CN105819519A - Preparation method of layered MoS2-Fe3O4 nano composite material - Google Patents

Preparation method of layered MoS2-Fe3O4 nano composite material Download PDF

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CN105819519A
CN105819519A CN201610144424.4A CN201610144424A CN105819519A CN 105819519 A CN105819519 A CN 105819519A CN 201610144424 A CN201610144424 A CN 201610144424A CN 105819519 A CN105819519 A CN 105819519A
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preparation
powder
molybdenum disulfide
solution
layered
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CN105819519B (en
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胡平
王快社
杨帆
胡卜亮
宋瑞
陈震宇
李秦伟
戴晓庆
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Xian University of Architecture and Technology
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    • C01G49/00—Compounds of iron
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    • C01G49/08—Ferroso-ferric oxide (Fe3O4)
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
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    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

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Abstract

The invention provides a preparation method of a layered MoS2-Fe3O4 nano composite material. The preparation method comprises the following steps: adding molybdenum disulfide powder into a layered solution to carry out layering reactions, after reactions, filtering the solution, drying to obtain layered molybdenum disulfide powder; mixing ferric nitrate and citric acid, adding the mixture into water to carry out chelating reactions so as to obtain a yellow sol solution; adding the layered molybdenum disulfide powder into the yellow sol solution, mixing and stirring to obtain a mixed gel solution; drying to obtain dry gel, grinding dry gel to obtain dry gel powder; mixing dry gel powder with a blasting agent to carry out explosive reactions, cooling to the room temperature, and taking out the explosive reaction products, namely the layered MoS2-Fe3O4 nano composite material. The sol-gel method and the explosive high temperature impact technology are combined; the layered molybdenum disulfide and sol are fused; the rapid reduction of Fe3O4 and peeling of MoS2 can be finished in one step; and the layered MoS2-Fe3O4 nano composite material is prepared successfully.

Description

A kind of stratiform MoS2-Fe3O4The preparation method of nano composite material
Technical field
The invention belongs to metal molybdenum technical field, relate to molybdenum bisuphide composite, be specifically related to a kind of layer Shape MoS2-Fe3O4The preparation method of nano composite material.
Background technology
Class Graphene molybdenum bisuphide (the Graphene-like MoS being made up of monolayer or few layer molybdenum bisuphide2) A kind of New Two Dimensional (2D) lamellar compound with similar graphene-structured and performance, in recent years with The physics of its uniqueness, chemical property and become emerging study hotspot.Class Graphene molybdenum bisuphide is by six The two dimension with " sandwich " layer structure of the single or multiple lift molybdenum bisuphide composition of prismatic crystal system is brilliant Body material, monolayer molybdenum bisuphide is made up of three layers of atomic layer, and middle one layer is molybdenum atom layer, upper and lower two-layer Being sulphur atom layer, molybdenum atom layer is formed class " sandwich " structure folded by two-layer sulphur atom layer, molybdenum is former Son is combined formation two-dimensional atomic crystal with sulphur atom with covalent bond；Multilamellar molybdenum bisuphide is by some monolayer two sulfur Changing molybdenum composition, be usually no more than five layers, there is weak Van der Waals force in interlayer, interlamellar spacing is about 0.65nm.
As the two-dimensional layer nano material that a class is important, monolayer or few layer molybdenum bisuphide with " the three of its uniqueness Mingzhi is sandwich " layer structure is in the application of the various fields such as lubricant, catalysis, energy storage, composite Extensively.Compared to zero band gap of Graphene, there is regulatable band gap in class Graphene molybdenum bisuphide, Brighter prospect is had at field of photoelectric devices；Compared to the said three-dimensional body phase structure of silicon materials, class graphite Alkene molybdenum bisuphide has the two-dimensional layered structure of nanoscale, can be used to manufacture quasiconductor or specification is less, The higher electronic chip of efficiency, will be used widely in fields such as follow-on nano-electric devices.
Although platelike molybdenumdisulfide has good greasy property and photoelectric properties, but it is in all many-sides Performance need to be further improved, by molybdenum bisuphide with other organic or inorganic microgranule compound use, utilize Their cooperative effect, is an up one of method of molybdenum bisuphide performance.Such as patent of invention CN201410369695 discloses a kind of molybdenum bisuphide-titanium dioxide compound and preparation method thereof, utilizes There is collaborative lubrication and concerted catalysis effect in titanium dioxide and molybdenum bisuphide, synthesizes curing by chemical method Molybdenum-titanium dioxide compound is the effective way improving molybdenum bisuphide with the lubrication of titanium dioxide with catalytic performance One of footpath；Patent of invention CN201510149438 discloses the graphite of a kind of monolayer curing molybdenum sheet that adulterates The preparation method of alkene laminated film, can improve composite by Graphene with the compound of molybdenum disulfide nano sheet Electric conductivity, strengthen the transmission of electronics in electrochemical electrode reaction and catalytic reaction process, thus improve The chemical property of composite and catalytic performance；Patent of invention CN201510349912 discloses one Molybdenum bisuphide-carbon composite and preparation method thereof, uses cheap silica dioxide granule and glucose As template and base material, it is prepared for being applied to molybdenum bisuphide lithium cell negative pole material molybdenum bisuphide lamella-carbon Hollow ball nano composite material, this structural composite material is conducive to the stability of holding electrode, Er Qieke To shorten the transmission range of lithium ion, the beneficially lifting of high rate performance.
Although molybdenum bisuphide composite disclosed above in greasy property and photoelectric properties to curing The performance of molybdenum stratified material has the biggest lifting, but for magnetic steering and adsorbing domain performance boost not There is the effective solution of proposition.
Compound by with magnetic medium, as with Fe3O4Functionalization is combined, and obtains the molybdenum bisuphide of functionalization Stratified material, can effectively increase its saturation magnetization, and make it have magnetic steering performance, biofacies Capacitive and strong adsorptivity, it is possible to apply to living things catalysis, drug targeting, environmental renovation and sea water light The fields such as change, are greatly expanded the range of application of class Graphene molybdenum bisuphide.
Patent of invention CN201210524859 discloses a kind of synthesis MoS2-Fe3O4Nano composite material Preparation method, with Fe3O4Nano-particle is raw material, distribute it in deionized water and add sodium molybdate, Sodium chloride, sodium rhodanate and Surfactant CTAB, react 6-10h, clearly in stainless steel cauldron Wash and obtain MoS after drying2The Fe of cladding3O4Nano-particle.Although the method uses hydro-thermal method to prepare MoS2-Fe3O4Nano composite material, but its preparation flow is complicated, and energy consumption is big, is not suitable for industrialized production, And its product structure is MoS2The Fe of cladding3O4Nano-particle, and in adsorbing domain and photocatalysis field Typically require large-area stratiform MoS2Composite, with Fe3O4Fe is needed after nano-particles reinforcement3O4 Nano-particle is uniformly attached on its lamella, and with its functionalization, obtain modification stratiform MoS2-Fe3O4 Nano composite material.It addition, MoS2The number of plies of stratified material is the fewest, and its band gap is the biggest, electron transfer Efficiency is the highest, and photoelectric properties are the best.Therefore, explore one and prepare few shape MoS layer by layer2-Fe3O4Nanometer is multiple The simple and easy method of condensation material is the most necessary.
Summary of the invention
Based on problems of the prior art, the present invention proposes a kind of stratiform MoS2-Fe3O4Nanometer is multiple Condensation material and preparation method thereof, it is thus achieved that there is stratiform MoS of nanoscale, superior performance2-Fe3O4Nanometer Composite, solves existing MoS2-Fe3O4Composite preparation flow is complicated, and energy consumption is big, is not suitable for Industrialized production, and granular composite material granule technology of poor performance in terms of absorption and photocatalysis asks Topic.
It should be noted that stratiform MoS in the application2-Fe3O4MoS in nano composite material2It is single Layer or few layer MoS2Nano material, described few layer refers to 2 layers to 5 layers.
In order to solve above-mentioned technical problem, the application adopts the following technical scheme that and is achieved:
A kind of stratiform MoS2-Fe3O4The preparation method of nano composite material, the method comprises the following steps:
Step one, adds molybdenum disulfide powder and carries out layering reaction, mistake after having reacted in layering solution Filter, dries, and obtains being layered molybdenum disulfide powder；
Step 2, is added to the water after being mixed with citric acid by ferric nitrate, carries out chelatropic reaction, obtains yellow Sol solution；
Step 3, adds layering molybdenum disulfide powder in yellow sol solution, is mixed after stirring mixing Close gel solution, obtain xerogel after drying, grind and obtain dry gel powder；
Step 4, mixes dry gel powder and burster, carries out explosive reaction, take after being cooled to room temperature Go out explosive reaction product, i.e. obtain stratiform MoS2-Fe3O4Nano composite material.
The present invention also has a following distinguishing feature:
Described layering solution is the ethanol solution of aromatic thioether；Described burster is picric acid.
Described aromatic thioether is polyphenylene sulfide or aromatic diamine monomer thioether, the second of aromatic thioether The mass concentration of alcoholic solution is 10%～60%.
The detailed process of described layering reaction is: molybdenum disulfide powder is ground to 200 mesh and sieves, will Molybdenum disulfide powder adds in the ethanol solution of aromatic thioether, is heated to 30～70 DEG C and stirs 5～12 H, filters, and dries, and obtains being layered molybdenum disulfide powder.
Described molybdenum disulfide powder is 1:(10～40 with the mass ratio of aromatic thioether).
The detailed process of chelatropic reaction is: be added to the water after being mixed with citric acid by ferric nitrate, adds ammonia The pH of regulation reaction system, 6.5～7.5, stirs chelatropic reaction 2～6h at 45～80 DEG C, obtains Huang Color sol solution.
In step 2, described ferric nitrate, citric acid are 1:(0.8～1.2 with distilled water in mass ratio): (1～3) prepare.
The detailed process of step 3 is: add layering molybdenum disulfide powder, stirring in yellow sol solution 1～3h, obtain mixed gel solution, after being dried 6～15h at 100～130 DEG C, obtain xerogel, will Xerogel is ground to 200 mesh and sieves and obtain dry gel powder.
In step 3, after described layering molybdenum disulfide powder adds sol solution, shared mass concentration is 2%～25%.
In step 4, the detailed process of described explosive reaction is: by dry gel powder with picric acid by matter Amount is than 1:(0.5～3) mix homogeneously, load in autoclave, by autoclave evacuation and be passed through Argon, is heated to 350～600 DEG C and explodes, and takes out explosive reaction product after cooling to room temperature with the furnace, I.e. obtain monolayer or few layer molybdenum disulfide nano material.
Compared with prior art, useful has the technical effect that the present invention
(I) present invention utilizes the close sulphur property of aromatic thioether, reduces the layer of molybdenum bisuphide material powder Between Van der Waals force, successfully it is carried out delamination in conjunction with blast impulse.
(II) present invention by sol-gel process with blast high temperature impact is combined, will be layered molybdenum bisuphide and After colloidal sol merges, only i.e. complete Fe with a step blast3O4Rapidly reduction and MoS2Stripping, success It is prepared for stratiform MoS2-Fe3O4Nano composite material.
(III) product prepared by the present invention is platelike molybdenumdisulfide and the Fe with high carrier mobility3O4 The nano material of nano-particles reinforcement, and Fe3O4Nano-particle is uniformly attached to monolayer molybdenum bisuphide lamella On, there is the fields such as preferable magnetic steering performance, drug targeting, environmental renovation and desalinization, It is greatly expanded the range of application of molybdenum bisuphide.
(IV) present invention prepares stratiform MoS2-Fe3O4Nano composite material, simple to operate, it is not necessary to multiple Miscellaneous and loaded down with trivial details preparation facilities, preparation efficiency is high, and yield is big, is suitable for industrialized production.
Accompanying drawing explanation
Fig. 1 is prepared stratiform MoS in embodiment 12-Fe3O4Nano composite material Raman collection of illustrative plates.
Fig. 2 is prepared stratiform MoS in embodiment 12-Fe3O4Nano composite material TEM is schemed.
Fig. 3 is MoS prepared in comparative example 12-Fe3O4The Raman collection of illustrative plates of composite.
Fig. 4 is MoS prepared in comparative example 12-Fe3O4The TEM figure of composite.
Below in conjunction with drawings and Examples, the particular content of the present invention is described in more detail.
Detailed description of the invention
Defer to technique scheme, the specific embodiment of the present invention given below, it should be noted that this The bright specific examples below that is not limited to, all equivalents done on the basis of technical scheme are equal Fall into protection scope of the present invention.Below in conjunction with embodiment, the present invention is described in further details.
It should be noted that ferric nitrate described herein i.e. Fe (NO3)3·9H2O。
Embodiment 1:
The present embodiment provides a kind of stratiform MoS2-Fe3O4The preparation method of nano composite material, the method has Body comprises the following steps:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 mesh and sieves, and being added into mass concentration is 10%, in the ethanol solution containing 100g polyphenylene sulfide, heating in water bath to 30 DEG C also stirs 12h, filters And filter cake is dried, it is ground to 200 mesh and sieves, obtain 3g and be layered molybdenum disulfide powder.
Step 2, takes 100g Fe (NO3)3·9H2O with 80g citric acid adds 100g distillation after mixing In water, adding ammonia regulation pH value is 6.5, obtains yellow sol molten at 45 DEG C after stirring chelating 6h Liquid.
Step 3, takes 150g sol solution and adds 3g layering molybdenum disulfide powder wherein, continuing to exist Stir 1h at 45 DEG C, obtain xerogel after mixed sols is dried 6h at 100 DEG C, and ground Sieve to 200 mesh and obtain dry gel powder.
Step 4, takes 3g dry gel powder and mixs homogeneously with 1.5g picric acid in loading autoclave, Evacuation is also passed through argon, reactor is heated to 500 DEG C and explodes, and takes out after cooling to room temperature with the furnace Explosive reaction thing, rinses repeatedly with deionized water, i.e. obtains stratiform MoS after filtration drying2-Fe3O4Nanometer Composite.
Stratiform MoS prepared by the present embodiment2-Fe3O4Nano composite material Raman collection of illustrative plates such as Fig. 1 institute Showing, high-resolution TEM is schemed as shown in Figure 2.
E in Raman collection of illustrative plates in Fig. 12g 1With Ag 1Value is respectively 381.85 and 404.71, and displacement difference is 22.86, belong to few Rotating fields MoS2, show MoS in sample prepared by the present embodiment2For stratified material.
Fig. 2 middle high-resolution TEM figure is shown as MoS2Laminar nano chip architecture and marginal fold corrugation shape Looks, and Fe3O4Nano-particle is uniformly attached to stratiform MoS2Nanometer sheet surface.
Comprehensive accompanying drawing can show that the sample prepared by the present embodiment is stratiform MoS2-Fe3O4Nano combined material Material.
Embodiment 2:
The present embodiment provides a kind of stratiform MoS2-Fe3O4The preparation method of nano composite material, the method has Body comprises the following steps:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 mesh and sieves, and being added into mass concentration is 20%, in the ethanol solution containing 200g polyphenylene sulfide, heating in water bath to 70 DEG C also stirs 5h, filters And filter cake is dried, it is ground to 200 mesh and sieves, obtain 3.2g and be layered molybdenum disulfide powder.
Step 2, takes 100g Fe (NO3)3·9H2O with 100g citric acid adds 150g distillation after mixing In water, adding ammonia regulation pH value is 7, obtains yellow sol solution at 50 DEG C after stirring chelating 5h.
Step 3, takes 64g sol solution and adds 3.2g layering molybdenum disulfide powder wherein, continuing to exist Stir 1.5h at 50 DEG C, obtain xerogel after colloidal sol is dried 7h at 105 DEG C, and be ground to 200 mesh sieve and obtain dry gel powder.
Step 4, takes 3g dry gel powder and mixs homogeneously with 3g picric acid in loading autoclave, take out Vacuum is also passed through argon, reactor is heated to 480 DEG C and explodes, take out quick-fried after cooling to room temperature with the furnace Fried reactant, repeatedly rinses with deionized water, i.e. obtains stratiform MoS after filtration drying2-Fe3O4Nanometer is multiple Condensation material.
The present embodiment products therefrom stratiform MoS2-Fe3O4The character of nano composite material is basic with embodiment 1 Identical.
Embodiment 3:
The present embodiment provides a kind of stratiform MoS2-Fe3O4The preparation method of nano composite material, the method has Body comprises the following steps:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 mesh and sieves, and being added into mass concentration is 30%, in the ethanol solution containing 300g polyphenylene sulfide, heating in water bath to 40 DEG C also stirs 8h, filters And filter cake is dried, it is ground to 200 mesh and sieves, obtain 2.8g and be layered molybdenum disulfide powder.
Step 2, takes 100g Fe (NO3)3·9H2O with 120g citric acid adds 200g distillation after mixing In water, adding ammonia regulation pH value is 7.5, obtains yellow sol molten at 60 DEG C after stirring chelating 4h Liquid.
Step 3, takes 28g sol solution and adds 2.8g layering molybdenum disulfide powder wherein, continuing to exist Stir 2h at 60 DEG C, obtain xerogel after colloidal sol is dried 9h at 110 DEG C, and be ground to 200 Mesh sieves and obtains dry gel powder.
Step 4, takes 3g dry gel powder and mixs homogeneously with 4.5g picric acid in loading autoclave, Evacuation is also passed through argon, reactor is heated to 450 DEG C and explodes, and takes out after cooling to room temperature with the furnace Explosive reaction thing, rinses repeatedly with deionized water, i.e. obtains stratiform MoS after filtration drying2-Fe3O4Nanometer Composite.
The present embodiment products therefrom stratiform MoS2-Fe3O4The character of nano composite material is basic with embodiment 1 Identical.
Embodiment 4:
The present embodiment provides a kind of stratiform MoS2-Fe3O4The preparation method of nano composite material, the method has Body comprises the following steps:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 mesh and sieves, and being added into mass concentration is 40%, in the ethanol solution containing 400g aromatic diamine monomer thioether, heating in water bath to 50 DEG C also stirs 10h, filters and is dried by filter cake, be ground to 200 mesh and sieve, and obtains 3.4g and is layered molybdenum disulfide powder.
Step 2, takes 100g Fe (NO3)3·9H2O with 120g citric acid adds 250g distillation after mixing In water, adding ammonia regulation pH value is 7.5, obtains yellow sol molten at 65 DEG C after stirring chelating 3h Liquid.
Step 3, takes 22g sol solution and adds 3.4g layering molybdenum disulfide powder wherein, continuing to exist Stir 2.5h at 65 DEG C, obtain xerogel after colloidal sol is dried 11h at 115 DEG C, and be ground to 200 mesh sieve and obtain dry gel powder.
Step 4, takes 3g dry gel powder and mixs homogeneously with 6g picric acid in loading autoclave, take out Vacuum is also passed through argon, reactor is heated to 550 DEG C and explodes, take out quick-fried after cooling to room temperature with the furnace Fried reactant, repeatedly rinses with deionized water, i.e. obtains stratiform MoS after filtration drying2-Fe3O4Nanometer is multiple Condensation material.
The present embodiment products therefrom stratiform MoS2-Fe3O4The character of nano composite material is basic with embodiment 1 Identical.
Embodiment 5:
The present embodiment provides a kind of stratiform MoS2-Fe3O4The preparation method of nano composite material, the method has Body comprises the following steps:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 mesh and sieves, and being added into mass concentration is 60%, in the ethanol solution containing 300g aromatic diamine monomer thioether, heating in water bath to 60 DEG C also stirs 12h, obtains mixed liquor, filters and is dried by filter cake, is ground to 200 mesh and sieves, and obtains 3.1g layering Molybdenum disulfide powder.
Step 2, takes 100g Fe (NO3)3·9H2O with 100g citric acid adds 300g distillation after mixing In water, adding ammonia regulation pH value is 7, obtains yellow sol solution at 70 DEG C after stirring chelating 2h.
Step 3, takes 16g sol solution and adds 3.1g layering molybdenum disulfide powder wherein, continuing to exist Stir 3h at 70 DEG C, obtain xerogel after colloidal sol is dried 13h at 120 DEG C, and be ground to 200 Mesh sieves and obtains dry gel powder.
Step 4, takes 3g dry gel powder and mixs homogeneously with 7.5g picric acid in loading autoclave, Evacuation is also passed through argon, reactor is heated to 510 DEG C and explodes, and takes out after cooling to room temperature with the furnace Explosive reaction thing, rinses repeatedly with deionized water, i.e. obtains stratiform MoS after filtration drying2-Fe3O4Nanometer Composite.
The present embodiment products therefrom stratiform MoS2-Fe3O4The character of nano composite material is basic with embodiment 1 Identical.
Embodiment 6:
The present embodiment provides a kind of stratiform MoS2-Fe3O4The preparation method of nano composite material, the method has Body comprises the following steps:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 mesh and sieves, and being added into mass concentration is 50%, in the ethanol solution containing 200g aromatic diamine monomer thioether, heating in water bath to 45 DEG C also stirs 8h, filters and is dried by filter cake, be ground to 200 mesh and sieve, and obtains 2.9g and is layered molybdenum disulfide powder.
Step 2, takes 100g Fe (NO3)3·9H2O with 80g citric acid adds 180g distillation after mixing In water, adding ammonia regulation pH value is 7, obtains yellow sol solution at 80 DEG C after stirring chelating 4h.
Step 3, takes 12g sol solution and adds 2.9g layering molybdenum disulfide powder wherein, continuing to exist Stir 2h at 80 DEG C, obtain xerogel after colloidal sol is dried 15h at 110 DEG C, and be ground to 200 Mesh sieves and obtains dry gel powder.
Step 4, takes 3g dry gel powder and mixs homogeneously with 9g picric acid in loading autoclave, take out Vacuum is also passed through argon, reactor is heated to 500 DEG C and explodes, take out quick-fried after cooling to room temperature with the furnace Fried reactant, repeatedly rinses with deionized water, i.e. obtains stratiform MoS after filtration drying2-Fe3O4Nanometer is multiple Condensation material.
The present embodiment products therefrom stratiform MoS2-Fe3O4The character of nano composite material is basic with embodiment 1 Identical.
Comparative example 1:
This comparative example provides a kind of MoS2-Fe3O4The preparation method of composite, the method specifically include with Lower step:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 mesh and sieves, and being added into mass concentration is 5%, in the ethanol solution containing 50g aromatic diamine monomer thioether, heating in water bath to 25 DEG C also stirs 5 H, filters and is dried by filter cake, be ground to 200 mesh and sieve, obtain 3.2g molybdenum bisuphide pretreatment powder.
Step 2, takes 100g Fe (NO3)3·9H2O with 60g citric acid adds 80g distilled water after mixing In, adding ammonia regulation pH value is 6, obtains sol solution at 40 DEG C after stirring chelating 3h.
Step 3, takes 10g sol solution and adds 3.2g molybdenum bisuphide pretreatment powder wherein, continuing At 40 DEG C, stir 1h, obtain xerogel after colloidal sol is dried 8h at 100 DEG C, and be ground to 200 mesh sieve and obtain dry gel powder.
Step 4, takes 3g dry gel powder and mixs homogeneously with 1g picric acid in loading autoclave, take out Vacuum is also passed through argon, reactor is heated to 600 DEG C and explodes, take out quick-fried after cooling to room temperature with the furnace Fried reactant, repeatedly rinses with deionized water, i.e. obtains MoS after filtration drying2-Fe3O4Complex.
The MoS that this comparative example is prepared2-Fe3O4Composite carries out Raman spectrum analysis and TEM Analyze.
Raman spectrum is as it is shown on figure 3, its E2g 1With Ag 1Value is respectively 381.83 and 408.14, displacement Difference is 26.31, belongs to block structure MoS2；
TEM image as shown in Figure 4, illustrates this product MoS2Block is piled up, and presents multiple structure, and At MoS2Surface or surrounding do not find obvious Fe3O4Granule, is not belonging to monolayer or few layer MoS2Nanometer Composite.
Comparative example 2:
This comparative example provides a kind of MoS2-Fe3O4The preparation method of composite, the method specifically include with Lower step:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 mesh and sieves, and being added into mass concentration is 70%, in the ethanol solution containing 500g aromatic diamine monomer thioether, heating in water bath to 20 DEG C also stirs Mix 4h, filter and filter cake is dried, be ground to 200 mesh and sieve, obtain 3g molybdenum bisuphide pretreatment powder End.
Step 2, takes 100g Fe (NO3)3·9H2O with 40g citric acid adds 200g distillation after mixing In water, adding ammonia regulation pH value is 8, obtains sol solution at 90 DEG C after stirring chelating 1h.
Step 3, takes 300g sol solution and adds 3g molybdenum bisuphide pretreatment powder wherein, continuing At 90 DEG C, stir 2h, obtain xerogel after colloidal sol is dried 5h at 90 DEG C, and be ground to 200 mesh sieve and obtain dry gel powder.
Step 4, takes 3g dry gel powder and mixs homogeneously with 0.5g picric acid in loading autoclave, Evacuation is also passed through argon, reactor is heated to 650 DEG C and explodes, and takes out after cooling to room temperature with the furnace Explosive reaction thing, rinses repeatedly with deionized water, obtains MoS after filtration drying i.e.2-Fe3O4Complex.
The MoS that this comparative example prepares2-Fe3O4Composite block as comparative example 1 is piled up, and Fe3O4 Granule occurs in MoS2Block surface and surrounding, be not belonging to monolayer or few layer molybdenum disulfide nano composite wood Material.
Comparative example 3:
This comparative example provides a kind of MoS2-Fe3O4The preparation method of composite, the method specifically include with Lower step:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 mesh and sieves, and being added into mass concentration is 8%, in the ethanol solution containing 60g aromatic diamine monomer thioether, heating in water bath to 90 DEG C also stirs 5 H, filters and is dried by filter cake, be ground to 200 mesh and sieve, obtain 3.5g molybdenum bisuphide pretreatment powder.
Step 2, takes 100g Fe (NO3)3·9H2O with 150g citric acid adds 350g distillation after mixing In water, adding ammonia regulation pH value is 7, obtains sol solution at 60 DEG C after stirring chelating 8h.
Step 3, takes 100g sol solution and adds 3.5g molybdenum bisuphide pretreatment powder wherein, continuing Continue stirring 1h at 60 DEG C, obtain xerogel after colloidal sol is dried 4h at 140 DEG C, and ground Sieve to 200 mesh and obtain dry gel powder.
Step 4, takes 3g dry gel powder and mixs homogeneously with 1g picric acid in loading autoclave, take out Vacuum is also passed through argon, reactor is heated to 620 DEG C and explodes, take out quick-fried after cooling to room temperature with the furnace Fried reactant, obtains MoS2-Fe3O4Complex.
The MoS that this comparative example prepares2-Fe3O4Composite block as comparative example 1 is piled up, and Fe3O4 Granule occurs in MoS2Block surface and surrounding, be not belonging to monolayer or few layer molybdenum disulfide nano composite wood Material.

Claims (10)

1. the preparation method of a stratiform MoS2-Fe3O4 nano composite material, it is characterised in that: the party Method comprises the following steps:
Step one, adds molybdenum disulfide powder and carries out layering reaction, mistake after having reacted in layering solution Filter, dries, and obtains being layered molybdenum disulfide powder；
Step 2, is added to the water after being mixed with citric acid by ferric nitrate, carries out chelatropic reaction, obtains yellow Sol solution；
Step 3, adds layering molybdenum disulfide powder in yellow sol solution, is mixed after stirring mixing Close gel solution, obtain xerogel after drying, grind and obtain dry gel powder；
Step 4, mixes dry gel powder and burster, carries out explosive reaction, take after being cooled to room temperature Go out explosive reaction product, i.e. obtain stratiform MoS2-Fe3O4Nano composite material.
2. preparation method as claimed in claim 1, it is characterised in that: described layering solution is fragrance The ethanol solution of race's thioether；Described burster is picric acid.
3. preparation method as claimed in claim 2, it is characterised in that: described aromatic thioether is poly- Diphenyl sulfide or aromatic diamine monomer thioether, the mass concentration of the ethanol solution of aromatic thioether be 10%～ 60%.
4. preparation method as claimed in claim 2, it is characterised in that: in step one, described layering The detailed process of reaction is: molybdenum disulfide powder is ground to 200 mesh and sieves, added by molybdenum disulfide powder Enter in the ethanol solution of aromatic thioether, be heated to 30～70 DEG C and stir 5～12h, filtering, drying, Obtain being layered molybdenum disulfide powder.
5. preparation method as claimed in claim 2, it is characterised in that: in step one, two described sulfur The mass ratio changing molybdenum powder and aromatic thioether is 1:(10～40).
6. preparation method as claimed in claim 2, it is characterised in that: in step 2, chelatropic reaction Detailed process is: be added to the water after being mixed with citric acid by ferric nitrate, adds ammonia regulation reaction system PH, 6.5～7.5, stirs chelatropic reaction 2～6h at 45～80 DEG C, obtains yellow sol solution.
7. preparation method as claimed in claim 2, it is characterised in that: in step 2, described nitric acid Ferrum, citric acid and distilled water are 1:(0.8～1.2 in mass ratio): (1～3) prepare.
8. preparation method as claimed in claim 2, it is characterised in that: the detailed process of step 3 is: In yellow sol solution, add layering molybdenum disulfide powder, stir 1～3h, obtain mixed gel solution, Obtain xerogel after being dried 6～15h at 100～130 DEG C, xerogel is ground to 200 mesh and sieves To dry gel powder.
9. preparation method as claimed in claim 2, it is characterised in that: in step 3, described layering After molybdenum disulfide powder addition sol solution, shared mass concentration is 2%～25%.
10. preparation method as claimed in claim 2, it is characterised in that: in step 4, described is quick-fried The detailed process of fried reaction is: by dry gel powder and picric acid 1:(0.5 in mass ratio～3) mix homogeneously, Load in autoclave, by autoclave evacuation and be passed through argon, be heated to 350～600 DEG C and send out Raw blast, takes out explosive reaction product after cooling to room temperature with the furnace, i.e. obtains monolayer or few layer molybdenum bisuphide Nano material.
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