CN102839388A - 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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- CN102839388A CN102839388A CN2012103260355A CN201210326035A CN102839388A CN 102839388 A CN102839388 A CN 102839388A CN 2012103260355 A CN2012103260355 A CN 2012103260355A CN 201210326035 A CN201210326035 A CN 201210326035A CN 102839388 A CN102839388 A CN 102839388A
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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 using now, to fifties 21 century will be near exhaustion, and this fuel has serious pollution to environment.International Technology circle is being sought the new energy, and hydrogen energy source is one of them.The combustion heat of hydrogen is 28900 kcal/kg, approximately is three times of gasoline combustion heat.Reaction product is a water, environment is not polluted, and the water that burning generates also can continue hydrogen manufacturing, recycles repeatedly.The product water non-corrosiveness, harmless to equipment, so people are called clean energy source to hydrogen.Generation, storage and the utilization of hydrogen are mainly studied by the International Association for Hydrogen Energy that formed in 1976.Liquid hydrogen is as rocket fuel at present; The hydrogen that liquid hydrogen, liquefied ammonia or hydrogen storage alloy are stored is as automobile fuel.But, promote the use of still and have any problem because the production cost of hydrogen is higher than fossil oil.Hydrogen energy source can be a kind of secondhand energy, and it utilizes other energy to produce through certain method, and unlike coal, oil and natural gas etc. can be directly from underground mining, almost completely rely on fossil oil.In industry, usually adopt following several method to produce hydrogen: the one, water vapour through scorching hot coke (being called carbon reduction method), is obtained purity and is about 75% hydrogen; The 2nd, water vapour through scorching hot iron, is obtained purity at the hydrogen below 97%; The 3rd, by extracting hydrogen in the water-gas, the hydrogen purity that obtains is also lower; The 4th kind of method is exactly water electrolysis method, and the hydrogen purity that makes can be up to more than 99%, and this is a kind of important method that preparation hydrogen is gone up in industry.But, use a kind of effective catalyzer in order to improve the efficient of water electrolysis hydrogen production.
Transition metal stratiform binary compound enjoys people's attention because of having performances such as good light, electricity, lubricated, catalysis.Moly-sulfide is one of typical case's representative wherein, MoS
2Be a kind of diamagnetism and the compound with semiconductor property, wherein the Mo-S faceted pebble is quite a lot of, and it is big that catalytic performance has specific surface area, high adsorption capacity, and the reactive behavior advantages of higher is so receive much concern this year.But, though MoS
2Laminate structure is a kind of up-and-coming electrochemical electrode material, but fails to obtain industrial applications, because MoS
2Conductivity relatively poor.Because Graphene has 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; Help the electron transport in the electrode process, the chemical property of intensifier electrode.
Aspect the combination electrode material of preparation Graphene/molybdenumdisulphide, people such as Kun Chang are with the graphene oxide of Hummer method preparation, and L-crysteine and Sodium orthomolybdate are raw material, in the aqueous solution, prepare matrix material, and have explored the application of lithium ion battery aspect.[Kun Chang and Weixiang Chen; L-Crysteine-assisted synthesis of layered MoS2/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 using.People such as Yangguang Li use pure organic solvent N; N-dimethylformamide (DMF; N; Dinethylformamide) synthesized two-dimentional molybdenumdisulphide evenly attached to the surperficial sandwich of two-dimentional Graphene; And the proof matrix material is as the excellent electrolytic hydrogen production characteristic [J.Am.Chem.Soc.133 (2011) 7296 for Yangguang Li et al., MoS2 nanoparticles grown on graphene:an advanced catalyst for the hydrogen evolution reaction] of electrode.But this method is all used DMF, and hydro-thermal synthetic raw material graphene oxide is hydrophilic not lipophilic, and therefore the dispersion in DMF is very difficult, and product is difficult to evenly, the expensive of its outer organic solvent own, and aftertreatment is also uneconomical.
Summary of the invention
The objective of the invention is to overcome the defective of prior art; A kind of Graphene/molybdenumdisulphide combination electrode material and preparation method thereof is provided; The preparation process of Graphene of the present invention/molybdenumdisulphide combination electrode material is carried out in the double solvents of water and organism composition; Not only greatly strengthen the homogeneity of product Graphene/molybdenumdisulphide in the hydrothermal reaction process, but also reduced the use of expensive organic solvent DMF.
The present invention at first discloses the preparation method of a kind of Graphene/molybdenumdisulphide combination electrode material, and concrete steps are following:
1) with graphite is raw material, prepares graphite oxide through the oxidation graft process;
2) graphite oxide of step 1) preparation is used deionized water dissolving, ultrasonic peeling off obtains graphene oxide solution, in graphene oxide solution, adds DMF, molybdate then, adds reductive agent at last, is uniformly dispersed, and obtains mixing solutions;
3) with step 2) preparation mixing solutions transfer in the reaction kettle; Insulation 5～10h under more than or equal to 180 ℃ temperature condition, with the product that obtains centrifugal after, repeatedly wash with deionized water and to remove DMF; Drying obtains Graphene/molybdenumdisulphide combination electrode material product.
More excellent, the said oxidation graft process of step 1) is selected from Hummer method or Staudenmair method.
Hummer method and Staudenmair method are prior art; The reaction process that adopts the Staudenmair legal system to be equipped with graphite oxide comprises: under the low temperature graphite is joined in nitric acid and the vitriolic mixing solutions; Stir the half a hour of lowering the temperature; Add oxygenant then, centrifugal or filtering separation acquisition graphite oxide after reaction for some time.
More excellent, the said graphite of step 1) is natural flake graphite.
More excellent, step 2) the ultrasonic time of peeling off is 5～20min described in.More excellent, step 2) the ultrasonic time of peeling off is 10min described in.
More excellent, step 2) DMF that adds in and the mass ratio of deionized water are 0.5～10:1.
More excellent, step 2) molybdate that adds in and the mol ratio of graphite oxide are 1:0.1～3.
More excellent, step 2) said molybdate is the solubility Thiomolybdate.
More excellent, step 2) said molybdate is four thio ammonium molybdate or tetrathiomolybdate sodium.
More excellent, step 2) said reductive agent is selected from Hydrazine Hydrate 80 or hydroiodic acid HI (HI).The consumption of reductive agent is decided according to the add-on and the reductive agent type of graphite oxide, and general reductive agent is excessive, makes graphene oxide by reduction fully.
More excellent, step 2) disperse to adopt ultra-sonic dispersion described in, the time of said ultra-sonic dispersion is 5～40min.More excellent, step 2) time of ultra-sonic dispersion is 10min described in.
More excellent, the temperature of reaction of step 3) reaction kettle is 300～600 ℃.The DMF in the reaction product is removed with deionized water wash 5～10 times in the centrifugal back of product.
More excellent, the product of in the step 3) washing being removed behind the DMF redissolves in deionized water, and drying obtains Graphene/molybdenumdisulphide combination electrode material.
More excellent, drying means can be selected from lyophilize or spraying drying.
The present invention also discloses the Graphene/molybdenumdisulphide combination electrode material that adopts the preceding method preparation on the other hand, and the mol ratio of Graphene and molybdenumdisulphide is 0.1～3:1 in said Graphene/molybdenumdisulphide combination electrode material.
More excellent, the mol ratio of Graphene and molybdenumdisulphide is 0.1～1:1 in said Graphene/molybdenumdisulphide combination electrode material, 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: the stannic oxide/graphene nano sheet contains abundant oxygen-containing functional group; In hydro-thermal reaction, reunited again no longer easily behind the ultra-sonic dispersion or be deposited in together; And the functional group on graphite oxide surface can be adsorbed on molybdate the surface of graphite oxide nanometer sheet through complexing action, in the reductibility hydrothermal reaction process, can make generated in-situ graphene nanometer sheet and the even combined heat treatment of molybdenumdisulphide material height obtain the matrix material of graphene nanometer sheet and molybdenumdisulphide.And; Because graphene nanometer sheet has excellent properties such as very high specific surface area, superpower mechanical property, high conduction and heat conduction; Therefore, invention prepares the chemical property that electrode helps the electron transport enhancing nano composite material electrode in the electrode process with the composite nano materials of graphene nanometer sheet and molybdenumdisulphide.
In the prior art; People such as Yangguang Li use pure organic solvent DMF to carry out synthetic [the Yangguang Li et al. of Graphene/molybdenumdisulphide combination electrode material; J.Am.Chem.Soc.133 (2011) 7296]; The present invention is dissolved in the water graphene oxide compound with organic solvent again; Graphene oxide is dispersed in the solvent system, has greatly strengthened the homogeneity of product Graphene/molybdenumdisulphide in the hydrothermal reaction process, but also reduced the use of expensive organic solvent DMF.People such as Kun Chang use Crysteine auxiliary hydrothermal method composite graphite alkene and molybdenumdisulphide [ACS Nano 5 (2011) 4720], and with this compared with techniques, the present invention need not use any subsidiary material, can directly synthesize final combination electrode material.
It is thus clear that Graphene of the present invention/molybdenumdisulphide combination electrode material preparation method is simple, reaction system is even, production cost is low, extremely is fit to the requirement of industrial mass production; Preparation product Graphene/molybdenumdisulphide combination electrode material has preferable chemical property.
Description of drawings
The TEM figure of the Graphene/molybdenumdisulphide matrix material of Fig. 1: embodiment 1 preparation
The Raman figure of the Graphene/molybdenumdisulphide matrix material of Fig. 2: embodiment 1 preparation
The electro-chemical test of the Graphene/molybdenumdisulphide material of Fig. 3: embodiment 1,2,3,4 preparations
The TEM figure of the Graphene/molybdenumdisulphide matrix material of Fig. 4: embodiment 2 preparations
The Raman figure of the Graphene/molybdenumdisulphide matrix material of Fig. 5: embodiment 2 preparations
The TEM figure of the Graphene/molybdenumdisulphide matrix material of Fig. 6: embodiment 3 preparations
The Raman figure of the Graphene/molybdenumdisulphide matrix material of Fig. 7: embodiment 3 preparations
The TEM figure of the Graphene/molybdenumdisulphide matrix material of Fig. 8: embodiment 4 preparations
The Raman figure of the Graphene/molybdenumdisulphide matrix material of Fig. 9: embodiment 4 preparations
The TEM figure of the Graphene/molybdenumdisulphide matrix material of Figure 10: embodiment 5 preparations
The Raman figure of the Graphene/molybdenumdisulphide matrix material of Figure 11: embodiment 5 preparations
The TEM figure of the Graphene/molybdenumdisulphide matrix material of Figure 12: embodiment 6 preparations
The Raman figure of the Graphene/molybdenumdisulphide matrix material of Figure 13: embodiment 6 preparations
The TEM figure of the Graphene/molybdenumdisulphide matrix material of Figure 14: embodiment 7 preparations
The Raman figure of the Graphene/molybdenumdisulphide matrix material of Figure 15: embodiment 7 preparations
The electro-chemical test of the Graphene/molybdenumdisulphide material of Figure 16: embodiment 5,6,7 preparations
Embodiment
Further set forth the present invention below in conjunction with embodiment.Should be understood that embodiment only is used to explain the present invention, and unrestricted scope of the present invention.
1. experimental technique
Adopt the Staudenmair method to prepare graphite oxide: temperature of reaction is 5 ℃, and natural flake graphite is joined in nitric acid and the vitriolic mixing solutions, stirs the half a hour of lowering the temperature; Add VAL-DROP then, reacted 12 hours down, water deposition at least 5 times at 5 ℃; So that remove disacidify, spinning then; Obtain graphite oxide 65 ℃ of oven dry.
Take by weighing the 1mg graphite oxide and add in the 10ml deionized water, the ultrasonic 5min that peels off obtains graphene oxide solution.Add 10ml DMF.Take by weighing the 22mg four thio ammonium molybdate, join in the solution, ultrasonic 10 minutes, this moment, solution was blood red; Add the 1ml Hydrazine Hydrate 80 then, ultrasonic 30 minutes.Transfer to above-mentioned solution in the reaction kettle of 100ml, be warming up to 200 ℃, be incubated 10 hours.The amount of substance ratio that obtains Graphene and molybdenumdisulphide is Graphene/molybdenumdisulphide matrix material of 1:10.11. embodiment result
Fig. 1 is the TEM figure according to the Graphene/molybdenumdisulphide matrix material of embodiment 1 preparation, and the result shows that matrix material is hollow ball; Fig. 2 is the Raman figure of this material, and Raman test shows that the characteristic peak of molybdenumdisulphide is more a lot of by force than the characteristic peak of Graphene, this with reactant in molybdenumdisulphide excessive consistent; Fig. 3 is an electro-chemical test, and wherein label is represented the electrochemical properties of this sample for the line of numeral 1.
1. experimental technique
The preparation method of graphite oxide takes by weighing the 10mg graphite oxide and adds in the 10ml deionized water with embodiment 1, and the ultrasonic 20min that peels off obtains graphene oxide solution.Add 10ml DMF, take by weighing the 22mg four thio ammonium molybdate, join in the reaction solution, ultrasonic 10 minutes, this moment, solution was blood red; Add the 1ml Hydrazine Hydrate 80 then, ultrasonic 40 minutes; Transfer to above-mentioned solution in the reaction kettle of 100ml, be warming up to 300 ℃, be incubated 5 hours.The amount of substance ratio that obtains Graphene and molybdenumdisulphide is Graphene/molybdenumdisulphide matrix material of 1:1.
2. experimental result
Fig. 4 is the TEM figure according to the Graphene/molybdenumdisulphide matrix material of embodiment 2 preparations, and the TEM test shows that this matrix material still is a hollow ball, and through measuring, interplanar distance is 0.625nm; Fig. 5 is the Raman figure of this material, and Raman tests demonstration, has the characteristic peak of molybdenumdisulphide.Fig. 3 is an electro-chemical test, and wherein label is represented the electrochemical properties of this sample for the line of numeral 2.
1. experimental technique
The preparation method of graphite oxide takes by weighing the 44mg graphite oxide and adds in the 20ml deionized water with embodiment 1, and the ultrasonic 20min that peels off obtains graphene oxide solution.Add 10ml DMF, take by weighing the 22mg four thio ammonium molybdate, join wherein, ultrasonic 10 minutes, this moment, solution was blood red; Add the 1ml Hydrazine Hydrate 80 then, ultrasonic 10 minutes;
Transfer to above-mentioned solution in the reaction kettle of 100ml, be warming up to 180 ℃, be incubated 10 hours.The amount of substance ratio that obtains Graphene and molybdenumdisulphide is Graphene/molybdenumdisulphide matrix material of 2:1.
2. experimental result
Like Fig. 6 is the TEM figure according to the Graphene/molybdenumdisulphide matrix material of embodiment 3 preparations; Fig. 7 is the Raman figure of this material, and test shows that the characteristic peak intensity of Graphene obviously strengthens, this with reactant in the increase of Graphene content consistent; Fig. 3 is an electro-chemical test, and wherein label is represented the electrochemical properties of this sample for the line of numeral 3.
1. experimental technique
The preparation method of graphite oxide takes by weighing the 66mg graphite oxide and adds in the 20ml deionized water with embodiment 1, and the ultrasonic 10min that peels off obtains graphene oxide solution.Add 10ml DMF, take by weighing the 22mg four thio ammonium molybdate, join wherein, ultrasonic 10 minutes, this moment, solution was blood red; Add the 1ml hydroiodic acid HI then, ultrasonic 5 minutes; Transfer to above-mentioned solution in the reaction kettle of 100ml, be warming up to 500 ℃ then, be incubated 10 hours.The amount of substance ratio that obtains Graphene and molybdenumdisulphide is Graphene/molybdenumdisulphide matrix material of 3:1.
2. experimental result
Like Fig. 8 is the TEM figure according to the redox graphene/molybdenumdisulphide matrix material of embodiment 4 preparations; Fig. 9 is the Raman figure of this material, and the Raman test shows graphene oxide by well reduction, but not reduction fully of molybdate has molybdic oxide to exist; Fig. 3 is an electro-chemical test, and wherein label is represented the electrochemical properties of this sample for the line of numeral 4.
1. experimental technique
The preparation method of graphite oxide takes by weighing the 2.2mg graphite oxide and adds in the 1ml deionized water with embodiment 1, and the ultrasonic 5min that peels off obtains graphene oxide solution.Add 10ml DMF, take by weighing the 22mg four thio ammonium molybdate, add wherein, ultrasonic 10 minutes, this moment, solution was blood red, added the 1ml Hydrazine Hydrate 80 again, ultrasonic 30 minutes; Transfer to above-mentioned solution in the reaction kettle of 100ml, be warming up in 600 ℃ the baking oven, be incubated 5 hours.The amount of substance ratio that obtains Graphene and molybdenumdisulphide is Graphene/molybdenumdisulphide matrix material of 1:10.
2. experimental result
Like Figure 10 is that TEM figure shows that molybdenumdisulphide is evenly distributed on the redox graphene according to the TEM figure of the Graphene/molybdenumdisulphide matrix material of embodiment 5 preparations; Figure 11 is the Raman figure of this material, and the Raman test shows graphene oxide by well reduction, and molybdate also well is reduced into molybdenumdisulphide, not assorted peak; Figure 16 is an electro-chemical test, and wherein label is represented the electrochemical properties of this sample for the line of numeral 6.
Embodiment 6
1. experimental technique
The preparation method of graphite oxide takes by weighing the 4.4mg graphite oxide and adds in the 2ml deionized water with embodiment 1, and ultrasonic peeling off obtains graphene oxide solution.Add 10ml DMF, take by weighing tetrathiomolybdate sodium (available from traditional Chinese medicines reagent group) 21.8mg, add wherein, ultrasonic 10 minutes, this moment, solution was blood red, added the 1ml Hydrazine Hydrate 80 again, sonicated 40 minutes; Transfer to above-mentioned solution in the reaction kettle of 100ml, be warming up in 700 ℃ the baking oven, be incubated 10 hours.The amount of substance ratio that obtains Graphene and molybdenumdisulphide is Graphene/molybdenumdisulphide matrix material of 1:5.
2. experimental result
Like Figure 12 is that TEM figure shows that molybdenumdisulphide also can be evenly distributed on the redox graphene according to the TEM figure of the redox graphene/molybdenumdisulphide matrix material of embodiment 5 preparations; Figure 13 is the Raman figure of this material, and the Raman test is similar with embodiment 5 results, and just the characteristic peak intensity of molybdenumdisulphide can be weak; Figure 16 is an electro-chemical test, and wherein label is represented the electrochemical properties of this sample for the line of numeral 7.
Embodiment 7
1. experimental technique
The preparation method of graphite oxide takes by weighing the 11mg graphite oxide and adds in the 20ml deionized water with embodiment 1, and ultrasonic peeling off obtains graphene oxide solution.Add 10ml DMF; And then take by weighing the 22mg four thio ammonium molybdate, and add wherein, ultrasonic 10 minutes, this moment, solution was blood red, added the 1ml Hydrazine Hydrate 80 again, in the ultrasonic reaction kettle of transferring to above-mentioned solution in 30 minutes 100ml, put into 200 ℃ baking oven then, was incubated 10 hours.Obtain Graphene/molybdenumdisulphide matrix material of the amount of substance ratio 1:2 of Graphene and molybdenumdisulphide.
2. experimental result
Like Figure 14 is that TEM figure shows the molybdenumdisulphide skewness according to the TEM figure of the redox graphene/molybdenumdisulphide matrix material of embodiment 5 preparations; Figure 15 is the Raman figure of this material, and the Raman test is similar with embodiment 5 results, because the increase of graphene oxide, the characteristic peak intensity of molybdenumdisulphide can be more weak; Figure 16 is an electro-chemical test, and wherein label is represented the electrochemical properties of this sample for the line of numeral 5.
The above; Being merely preferred embodiment of the present invention, is not to any formal and substantial restriction of the present invention, should be understood that; For those skilled in the art; Under the prerequisite that does not break away from the inventive method, also can make some improvement and replenish, these improvement and replenish and also should be regarded as protection scope of the present invention.Allly be familiar with the professional and technical personnel, under the situation that does not break away from the spirit and scope of the present invention, the technology contents that is disclosed more than capable of using and a little change of making, modify the equivalent variations with differentiation, be equivalent embodiment of the present invention; Simultaneously, the change of any equivalent variations that all foundations essence technology of the present invention is done the foregoing description, modify and differentiation, all still belong in the scope of technical scheme of the present invention.
Claims (10)
1. the preparation method of Graphene/molybdenumdisulphide combination electrode material, concrete steps are following:
1) with graphite is raw material, prepares graphite oxide through the oxidation graft process;
2) graphite oxide of step 1) preparation is used deionized water dissolving, ultrasonic peeling off obtains graphene oxide solution, in graphene oxide solution, adds DMF, molybdate then, adds reductive agent at last, is uniformly dispersed, and obtains mixing solutions;
3) with step 2) preparation mixing solutions transfer in the reaction kettle; Insulation 5～10h under more than or equal to 180 ℃ temperature condition, with the product that obtains centrifugal after, repeatedly wash with deionized water and to remove DMF; Drying obtains Graphene/molybdenumdisulphide combination electrode material product.
2. preparation method as claimed in claim 1 is characterized in that step 2) the said ultrasonic time of peeling off is 5～20min.
3. preparation method as claimed in claim 1 is characterized in that step 2) in the mass ratio of graphite oxide and deionized water be 0.1～10:1000.
4. preparation method as claimed in claim 1 is characterized in that step 2) in the DMF that adds and the mass ratio of deionized water be 0.5～10:1.
5. preparation method as claimed in claim 1 is characterized in that step 2) in the molybdate that adds and the mol ratio of graphite oxide be 1:0.1～3.
6. like claim 1 or the described preparation method of 5 arbitrary claims, it is characterized in that step 2) said molybdate is the solubility Thiomolybdate.
7. preparation method as claimed in claim 6 is characterized in that step 2) said molybdate is four thio ammonium molybdate or tetrathiomolybdate sodium.
8. preparation method as claimed in claim 1 is characterized in that step 2) said reductive agent is selected from Hydrazine Hydrate 80 or hydroiodic acid HI.
9. preparation method as claimed in claim 1 is characterized in that, the temperature of reaction of step 3) reaction kettle is 300～600 ℃.
10. according to the Graphene/molybdenumdisulphide combination electrode material of the said method preparation of the arbitrary claim of claim 1-9, the mol ratio of Graphene and molybdenumdisulphide is 0.1～3:1 in said Graphene/molybdenumdisulphide combination electrode material.
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