CN103613136A - Preparation method of square MoO3 nanosheet - Google Patents
Preparation method of square MoO3 nanosheet Download PDFInfo
- Publication number
- CN103613136A CN103613136A CN201310589644.4A CN201310589644A CN103613136A CN 103613136 A CN103613136 A CN 103613136A CN 201310589644 A CN201310589644 A CN 201310589644A CN 103613136 A CN103613136 A CN 103613136A
- Authority
- CN
- China
- Prior art keywords
- preparation
- directions
- source
- nanometer sheet
- nano material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a preparation method of a square MoO3 nanosheet. The preparation method is characterized by comprising the following steps: dissolving a molybdenum source, a sulfur source and a reducing agent into a solvent, centrifugally stirring to enable the molybdenum source, the sulfur source and the reducing agent to be uniformly dispersed into a solution, transferring the solution into a stainless steel reaction kettle, sealing, reacting at the constant temperature of 100-300 DEG C for 24h, then, cooling to the room temperature to obtain a reaction product, separating the reaction product, cleaning and drying to obtain a precursor MoS2; placing the MoS2 nano material into a tube furnace, preserving the constant temperature of 300-600 DEG C at the air or oxygen atmosphere for 24h, and annealing for 0.5-5h to obtain the square MoO3 nanosheet with the thickness of 100-150nm and the size of 1-2mum. The raw materials used in the method provided by the invention are easy to obtain and low in cost; the preparation method is simple in process, easy to control parameters as well as safe and environment friendly in production process and can be widely applied to the aspects such as air sensitivity, magnetism, lithium battery material and the like.
Description
Technical field
The present invention relates to nano magnetic material field, particularly, is a kind of MoO
3the preparation method of four directions nanometer sheet.
Background technology
Molybdic oxide is a kind of very potential semiconductor material, at aspects such as solar cell, photochemical catalysis, air-sensitive and magnetic, has important application.Particularly nano level molybdic oxide tool more has excellent reversible photochromism and higher optical contrast, its performance has potential using value at aspects such as information storage, image demonstration and light regulatings, the core material that can be used as the devices such as electrochromism, photochromic, intelligent camouflage, has wide using value in fields such as display equipment and military equipments.
In recent years, along with scientific and technical progress, constantly there are many novel molybdic oxide powder preparing methods.The at present existing multiple method of preparing powder, as the precipitator method, hydrothermal method, electrochemical deposition method, sputtering method, sol-gel method etc.Yet, for the regulation and control of molybdenum trioxide nano material morphology, be the focus of nano material study on the synthesis always.
Summary of the invention
The object of the present invention is to provide and a kind ofly using molybdenum disulfide nano material as presoma, by the synthetic MoO of low sintering mode
3the method of four directions nanometer sheet, with low cost, technique is simple and productive rate is high, synthesized MoO
3four directions nanometer sheet has better air-sensitive and chemical property.
Above-mentioned purpose is achieved by the following technical solution:
A preparation method for molybdic oxide four directions nanometer sheet, step is as follows:
(1) presoma MoS
2nano material preparation:
,Liu source, molybdenum source and reductive agent are dissolved in solvent, by centrifugal mixer, it are distributed in solution uniformly, move into stainless steel cauldron, sealing, after 100 ℃～300 ℃ reaction 24h of constant temperature, be cooled to room temperature, obtain reaction product, separated above-mentioned reaction product, washing, dry, obtains presoma MoS
2;
The ratio of the amount of substance in Yu Liu source, molybdenum source is 1:2-1:4; Molybdenum source is 1:1-1:3 with the ratio of the amount of substance of reductive agent;
Described molybdenum source is soluble molybdenum salt, as Sodium orthomolybdate, ammonium molybdate, hexacarbonylmolybdenum;
Sulphur source is dissolvable sulfide, as sodium sulphite, potassium sulphide, thiocarbamide;
Reductive agent is organic reducing agent, as, citric acid, xitix etc.;
Solvent is deionized water or ethanol;
(2) the synthetic MoO of aerobic annealing sintering
3four directions nanometer sheet:
By synthetic MoS
2nano material is placed in tube furnace, and in air or oxygen atmosphere, the 0.5～5h that anneals at 300 ℃～600 ℃ of glucose obtains MoO
3four directions nanometer sheet, thickness is greatly about 100nm, and size is in the cubic nanometer sheet of 1～2 μ m.
The cost of the inventive method is inexpensive, and production technique is simple and easy to control, and product rate is high, is applicable to large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is the MoO that the embodiment of the present invention 1 makes
3the XRD of four directions nanometer sheet, illustrates that XRD peak position is consistent with standard diffractogram (PDF No.35-0609), and product is mainly MoO
3four directions nanometer sheet;
Fig. 2 is the MoO that the embodiment of the present invention 1 makes
3four directions nanometer sheet field emission scanning electron microscope (SEM) photo, Fig. 2 a and 2b are the SEM photo of product different multiples, can clearly see that product is that thickness is approximately 200nm, the MoO of diameter 1～2 μ m from figure
3four directions nanometer sheet.
Fig. 3 is the MoO that the embodiment of the present invention 1 makes
3the transmission electron microscope (TEM figure) of four directions nanometer sheet, its result is consistent with SEM, further proves that product is MoO
3four directions nanometer sheet (unit scaling refers to 0.5nm).
Embodiment
By embodiment, further describe the present invention below, as known by the technical knowledge, the present invention also can describe by other the scheme that does not depart from the technology of the present invention feature, and therefore changes within the scope of the present invention all or that be equal in the scope of the invention are all included in the invention.
Embodiment 1:
0.44g Na
2mO
4, 0.6g Na
2s and 0.4g glucose sugar are dissolved in the deionized water of 60mL completely, continue to stir after 30min, mixed solution are transferred in the stainless steel cauldron of 100ml, are placed in vacuum drying oven in 180 ℃ of insulation 24h, are cooled to room temperature.Reaction product, after centrifugation, is used respectively deionized water and dehydrated alcohol repetitive scrubbing, last under vacuum condition 80 ℃ of dry 10h obtain the powder of grey black, i.e. presoma MoS
2nano material.By under 400 ℃ of conditions of above-mentioned product, the product powder that the 2h that anneals in tube furnace obtains black is MoO
3four directions nanometer sheet.
Embodiment 2:
0.44g Na
2mO
4, 0.6g Na
2s and 0.6g citric acid are dissolved in going in ethanol of 60mL completely, continue to stir after 30min, mixed solution are transferred in the stainless steel cauldron of 100ml, are placed in vacuum drying oven in 160 ℃ of insulation 24h, are cooled to room temperature.Reaction product, after centrifugation, is used respectively deionized water and dehydrated alcohol repetitive scrubbing, last under vacuum condition 80 ℃ of dry 10h obtain the powder of grey black, i.e. presoma MoS
2nano material.By under 450 ℃ of conditions of above-mentioned product, the product powder that the 1h that anneals in tube furnace obtains black is MoO
3four directions nanometer sheet, thickness is approximately 200nm, diameter 1～2 μ m.
The reagent different from embodiment 1 that embodiment 3-5 adopts and parameter are in Table 1.
Table 1
Claims (3)
1. a preparation method for molybdic oxide four directions nanometer sheet, is characterized in that step is as follows:
(1) presoma MoS
2nano material preparation:
,Liu source, molybdenum source and reductive agent are dissolved in solvent, by centrifugal mixer, it are distributed in solution uniformly, move into stainless steel cauldron, sealing, after 100 ℃～300 ℃ reaction 24h of constant temperature, be cooled to room temperature, obtain reaction product, reaction product isolated, washing, dry, obtains presoma MoS
2nano material;
(2) the synthetic MoO of aerobic annealing sintering
3four directions nanometer sheet:
By synthetic MoS
2nano material is placed in tube furnace, and in air or oxygen atmosphere, the 0.5～5h that anneals at 300 ℃～600 ℃ obtains MoO
3four directions nanometer sheet, thickness is at 100-150nm, size 1～2 μ m.
2. the preparation method of molybdic oxide according to claim 1 four directions nanometer sheet, it is characterized in that the molybdenum source described in step (1) be Sodium orthomolybdate, ammonium molybdate or hexacarbonylmolybdenum it; Sulphur source is sodium sulphite, potassium sulphide or thiocarbamide; Reductive agent is citric acid or xitix; Described solvent is deionized water, ethanol or ethylene glycol.
3. the preparation method of molybdic oxide according to claim 1 four directions nanometer sheet, is characterized in that the ratio of the amount of substance in described Yu Liu source, molybdenum source is 1:2-1:4; Molybdenum source is 1:1-1:3 with the ratio of the amount of substance of reductive agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310589644.4A CN103613136B (en) | 2013-11-21 | 2013-11-21 | A kind of preparation method of square MoO3 nanosheet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310589644.4A CN103613136B (en) | 2013-11-21 | 2013-11-21 | A kind of preparation method of square MoO3 nanosheet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103613136A true CN103613136A (en) | 2014-03-05 |
| CN103613136B CN103613136B (en) | 2015-09-16 |
Family
ID=50163866
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310589644.4A Active CN103613136B (en) | 2013-11-21 | 2013-11-21 | A kind of preparation method of square MoO3 nanosheet |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103613136B (en) |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104241624A (en) * | 2014-09-24 | 2014-12-24 | 南京大学 | Method for preparing anode material of molybdenum oxide lithium ion battery by controlling oxidation |
| CN104649323A (en) * | 2015-01-21 | 2015-05-27 | 济南大学 | Preparation method of strip-shaped molybdenum trioxide |
| CN104709943A (en) * | 2015-03-13 | 2015-06-17 | 济南大学 | Preparation method of molybdenum trioxide microsphere in three-dimensional hierarchical structure |
| CN105789030A (en) * | 2016-03-14 | 2016-07-20 | 暨南大学 | Preparation method of molybdenum trioxide two-dimensional atomic crystals with reduced layers |
| CN105944712A (en) * | 2016-05-23 | 2016-09-21 | 南京信息工程大学 | Preparation method of novel cerium sodium molybdate/molybdenum trioxide composite photocatalyst |
| CN106745262A (en) * | 2016-12-12 | 2017-05-31 | 郑州大学 | A kind of method for preparing amorphous oxide molybdenum nanometer sheet using the few layer molybdenum sulfide of oxidation |
| CN108279540A (en) * | 2018-02-01 | 2018-07-13 | 深圳市光羿科技有限公司 | A kind of inorganic, metal oxide ion storage layer, its cryogenic fluid processing method and purposes |
| CN108996549A (en) * | 2018-10-10 | 2018-12-14 | 金堆城钼业光明（山东）股份有限公司 | A kind of MoO3The network structure nanometer material and preparation method thereof of piece assembling |
| CN109205676A (en) * | 2018-08-30 | 2019-01-15 | 济南大学 | A kind of MoO3The electrostatic spinning synthetic method of laminated structure |
| CN110441380A (en) * | 2019-08-07 | 2019-11-12 | 暨南大学 | A kind of electrochemical sensor and its preparation method and application based on molecular engram electrode technology |
| CN110879238A (en) * | 2019-10-25 | 2020-03-13 | 东北大学 | Molybdenum trioxide nano-structure sensitive material, corresponding ammonia gas sensor and preparation method |
| CN112520789A (en) * | 2020-12-29 | 2021-03-19 | 杭州电子科技大学 | Preparation method of molybdenum trioxide nano film |
| CN113697857A (en) * | 2021-09-14 | 2021-11-26 | 河北地质大学 | Preparation method and application of two-dimensional flaky molybdenum oxide nano material |
| CN114609197A (en) * | 2022-03-25 | 2022-06-10 | 电子科技大学 | Gas sensitive material, preparation method and application thereof in NH3Application in gas sensor |
| CN115347083A (en) * | 2022-09-19 | 2022-11-15 | 陕西科技大学 | Morphology-controllable molybdenum disulfide nano material and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3941867A (en) * | 1974-09-04 | 1976-03-02 | Canadian Patents And Development Limited | Production of molybdenum trioxide from molybdenite in a fluidized bed |
| DE2830394A1 (en) * | 1978-07-11 | 1980-01-31 | Elektrometallurgie Gmbh | Molybdenum oxide prodn. from molybdenum sulphide concentrate - by oxidn. in aq. slurry, with recirculation for higher yield and recovery of metallic impurities |
| CN101535186A (en) * | 2006-11-16 | 2009-09-16 | 雅宝荷兰有限责任公司 | Purification of molybdenum technical oxide |
| CN101851006A (en) * | 2010-06-08 | 2010-10-06 | 南开大学 | Method for preparing MoS2 microspheres by solvent hot method |
| CN102126757A (en) * | 2010-01-19 | 2011-07-20 | 中国环境科学研究院 | Method for pollution-free production of molybdenum oxide |
-
2013
- 2013-11-21 CN CN201310589644.4A patent/CN103613136B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3941867A (en) * | 1974-09-04 | 1976-03-02 | Canadian Patents And Development Limited | Production of molybdenum trioxide from molybdenite in a fluidized bed |
| DE2830394A1 (en) * | 1978-07-11 | 1980-01-31 | Elektrometallurgie Gmbh | Molybdenum oxide prodn. from molybdenum sulphide concentrate - by oxidn. in aq. slurry, with recirculation for higher yield and recovery of metallic impurities |
| CN101535186A (en) * | 2006-11-16 | 2009-09-16 | 雅宝荷兰有限责任公司 | Purification of molybdenum technical oxide |
| CN102126757A (en) * | 2010-01-19 | 2011-07-20 | 中国环境科学研究院 | Method for pollution-free production of molybdenum oxide |
| CN101851006A (en) * | 2010-06-08 | 2010-10-06 | 南开大学 | Method for preparing MoS2 microspheres by solvent hot method |
Non-Patent Citations (2)
| Title |
|---|
| G. NAGARAJU ET AL.: "Hydrothermal synthesis of amorphous MoS2 nanofiber bundles via acidification of ammonium heptamolybdate tetrahydrate", 《NANOSCALE RES LETT》 * |
| 耿丁新: "二硫化钼分级纳米结构的制备与光催化性能", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104241624A (en) * | 2014-09-24 | 2014-12-24 | 南京大学 | Method for preparing anode material of molybdenum oxide lithium ion battery by controlling oxidation |
| CN104649323A (en) * | 2015-01-21 | 2015-05-27 | 济南大学 | Preparation method of strip-shaped molybdenum trioxide |
| CN104709943A (en) * | 2015-03-13 | 2015-06-17 | 济南大学 | Preparation method of molybdenum trioxide microsphere in three-dimensional hierarchical structure |
| CN105789030A (en) * | 2016-03-14 | 2016-07-20 | 暨南大学 | Preparation method of molybdenum trioxide two-dimensional atomic crystals with reduced layers |
| CN105944712A (en) * | 2016-05-23 | 2016-09-21 | 南京信息工程大学 | Preparation method of novel cerium sodium molybdate/molybdenum trioxide composite photocatalyst |
| CN106745262A (en) * | 2016-12-12 | 2017-05-31 | 郑州大学 | A kind of method for preparing amorphous oxide molybdenum nanometer sheet using the few layer molybdenum sulfide of oxidation |
| CN106745262B (en) * | 2016-12-12 | 2017-12-29 | 郑州大学 | A kind of method for preparing amorphous oxide molybdenum nanometer sheet using the few layer molybdenum sulfide of oxidation |
| CN108279540A (en) * | 2018-02-01 | 2018-07-13 | 深圳市光羿科技有限公司 | A kind of inorganic, metal oxide ion storage layer, its cryogenic fluid processing method and purposes |
| CN109205676B (en) * | 2018-08-30 | 2021-02-02 | 济南大学 | MoO (MoO)3Electrostatic spinning synthetic method of sheet structure |
| CN109205676A (en) * | 2018-08-30 | 2019-01-15 | 济南大学 | A kind of MoO3The electrostatic spinning synthetic method of laminated structure |
| CN108996549A (en) * | 2018-10-10 | 2018-12-14 | 金堆城钼业光明（山东）股份有限公司 | A kind of MoO3The network structure nanometer material and preparation method thereof of piece assembling |
| CN108996549B (en) * | 2018-10-10 | 2021-06-15 | 金堆城钼业光明（山东）股份有限公司 | MoO (MoO)3Sheet-assembled network structure nano material and preparation method thereof |
| CN110441380A (en) * | 2019-08-07 | 2019-11-12 | 暨南大学 | A kind of electrochemical sensor and its preparation method and application based on molecular engram electrode technology |
| CN110441380B (en) * | 2019-08-07 | 2021-07-23 | 暨南大学 | Electrochemical sensor based on molecular imprinting electrode technology and preparation method and application thereof |
| CN110879238A (en) * | 2019-10-25 | 2020-03-13 | 东北大学 | Molybdenum trioxide nano-structure sensitive material, corresponding ammonia gas sensor and preparation method |
| CN110879238B (en) * | 2019-10-25 | 2021-08-24 | 东北大学 | Molybdenum trioxide nano-structure sensitive material, corresponding ammonia gas sensor and preparation method |
| CN112520789A (en) * | 2020-12-29 | 2021-03-19 | 杭州电子科技大学 | Preparation method of molybdenum trioxide nano film |
| CN113697857A (en) * | 2021-09-14 | 2021-11-26 | 河北地质大学 | Preparation method and application of two-dimensional flaky molybdenum oxide nano material |
| CN113697857B (en) * | 2021-09-14 | 2023-01-24 | 河北地质大学 | Preparation method and application of two-dimensional flaky molybdenum oxide nano material |
| CN114609197A (en) * | 2022-03-25 | 2022-06-10 | 电子科技大学 | Gas sensitive material, preparation method and application thereof in NH3Application in gas sensor |
| CN114609197B (en) * | 2022-03-25 | 2023-11-21 | 电子科技大学 | Gas-sensitive material, preparation method and NH (NH) thereof 3 Application in gas sensor |
| CN115347083A (en) * | 2022-09-19 | 2022-11-15 | 陕西科技大学 | Morphology-controllable molybdenum disulfide nano material and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103613136B (en) | 2015-09-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103613136A (en) | Preparation method of square MoO3 nanosheet | |
| CN103613137B (en) | Hydrothermal synthesis method of molybdenum disulfide nanoflower | |
| CN106277064B (en) | A kind of method for preparing rhenium disulfide nanometer sheet | |
| CN102070184B (en) | Preparation method of CuInS2 nanoparticles | |
| CN102992405B (en) | Preparation method for molybdenum disulfide nanometer nuclear shell nano-structure | |
| CN105381807B (en) | A kind of preparation method of the selenizing cobalt nanocomposites of two selenizings molybdenum/bis- | |
| CN108439470A (en) | A kind of preparation method and application of molybdenum disulfide nano sheet | |
| CN106952743A (en) | The preparation and its application of a kind of cobaltosic oxide/carbon@molybdenum disulfide core-shell materials | |
| CN104556230B (en) | Molybdenum disulfide nano laurustinus structural semiconductor material and preparation method thereof | |
| CN105819507A (en) | Preparation method and application of nanosheet self-assembled microflower-shaped VS2 | |
| CN110203972A (en) | The preparation method of phase-M vanadium dioxide nanometre powder | |
| CN101857273A (en) | Preparation method of nanoscale flaky molybdenum disulfide | |
| CN110690419B (en) | Transition metal chalcogenide composite material and preparation method and application thereof | |
| WO2017059659A1 (en) | New silver nanowires with uniform aspect ratio and nodes preparation method | |
| CN108483502A (en) | A kind of preparation method and application of rhenium disulfide nanometer sheet | |
| CN109734132A (en) | A method of controlling synthesis of carbon/molybdenum disulfide particle in mixed solvent system | |
| CN105384192A (en) | Method for preparing one-dimensional nanorod self-assembled flower type three-dimensional Nb2O5 | |
| CN105060347A (en) | Method for synthesizing ultrathin molybdenum disulfide nanocrystals | |
| CN103833080B (en) | A kind of preparation method of molybdic acid cadmium porous ball | |
| CN105449177A (en) | Porous cubic ZnSO3@graphene negative electrode material used for sodium ion battery and preparation method for porous cubic ZnSO3@graphene negative electrode material | |
| CN104001494A (en) | Synthetic method of graphite-like modified nano-zinc stannate | |
| CN103496744A (en) | Preparation method of as-reduced ammonium tungsten bronze nanoparticles | |
| CN104941667A (en) | Petal-shaped magnetic ferric oxide molybdenum sulfide compound and preparation method thereof | |
| CN103774229B (en) | A kind of synthetic method of pucherite dendrite | |
| CN103819098A (en) | Method for preparing stannous sulfide nanosheet array film |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP02 | Change in the address of a patent holder | ||
| CP02 | Change in the address of a patent holder |
Address after: 212028 No. 518, Chang Xiang Road, University Park, Zhenjiang, Jiangsu Patentee after: Zhenjiang College Address before: Zhenjiang City, Jiangsu Province, 212003 Jingkou District Road No. 61 Patentee before: Zhenjiang College |