CN110280232A - A kind of preparation method of richness defect metal oxygen (sulphur) compound/graphene oxide composite material - Google Patents
A kind of preparation method of richness defect metal oxygen (sulphur) compound/graphene oxide composite material Download PDFInfo
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- CN110280232A CN110280232A CN201910414165.6A CN201910414165A CN110280232A CN 110280232 A CN110280232 A CN 110280232A CN 201910414165 A CN201910414165 A CN 201910414165A CN 110280232 A CN110280232 A CN 110280232A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 230000007547 defect Effects 0.000 title claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 10
- 239000002184 metal Substances 0.000 title claims abstract description 10
- -1 oxygen (sulphur) compound Chemical class 0.000 title claims abstract description 8
- 239000002131 composite material Substances 0.000 title claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 21
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 16
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 229910052961 molybdenite Inorganic materials 0.000 claims description 2
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 2
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 150000003839 salts Chemical group 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 7
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 238000004146 energy storage Methods 0.000 abstract description 5
- 230000001747 exhibiting effect Effects 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract description 2
- 238000003487 electrochemical reaction Methods 0.000 abstract description 2
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 239000011232 storage material Substances 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 12
- 239000004065 semiconductor Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 5
- 239000011787 zinc oxide Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000013019 agitation Methods 0.000 description 4
- 229960000935 dehydrated alcohol Drugs 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000011888 foil Substances 0.000 description 4
- RRMGGYGDQCMPKP-UHFFFAOYSA-N gold lithium Chemical compound [Li].[Au] RRMGGYGDQCMPKP-UHFFFAOYSA-N 0.000 description 4
- 229910003002 lithium salt Inorganic materials 0.000 description 4
- 159000000002 lithium salts Chemical class 0.000 description 4
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 4
- 230000001376 precipitating effect Effects 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229910052976 metal sulfide Inorganic materials 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 229910001868 water Inorganic materials 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000002305 electric material Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 210000004709 eyebrow Anatomy 0.000 description 1
- 210000000720 eyelash Anatomy 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/28—Molybdenum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B01J35/39—
Abstract
The present invention provides a kind of preparation method of rich defect metal oxygen (sulphur) compound/graphene oxide composite material.Metal lithium sheet, graphene oxide colloidal sol and selected oxide or sulfide are stirred evenly in the liquid phase, the composite material of certain defect concentration can be obtained after washing is dry.This method whipping step carries out under the anhydrous environment of anaerobic, and excessive hydrochloric acid is added to remove residual lithium piece after abundant reaction.The material that the present invention is prepared has exhibiting high surface defect, may advantageously facilitate the progress of photochemistry and electrochemical reaction；With graphene oxide it is compound can substantially extend light abstraction width, increasing specific surface area, improve conductive capability, to improve the photochemistry and chemical property of oxygen (sulphur) compound material.This method carries out at room temperature, easy to operate, low in cost, provides a kind of new thinking for the preparation of photochemical catalyst and energy storage material.
Description
Technical field
The invention belongs to technical field of nano material, in particular to a kind of rich defect metal oxygen (sulphur) compound/graphite oxide
The preparation method of alkene composite material.
Background technique
Environment and energy problem have caused whole world extensive concern, and the development for seeking new cleaning fuel and energy storage technology is compeled
In the eyebrows and eyelashes.Semiconductor material uses very extensive, especially many transition metal oxides and its sulfide, such as titanium dioxide wherein
Titanium (TiO2), molybdenum sulfide (MoS2), zinc oxide (ZnO) and molybdenum trioxide (MoO3) etc., they are the extensive semiconductors of research in recent years
Material, they all have the characteristics that chemical property is stable, cheap, abundance and prepares relatively simple at a low price, are outstanding light
Electric material.However, wider forbidden bandwidth limits the carrier transport and separating capacity of these materials, Carrier recombination rate also by
It is influenced.Therefore, by adjusting their forbidden bandwidth, improve its carrier transport and separating capacity, improve its light absorption energy
Power, and then it is particularly important to improve photocatalysis performance.Metal oxide and sulfide are the main forces of the energy storage material in addition to carbon material
Army, for semiconductor material, poorly conductive and ionic diffusion coefficient coefficient it is low be its energy-storage property limiting factor, from this
The energy-storage property that two aspects improve semiconductor material is also even more important.
On the other hand on the one hand electric conductivity that surface defect is conducive to improve material is Active sites, is conducive to promote
The progress of entering light chemistry and electrochemical reaction.Importantly, the ratio table of the excellent electricity of graphene, mechanical property and its super large
Area, and semiconductor material is compound greatly improves its electrochemistry and optical property.The unique gauffer pattern of graphene can be effective
Increase specific surface area, improves the adsorption capacity of material surface；Graphene has higher conductivity, for improving leading for compound
Electric energy power has great role, to improve its chemical property, graphene oxide can be used as the gatherer and transmitter of electronics,
Promote the migration of electronics to reduce the probability of recombination of carrier；Also, the chemical action between semiconductor and graphene oxide
Doping chemical bond can be formed, to extend the light abstraction width of catalysis material.It is existing to oxide and sulfide at present
The method for carrying out defect regulation mainly under the high temperature conditions restores it, manufacturing conditions are more harsh and preparation cost compared with
It is high.In addition, by graphene oxide auxiliary preparation there is the method for the semiconductor material of exhibiting high surface defect not report also.Pass through
Solution at room temperature method is to TiO2、MoS2, ZnO and MoO3Several difference nano materials are handled, and exhibiting high surface defect are introduced, into one
Step is compound with graphene oxide, can reduce the complexity of expensive cost and preparation condition needed for preparing material, and can be effective
Prepare the semiconductor material with excellent optical, chemical property in ground.
Summary of the invention
The present invention is directed to propose a kind of simple and effective oxygen (sulphur) compound and graphene oxide with vacancy are compound
Preparation method.We by stirring metal lithium sheet, graphene oxide colloidal sol and selected oxide or sulfide in the liquid phase
It is even, the composite material of certain defect concentration is obtained, this method carries out at room temperature, and it is easy to operate, low in cost, and pass through the party
The material of method preparation has excellent absorbing properties and chemical property.
The metal oxide and sulfide include TiO2、MoS2, ZnO and MoO3Deng.Due to experimentation and method one
It causes, with TiO2For, the specific steps are as follows:
(1) TiO that 100~600mg is dry2Nano particle pours into beaker, and addition 20~40ml EDA and 1~
Magneton is added in the graphene oxide gel of 3mL.
(2) 12~36mg metallic lithium foil is dissolved in and is added in above-mentioned solution, seal simultaneously magnetic agitation.
(3) sufficiently after reaction, hydrochloric acid stirring is gradually added dropwise, extinguishes excessive lithium piece, and forms lithium salts to remove residual lithium gold
Belong to.
(4) precipitating obtained after reaction is washed with deionized water and dehydrated alcohol, is then freeze-dried.
The TiO being added in the step (1)2Nano particle is 100~600mg, and anatase crystal, purity is
99.9%, EDA additional amount are 20mL, graphene oxide gel is 1~3mL, concentration 1wt.%.
The quality of lithium metal be added is 12~36mg in the step (2), and mixing time is 24 hours, and the process must
It must be carried out in the glove box of no water oxygen environment, avoid the reaction between lithium metal and water, oxygen.
Concentration of hydrochloric acid be added is 36%~38% in the step (3), and hydrochloric acid is added excessively, until not having reaction to be
Only, it stirs 3 hours.
Drying condition is vacuum freezedrying in affiliated step (4), and temperature is -40 DEG C, the time 24 hours or more.
The processing method is equally applicable to MoS2, ZnO and MoO3Equal materials.This method operating procedure is extremely simple, at low cost
Honest and clean, the material band gap width being prepared narrows, and is conducive to promote its absorbing properties, and defect density improves, and is conducive to mention
High photocatalysis performance.This method provides a kind of new thinking for the preparation of photochemical catalyst.
Detailed description of the invention
Fig. 1 is oxide and sulfide optical photograph figure before and after the processing.
Fig. 2 is TiO before and after the processing2Light absorption comparison diagram.
Fig. 3 is transmission electron microscope (TEM) figure: (a) TiO2(b)ZnO(c)MoO3。
Fig. 4 is MoO after processing3XPS figure.
Fig. 5 is the cycle performance of lithium ion battery figure of titanium oxide (anatase) before and after the processing, circulating ratio 5C.
Specific embodiment
Embodiment 1
It is proposed by the present invention to prepare lithium reduction GO@MoS2Material can be implemented by following method, specific preparation method
Include the following steps:
(1) MoS that 100~600mg is dry2Nano particle pours into beaker, and addition 20~40ml EDA and 1~
Magneton is added in the graphene oxide gel of 3mL.
(2) 12~36mg metallic lithium foils, which are dissolved in, to be added in above-mentioned solution, sealer and magnetic agitation.
(3) sufficiently after reaction, hydrochloric acid stirring is gradually added dropwise, extinguishes excessive lithium piece, and forms lithium salts to remove residual lithium gold
Belong to.
(4) precipitating obtained after reaction is washed with deionized water and dehydrated alcohol, is then freeze-dried.
Embodiment 2
The lithium reduction GO@ZnO material proposed by the present invention for preparing can be implemented by following method, specific preparation method packet
Include following steps:
(1) the dry ZnO nano particle of 100~600mg is poured into beaker, and 20~40ml EDA and 1~3mL is added
Graphene oxide gel, be added magneton.
(2) 12~36mg metallic lithium foils, which are dissolved in, to be added in above-mentioned solution, sealer and magnetic agitation.
(3) sufficiently after reaction, hydrochloric acid stirring is gradually added dropwise, extinguishes excessive lithium piece, and forms lithium salts to remove residual lithium gold
Belong to.
(4) precipitating obtained after reaction is washed with deionized water and dehydrated alcohol, is then freeze-dried.
Embodiment 3
It is proposed by the present invention to prepare lithium reduction GO@MoO3Material can be implemented by following method, specific preparation method
Include the following steps:
(1) MoO that 100~600mg is dry3Nano particle pours into beaker, and addition 20~40ml EDA and 1~
Magneton is added in the graphene oxide gel of 3mL.
(2) 12~36mg metallic lithium foils, which are dissolved in, to be added in above-mentioned solution, sealer and magnetic agitation.
(3) sufficiently after reaction, hydrochloric acid stirring is gradually added dropwise, extinguishes excessive lithium piece, and forms lithium salts to remove residual lithium gold
Belong to.
(4) precipitating obtained after reaction is washed with deionized water and dehydrated alcohol, is then freeze-dried.
Claims (6)
1. a kind of preparation method of richness defect metal oxygen (sulphur) compound/graphene oxide composite material, it is characterised in that: by metal
Lithium piece, graphene oxide gel and metal target oxygen (sulphur) compound are added to ethylenediamine (EDA) solution, carry out under normal temperature conditions
Stirring.After sufficiently reacting, hydrochloric acid is added dropwise and stirs.Finally, the product obtained after cleaning is freeze-dried.
2. preparation method according to claim 1, it is characterised in that: TiO2Dosage be 100~600mg, the dosage of EDA
For 20~40ml, graphene oxide gel concentration is 1wt%, and dosage is 1~3mL, and whipping step is in the environment of anhydrous and oxygen-free
It carries out.
3. preparation method according to claim 1, it is characterised in that: the dosage of metal lithium sheet is 12~36mg.
4. preparation method according to claim 1, it is characterised in that: solvent for use is salt in removal residual lithium piece step
Acid, hydrochloric acid addition needs excess, until not having reaction.
5. preparation method according to claim 1, it is characterised in that: drying condition is vacuum freezedrying, drying time
At 24 hours or more.
6. according to the method described in claim 1, this method is applicable not only to TiO2Material, equally applicable ZnO and MoO3Deng oxidation
Object, it may also be used for MoS2Sulfides are to introduce sulphur vacancy.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910414165.6A CN110280232A (en) | 2019-05-17 | 2019-05-17 | A kind of preparation method of richness defect metal oxygen (sulphur) compound/graphene oxide composite material |
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| CN201910414165.6A CN110280232A (en) | 2019-05-17 | 2019-05-17 | A kind of preparation method of richness defect metal oxygen (sulphur) compound/graphene oxide composite material |
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| CN110280232A true CN110280232A (en) | 2019-09-27 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111389417A (en) * | 2020-03-24 | 2020-07-10 | 武汉理工大学 | Sulfur-rich vacancy bismuth sulfide nanowire and preparation method and application thereof |
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|---|---|---|---|---|
| CN104069807A (en) * | 2014-06-19 | 2014-10-01 | 北京师范大学 | Preparation method and application of ZnO nano particle/graphene oxide composite material |
| US20160355405A1 (en) * | 2015-06-02 | 2016-12-08 | Korea Advanced Institute Of Science And Technology | Method of fabricating array of nanoparticle clusters using thermal transformation of sublimable liquid crystal film |
| CN107342405A (en) * | 2017-06-14 | 2017-11-10 | 三峡大学 | A kind of MoS2‑xOx/ carbon negative pole material and preparation method thereof |
-
2019
- 2019-05-17 CN CN201910414165.6A patent/CN110280232A/en active Pending
Patent Citations (3)
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| CN104069807A (en) * | 2014-06-19 | 2014-10-01 | 北京师范大学 | Preparation method and application of ZnO nano particle/graphene oxide composite material |
| US20160355405A1 (en) * | 2015-06-02 | 2016-12-08 | Korea Advanced Institute Of Science And Technology | Method of fabricating array of nanoparticle clusters using thermal transformation of sublimable liquid crystal film |
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| MING MA ET AL.: ""Dual Oxygen and Tungsten Vacancies on a WO3 Photoanode for Enhanced Water Oxidation"", 《ANGEWANDTE CHEMIE INTERNATIONAL EDITION》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111389417A (en) * | 2020-03-24 | 2020-07-10 | 武汉理工大学 | Sulfur-rich vacancy bismuth sulfide nanowire and preparation method and application thereof |
| CN111389417B (en) * | 2020-03-24 | 2021-06-08 | 武汉理工大学 | Sulfur-rich vacancy bismuth sulfide nanowire and preparation method and application thereof |
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Application publication date: 20190927 |