CN103771406B - The preparation method of Graphene/trimanganese tetroxide nano matrix material - Google Patents
The preparation method of Graphene/trimanganese tetroxide nano matrix material Download PDFInfo
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Abstract
The invention discloses a kind of Graphene/trimanganese tetroxide nano matrix material and preparation method thereof, described method comprises the following steps: step one: 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 ice-water bath, and ultrasonic under probe sonication ripple treater, products therefrom is graphene oxide solution; Step 2: add permanganate in graphene oxide solution, is stirred to permanganate and dissolves completely, add reductive agent, stir; Step 3: solution step 2 obtained reacts at 80 ~ 120 DEG C, reaction terminates rear cooling, centrifuge washing, vacuum-drying, can obtain Graphene/trimanganese tetroxide nano matrix material.The present invention's Graphene/trimanganese tetroxide nano matrix material that adopted one step hydro thermal method to prepare, reductive agent serves the effect of reduction to two kinds of starting material simultaneously, and the method is simple, easy to operate.
Description
Technical field
The invention belongs to field of inorganic nano-material preparation, be specifically related to the preparation method of a kind of Graphene/trimanganese tetroxide nano matrix material.
Background technology
Nano material, also known as nano structural material, refers to the material that three-dimensional space has one dimension at least and is in nanoscale scope (1-100nm) or 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 atypical meta system also atypical microsystem both, but a kind of mesoscopic systems, therefore there is the special effectses such as small-size effect, surface effects, quantum size effect, macro quanta tunnel effect, also give the specific physical chemical property that it had not only been different from individual molecule but also had been different from body phase material simultaneously.Because different nano materials has different physicochemical property, in actual applications, sometimes need two kinds or more of nano material to combine, be prepared into matrix material, differing materials is learnt from other's strong points to offset one's weaknesses, plays 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, large specific surface area and the quantum hall effect etc. of uniqueness, be therefore widely used in multiple fields such as field-effect transistor, liquid crystal apparatus and stored energy.But interact owing to there is Van der Waals force between graphene sheet layer, reuniting very easily appears in graphene sheet layer, and this not only substantially reduces the specific surface area of Graphene, and directly has influence on the physical and chemical performance of its excellence.So far, solving the most effective means of Graphene agglomeration traits is inorganic nano-particle is distributed to graphene nano lamella surface to 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 nanometer of several nanometer, thus 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.Current Graphene/inorganic nano composite material based on the various inorganic nanometer oxide of Graphene compound, as Graphene/zinc oxide, Graphene/Mn oxide, Graphene/bismuth oxide compound, Graphene/titanium oxide etc.Wherein, because of multiple advantages such as manganese element rich reserves, 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 stable charge/discharge that effectively can improve battery in electrode materials, extend the work-ing life of battery, be therefore used as the electrode materials of lithium ion battery and ultracapacitor in recent years gradually.
Graphene and manganic manganous oxide nano-material are carried out compound, not only combines carbon material good stability, quality is light and Mn oxide specific energy is high advantage, and the reunion of Graphene can be prevented, increase the specific surface area of matrix material.Meanwhile, Graphene, as the propping material of trimanganese tetroxide nano particle, can play the effect of electron transmission passage, thus effectively improves the conductivity of manganic manganous oxide nano-material.In addition, because the ground load of trimanganese tetroxide nano uniform particles is on graphene sheet layer, make this matrix material have open cavernous structure, be conducive to the migration of electrolyte ion, this is also very helpful to the performance improving device.But the report about the preparation of Graphene/trimanganese tetroxide nano matrix material is less, and the general more complicated of synthesis technique.Therefore, the preparation method developing a kind of easy Graphene/trimanganese tetroxide nano matrix material to seem outbalance for the exploitation of new energy materials.
Summary of the invention
The object of this invention is to provide a kind of technique simple, with low cost, product property is stablized and the preparation method of the Graphene/trimanganese tetroxide nano matrix material of energy suitability for industrialized production.
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 one: 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 ice-water bath, and ultrasonic under probe sonication ripple treater, and products therefrom is graphene oxide solution;
Step 2: add permanganate in graphene oxide solution, is stirred to permanganate and dissolves completely, add reductive agent, stir;
Step 3: solution step 2 obtained reacts at 80 ~ 120 DEG C, reaction terminates rear cooling, centrifuge washing, vacuum-drying, can obtain Graphene/trimanganese tetroxide nano matrix material.
Further technical scheme is: the time of water bath sonicator is 10 ~ 50min; Time ultrasonic under probe sonication ripple treater 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, preferred 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, preferred hydrazine hydrate.
Further technical scheme is: the ultrasonic power of described probe sonication ripple treater is 50 ~ 500W.
Further technical scheme is: the volume of described 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 DEG C, and the time is 12 ~ 24h.
Further technical scheme is: described graphite oxide concentrated solution adopts the Hummers method liquid-phase oxidation synthesis improved to obtain, Hummers method liquid-phase oxidation synthetic method is specifically shown in J.Am.Chem.Soc.1958,80,1339, the Hummers method of described improvement is the improvement carried out on the basis of Hummers method, the Hummers method improved specifically is 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 load is 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's Graphene/trimanganese tetroxide nano matrix material that adopted one step hydro thermal method to prepare, reductive agent serves the effect of reduction to two kinds of starting material simultaneously, and the method is simple, easy to operate.
(2) particle diameter of the trimanganese tetroxide in Graphene/trimanganese tetroxide nano matrix material of obtaining of the present invention can controlled adjustment between several nanometer to hundreds of nanometer, and is evenly distributed.
(3) the effective ground resistance of existence of trimanganese tetroxide nano particle in Graphene/trimanganese tetroxide nano matrix material of obtaining of the present invention has stopped the reunion of Graphene, makes the performance of matrix material more stable.
(4) large, the good conductivity of the specific surface area of Graphene/trimanganese tetroxide nano matrix material that obtains of the present invention.
(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 that the XRD spectra of Graphene/trimanganese tetroxide nano matrix material and pure trimanganese tetroxide material contrasts;
The SEM figure of Fig. 2 is Graphene concentration when being 0.5mg/mL product;
Fig. 3 be embodiment 3 at 80 DEG C after hydro-thermal reaction 8h Graphene/trimanganese tetroxide nano matrix material SEM figure;
Fig. 4 is the SEM figure of Graphene/trimanganese tetroxide nano matrix material prepared by embodiment 4, and wherein (a) is the SEM figure under 50 times; B () is 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 getting 1mL10mg/mL is placed in beaker, add 39mL deionized water, obtain the graphene oxide solution that concentration is 0.25mg/mL, stir, the ultrasonic 10min of room-temperature water bath, then beaker is placed in ice-water bath, and under probe sonication ripple treater 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 to add 1000 μ L massfractions be wherein the hydrazine hydrate of 35%, stir 20min and make it Homogeneous phase mixing; Above-mentioned mixing solutions is poured in 50mL reactor, 8h is reacted at 100 DEG C, react and taken out after cooling, reaction product is brown color, indicate the generation of Mn oxide, product through centrifuge washing repeatedly, at 80 DEG C vacuum-drying 12h, obtain chocolate brown powder, determine that product is Graphene/trimanganese tetroxide nano matrix material (Fig. 1) through X-ray powder diffraction (XRD) analysis.
Embodiment 2:
The graphite oxide concentrated solution 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 ice-water bath, and under probe sonication ripple treater 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, adding 1000 μ L massfractions is the hydrazine hydrate of 35%, stirs 20min and makes it Homogeneous phase mixing; Above-mentioned mixing solutions is poured in 50mL reactor, 8h is reacted at 100 DEG C, reaction product through centrifuge washing repeatedly, at 80 DEG C vacuum-drying 12h, obtain Graphene/trimanganese tetroxide nano matrix material, and trimanganese tetroxide particle is evenly attached to graphenic surface, and trimanganese tetroxide is spherical in shape or square, as shown in Figure 2.
Embodiment 3:
The graphite oxide concentrated solution 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 ice-water bath, and under probe sonication ripple treater 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, adding 1000 μ L massfractions is the hydrazine hydrate of 35%, stirs 20min and makes it Homogeneous phase mixing; Above-mentioned mixing solutions is poured in 50mL reactor, at 80 DEG C, reacts 8h, reaction product through centrifuge washing repeatedly, at 80 DEG C vacuum-drying 12h, obtain Graphene/trimanganese tetroxide nano matrix material, and trimanganese tetroxide is spherical in shape, diameter is about 20nm, as shown in Figure 3.
Embodiment 4:
The graphite oxide concentrated solution 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 ice-water bath, and under probe sonication ripple treater 240W power ultrasonic 60min; In above-mentioned 1mg/mL graphene oxide solution, add 1mmol potassium permanganate, be stirred to potassium permanganate and dissolve completely, adding 1000 μ L massfractions is the hydrazine hydrate of 35%, stirs 20min and makes it Homogeneous phase mixing; Above-mentioned mixing solutions is poured in 50mL reactor, at 100 DEG C, react 8h, reaction product through centrifuge washing repeatedly, at 80 DEG C vacuum-drying 12h, obtain Graphene/trimanganese tetroxide nano matrix material, trimanganese tetroxide nano is of a size of about 80nm, as shown in Figure 4.
Embodiment 5:
Preparation 40mL concentration is the graphene oxide solution of 0.25mg/mL, and stir, 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 to add 800 μ L massfractions be wherein the hydrazine hydrate of 35%, stir 20min; Then above-mentioned mixing solutions is poured in 50mL reactor, at 100 DEG C, react 8h, reacted rear cooling and taken out and centrifuge washing, at 80 DEG C, Graphene/trimanganese tetroxide nano matrix material can have been obtained after vacuum-drying 12h.
Embodiment 6:
Preparation 40mL concentration is the graphene oxide solution of 0.25mg/mL, and stir, 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 to add 1000 μ L massfractions be wherein the hydrazine hydrate of 35%, vigorous stirring 10min; Then above-mentioned mixing solutions is poured in 50mL reactor, at 110 DEG C, react 8h, reacted rear cooling and taken out and centrifuge washing, at 80 DEG C, Graphene/trimanganese tetroxide nano matrix material can have been obtained after vacuum-drying 12h.
Embodiment 7:
Preparation 40mL concentration is the graphene oxide solution of 0.25mg/mL, and stir, 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 to add 1000 μ L massfractions be wherein the sodium citrate solution of 35%, stir 20min; Then above-mentioned mixing solutions is poured in 50mL reactor, at 100 DEG C, react 8h, reacted rear cooling and taken out and centrifuge washing, at 80 DEG C, Graphene/trimanganese tetroxide nano matrix material can have been obtained after vacuum-drying 12h.
Although only give the specific embodiment that reductive agent is hydrazine hydrate and Trisodium Citrate in embodiments of the invention, but the present invention is not limited only to adopt above-mentioned two kinds of reductive agents, and 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 the present invention's preferably embodiment, 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 amendment and embodiment, these amendments and embodiment will drop within spirit disclosed in the present application and spirit.
Claims (7)
1. a preparation method for Graphene/trimanganese tetroxide nano matrix material, is characterized in that comprising the following steps:
Step one: 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 ice-water bath, and ultrasonic under probe sonication ripple treater, and products therefrom is graphene oxide solution;
Step 2: add permanganate in graphene oxide solution, is stirred to permanganate and dissolves completely, add reductive agent, stir;
Step 3: solution step 2 obtained reacts at 80 ~ 120 DEG C, reaction terminates rear cooling, centrifuge washing, vacuum-drying, can obtain Graphene/trimanganese tetroxide nano matrix material;
Described Graphene/trimanganese tetroxide nano matrix material is made up of Graphene and trimanganese tetroxide, trimanganese tetroxide load is 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 described water bath sonicator time is 10 ~ 50min; Time ultrasonic under probe sonication ripple treater is 30 ~ 120min;
The ultrasonic power of described probe sonication ripple treater is 50 ~ 500W.
2. the preparation method of Graphene according to claim 1/trimanganese tetroxide nano matrix material, 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 according to claim 1/trimanganese tetroxide nano matrix material, 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 according to claim 1/trimanganese tetroxide nano matrix material, is characterized in that the volume of described graphene oxide solution is 40mL:(1 ~ 4mmol with the amount of substance ratio of permanganate).
5. the preparation method of Graphene according to claim 1/trimanganese tetroxide nano matrix material, is characterized in that the volume ratio of described graphene oxide solution and reductive agent is 40:(0.1 ~ 1).
6. the preparation method of Graphene according to claim 1/trimanganese tetroxide nano matrix material, it is characterized in that described vacuum drying temperature is 80 ~ 120 DEG C, the time is 12 ~ 24h.
7. the preparation method of Graphene according to claim 1/trimanganese tetroxide nano matrix material, is characterized in that described graphite oxide concentrated solution adopts the Hummers method liquid-phase oxidation synthesis improved to obtain.
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