CN102839388B - Graphene/molybdenum disulfide composite electrode material and preparation method thereof - Google Patents
Graphene/molybdenum disulfide composite electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the fields of a novel chemical electric power source and a new energy material, and particularly discloses a graphene/molybdenum disulfide composite electrode material and a preparation method of the composite electrode material. The preparation method comprises the steps of: (1) preparing graphite oxide from graphite as a raw material by an oxidation and intercalation method; (2) dissolving prepared graphite oxide with deionized water, carrying out ultrasonic stripping to obtain a graphene oxide solution, then adding DMF (dimethyl formamide) and molybdate, finally adding a reducing agent, and dispersing uniformly to obtain a mixed solution; and (3) transferring the mixed solution to a reaction kettle, keeping the temperature in the temperature condition of greater than or equal to 180 DEG C for 5-10h, centrifuging and washing the product to remove DMF, and drying to obtain the graphene/molybdenum disulfide composite electrode material product. The preparation method of the graphene/molybdenum disulfide composite electrode material is simple, uniform in reaction system and low in production cost, and is particularly suitable for requirements of industrial large scale production; and the prepared product graphene/molybdenum disulfide composite electrode material has better electrochemical performances.
Description
Technical field
The present invention relates to mechanism of new electrochemical power sources and new energy materials field, specifically disclose combination electrode material of a kind of Graphene/molybdenumdisulphide and preparation method thereof.
Background technology
Fossil oil (oil and the coal) resource of present use, will close to exhausted to fifties 21 century, and this fuel has serious pollution to environment.International Technology circle is finding the new energy, and hydrogen energy source is one of them.The combustion heat of hydrogen is 28900 kcal/kg, is approximately three times of gasoline combustion heat.Reaction product is water, does not pollute environment, and the water that burning generates also can continue hydrogen manufacturing, and iterative cycles uses.Product water non-corrosiveness, can't harm, so people are called clean energy source hydrogen equipment.The International Association for Hydrogen Energy of composition in 1976, the generation of main Study of Hydrogen, storage and utilization.Current liquid hydrogen is used as rocket fuel; The hydrogen of liquid hydrogen, liquefied ammonia or hydrogen storage alloy storage is used as automobile fuel.But because the production cost of hydrogen is higher than fossil oil, promotes the use of and still have any problem.Hydrogen energy source can be a kind of secondary energy, and it utilizes other energy to produce by certain method, and can directly from underground mining, almost rely on fossil oil completely unlike coal, oil and natural gas etc.Industrially usually adopt following several method hydrogen making: one be by water vapour by scorching hot coke (being called carbon reduction method), obtain the hydrogen that purity is about 75%; Two be by water vapour by scorching hot iron, obtain the hydrogen of purity below 97%; Three is extract hydrogen by water-gas, and the hydrogen purity obtained is also lower; 4th kind of method is exactly water electrolysis method, and obtained hydrogen purity can up to more than 99%, and this is the industrial a kind of important method preparing hydrogen.But in order to improve the efficiency of water electrolysis hydrogen production, a kind of effective catalyzer be used.
Transition metal stratiform binary compound, because having the performances such as good optical, electrical, lubrication, catalysis, enjoys the concern of people.Moly-sulfide is one of Typical Representative wherein, MoS
2be a kind of diamagnetism and have the compound of semiconductor property, wherein Mo-S faceted pebble is quite a lot of, and it is large that catalytic performance has specific surface area, and high adsorption capacity, reactive behavior advantages of higher, so receive much concern this year.But, although MoS
2laminate structure is a kind of up-and-coming electrochemical electrode material, but fails to obtain industrial applications, because MoS
2conductivity poor.There is due to Graphene the excellent properties such as very high specific surface area, superpower mechanical property, high conduction and heat conduction, therefore, the present invention uses the composite nanostructure material of Graphene and molybdenumdisulphide as electrode, be conducive to the electron transmission in electrode process, the chemical property of intensifier electrode.
In the combination electrode material preparing Graphene/molybdenumdisulphide, the people such as Kun Chang are with the standby graphene oxide of Hummer legal system, and L-crysteine and Sodium orthomolybdate are raw material, prepare matrix material in aqueous, and explore the application of lithium ion battery aspect.[Kun Chang and Weixiang Chen, L-Crysteine-assisted synthesis of layeredMoS2/Graphene composites with excellent electrochemical performances for lithium ion batteries, ACS Nano 5 (2011) 4720], matrix material is mainly used in Study on Li-ion batteries.The people such as Yangguang Li use pure organic solvent N, N-dimethylformamide (DMF, N, dinethylformamide) synthesize the sandwich that two-dimentional molybdenumdisulphide is evenly attached to two-dimensional graphene surface, and prove electrolytic hydrogen production characteristic [the Yangguang Li et al. of matrix material as electrode excellence, MoS2 nanoparticles grown on graphene:an advanced catalyst for thehydrogen evolution reaction, J.Am.Chem.Soc.133 (2011) 7296].But this method all uses DMF, and the material oxidation Graphene of Hydrothermal Synthesis is hydrophilic not oleophylic, and the dispersion therefore in DMF is very difficult, and product is difficult to evenly, and the price of its outer organic solvent own, aftertreatment is also uneconomical.
In prior art, the people such as Yangguang Li use pure organic solvent DMF to carry out the synthesis of Graphene/molybdenum disulfide composite electrode material [Yangguang Li et al., J.Am.Chem.Soc.133 (2011) 7296], the present invention be then graphene oxide is dissolved in the water again with organic solvent compound, graphene oxide is so not only made to be dispersed in solvent system, significantly enhance the homogeneity of product Graphene/molybdenumdisulphide in hydrothermal reaction process, but also decrease the use of expensive organic solvent DMF.The hydrothermal method composite graphite alkene that the people such as Kun Chang use Crysteine auxiliary and molybdenumdisulphide [ACS Nano 5 (2011) 4720], compared with this technology, the present invention does not need to use any subsidiary material, can directly synthesize final combination electrode material.
Visible Graphene/molybdenum disulfide composite electrode material preparation method of the present invention is simple, reaction system even, and production cost is low, is extremely applicable to the requirement of industrial mass production; Prepare product Graphene/molybdenum disulfide composite electrode material and there is preferably chemical property.
Summary of the invention
The object of the invention is to the defect overcoming prior art, a kind of Graphene/molybdenum disulfide composite electrode material and preparation method thereof is provided, the preparation process of Graphene/molybdenum disulfide composite electrode material of the present invention is carried out in the double solvents of water and organism composition, not only significantly enhance the homogeneity of product Graphene/molybdenumdisulphide in hydrothermal reaction process, but also decrease the use of expensive organic solvent DMF.
First the present invention discloses a kind of preparation method of Graphene/molybdenum disulfide composite electrode material, and concrete steps are as follows:
1) take graphite as raw material, prepare graphite oxide by oxidation graft process;
2) the graphite oxide deionized water dissolving prepared by step 1), ultrasonic stripping obtains graphene oxide solution, then in graphene oxide solution, adds DMF, molybdate, finally adds reductive agent, be uniformly dispersed, and obtains mixing solutions;
3) by step 2) mixing solutions prepared transfers in reactor, be incubated 5 ~ 10h being more than or equal under the temperature condition of 180 DEG C, after the product that obtains is centrifugal, repeatedly wash removing DMF with deionized water, drying, obtains Graphene/molybdenum disulfide composite electrode material product.
Preferably, be oxidized graft process described in step 1) and be selected from Hummer method or Staudenmair method.
Hummer method and Staudenmair method are prior art, Staudenmair legal system is adopted to comprise for the reaction process of graphite oxide: to be joined by graphite in the mixing solutions of nitric acid and sulfuric acid under low temperature, stir half an hour of lowering the temperature, then oxygenant is added, centrifugal or filtering separation acquisition graphite oxide after reaction for some time.
Preferably, graphite described in step 1) is natural flake graphite.
Preferably, step 2) described in time of ultrasonic stripping be 5 ~ 20min.More excellent, step 2) described in time of ultrasonic stripping be 10min.
Step 2 of the present invention) in the consumption of deionized water add according to the concrete consumption of the graphite oxide for reacting, the minimum addition of deionized water is the graphite oxide that just can dissolve completely for reacting.Preferably, the mass ratio of described graphite oxide and deionized water is 0.1 ~ 10:1000.More excellent, the mass ratio of described graphite oxide and deionized water is 0.1 ~ 3.3:1000.
Preferably, step 2) in the mass ratio of the DMF that adds and deionized water be 0.5 ~ 10:1.
Preferably, step 2) in the mol ratio of the molybdate that adds and graphite oxide be 1:0.1 ~ 3.
Preferably, step 2) described molybdate is solubility Thiomolybdate.
More excellent, step 2) described molybdate is four thio ammonium molybdate or tetrathiomolybdate sodium.
Preferably, step 2) described reductive agent is selected from hydrazine hydrate or hydroiodic acid HI (HI).The consumption of reductive agent is determined according to the add-on of graphite oxide and reductive agent type, and general reductive agent is excessive, and graphene oxide is completely reduced.
Preferably, step 2) described in dispersion adopt ultrasonic disperse, the time of described ultrasonic disperse is 5 ~ 40min.More excellent, step 2) described in time of ultrasonic disperse be 10min.
Preferably, the temperature of reaction of step 3) reactor is 300 ~ 600 DEG C.The centrifugal rear deionized water wash of product 5 ~ 10 times, the DMF in removing reaction product.
Preferably, in step 3), the product after washing removing DMF is redissolved in deionized water, dry, obtain Graphene/molybdenum disulfide composite electrode material.
More excellent, drying means can be selected from lyophilize or spraying dry.
The present invention also discloses the Graphene/molybdenum disulfide composite electrode material adopting preceding method to prepare on the other hand, and in described Graphene/molybdenum disulfide composite electrode material, the mol ratio of Graphene and molybdenumdisulphide is 0.1 ~ 3:1.
Preferably, in described Graphene/molybdenum disulfide composite electrode material, the mol ratio of Graphene and molybdenumdisulphide is 0.1 ~ 1:1, and the mol ratio of Graphene and molybdenumdisulphide is except the end points of 1:1.
The principle of preparation feedback of the present invention is: stannic oxide/graphene nano sheet contains abundant oxygen-containing functional group, no longer easily again reunited by after ultrasonic disperse or be deposited in together in hydro-thermal reaction, and molybdate can be adsorbed on the surface of graphite oxide nanometer sheet by complexing action by the functional group on graphite oxide surface, generated in-situ graphene nanometer sheet and the even combined heat treatment of molybdenumdisulphide material height can be made in reductibility hydrothermal reaction process to obtain the matrix material of graphene nanometer sheet and molybdenumdisulphide.And, there is due to graphene nanometer sheet the excellent properties such as very high specific surface area, superpower mechanical property, high conduction and heat conduction, therefore, the composite nano materials of invention graphene nanometer sheet and molybdenumdisulphide prepares the chemical property that the electrode electron transmission be conducive in electrode process strengthens nano composite material electrode.
Accompanying drawing explanation
Fig. 1: the TEM figure of Graphene/molybdenumdisulphide matrix material prepared by embodiment 1
Fig. 2: the Raman figure of Graphene/molybdenumdisulphide matrix material prepared by embodiment 1
Fig. 3: embodiment 1,2, the electro-chemical test of the Graphene/molybdenumdisulphide material of 3,4 preparations
Fig. 4: the TEM figure of Graphene/molybdenumdisulphide matrix material prepared by embodiment 2
Fig. 5: the Raman figure of Graphene/molybdenumdisulphide matrix material prepared by embodiment 2
Fig. 6: the TEM figure of Graphene/molybdenumdisulphide matrix material prepared by embodiment 3
Fig. 7: the Raman figure of Graphene/molybdenumdisulphide matrix material prepared by embodiment 3
Fig. 8: the TEM figure of Graphene/molybdenumdisulphide matrix material prepared by embodiment 4
Fig. 9: the Raman figure of Graphene/molybdenumdisulphide matrix material prepared by embodiment 4
Figure 10: the TEM figure of Graphene/molybdenumdisulphide matrix material prepared by embodiment 5
Figure 11: the Raman figure of Graphene/molybdenumdisulphide matrix material prepared by embodiment 5
Figure 12: the TEM figure of Graphene/molybdenumdisulphide matrix material prepared by embodiment 6
Figure 13: the Raman figure of Graphene/molybdenumdisulphide matrix material prepared by embodiment 6
Figure 14: the TEM figure of Graphene/molybdenumdisulphide matrix material prepared by embodiment 7
Figure 15: the Raman figure of Graphene/molybdenumdisulphide matrix material prepared by embodiment 7
Figure 16: embodiment 5,6, the electro-chemical test of the Graphene/molybdenumdisulphide material of 7 preparations
Embodiment
The present invention is set forth further below in conjunction with embodiment.Should be understood that embodiment only for illustration of the present invention, but not limit the scope of the invention.
Embodiment 1
1. experimental technique
Adopt Staudenmair method to prepare graphite oxide: temperature of reaction is 5 DEG C, is joined by natural flake graphite in the mixing solutions of nitric acid and sulfuric acid, stir half an hour of lowering the temperature, then add sodium chlorate, react 12 hours at 5 DEG C, with water precipitation at least 5 times, so that except disacidify, then centrifugation; Graphite oxide is obtained 65 DEG C of oven dry.
Taking 1mg graphite oxide adds in 10ml deionized water, and ultrasonic stripping 5min obtains graphene oxide solution.Add 10ml DMF.Take 22mg four thio ammonium molybdate, join in solution, ultrasonic 10 minutes, now solution was blood red; Then 1ml hydrazine hydrate is added, ultrasonic 30 minutes.Above-mentioned solution is transferred in the reactor of 100ml, is warming up to 200 DEG C, be incubated 10 hours.The amount of substance ratio obtaining Graphene and molybdenumdisulphide is the Graphene/molybdenumdisulphide matrix material of 1:10.11. embodiment results
Fig. 1 is the TEM figure of the Graphene/molybdenumdisulphide matrix material according to embodiment 1 preparation, and result display matrix material is hollow ball; Fig. 2 is that the characteristic peak of the Raman figure of this material, Raman test display molybdenumdisulphide is more a lot of by force than the characteristic peak of Graphene, and this is excessive consistent with molybdenumdisulphide in reactant; Fig. 3 is electro-chemical test, and wherein label is that the line of numeral 1 represents the electrochemical properties of this sample.
Embodiment 2
1. experimental technique
The preparation method of graphite oxide, with embodiment 1, takes 10mg graphite oxide and adds in 10ml deionized water, and ultrasonic stripping 20min obtains graphene oxide solution.Add 10ml DMF, take 22mg four thio ammonium molybdate, join in reaction solution, ultrasonic 10 minutes, now solution was blood red; Then 1ml hydrazine hydrate is added, ultrasonic 40 minutes; Above-mentioned solution is transferred in the reactor of 100ml, is warming up to 300 DEG C, be incubated 5 hours.The amount of substance ratio obtaining Graphene and molybdenumdisulphide is the Graphene/molybdenumdisulphide matrix material of 1:1.
2. experimental result
Fig. 4 is the TEM figure of the Graphene/molybdenumdisulphide matrix material according to embodiment 2 preparation, and this matrix material of TEM test display is still hollow ball, and through measuring, interplanar distance is 0.625nm; Fig. 5 is the Raman figure of this material, and Raman tests display, there is the characteristic peak of molybdenumdisulphide.Fig. 3 is electro-chemical test, and wherein label is that the line of numeral 2 represents the electrochemical properties of this sample.
Embodiment 3
1. experimental technique
The preparation method of graphite oxide, with embodiment 1, takes 44mg graphite oxide and adds in 20ml deionized water, and ultrasonic stripping 20min obtains graphene oxide solution.Add 10ml DMF, take 22mg four thio ammonium molybdate, join wherein, ultrasonic 10 minutes, now solution was blood red; Then 1ml hydrazine hydrate is added, ultrasonic 10 minutes;
Above-mentioned solution is transferred in the reactor of 100ml, is warming up to 180 DEG C, be incubated 10 hours.The amount of substance ratio obtaining Graphene and molybdenumdisulphide is the Graphene/molybdenumdisulphide matrix material of 2:1.
2. experimental result
As the TEM figure that Fig. 6 is the Graphene/molybdenumdisulphide matrix material according to embodiment 3 preparation; Fig. 7 is the Raman figure of this material, and the characteristic peak intensity of test display Graphene obviously strengthens, and this increases consistent with Graphene content in reactant; Fig. 3 is electro-chemical test, and wherein label is that the line of numeral 3 represents the electrochemical properties of this sample.
Embodiment 4
1. experimental technique
The preparation method of graphite oxide, with embodiment 1, takes 66mg graphite oxide and adds in 20ml deionized water, and ultrasonic stripping 10min obtains graphene oxide solution.Add 10ml DMF, take 22mg four thio ammonium molybdate, join wherein, ultrasonic 10 minutes, now solution was blood red; Then 1ml hydroiodic acid HI is added, ultrasonic 5 minutes; Above-mentioned solution is transferred in the reactor of 100ml, is then warming up to 500 DEG C, be incubated 10 hours.The amount of substance ratio obtaining Graphene and molybdenumdisulphide is the Graphene/molybdenumdisulphide matrix material of 3:1.
2. experimental result
As the TEM figure that Fig. 8 is the redox graphene/molybdenumdisulphide matrix material according to embodiment 4 preparation; Fig. 9 is that the Raman figure of this material, Raman test display graphene oxide is well restored, but molybdate does not reduce completely, has molybdic oxide to exist; Fig. 3 is electro-chemical test, and wherein label is that the line of numeral 4 represents the electrochemical properties of this sample.
Embodiment 5
1. experimental technique
The preparation method of graphite oxide, with embodiment 1, takes 2.2mg graphite oxide and adds in 1ml deionized water, and ultrasonic stripping 5min obtains graphene oxide solution.Add 10ml DMF, take 22mg four thio ammonium molybdate, add wherein, ultrasonic 10 minutes, now solution was blood red, then added 1ml hydrazine hydrate, ultrasonic 30 minutes; Above-mentioned solution is transferred in the reactor of 100ml, is warming up in the baking oven of 600 DEG C, be incubated 5 hours.The amount of substance ratio obtaining Graphene and molybdenumdisulphide is the Graphene/molybdenumdisulphide matrix material of 1:10.
2. experimental result
As the TEM figure that Figure 10 is the Graphene/molybdenumdisulphide matrix material according to embodiment 5 preparation, TEM figure shows molybdenumdisulphide and is evenly distributed on redox graphene; Figure 11 is that the Raman figure of this material, Raman test display graphene oxide is well restored, and molybdate is also well restored into molybdenumdisulphide, not assorted peak; Figure 16 is electro-chemical test, and wherein label is that the line of numeral 6 represents the electrochemical properties of this sample.
Embodiment 6
1. experimental technique
The preparation method of graphite oxide, with embodiment 1, takes 4.4mg graphite oxide and adds in 2ml deionized water, and ultrasonic stripping obtains graphene oxide solution.Add 10ml DMF, take tetrathiomolybdate sodium (purchased from traditional Chinese medicines reagent group) 21.8mg, add wherein, ultrasonic 10 minutes, now solution was blood red, then added 1ml hydrazine hydrate, ultrasonication 40 minutes; Above-mentioned solution is transferred in the reactor of 100ml, is warming up in the baking oven of 700 DEG C, be incubated 10 hours.The amount of substance ratio obtaining Graphene and molybdenumdisulphide is the Graphene/molybdenumdisulphide matrix material of 1:5.
2. experimental result
As the TEM figure that Figure 12 is the redox graphene/molybdenumdisulphide matrix material according to embodiment 5 preparation, TEM figure shows molybdenumdisulphide and also can be evenly distributed on redox graphene; Figure 13 is the Raman figure of this material, and Raman testing and implementation example 5 result is similar, and just the characteristic peak intensity of molybdenumdisulphide can be more weak; Figure 16 is electro-chemical test, and wherein label is that the line of numeral 7 represents the electrochemical properties of this sample.
Embodiment 7
1. experimental technique
The preparation method of graphite oxide, with embodiment 1, takes 11mg graphite oxide and adds in 20ml deionized water, and ultrasonic stripping obtains graphene oxide solution.Add 10ml DMF; And then take 22mg four thio ammonium molybdate, add wherein, ultrasonic 10 minutes, now solution was blood red, then added 1ml hydrazine hydrate, within ultrasonic 30 minutes, above-mentioned solution is transferred in the reactor of 100ml, then puts into the baking oven of 200 DEG C, be incubated 10 hours.Obtain the Graphene/molybdenumdisulphide matrix material of the amount of substance ratio 1:2 of Graphene and molybdenumdisulphide.
2. experimental result
As the TEM figure that Figure 14 is the redox graphene/molybdenumdisulphide matrix material according to embodiment 5 preparation, TEM figure shows molybdenumdisulphide skewness; Figure 15 is the Raman figure of this material, and Raman testing and implementation example 5 result is similar, because the increase of graphene oxide, the characteristic peak intensity of molybdenumdisulphide can be more weak; Figure 16 is electro-chemical test, and wherein label is that the line of numeral 5 represents the electrochemical properties of this sample.
The above; be only preferred embodiment of the present invention; not to any formal and substantial restriction of the present invention; should be understood that; for those skilled in the art; under the prerequisite not departing from the inventive method, also can make some improvement and supplement, these improve and supplement and also should be considered as protection scope of the present invention.All those skilled in the art, without departing from the spirit and scope of the present invention, a little change made when utilizing disclosed above technology contents, the equivalent variations of modifying and developing, be Equivalent embodiments of the present invention; Meanwhile, all according to substantial technological of the present invention to the change of any equivalent variations that above-described embodiment is done, modify and differentiation, all still belong in the scope of technical scheme of the present invention.
Claims (6)
1. a preparation method for Graphene/molybdenum disulfide composite electrode material, concrete steps are as follows:
1) take graphite as raw material, prepare graphite oxide by oxidation graft process;
2) by step 1) the graphite oxide deionized water dissolving prepared, ultrasonic stripping obtains graphene oxide solution, then in graphene oxide solution, adds DMF, molybdate, finally adds reductive agent, be uniformly dispersed, and obtains mixing solutions;
3) by step 2) mixing solutions prepared transfers in reactor, be incubated 5 ~ 10h being more than or equal under the temperature condition of 180 DEG C, after the product that obtains is centrifugal, repeatedly wash removing DMF with deionized water, drying, obtains Graphene/molybdenum disulfide composite electrode material product;
Step 2) described reductive agent is selected from hydrazine hydrate or hydroiodic acid HI;
Step 2) described molybdate is solubility Thiomolybdate;
Step 2) in the mass ratio of graphite oxide and deionized water be 0.1 ~ 10:1000, the DMF added and the mass ratio of deionized water are 0.5 ~ 10:1.
2. preparation method as claimed in claim 1, is characterized in that, step 2) time of described ultrasonic stripping is 5 ~ 20min.
3. preparation method as claimed in claim 1, is characterized in that, step 2) in the mol ratio of the molybdate that adds and graphite oxide be 1:0.1 ~ 3.
4. preparation method as claimed in claim 1, is characterized in that, step 2) described molybdate is four thio ammonium molybdate or tetrathiomolybdate sodium.
5. preparation method as claimed in claim 1, is characterized in that, step 3) temperature of reaction of reactor is 300 ~ 600 DEG C.
6., according to Graphene/molybdenum disulfide composite electrode material prepared by method described in the arbitrary claim of claim 1-5, in described Graphene/molybdenum disulfide composite electrode material, the mol ratio of Graphene and molybdenumdisulphide is 0.1 ~ 3:1.
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| CN102142551A (en) * | 2011-02-25 | 2011-08-03 | 浙江大学 | Graphene nano sheet/MoS2 composite nano material and synthesis method thereof |
| CN102142537A (en) * | 2011-02-25 | 2011-08-03 | 浙江大学 | Graphene/MoS2 compound nano material lithium ion battery electrode and preparation method thereof |
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| CN102142551A (en) * | 2011-02-25 | 2011-08-03 | 浙江大学 | Graphene nano sheet/MoS2 composite nano material and synthesis method thereof |
| CN102142537A (en) * | 2011-02-25 | 2011-08-03 | 浙江大学 | Graphene/MoS2 compound nano material lithium ion battery electrode and preparation method thereof |
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