CN106057471A - Preparation method and application of three-dimensional graphene aerogel load molybdenum disulfide nano-sheet hybridization material - Google Patents
Preparation method and application of three-dimensional graphene aerogel load molybdenum disulfide nano-sheet hybridization material Download PDFInfo
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention belongs to the technical field of a new energy nano function material, and specifically relates to a preparation method and application of a three-dimensional graphene load molybdenum disulfide nano-sheet hybridization material. A three-dimensional graphene aerogel macroscopic body is prepared through a hydrothermal reduction self-assembly method, and nano-sheet layer crystal-phase molybdenum disulfide grows on a three-dimensional graphene aerogel skeleton through adoption of a H<2> reduction method. According to the three-dimensional graphene load molybdenum disulfide nano-sheet hybridization material prepared in the invention, a large specific surface of three-dimensional graphene provides more active sites for growth of molybdenum disulfide nano sheets, the nano-sheet layer crystal-phase molybdenum disulfide as an active catalyst disperse on a surface of a three-dimensional graphene aerogel, heterojunction structure is formed between the molybdenum disulfide nano sheet and the three-dimensional graphene aerogel through intermolecular forces, and edge activity of the molybdenum disulfide nano sheet is fully exposed. The high catalytic property of molybdenum disulfide is combined with the high specific surface area and excellent eectrical conductivity of the three-dimensional graphene. The hybridization material is applied to fuel cell counter electrode preparation to perform cell assembly so that photoelectric conversion efficiency is improved.
Description
Technical field
The invention belongs to new forms of energy nano-functional material technical field, be specifically related to a kind of three-dimensional grapheme load molybdenum bisuphide
Nanometer sheet hybrid material preparation method and applications.
Background technology
Along with the world economic development huge consumption to fossil energy, energy shortage and Environmental and ecological problems become system
The about obstacle of various countries' sustainable development, solar energy receives the extensive concern of various countries' researcher as a kind of clean energy resource,
The development maked rapid progress of nanotechnology, becomes the powerful motive force of current new type solar energy technology development.At present, scientists
It is devoted to the research of novel solar battery material and structure.1991, the Gratzel professor of Lausanne, SUI Gao Deng engineering institute
Use the nano-porous TiO_2films of high-specific surface area to make semi-conducting electrode with his research group, organise with transition metal Ru etc.
Compound makees dyestuff, and selects suitable electrolyte development to assemble nanocrystalline DSSC.Compared to the silica-based sun
Battery, DSSC (DSSC) is with low cost with it, technique is simple and of a relatively high photoelectric transformation efficiency and
Cause the extensive concern of relevant scholar, and rapidly become solar energy research focus.Classical DSSC (DSSC)
Middle employing Pt is to electrode material, but the price of its costliness, easily react with I3-and be corroded etc. drawbacks limit its extensively apply.
Therefore, recent domestic researchers put forth effort to find platinum substitution material cheap, efficient, thus advance dye sensitization of solar
The extensive application of battery.
Graphene is the two dimensional surface material of the Nidus Vespae lattice structure of the atomic thickness that carbon atom is formed with sp2 hydridization
Material, is the elementary cell of the carbonaceous material (such as zero dimension fullerene, one-dimensional CNT and three-dimensional graphite) constituting other dimension, tool
There are the electric conductivity of excellence, (electron mobility 15000cm under room temperature2/ V s), high heat conductance (～5000W/ (mK)), high saturating
Light rate (～97.7%) and extra specific surface area (2630m2/ g), and the mechanical strength of excellence is it is considered to be have now most
One of nano material of potentiality.But, the π-π of graphene film interlayer interacts and Van der Waals force is bigger so that layer and layer it
Between occur the most serious nanometer to reunite and lamella stacking phenomenon, greatly reduce the effective area of Graphene, so that it should
Have a greatly reduced quality with potential.Currently, Graphene prepared by conventional method, all in superfine powdery, in use can be imitated due to size
There are the problems such as reunion, skewness in answer, surface inertness etc., thus causes the excellent properties of material itself to can not get effectively and send out
Wave.Three-dimensional grapheme hydrogel, aeroge are then the macroscopic form materials assembling with Graphene for skeleton and forming three-dimensional net structure
Material, effectively prevent the reunion between graphene sheet layer, and while retaining Graphene intrinsic property, improves other property
Can, flourishing three dimensional pore structures is also electric transmission, gas-liquid mass transfer and storage while providing bigger specific surface area
More space is provided.
Molybdenum bisuphide is the Transition-metal dichalcogenide of a quasi-representative, and it belongs to hexagonal crystal system, is the strongest Mo-in layer
S covalent bond, interlayer is more weak Van der Waals force, and thickness in monolayer is about 0.65nm.Monolayer molybdenum bisuphide has similar with Graphene
Two-dimensional nano sheet pattern, both have good similarity on microscopic appearance and crystal structure.In three-dimensional grapheme airsetting
The method using chemical heat reaction on glue skeleton prepares nanoscale twins crystalline phase molybdenum bisuphide, on the one hand three-dimensional grapheme greatly than table
Face provides more avtive spots for molybdenum disulfide nano sheet growth, is dispersed in three-dimensional grapheme airsetting as active catalyst
Glue surface, forms heterojunction structure by intermolecular force between the two, fully exposes molybdenum disulfide nano sheet edge active.
Therefore molybdenum bisuphide high catalytic property can be combined with three-dimensional grapheme high-specific surface area, superior electrical conductivity, should by this hybrid material
Use dye cell electrode preparation is carried out set of cells and is filled with raising electricity conversion.
Summary of the invention
Present invention aim to overcome that the deficiencies in the prior art, it is provided that a kind of graphene-supported molybdenum disulfide nano sheet hydridization
The preparation method and applications of material.It is summarised as: there is three-dimensional porous structure graphene aerogel as skeleton, with tetrathio molybdenum
Acid ammonium is that raw material passes through chemical heat reducing process growth in situ molybdenum disulfide nano sheet on three-dimensional grapheme aeroge skeleton, is formed
Graphene molybdenum bisuphide heterojunction structure；Use instillation to prepare Graphene/molybdenum disulfide nano sheet hybrid material to electrode, obtain
Obtain high efficiency dye sensitization solar battery.
This three-dimensional grapheme load molybdenum disulfide nano sheet hybrid material preparation method, it is characterised in that by hydrothermal reduction certainly
The method assembled prepares Graphene hydrogel, prepares graphene aerogel by cryodesiccated method afterwards；With tetrathio molybdenum
Acid ammonium is that raw material passes through chemical heat reducing process growth in situ molybdenum disulfide nano sheet on three-dimensional grapheme aeroge skeleton, is formed
Graphene molybdenum bisuphide heterojunction structure.
The technical scheme that the present invention is given:
The preparation method of a kind of graphene-supported molybdenum disulfide nano sheet hybrid material, specifically comprises the following steps that
(1) being dissolved in deionized water by graphene oxide (Go), ultrasonic 5-6h makes its acquisition 1～2mg/ml oxidation stone that is uniformly dispersed
Ink alkene solution；
(2) in reductive glutathione in above-mentioned solution: graphene oxide mass ratio is the ratio of 2:1, reproducibility paddy is added
The sweet peptide of Guang, rear ultrasonic 0.5～1h, it is stirred continuously the homogeneous dispersion soln of acquisition；
(3) (2) step acquisition solution is placed in 85～90 DEG C of thermostat water baths, the most persistently 12-13h,
(4) the redox graphene hydrogel tert-butyl alcohol obtaining (3) step soaks 48h, and the tert-butyl alcohol is changed twice in centre,
After carry out lyophilization and prepare graphene aerogel, and carry out making annealing treatment 1～2h at argon and 800 DEG C of conditions；
(5) cotton-shaped graphene aerogel and four thio ammonium molybdate [(NH4) 2MoS4] that (4) obtain are taken in mass ratio for the ratio of 4:1
Example is scattered in ethanol solution (20%), carries out supersound process 2～3h after being stirred continuously；
(6) in (5) obtain dispersion liquid, add some milliliters of concentrated hydrochloric acid (37.5%), be stirred continuously, it is thus achieved that black mixed solution；
(7) above-mentioned dark solution is carried out vacuum filtration, and the black solid material deionized water obtaining sucking filtration is washed
Wash several times, after be scattered in deionized water, ultrasonic 4～5h, it is thus achieved that stable homogeneous solution.
(8) above-mentioned solution is carried out lyophilization and obtain Graphene/molybdenum trisulfide black solid powdered rubber；
(9) logical hydrogen in tube furnace, carries out above-mentioned black solid material making annealing treatment 2h, it is thus achieved that three under the conditions of 650 DEG C
Dimension Graphene/molybdenum disulfide nano sheet hybrid material.
The three-dimensional grapheme load molybdenum disulfide nano sheet hybrid material that the present invention provides is with bigger serface and mesoporous
The three-dimensional grapheme aeroge of structure is skeleton, uses chemical heat reducing process in Graphene airsetting with four thio ammonium molybdate for raw material
Growth in situ molybdenum disulfide nano sheet composition on glue skeleton；Prepare raw material to include: graphene oxide, concentrated hydrochloric acid, reproducibility paddy Guang
Sweet peptide, the tert-butyl alcohol.
Step (2) uses reductive glutathione as reducing agent, and glutathion is with graphene-supported molybdenum disulfide nano
The mass ratio of sheet hybrid material is 2:1.
Step (4) uses tert-butyl alcohol soaking and reducing graphene oxide hydrogel, replaces hydrogel internal water.
The graphene aerogel of step (5) and four thio ammonium molybdate [(NH4) 2MoS4] are 4:1 in mass ratio.
Step (9) is under the conditions of 650 DEG C, and logical hydrogen reduces.
Transmission electron microscope (TEM), scanning electron microscope (SEM) is used to characterize the curing that the present invention is obtained
The structure and morphology of molybdenum nanometer sheet/graphene nanobelt hybrid material, its result is as follows: SEM, TEM test result shows to use water
The graphene aerogel that thermal reduction-freeze-drying method is prepared, has the most three-dimensional cavernous structure, and Graphene thin layer
Number is less, about 6-8 layer, is prevented effectively from graphene sheet layer stacking；Molybdenum bisuphide presents flaky nanometer structure, lamella overall dimensions
Less.In hybrid material, the effective uniform load of molybdenum bisuphide is to graphenic surface, and prepared three-dimensional grapheme aeroge is bigger
The growth that specific surface area is molybdenum disulfide nano sheet provide more avtive spot, make to have the molybdenum bisuphide of catalysis activity
The edge of nanoscale twins is sufficiently exposed.
Three-dimensional grapheme prepared by present invention load molybdenum disulfide nano sheet hybrid material, can be used as catalysis material and
The ideal electrode material of the novel energy such as lithium ion battery, solaode.
Accompanying drawing explanation
Redox graphene hydrogel optics picture obtained in Fig. 1 embodiment 1.
Redox graphene aeroge optics picture obtained in Fig. 2 embodiment 1.
Graphene aerogel field emission scanning electron microscope picture obtained in Fig. 3 embodiment 1
Graphene-supported molybdenum disulfide nano sheet field emission scanning electron microscope picture obtained in Fig. 4 embodiment 1
Graphene aerogel transmission electron micrograph obtained in Fig. 5 embodiment 1
Graphene-supported molybdenum disulfide nano sheet field transmission electron micrograph obtained in Fig. 6 embodiment 1
In Fig. 7 embodiment 1, electrode is assembled by graphene-supported molybdenum disulfide nano sheet hybrid material by electrode and Pt respectively
Dye cell I-V test curve.
Detailed description of the invention
Below in conjunction with instantiation, the present invention is expanded on further.It should be noted that these embodiments are merely to illustrate this
Bright rather than limit the scope of the present invention.Additionally, after having read the content that the present invention lectures, those skilled in the art can
So that the present invention to make various change or amendment, these equivalent form of values fall within the model that the application appended claims is limited equally
Enclose.
Embodiment 1
The present embodiment comprises the following steps:
(1) weighing 100mg graphene oxide (Go) to be dissolved in 100ml deionized water, ultrasonic 5-6h makes its acquisition that is uniformly dispersed
1mg/ml graphene oxide solution；
(2) in above-mentioned solution, add 200mg reductive glutathione, rear ultrasonic 1h, be stirred continuously the homogeneous dispersion soln of acquisition；
(3) (2) step acquisition solution is placed in 85 DEG C of thermostat water baths, the most persistently 12h, it is thus achieved that cylindric oxygen reduction fossil
Ink alkene hydrogel (Fig. 1)
(4) the redox graphene hydrogel tert-butyl alcohol obtaining (3) step soaks 48h, and the tert-butyl alcohol is changed twice in centre,
After carry out lyophilization 48h and prepare graphene aerogel (Fig. 2), graphene aerogel is fine the most after drying
Maintain initial condition gel shape, after carry out making annealing treatment 1h at argon and 800 DEG C of conditions；To the graphene aerogel prepared
Carry out morphology characterization (Fig. 3～6): SEM, TEM test result shows to use hydrothermal reduction-freeze-drying method successfully to prepare aobvious
Write three-dimensional poroid structure graphite alkene aeroge, and the Graphene thin layer number of plies is less, about 6-8 layer, can be prevented effectively from graphene film
Layer stack is folded；Molybdenum bisuphide presents flaky nanometer structure, and lamella overall dimensions is less.In hybrid material, molybdenum bisuphide is the most uniformly born
Being loaded onto graphenic surface, the growth that specific surface area is molybdenum disulfide nano sheet that prepared three-dimensional grapheme aeroge is bigger carries
Supply more avtive spot, made the edge with the molybdenum disulfide nano sheet layer of catalysis activity sufficiently be exposed.
(5) weigh cotton-shaped graphene aerogel 20mg and four thio ammonium molybdate 5mg that (4) obtain, be scattered in 5ml ethanol solution
(20%), in, supersound process 2h after being stirred continuously, is carried out；
(6) in (5) obtain dispersion liquid, add 2ml concentrated hydrochloric acid (37.5%), be stirred continuously, it is thus achieved that black mixed solution；
(7) above-mentioned dark solution is carried out vacuum filtration, and the black solid material deionized water obtaining sucking filtration is washed
Wash several times, after be scattered in deionized water, ultrasonic 4h, it is thus achieved that stable homogeneous solution.
(8) above-mentioned solution is carried out lyophilization 48h and obtain Graphene/molybdenum trisulfide black solid powdered rubber；
(9) logical hydrogen in tube furnace, carries out above-mentioned black solid material making annealing treatment 1h, it is thus achieved that three under the conditions of 650 DEG C
Dimension Graphene/molybdenum disulfide nano sheet hybrid material, is designated as MG.
(10) use MG electrode is carried out set of cells put into row I-V test (Fig. 7), MG electrode is shown excellence electric conductivity and
To I3 -Catalytic, final electricity conversion is up to 7.86%, is better than platinum 7.2% to electrode.
The present invention prepares three-dimensional grapheme aeroge macroscopic body by hydrothermal reduction self-assembly method, at three-dimensional grapheme aeroge bone
H is used on frame2The method long nanoscale twins crystalline phase molybdenum bisuphide of reduction.Three-dimensional grapheme load molybdenum bisuphide prepared by the present invention
Nanometer sheet hybrid material, the Large ratio surface of three-dimensional grapheme provides more avtive spots, by it for molybdenum disulfide nano sheet growth
It is dispersed in three-dimensional grapheme aeroge surface as active catalyst, forms hetero-junctions by intermolecular force between the two and tie
Structure, fully exposes molybdenum disulfide nano sheet edge active.Molybdenum bisuphide high catalytic property is with three-dimensional grapheme high-specific surface area, excellence
Electric conductivity combines, and this hybrid material is applied to dye cell electrode preparation carries out battery assembling acquisition efficient photoelectricity treater conversion
Efficiency.
Embodiment 2
Changing four thio ammonium molybdate quality in embodiment 1 into 10mg, remaining is all with embodiment 1, final obtained hybrid material mark
It is designated as MG-1
Embodiment 3
Changing four thio ammonium molybdate quality in embodiment 1 into 20mg, remaining is all with embodiment 1, final obtained hybrid material mark
It is designated as MG-2.
Claims (9)
1. three-dimensional grapheme load molybdenum disulfide nano sheet hybrid material preparation method and applications, it is characterised in that: with
Having three-dimensional porous structure graphene aerogel is skeleton, with four thio ammonium molybdate for raw material by chemical heat reducing process in three-dimensional
Growth in situ molybdenum disulfide nano sheet on graphene aerogel skeleton, forms Graphene molybdenum bisuphide heterojunction structure；Use and drip
Note method prepares Graphene/molybdenum disulfide nano sheet hybrid material to electrode, it is thus achieved that high efficiency dye sensitization solar battery.
2. method as claimed in claim 2, is characterised by, specifically comprises the following steps that
(1) being dissolved in deionized water by graphene oxide (GO), ultrasonic 5-6h makes its acquisition 1～2mg/ml oxidation stone that is uniformly dispersed
Ink alkene solution；
(2) in reductive glutathione in above-mentioned solution: graphene oxide mass ratio is the ratio of 2:1, reproducibility paddy is added
The sweet peptide of Guang, rear ultrasonic 0.5～1h, it is stirred continuously the homogeneous dispersion soln of acquisition；
(3) (2) step acquisition solution is placed in 85～90 DEG C of thermostat water baths, the most persistently 12-13h,
(4) the redox graphene hydrogel tert-butyl alcohol obtaining (3) step soaks 48h, and the tert-butyl alcohol is changed twice in centre,
After carry out lyophilization and prepare graphene aerogel, and carry out making annealing treatment 1～2h at argon and 800 DEG C of conditions；
(5) cotton-shaped graphene aerogel and four thio ammonium molybdate [(NH4) 2MoS4] that (4) obtain are taken in mass ratio for the ratio of 4:1
Example is scattered in ethanol solution (20%), carries out supersound process 2～3h after being stirred continuously；
(6) in (5) obtain dispersion liquid, add concentrated hydrochloric acid (37.5%), be stirred continuously, it is thus achieved that black mixed solution；
(7) above-mentioned dark solution is carried out vacuum filtration, and the black solid material deionized water obtaining sucking filtration is washed
Wash several times, after be scattered in deionized water, ultrasonic 4～5h, it is thus achieved that stable homogeneous solution；
(8) above-mentioned solution is carried out lyophilization and obtain Graphene/molybdenum trisulfide black solid powdered rubber；
(9) logical hydrogen in tube furnace, carries out above-mentioned black solid material making annealing treatment 2h, it is thus achieved that three under the conditions of 650 DEG C
Dimension Graphene/molybdenum disulfide nano sheet hybrid material.
Method the most according to claim 2, it is characterised in that step (2) described reducing agent use for reproducibility gluathione
Peptide, reductive glutathione is 2:1 with graphene oxide mass ratio.
Method the most according to claim 2, it is characterised in that with the tert-butyl alcohol, Graphene hydrogel is soaked described in step (4)
Bubble replaces wherein deionized water.
Method the most according to claim 2, it is characterised in that use cryodesiccated method to prepare stone described in step (4)
Ink alkene aeroge.
Method the most according to claim 2, it is characterised in that graphene aerogel and four thio ammonium molybdate matter in step (5)
Amount ratio is 4:1.
Method the most according to claim 2, it is characterised in that the reaction reagent used in step (6) is hydrochloric acid.
Method the most according to claim 2, it is characterised in that step (7) described vacuum filtration carries out solid-liquid separation, go from
Sub-water is washed.
Method the most according to claim 2, it is characterised in that be passed through hydrogen at 650 DEG C described in step (8) and reduce.
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