HI, sodium borohydride, preferably hydrazine hydrate.
Further technical scheme is: the ultrasonic power of described probe processor for ultrasonic wave is 50～500W.
Further technical scheme is: the described volume of graphene oxide solution and the amount of substance of permanganate are than being 40mL:(1～4mmol).
Further technical scheme is: described graphene oxide solution and the volume ratio of reductive agent are 40:(0.1～1).
Further technical scheme is: described vacuum drying temperature is 80～120 ℃, and the time is 12～24h.
Further technical scheme is: described graphite oxide concentrated solution adopts the liquid-phase oxidation of improved Hummers method to synthesize and obtains, Hummers method liquid-phase oxidation synthetic method is specifically shown in J.Am.Chem.Soc.1958,80,1339, described improved Hummers method is the improvement of carrying out on the basis of Hummers method, improved Hummers method is specifically shown in DAN LI, MARCB.MU ¨ LLER, SCOTT GILJE, et al.Nature nanotechnology, 2008,3,101～105.
A kind of Graphene/trimanganese tetroxide nano matrix material, it is characterized in that Graphene/trimanganese tetroxide nano matrix material is made up of Graphene and trimanganese tetroxide, trimanganese tetroxide loads on graphene film, trimanganese tetroxide is spherical or cubic, the particle diameter of trimanganese tetroxide is 5～100nm, the thickness of graphene film is 0.8～1.6nm, and wherein the massfraction of graphene film is 1～85wt%.
The present invention compared with prior art, has following beneficial effect:
(1) the present invention adopts one step hydro thermal method to prepare Graphene/trimanganese tetroxide nano matrix material, and reductive agent has played the effect of reduction simultaneously to two kinds of starting material, and the method is simple, easy to operate.
(2) particle diameter of the trimanganese tetroxide in Graphene/trimanganese tetroxide nano matrix material that the present invention obtains can arrive controlled adjustment between hundreds of nanometers in several nanometers, and is evenly distributed.
(3) the effective ground resistance of existence of the trimanganese tetroxide nano particle in Graphene/trimanganese tetroxide nano matrix material that the present invention obtains has been stopped the reunion of Graphene, makes the performance of matrix material more stable.
(4) specific surface area of Graphene/trimanganese tetroxide nano matrix material that the present invention obtains is large, good conductivity.
(5) gained nano composite material of the present invention can be widely used in the fields such as lithium cell, ultracapacitor, eelctro-catalyst and dye cell.
Accompanying drawing explanation
Fig. 1 is the XRD spectra contrast of Graphene/trimanganese tetroxide nano matrix material and pure trimanganese tetroxide material;
Fig. 2 is the SEM figure of Graphene concentration product while being 0.5mg/mL;
Fig. 3 is embodiment 3 SEM of Graphene/trimanganese tetroxide nano matrix material figure after hydro-thermal reaction 8h at 80 ℃;
Fig. 4 is the SEM figure of Graphene/trimanganese tetroxide nano matrix material of preparing of embodiment 4, and wherein (a) is the SEM figure under 50 times; (b) be the SEM figure under 100 times.
Embodiment
Below in conjunction with embodiments of the invention, the invention will be further elaborated.
Embodiment 1:
The graphite oxide concentrated solution of getting 1mL10mg/mL is placed in beaker, add 39mL deionized water, obtaining concentration is the graphene oxide solution of 0.25mg/mL, stir, the ultrasonic 10min of room-temperature water bath, then beaker is placed in to ice-water bath, and under probe processor for ultrasonic wave 240W power further ultrasonic 60min; In above-mentioned 0.25mg/mL graphene oxide solution, add 1mmol potassium permanganate, be stirred to potassium permanganate and dissolve completely, then add wherein the hydrazine hydrate that 1000 μ L massfractions are 35%, stir 20min and make it even mixing; Above-mentioned mixing solutions is poured in 50mL reactor, at 100 ℃, react 8h, react after cooling and taken out, reaction product is brown color, show the generation of Mn oxide, product through centrifuge washing repeatedly, at 80 ℃ vacuum-drying 12h, obtain chocolate brown powder, be Graphene/trimanganese tetroxide nano matrix material (Fig. 1) through X-ray powder diffraction (XRD) Analysis deterrmination product.
Embodiment 2:
The graphite oxide concentrated solution of getting 2mL10mg/mL is placed in beaker, adds 38mL deionized water, makes graphite oxide solution concentration dilution to 0.5mg/mL, stir, after the ultrasonic 10min of room-temperature water bath, beaker is placed in to ice-water bath, and under probe processor for ultrasonic wave 240W power ultrasonic 60min; In above-mentioned 0.5mg/mL graphene oxide solution, add 1mmol potassium permanganate, be stirred to potassium permanganate and dissolve completely, add the hydrazine hydrate that 1000 μ L massfractions are 35%, stir 20min and make it even mixing; Above-mentioned mixing solutions is poured in 50mL reactor, at 100 ℃, react 8h, reaction product through centrifuge washing repeatedly, at 80 ℃ vacuum-drying 12h, obtain Graphene/trimanganese tetroxide nano matrix material, and trimanganese tetroxide particle is evenly attached to Graphene surface, and trimanganese tetroxide is spherical in shape or square, as shown in Figure 2.
Embodiment 3:
The graphite oxide concentrated solution of getting 1mL10mg/mL is placed in beaker, adds 39mL deionized water, makes graphite oxide solution concentration dilution to 0.25mg/mL, stir, after the ultrasonic 10min of room-temperature water bath, beaker is placed in to ice-water bath, and under probe processor for ultrasonic wave 240W power ultrasonic 60min; In above-mentioned 0.25mg/mL graphene oxide solution, add 1mmol potassium permanganate, be stirred to potassium permanganate and dissolve completely, add the hydrazine hydrate that 1000 μ L massfractions are 35%, stir 20min and make it even mixing; Above-mentioned mixing solutions is poured in 50mL reactor, at 80 ℃, is reacted 8h, reaction product through centrifuge washing repeatedly, at 80 ℃ vacuum-drying 12h, obtain Graphene/trimanganese tetroxide nano matrix material, and trimanganese tetroxide is spherical in shape, diameter is 20nm left and right, as shown in Figure 3.
Embodiment 4:
The graphite oxide concentrated solution of getting 4mL10mg/mL is placed in beaker, adds 36mL deionized water, makes graphite oxide solution concentration dilution to 1mg/mL, stir, after the ultrasonic 10min of room-temperature water bath, beaker is placed in to ice-water bath, and under probe processor for ultrasonic wave 240W power ultrasonic 60min; In above-mentioned 1mg/mL graphene oxide solution, add 1mmol potassium permanganate, be stirred to potassium permanganate and dissolve completely, add the hydrazine hydrate that 1000 μ L massfractions are 35%, stir 20min and make it even mixing; Above-mentioned mixing solutions is poured in 50mL reactor, at 100 ℃, react 8h, reaction product through centrifuge washing repeatedly, at 80 ℃ vacuum-drying 12h, obtain Graphene/trimanganese tetroxide nano matrix material, trimanganese tetroxide nano is of a size of 80nm left and right, as shown in Figure 4.
Embodiment 5:
The graphene oxide solution that preparation 40mL concentration is 0.25mg/mL, stirs, and the ultrasonic 10min of room-temperature water bath, is then placed in ice-water bath by beaker, and under 240W power further ultrasonic 60min; In this solution, add 1mmol high manganese lithium, be stirred to high manganese lithium and dissolve completely, then add wherein the hydrazine hydrate that 800 μ L massfractions are 35%, stir 20min; Then above-mentioned mixing solutions is poured in 50mL reactor, at 100 ℃, reacted 8h, reacted rear cooling taking-up centrifuge washing, at 80 ℃, after vacuum-drying 12h, can obtain Graphene/trimanganese tetroxide nano matrix material.
Embodiment 6:
The graphene oxide solution that preparation 40mL concentration is 0.25mg/mL, stirs, and the ultrasonic 10min of room-temperature water bath, is then placed in ice-water bath by beaker, and under 240W power further ultrasonic 60min; In this solution, add 1.2mmol magnesium permanganate, be stirred to magnesium permanganate and dissolve completely, then add wherein the hydrazine hydrate that 1000 μ L massfractions are 35%, vigorous stirring 10min; Then above-mentioned mixing solutions is poured in 50mL reactor, at 110 ℃, reacted 8h, reacted rear cooling taking-up centrifuge washing, at 80 ℃, after vacuum-drying 12h, can obtain Graphene/trimanganese tetroxide nano matrix material.
Embodiment 7:
The graphene oxide solution that preparation 40mL concentration is 0.25mg/mL, stirs, and the ultrasonic 10min of room-temperature water bath, is then placed in ice-water bath by beaker, and under 240W power further ultrasonic 60min; In this solution, add 1mmol potassium permanganate, be stirred to potassium permanganate and dissolve completely, then add wherein the sodium citrate solution that 1000 μ L massfractions are 35%, stir 20min; Then above-mentioned mixing solutions is poured in 50mL reactor, at 100 ℃, reacted 8h, reacted rear cooling taking-up centrifuge washing, at 80 ℃, after vacuum-drying 12h, can obtain Graphene/trimanganese tetroxide nano matrix material.
Be the specific embodiment of hydrazine hydrate and Trisodium Citrate although only provided reductive agent in embodiments of the invention, but the present invention is not limited only to adopt above-mentioned two kinds of reductive agents, reductive agent of the present invention can also be one or more in quadrol, xitix, Cys, ammoniacal liquor, hydroiodic acid HI, sodium borohydride.
Although with reference to explanatory embodiment of the present invention, invention has been described here, above-described embodiment is only preferably embodiment of the present invention, embodiments of the present invention are not restricted to the described embodiments, should be appreciated that, those skilled in the art can design a lot of other modification and embodiments, and these are revised and within embodiment will drop on the disclosed principle scope and spirit of the application.
Claims (9)
1. a preparation method for Graphene/trimanganese tetroxide nano matrix material, is characterized in that comprising the following steps:
Step 1: with deionized water dilution graphite oxide concentrated solution to 0.1～5mg/mL, stir, after room-temperature water bath is ultrasonic, beaker is placed in to ice-water bath, and ultrasonic under probe processor for ultrasonic wave, products therefrom is graphene oxide solution;
Step 2: add permanganate in graphene oxide solution, be stirred to permanganate and dissolve completely, add reductive agent, stir;
Step 3: the solution that step 2 is obtained reacts at 80～120 ℃, reaction finishes rear cooling, and centrifuge washing, vacuum-drying, can obtain Graphene/trimanganese tetroxide nano matrix material.
2. the preparation method of Graphene/trimanganese tetroxide nano matrix material according to claim 1, is characterized in that described permanganate is one or more in high manganese lithium, sodium permanganate, potassium permanganate, ammonium permanganate, calcium permanganate, barium permanganate, magnesium permanganate, permanganic acid mercury, cadmium permanganate, permanganic acid rubidium.
3. the preparation method of Graphene/trimanganese tetroxide nano matrix material according to claim 1, is characterized in that described reductive agent is one or more in hydrazine hydrate, quadrol, xitix, Trisodium Citrate, Cys, ammoniacal liquor, hydroiodic acid HI, sodium borohydride.
4. the preparation method of Graphene/trimanganese tetroxide nano matrix material according to claim 1, is characterized in that the ultrasonic power of described probe processor for ultrasonic wave is 50～500W.
5. the preparation method of Graphene/trimanganese tetroxide nano matrix material according to claim 1, is characterized in that the described volume of graphene oxide solution and the amount of substance of permanganate than being 40mL:(1～4mmol).
6. the preparation method of Graphene/trimanganese tetroxide nano matrix material according to claim 1, is characterized in that described graphene oxide solution and the volume ratio of reductive agent are 40:(0.1～1).
7. the preparation method of Graphene/trimanganese tetroxide nano matrix material according to claim 1, is characterized in that described vacuum drying temperature is 80～120 ℃, and the time is 12～24h.
8. the preparation method of Graphene/trimanganese tetroxide nano matrix material according to claim 1, is characterized in that described graphite oxide concentrated solution adopts the liquid-phase oxidation of improved Hummers method to synthesize and obtains.
9. Graphene/trimanganese tetroxide nano matrix material that prepared by the preparation method described in claim 1～8 any one, it is characterized in that Graphene/trimanganese tetroxide nano matrix material is made up of Graphene and trimanganese tetroxide, trimanganese tetroxide loads on graphene film, trimanganese tetroxide is spherical or cubic, the particle diameter of trimanganese tetroxide is 5～100nm, the thickness of graphene film is 0.8～1.6nm, and wherein the massfraction of graphene film is 1～85wt%.
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