CN104183830A - Preparation method of two-dimensional inorganic layered compound/graphene composite material - Google Patents
Preparation method of two-dimensional inorganic layered compound/graphene composite material Download PDFInfo
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
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Abstract
The invention discloses a preparation method of a two-dimensional inorganic layered compound/graphene composite material. The preparation method of the composite material comprises the following steps: preparing layered compound dispersion liquid with positive charges on the surface and oxidized graphene dispersion liquid with negative charges; mixing the two kinds of solution to perform self-assembling under an electrostatic interaction to obtain the ordered two-dimensional inorganic layered compound/graphene composite material assembled alternatively layer by layer; and carrying out reduction reaction on the composite material under certain conditions to obtain the two-dimensional inorganic layered compound/graphene composite material. According to the two-dimensional inorganic layered compound/graphene composite material, the two-dimensional inorganic layered compound and the graphene are assembled alternatively layer by layer under the electrostatic interaction; the required equipment has low requirement and is easy to operate; the graphene can provide a good electronic transmission channel for the inorganic layered material, so as to enhance the electrical conductivity of the inorganic layered material, prevent agglomeration, and achieve an important effect on the material structure stability. The two-dimensional inorganic layered compound/graphene composite material can be widely applied to the fields of catalytic and electrochemical energy storage fields.
Description
Technical field
The present invention relates to a kind of preparation method of Two-dimensional Inorganic lamellar compound/graphene composite material, belong to nano material and preparing technical field thereof.
Background technology
Two-dimensional Inorganic lamellar compound as stratiform transition metal hydroxide, stratiform transition metal oxide, laminated metal chalcogenide etc. because its unique layer structure attracted a lot of concerns.And research shows, these Two-dimensional Inorganic nonwoven fabric from filaments are peeled off into the thinner nanometer sheet of stable existence, these materials can show more excellent performance, have very large application potential aspect electrochemical energy storage.Yet poorly conductive is the main cause that limits these material application.
Than these semiconductors Two-dimensional Inorganic lamellar compound of insulating property (properties) even, Graphene is a kind of material with carbon element of monoatomic layer, has specific area large, good conductivity, intensity high.Yet Graphene is used separately and is easy to reunite, its actual specific area is significantly less than theoretical specific area, therefore, can not bring into play better its effect.
Patent CN103093967A discloses a kind of preparation method who prepares the cobalt aluminum bimetal hydroxide/redox graphene of lamellar structure, and the method is by being directly added to cobalt nitrate and aluminum nitrate mixed solution in graphene oxide, and backflow obtains.But the metal ion that this method is removed on absorption position grows into outside nano particle, in solution, also have a large amount of metal ions to generate double-metal hydroxide, form aggregating state and the contact of discord Graphene.Patent CN103641174A has described a kind of by the direct ultrasonic nano-sheet MnO that obtains of mixing of the dispersion liquid of nano-sheet manganese dioxide powder dispersion and graphene powder
2the preparation method of/graphene composite material.Yet composite material prepared by this method, only relies on ultrasonic effect, MnO
2with evenly combination effectively of Graphene.In patent CN102496480A, alkali source compound, nickel and aluminium salt precursor body are joined to hydro-thermal reaction in Graphene filter cake and make graphene/nickel-aluminum bimetal hydroxide.The method is high to equipment requirement, and nickel aluminum bimetal hydroxide differs and effectively grows into surely on the Graphene filter cake having reduced.
Summary of the invention
The object of the invention is to, for Two-dimensional Inorganic lamellar compound and the independent deficiency of using of Graphene, provides a kind of compound Two-dimensional Inorganic lamellar compound of simple possible and the preparation method of Graphene.
The present invention specifically comprises the following steps:
(1) Two-dimensional Inorganic lamellar compound presoma is peeled off into nanometer sheet in can reducing its solvent of peeling off energy, make positive charge on lamellar compound surface band, obtain positively charged lamellar compound solution, the mass ratio of lamellar compound and solvent is 1:1 ~ 1:20.
(2) by the surface of preparation with the lamellar compound solution of positive charge and with the graphene oxide solution of negative electrical charge in proportion 1:1 ~ 50:1 mix, standing 6 ~ 60h, there is precipitation, pour out supernatant liquor, centrifuge washing lower floor solution, obtains Two-dimensional Inorganic lamellar compound/graphene oxide composite material I.
(3) by Two-dimensional Inorganic lamellar compound/graphene oxide composite material I reduction, obtain Two-dimensional Inorganic lamellar compound/graphene composite material II.
Two-dimensional Inorganic lamellar compound presoma described in step (1) is stratiform transition metal hydroxide, stratiform transition metal oxide, laminated metal chalcogenide.
Described its solvent of peeling off energy that can reduce is formamide, Tetramethylammonium hydroxide, 1-METHYLPYRROLIDONE, isopropyl alcohol or N-N-dimethyl formamide etc.
Described make the lamellar compound lotus that becomes positively charged, if the positively charged of lamellar compound nanometer sheet own is directly peeled off into nanometer sheet, if lamellar compound itself is electronegative, with cationic surfactant, modify.Cationic surfactant can be hexadecyltrimethylammonium chloride, polyethylene propyl-dimethyl ammonium chloride, polypropylene amine hydrochloride, poly 4 vinyl pyridine etc.Described lamellar compound and the mass ratio of solvent are 1:1 ~ 1:20.
The solution with positive charge described in step (2) and with the graphene solution of negative electrical charge in proportion 1:1 ~ 20:1 mix.
Method of reducing described in step (3) has electronation, thermal reduction etc.Described its conductivity of Two-dimensional Inorganic lamellar compound/graphene composite material II is obviously better than Two-dimensional Inorganic lamellar compound/graphene oxide composite material I.
The present invention utilizes electrostatic interaction by Two-dimensional Inorganic lamellar compound and Graphene alternate group dress layer by layer, and both can carry out combination effectively by electrostatic force, the nano composite material that height of formation is orderly, and equipment needed thereby requires low, easy operating.Graphene not only can strengthen its conductivity for inorganic lamellar material provides good electron propagation ducts, has also prevented the reunion of self, the structural stability of material has been play a part important, has guaranteed that it is in many-sided application.
Accompanying drawing explanation
Fig. 1 is the mechanism schematic diagram of Two-dimensional Inorganic lamellar compound (surface band the positive charge)/graphene composite material prepared of the present invention.
Fig. 2 is the mechanism schematic diagram of Two-dimensional Inorganic lamellar compound (surface band the negative electrical charge)/graphene composite material prepared of the present invention.
Embodiment
Below in conjunction with embodiment, be intended to further illustrate the present invention, and unrestricted the present invention.
Embodiment 1
2.617g is analyzed to pure nickel nitrate and 1.125g to be analyzed in the deionized water that pure aluminum nitrate is dissolved in 50ml, 2.4g urea is dissolved in the deionized water of 50ml, two kinds of solution are mixed, proceed in autoclave, 100 ℃ of reaction 24h, filter, washing, obtains nickel aluminum bimetal hydroxide 60 ℃ of vacuumizes.The nickel aluminum bimetal hydroxide of 1g is joined in the nitric acid 1000ml solution of the sodium nitrate that contains 1.5M and 0.005M, in solution, pass into nitrogen 15min, drive carbon dioxide away.Above-mentioned solution is at room temperature shaken 1 day, the product obtaining is filtered, washing, obtains the nickel aluminum bimetal hydroxide after anion exchange 60 ℃ of vacuumizes.By the nickel aluminum bimetal hydroxide after anion exchange and formamide solution 1:1 mixing in mass ratio, shake 1 day, 2000rpm centrifuging and taking supernatant liquor, obtains the positively charged stratiform nickel aluminum bimetal hydroxide nanometer sheet solution 1 of peeling off.By the positively charged stratiform nickel aluminum bimetal hydroxide nanometer sheet solution 1 of peeling off and stannic oxide/graphene nano sheet solution 2 50:1 mixing in proportion, stir 10min, standing 24h, 8000rpm is centrifugal, washing, 60 ℃ of vacuumizes, obtain nickel aluminum bimetal hydroxide/graphene oxide composite material 3, as shown in Figure 1.By composite material 200 ℃ of heat treatment 6h under nitrogen atmosphere, obtain nickel aluminum bimetal hydroxide/graphene composite material.Above-mentioned composite material is loaded on glass-carbon electrode, and in 1mol/L potassium hydroxide electrolyte, test has good electrocatalysis characteristic, can be applied to alkaline fuel cell.
Embodiment 2
1.746g is analyzed to pure nickel nitrate and 1.125g to be analyzed in the deionized water that pure aluminum nitrate is dissolved in 50ml, 1.8g urea is dissolved in the deionized water of 50ml, two kinds of solution are mixed, proceed in autoclave, 100 ℃ of reaction 24h, filter, washing, obtains nickel aluminum bimetal hydroxide 60 ℃ of vacuumizes.The nickel aluminum bimetal hydroxide of 1g is joined in the nitric acid 1000ml solution of the sodium nitrate that contains 1.5M and 0.005M, in solution, pass into nitrogen 15min, drive carbon dioxide away.Above-mentioned solution is at room temperature shaken 1 day, the product obtaining is filtered, washing, obtains the nickel aluminum bimetal hydroxide after anion exchange 60 ℃ of vacuumizes.By the nickel aluminum bimetal hydroxide after anion exchange and formamide solution 1:1 mixing in mass ratio, shake 1 day, 2000rpm centrifuging and taking supernatant liquor, obtains the positively charged stratiform nickel aluminum bimetal hydroxide nanometer sheet of peeling off.By the positively charged stratiform nickel aluminum bimetal hydroxide nanometer sheet solution of peeling off and the 20:1 mixing in proportion of stannic oxide/graphene nano sheet solution, stir 10min, standing 24h, 8000rpm is centrifugal, washing, 60 ℃ of vacuumizes, obtain nickel aluminum bimetal hydroxide/graphene oxide composite material.By composite material 200 ℃ of heat treatment 6h under nitrogen atmosphere, obtain nickel aluminum bimetal hydroxide/graphene composite material.Above-mentioned composite material is loaded on glass-carbon electrode, and in 1mol/L potassium hydroxide electrolyte, test has good electrocatalysis characteristic, can be applied to alkaline fuel cell.
Embodiment 3
2.619g is analyzed to pure cobalt nitrate and 1.125g to be analyzed in the deionized water that pure aluminum nitrate is dissolved in 50ml, 2.4g urea is dissolved in the deionized water of 50ml, two kinds of solution are mixed, proceed in autoclave, 120 ℃ of reaction 24h, filter, washing, obtains cobalt aluminum bimetal hydroxide 60 ℃ of vacuumizes.The cobalt aluminum bimetal hydroxide of 1g is joined in the nitric acid 1000ml solution of the sodium nitrate that contains 1.5M and 0.005M, in solution, pass into nitrogen 15min, drive carbon dioxide away.Above-mentioned solution is at room temperature shaken 1 day, the product obtaining is filtered, washing, obtains the cobalt aluminum bimetal hydroxide after anion exchange 60 ℃ of vacuumizes.By the cobalt aluminum bimetal hydroxide after anion exchange and formamide solution 1:5 mixing in mass ratio, shake 1 day, 2000rpm centrifuging and taking supernatant liquor, obtains the layered cobalt aluminium duplex metal hydroxide nanometer sheet of peeling off.By the layered cobalt aluminium duplex metal hydroxide nanometer sheet solution of peeling off and the 50:1 mixing in proportion of stannic oxide/graphene nano sheet solution, stir 10min, standing 36h, 8000rpm is centrifugal, washing, 60 ℃ of vacuumizes, obtain cobalt aluminum bimetal hydroxide/graphene oxide composite material.By composite material 200 ℃ of heat treatment 6h under nitrogen atmosphere, obtain cobalt aluminum bimetal hydroxide/graphene composite material.Above-mentioned composite material is made into electrode, and in 6mol/L potassium hydroxide electrolyte, test has good chemical property, can be applied to ultracapacitor.
Embodiment 4
1.746g is analyzed to pure cobalt nitrate and 1.125g to be analyzed in the deionized water that pure aluminum nitrate is dissolved in 50ml, 1.8g urea is dissolved in the deionized water of 50ml, two kinds of solution are mixed, proceed in autoclave, 120 ℃ of reaction 24h, filter, washing, obtains cobalt aluminum bimetal hydroxide 60 ℃ of vacuumizes.The cobalt aluminum bimetal hydroxide of 1g is joined in the nitric acid 1000ml solution of the sodium nitrate that contains 1.5M and 0.005M, in solution, pass into nitrogen 15min, drive carbon dioxide away.Above-mentioned solution is at room temperature shaken 1 day, the product obtaining is filtered, washing, obtains the cobalt aluminum bimetal hydroxide after anion exchange 60 ℃ of vacuumizes.By the cobalt aluminum bimetal hydroxide after anion exchange and formamide solution 1:5 mixing in mass ratio, shake 1 day, 2000rpm centrifuging and taking supernatant liquor, obtains the layered cobalt aluminium duplex metal hydroxide nanometer sheet of peeling off.By the layered cobalt aluminium duplex metal hydroxide nanometer sheet solution of peeling off and the 20:1 mixing in proportion of stannic oxide/graphene nano sheet solution, stir 10min, standing 36h, 8000rpm is centrifugal, washing, 60 ℃ of vacuumizes, obtain cobalt aluminum bimetal hydroxide/graphene oxide composite material.By composite material 200 ℃ of heat treatment 6h under nitrogen atmosphere, obtain cobalt aluminum bimetal hydroxide/graphene composite material.Above-mentioned composite material is made into electrode, and in 6mol/L potassium hydroxide electrolyte, test has good chemical property, can be applied to ultracapacitor.
Embodiment 5
30% the hydrogen peroxide that measures 10% the tetramethyl ammonium hydroxide solution of 10ml and 2ml is made into the solution A of 20ml.The manganese chloride that weighs 0.594g is dissolved in the deionized water of 10ml and forms solution B.Solution A is joined in 15s in solution B, vigorous stirring 24h at room temperature then, 8000rpm centrifuge washing, is dispersed in water centrifugal precipitation of getting off, and ultrasonic 30min can form electronegative manganese dioxide nano-plates solution 4.20% the diallyl dimethyl ammoniumchloride solution 5 that measures 1ml joins in the manganese dioxide nano-plates solution of 100ml, under room temperature, stirs 2h, forms the modified manganese dioxide solution 6 of surface band positive charge, as shown in Figure 2.By the layered manganese oxide nanometer sheet solution of modification and the 1:1 mixing in proportion of stannic oxide/graphene nano sheet solution, stir 10min, standing 60h, 8000rpm is centrifugal, washing, 60 ℃ of vacuumizes, obtain manganese dioxide/graphene oxide composite material 7.100mg composite material is dispersed in 100ml deionized water, adds the hydrazine hydrate of 1ml to the inside, 95 ℃ of oil bath reaction 6h, obtain manganese dioxide/graphene composite material.Above-mentioned composite material is made into electrode, in the metabisulfite solution of 1mol/L, has good capacitive property, can be applied to ultracapacitor.
Embodiment 6
The thioacetamide of the sodium vanadate of 2.399g and 2.254g is dissolved in the deionized water of 80ml, stirring at room 1h, then proceeds in autoclave, and 160 ℃ of reaction 24h, obtain vanadium disulfide presoma.Then the vanadium disulfide presoma of getting 40mg is dispersed in the deionized water of 60ml, passes into argon gas half an hour, drives oxygen away, sealing, ice-bath ultrasonic 3h, the electronegative vanadium disulfide nanometer sheet that obtains peeling off.Take 1mg hexadecyltrimethylammonium chloride and be made into 10ml solution, join in the vanadium disulfide nanometer sheet solution of 100ml, under room temperature, stir 2h, form the modification vanadium disulfide solution of surface band positive charge.By the stratiform vanadium disulfide nanometer sheet solution of modification and the 50:1 mixing in proportion of stannic oxide/graphene nano sheet solution, stir 10min, standing 10h, 8000rpm is centrifugal, washing, 60 ℃ of vacuumizes, obtain vanadium disulfide/graphene oxide composite material.100mg composite material is dispersed in 100ml deionized water, adds the hydrazine hydrate of 1ml to the inside, 95 ℃ of oil bath reaction 6h, obtain vanadium disulfide/graphene composite material.Above-mentioned material is made into electrode, and the negative material as lithium battery, shows to have good application prospect.
Claims (6)
1. a preparation method for Two-dimensional Inorganic lamellar compound/graphene composite material, is characterized in that preparation process is as follows:
(1) Two-dimensional Inorganic lamellar compound presoma is peeled off into nanometer sheet in can reducing its solvent of peeling off energy; make positive charge on lamellar compound surface band; obtain positively charged lamellar compound solution, the mass ratio of lamellar compound and solvent is 1:1 ~ 1:20;
(2) by the surface of preparation with the nanometer sheet solution of positive charge and with the graphene oxide solution of negative electrical charge in proportion 1:1 ~ 50:1 mix, standing 6 ~ 60h, pour out supernatant liquor, centrifuge washing lower floor solution, obtains Two-dimensional Inorganic lamellar compound/graphene oxide composite material I;
(3) by Two-dimensional Inorganic lamellar compound/graphene oxide composite material I reduction, obtain Two-dimensional Inorganic lamellar compound/graphene composite material II.
2. according to the preparation method of the Two-dimensional Inorganic lamellar compound/graphene composite material described in claims 1, it is characterized in that: the Two-dimensional Inorganic lamellar compound presoma described in step (1) is stratiform transition metal hydroxide, stratiform transition metal oxide or laminated metal chalcogenide.
3. according to the preparation method of the Two-dimensional Inorganic lamellar compound/graphene composite material described in claims 1, it is characterized in that: its solvent of peeling off energy that can reduce described in step (1) is formamide, Tetramethylammonium hydroxide, 1-METHYLPYRROLIDONE, isopropyl alcohol or N-N-dimethyl formamide.
4. according to the preparation method of the Two-dimensional Inorganic lamellar compound/graphene composite material described in claims 1, it is characterized in that: described in step (1), make the lamellar compound lotus that becomes positively charged, if the positively charged of lamellar compound nanometer sheet of peeling off own, directly use, if the lamellar compound nanometer sheet of peeling off is electronegative, with cationic surfactant, modify, described cationic surfactant is hexadecyltrimethylammonium chloride, polyethylene propyl-dimethyl ammonium chloride, polypropylene amine hydrochloride or poly 4 vinyl pyridine.
5. according to the preparation method of the Two-dimensional Inorganic lamellar compound/graphene composite material described in claims 1, it is characterized in that: the solution with positive charge described in step (2) and with the graphene solution of negative electrical charge in proportion 1:1 ~ 20:1 mix.
6. according to the preparation method of the Two-dimensional Inorganic lamellar compound/graphene composite material described in claims 1, it is characterized in that: the method for reducing described in step (3) has electronation or thermal reduction.
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