CN103147128A - Manganese vanadate nanoneedle structure and synthesis method thereof - Google Patents
Manganese vanadate nanoneedle structure and synthesis method thereof Download PDFInfo
- Publication number
- CN103147128A CN103147128A CN2013100749985A CN201310074998A CN103147128A CN 103147128 A CN103147128 A CN 103147128A CN 2013100749985 A CN2013100749985 A CN 2013100749985A CN 201310074998 A CN201310074998 A CN 201310074998A CN 103147128 A CN103147128 A CN 103147128A
- Authority
- CN
- China
- Prior art keywords
- vanadic acid
- sds
- water
- chloride tetrahydrate
- manganous chloride
- 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
Abstract
The invention discloses a manganese vanadate nanoneedle structure and a synthesis method thereof, belonging to the technical field of preparation of nano materials. The manganese vanadate nanoneedle structure disclosed by the invention is composed of an MnV2O5 orthorhombic phase which is about 10 mu m long, and the diameter of the nanoneedle tip is about 50 nm. The synthesis method comprises the following steps: by using manganese chloride and sodium vanadate as raw materials, sodium dodecylsulfate (SDS) as a surfactant and water as a solvent, evenly mixing the manganese chloride, sodium vanadate, SDS and water, sealing the mixture in a reaction vessel, and keeping at the temperature of 120-180 DEG C for 6-24 hours, thereby finally obtaining the brown flocculent manganese vanadate nanoneedle structure, wherein the amount of the manganese chloride and sodium vanadate is not greater than 10 wt% of the water, and the amount of the SDS is not greater than 10 wt% of the water. The invention has the advantages of simple synthetic process, and no environmental pollution by the raw materials and synthetic process, conforms to the trend of modern industry requiring environmental protection, and can implement mass synthesis of the manganese vanadate nanoneedle structure.
Description
Technical field:
The invention belongs to the nano material preparing technical field, be specifically related to a kind of vanadic acid manganese nanometer acicular structure and synthetic method thereof.
Background technology:
Vanadic acid manganese is a kind of important inorganic vanadium hydrochlorate, has laminate structure, has caused people's research interest, has a good application prospect at optics, electrochemical sensor and lithium ion battery field.Can prepare the vanadic acid manganese powder end of random form by high temperature solid-state method.Inorganic nano material with certain dimension novel functionalization characteristic can occur on the basis of conventional blocks material physical properties, it is the important tectonic element of following nanocomposite optical device, electron device, has good development potentiality aspect the fundamental and applied research of inorganic materials, therefore, the form of vanadic acid manganese nanostructure is to its performance important.At present also relevant for the vanadic acid manganese nanostructure of specific form, the report of vanadic acid manganese nanometer rod and vanadic acid manganese nano belt for example.
Compare with diameter uniform vanadic acid manganese nanometer rod and nano belt, vanadic acid manganese nanometer acicular structure has the conical needle-like nanostructure that an end size is large, the other end is small-sized, can be applied to some specific area, for example it is used the tip member of probe as various detection analysis, can improve the spatial resolution of equipment, also much smaller to the destructiveness of test material simultaneously.Yet, up to the present, not yet relevant for the report of vanadic acid manganese nanometer acicular structure.Compare with diameter uniform vanadic acid manganese nanometer rod and nano belt, this vanadic acid manganese nanometer acicular structure is difficult to synthesize.
Summary of the invention:
The purpose of this invention is to provide a kind of vanadic acid manganese nanometer acicular structure and synthetic method thereof.
Vanadic acid manganese nanometer acicular structure provided by the present invention is by MnV
2O
5Crystalline phase consists of, and length is 10 μ m approximately, nanoneedle tip diameter 50nm, and described vanadic acid manganese nanoneedle is oblique square structure.
The synthetic method of vanadic acid manganese nanometer acicular structure provided by the present invention, that employing Manganous chloride tetrahydrate, vanadic acid sodium are raw material, sodium laurylsulfonate (SDS) is as structure directing agent, synthetic vanadic acid manganese nanometer acicular structure of low-temperature heat insulation for some time in encloses container, synthetic method is specific as follows:
Take Manganous chloride tetrahydrate, vanadic acid sodium as raw material, SDS is tensio-active agent, and water is solvent, and wherein the mol ratio of Manganous chloride tetrahydrate and vanadic acid sodium is 1: 2.Manganous chloride tetrahydrate, vanadic acid sodium, SDS are evenly mixed being placed in reaction vessel and sealing with water, in temperature 120-180 ℃, soaking time 6-24h, the amount of described Manganous chloride tetrahydrate and vanadic acid sodium is not more than 10% of water weight, and the amount of SDS is not more than 10% of water weight.Finally can obtain the cotton-shaped product of brown, be vanadic acid manganese nanometer acicular structure.
Manganous chloride tetrahydrate of the present invention and vanadic acid sodium account for 8% of water weight, and SDS accounts for 5% of water weight.
Manganous chloride tetrahydrate of the present invention and vanadic acid sodium account for 5% of water weight, and SDS accounts for 3% of water weight.
The better synthesis condition of the present invention is 150-180 ℃, insulation 12-18h.
The present invention adopts above-mentioned building-up process, Manganous chloride tetrahydrate, vanadic acid sodium are dissolved in the water, reaction generates vanadic acid manganese under certain temperature in sealed vessel, vanadic acid manganese reaches degree of supersaturation and separates out in water, form vanadic acid manganese nucleus, it is surperficial that surfactant SDS is adsorbed in vanadic acid manganese core, induced the formation of vanadic acid manganese nanometer acicular structure as structure directing agent, has oblique side MnV so can synthesize in a large number by this kind method
2O
5The vanadic acid manganese nanometer acicular structure of crystalline phase.Simple due to building-up process, synthesis temperature is low, so the cost of gained vanadic acid manganese nanometer acicular structure is low, for the practical application of vanadic acid manganese nanometer acicular structure provides condition.The vanadic acid manganese nanometer acicular structure and the cryochemistry process that the invention provides a kind of novelty are synthesized the method for vanadic acid manganese nanometer acicular structure in a large number, this has opened up new approaches for the research of novel inorganic nano-functional material, and has more important Research Significance for formation and the process of growth of inquiring into novel inorganic nanometer functional material.What the present invention adopted is nontoxic Manganous chloride tetrahydrate, vanadic acid sodium, water and cryochemistry reaction process, and raw material and building-up process environmentally safe meet the development of modern industry direction of environmental requirement, can realize a large amount of synthetic of vanadic acid manganese nanometer acicular structure.
Description of drawings:
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the present invention's vanadic acid manganese nanometer acicular structure of synthesizing.
(the JCPDS card PDF51-0203), can retrieve gained germanic acid manganese nanometer acicular structure by MnV according to JCPDS PDF card
2O
5Crystalline phase consists of, and is oblique square structure.
Fig. 2 is the SDS that the present invention adds 5wt.%, in 180 ℃, the insulation vanadic acid manganese nanometer acicular structure that 24h synthesized scanning electronic microscope (SEM) image.
As can be seen from the figure can synthesize the uniform vanadic acid manganese of form nanometer acicular structure by the present invention, mix in together without other nanostructures.Add the SDS of 5wt.%, in the about 10 μ m of 180 ℃, the length of insulation 24h gained germanium vanadic acid manganese nanometer acicular structure, nanoneedle is dwindled gradually from a large-sized end, smooth surface, larger-size end diameter 1 a μ m, and the about 50nm of the tip diameter of acicular structure.
Fig. 3 is the SDS that the present invention adds 3wt.%, in 180 ℃, the insulation vanadic acid manganese nanometer acicular structure that 24h synthesized the SEM image.
As can be seen from the figure add the SDS of 3wt.%, in the about 10 μ m of 180 ℃, the length of insulation 24h gained germanium vanadic acid manganese nanometer acicular structure, the nanoneedle smooth surface, larger-size end diameter 1 a μ m, and the tip diameter of acicular structure is approximately 50nm.
Fig. 4 is the SDS that the present invention adds 5wt.%, in 180 ℃, the insulation vanadic acid manganese nanometer acicular structure that 6h synthesized the SEM image.
As can be seen from the figure add the SDS of 5wt.%, in the about 10 μ m of 180 ℃, the length of insulation 6h gained germanium vanadic acid manganese nanometer acicular structure, the nanoneedle smooth surface, larger-size end diameter 1 a μ m, and the tip diameter of acicular structure is approximately 50nm.
Embodiment:
Embodiment 1: insert in reaction vessel with Manganous chloride tetrahydrate, vanadic acid sodium, SDS and after water evenly mixes and sealing, wherein the mol ratio of Manganous chloride tetrahydrate and vanadic acid sodium is 1: 2, and Manganous chloride tetrahydrate, vanadic acid sodium account for 10% of water solvent weight, and SDS accounts for 8% of water solvent weight.Then be incubated 24h at 180 ℃ of temperature, finally obtained the approximately velvet-like brown product of vanadic acid manganese nanometer acicular structure of 10 μ m, nanoneedle tip diameter 50nm of length.
Embodiment 2: insert in reaction vessel with Manganous chloride tetrahydrate, vanadic acid sodium, SDS and after water evenly mixes and sealing, wherein the mol ratio of Manganous chloride tetrahydrate and vanadic acid sodium is 1: 2, and Manganous chloride tetrahydrate, vanadic acid sodium account for 5% of water solvent weight, and SDS accounts for 5% of water solvent weight.Then be incubated 24h at 180 ℃ of temperature, finally obtained the approximately velvet-like brown product of vanadic acid manganese nanometer acicular structure of 10 μ m, nanoneedle tip diameter 50nm of length.
Embodiment 3: insert in reaction vessel with Manganous chloride tetrahydrate, vanadic acid sodium, SDS and after water evenly mixes and sealing, wherein the mol ratio of Manganous chloride tetrahydrate and vanadic acid sodium is 1: 2, and Manganous chloride tetrahydrate, vanadic acid sodium account for 10% of water solvent weight, and SDS accounts for 8% of water solvent weight.Then be incubated 18h at 180 ℃ of temperature, finally obtained the approximately velvet-like brown product of vanadic acid manganese nanometer acicular structure of 10 μ m, nanoneedle tip diameter 50nm of length.
Embodiment 4: insert in reaction vessel with Manganous chloride tetrahydrate, vanadic acid sodium, SDS and after water evenly mixes and sealing, wherein the mol ratio of Manganous chloride tetrahydrate and vanadic acid sodium is 1: 2, and Manganous chloride tetrahydrate, vanadic acid sodium account for 10% of water solvent weight, and SDS accounts for 8% of water solvent weight.Then be incubated 12h at 180 ℃ of temperature, finally obtained the approximately velvet-like brown product of vanadic acid manganese nanometer acicular structure of 10 μ m, nanoneedle tip diameter 50nm of length.
Embodiment 5: insert in reaction vessel with Manganous chloride tetrahydrate, vanadic acid sodium, SDS and after water evenly mixes and sealing, wherein the mol ratio of Manganous chloride tetrahydrate and vanadic acid sodium is 1: 2, and Manganous chloride tetrahydrate, vanadic acid sodium account for 10% of water solvent weight, and SDS accounts for 3% of water solvent weight.Then be incubated 6h at 150 ℃ of temperature, finally obtained the approximately velvet-like brown product of vanadic acid manganese nanometer acicular structure of 10 μ m, nanoneedle tip diameter 50nm of length.
Embodiment 6: insert in reaction vessel with Manganous chloride tetrahydrate, vanadic acid sodium, SDS and after water evenly mixes and sealing, wherein the mol ratio of Manganous chloride tetrahydrate and vanadic acid sodium is 1: 2, and Manganous chloride tetrahydrate, vanadic acid sodium account for 10% of water solvent weight, and SDS accounts for 3% of water solvent weight.Then be incubated 12h at 120 ℃ of temperature, finally obtained the approximately velvet-like brown product of vanadic acid manganese nanometer acicular structure of 10 μ m, nanoneedle tip diameter 50nm of length.
Embodiment 7: insert in reaction vessel with Manganous chloride tetrahydrate, vanadic acid sodium, SDS and after water evenly mixes and sealing, wherein the mol ratio of Manganous chloride tetrahydrate and vanadic acid sodium is 1: 2, and Manganous chloride tetrahydrate, vanadic acid sodium account for 3% of water solvent weight, and SDS accounts for 5% of water solvent weight.Then be incubated 6h at 180 ℃ of temperature, finally obtained the approximately velvet-like brown product of vanadic acid manganese nanometer acicular structure of 10 μ m, nanoneedle tip diameter 50nm of length.
Embodiment 8: insert in reaction vessel with Manganous chloride tetrahydrate, vanadic acid sodium, SDS and after water evenly mixes and sealing, wherein the mol ratio of Manganous chloride tetrahydrate and vanadic acid sodium is 1: 2, and Manganous chloride tetrahydrate, vanadic acid sodium account for 8% of water solvent weight, and SDS accounts for 3% of water solvent weight.Then be incubated 24h at 150 ℃ of temperature, finally obtained the approximately velvet-like brown product of vanadic acid manganese nanometer acicular structure of 10 μ m, nanoneedle tip diameter 50nm of length.
Claims (5)
1. a vanadic acid manganese nanometer acicular structure, is characterized in that this vanadic acid manganese nanometer acicular structure is by MnV
2O
5Crystalline phase consists of, and length is 10 μ m approximately, nanoneedle tip diameter 50nm, and described vanadic acid manganese nanoneedle is oblique square structure.
2. synthetic method of vanadic acid manganese nanometer acicular structure as claimed in claim 1 is characterized in that this synthetic method is as follows:
Take Manganous chloride tetrahydrate, vanadic acid sodium as raw material, sodium laurylsulfonate (SDS) is tensio-active agent, water is solvent, wherein the mol ratio of Manganous chloride tetrahydrate and vanadic acid sodium is 1: 2, Manganous chloride tetrahydrate, vanadic acid sodium, SDS are evenly mixed with water to be placed in reaction vessel and sealing, in temperature 120-180 ℃, soaking time 6-24h, the amount of described Manganous chloride tetrahydrate and vanadic acid sodium is not more than 10% of water weight, and the amount of SDS is not more than 10% of water weight.
3. synthetic method according to claim 2, it is characterized in that: Manganous chloride tetrahydrate and vanadic acid sodium account for 8% of water weight, and SDS accounts for 5% of water weight.
4. synthetic method according to claim 2, it is characterized in that: Manganous chloride tetrahydrate and vanadic acid sodium account for 5% of water weight, and SDS accounts for 3% of water weight.
5. synthetic method according to claim 2, it is characterized in that: described temperature is 150-180 ℃, soaking time 12-18h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310074998.5A CN103147128B (en) | 2013-02-28 | 2013-02-28 | Manganese vanadate nanoneedle structure and synthesis method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310074998.5A CN103147128B (en) | 2013-02-28 | 2013-02-28 | Manganese vanadate nanoneedle structure and synthesis method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103147128A true CN103147128A (en) | 2013-06-12 |
| CN103147128B CN103147128B (en) | 2015-05-13 |
Family
ID=48545431
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310074998.5A Expired - Fee Related CN103147128B (en) | 2013-02-28 | 2013-02-28 | Manganese vanadate nanoneedle structure and synthesis method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103147128B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466693A (en) * | 2013-09-29 | 2013-12-25 | 安徽工业大学 | Copper titanate nanoneedle and preparation method thereof |
| CN104118912A (en) * | 2014-08-14 | 2014-10-29 | 安徽工业大学 | Method for preparing manganese vanadate nano-ribbons |
| CN104528830A (en) * | 2014-12-03 | 2015-04-22 | 石家庄学院 | Manganese vanadate nano-micro material, and synthetic method and application thereof |
| CN105970281A (en) * | 2016-05-06 | 2016-09-28 | 黑龙江大学 | Simple preparation method of cadmium vanadate monocrystalline nanometer wire |
| CN110350186A (en) * | 2019-07-09 | 2019-10-18 | 齐鲁工业大学 | A kind of preparation method of novel water system Zinc ion battery positive electrode |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0071190B1 (en) * | 1981-07-24 | 1985-05-15 | E.I. Du Pont De Nemours And Company | Thick film resistor compositions |
| CN1059762A (en) * | 1991-07-18 | 1992-03-25 | 丁中南 | The novel process of V 2 O 5 production by chloric acid chlorination method |
-
2013
- 2013-02-28 CN CN201310074998.5A patent/CN103147128B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0071190B1 (en) * | 1981-07-24 | 1985-05-15 | E.I. Du Pont De Nemours And Company | Thick film resistor compositions |
| CN1059762A (en) * | 1991-07-18 | 1992-03-25 | 丁中南 | The novel process of V 2 O 5 production by chloric acid chlorination method |
Non-Patent Citations (6)
| Title |
|---|
| FAN ZHANG, ET.AL: "Hydrothermal synthesis and electrochemistry of δ-type manganese vanadium oxide", 《ELECTROCHEMISTRY COMMUNICATIONS》 * |
| FAN ZHANG,ET.AL: "Hydrothermal synthesis and electrochemistry of a manganese vanadium oxide,γ-MnV2O5", 《ELECTROCHEMISTRY COMMUNICATIONS》 * |
| FAN ZHANG,ET.AL: "Synthesis and characterization of a pipe-structure manganese vanadium oxide by hydrothermal reaction", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
| L. Z. PEI,ET.AL: "Synthesis and characterization of manganese vanadate nanorods as glassy carbon electrode modified materials for the determination of L-cysteine", 《CRYSTENGCOMM》 * |
| 房晓燕，等: "十二烷基磺酸钠溶剂效应的理论研究", 《计算机与应用化学》 * |
| 裴立宅，等: "水热法及溶剂热合成法制备Ⅳ族一维无机纳米材料", 《稀有金属》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466693A (en) * | 2013-09-29 | 2013-12-25 | 安徽工业大学 | Copper titanate nanoneedle and preparation method thereof |
| CN103466693B (en) * | 2013-09-29 | 2014-09-03 | 安徽工业大学 | Copper titanate nanoneedle and preparation method thereof |
| CN104118912A (en) * | 2014-08-14 | 2014-10-29 | 安徽工业大学 | Method for preparing manganese vanadate nano-ribbons |
| CN104528830A (en) * | 2014-12-03 | 2015-04-22 | 石家庄学院 | Manganese vanadate nano-micro material, and synthetic method and application thereof |
| CN105970281A (en) * | 2016-05-06 | 2016-09-28 | 黑龙江大学 | Simple preparation method of cadmium vanadate monocrystalline nanometer wire |
| CN105970281B (en) * | 2016-05-06 | 2018-03-20 | 黑龙江大学 | A kind of simple preparation method of cadmium vanadate monocrystal nanowire |
| CN110350186A (en) * | 2019-07-09 | 2019-10-18 | 齐鲁工业大学 | A kind of preparation method of novel water system Zinc ion battery positive electrode |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103147128B (en) | 2015-05-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103147128B (en) | Manganese vanadate nanoneedle structure and synthesis method thereof | |
| Xiong et al. | Controllable synthesis of mesoporous Co3O4 nanostructures with tunable morphology for application in supercapacitors | |
| Chen et al. | A new and facile route to ultrafine nanowires, superthin flakes and uniform nanodisks of nickel hydroxide | |
| CN103193273B (en) | Preparation method of extra-long manganese dioxide nanowires | |
| CN103482712B (en) | Method for preparing beta-Ni(OH)2 flower-like microsphere | |
| CN103523824B (en) | The preparation method of nano-sheet ferroelectric material for a kind of photocatalysis | |
| CN101544408A (en) | Method for preparing laminated Co(OH)2 or Co3O4 nano-rod by hydro-thermal method | |
| CN102259929B (en) | Method for preparing porous nano or submicron rod-like manganese oxide | |
| Sannasi et al. | High-pseudocapacitance of MnCo2O4 nanostructures prepared by phenolphthalein assisted hydrothermal and microwave methods | |
| CN105870384A (en) | Nitrogen-doped carbon nanotube/manganese-cobalt oxide nano composite material for lithium battery electrodes | |
| CN104129770B (en) | A kind of nanoscale iron phosphate and preparation method thereof | |
| CN104787806B (en) | A kind of rose-shaped nano Cobalto-cobaltic oxide and preparation method thereof | |
| CN103253699A (en) | Self-assembled structure of perovskite/lead titanate nanosheet and preparation method thereof | |
| Li et al. | SnO 2/C composites fabricated by a biotemplating method from cotton and their electrochemical performances | |
| CN110203976A (en) | Rapid synthesis flakes ZnCo2O4The preparation method of-ZnO compound electric grade material | |
| Xu et al. | Green synthesis of Bi 2 Se 3 hierarchical nanostructure and its electrochemical properties | |
| CN102774893B (en) | Preparation method of nano petaline Ni(OH)2 | |
| CN103011215A (en) | Boehmite micro-nano structure sphere and preparation method thereof | |
| WO2008007752A1 (en) | Lithium composite metal oxide | |
| CN101734711A (en) | Method for synthesis of nano-zinc oxide powder through microwave solid state reaction | |
| CN108101123B (en) | Square prism vanadic acid nickel nano material and preparation method thereof | |
| CN101555042A (en) | Method for preparing spinel type iron-containing oxide nano-materials by low heat solid state reaction | |
| Xiao et al. | LiNi 0.5 Mn 1.5 O 4 hollow nano-micro hierarchical microspheres as advanced cathode for lithium ion batteries | |
| CN105565348A (en) | Nano particle size borate radical intercalation hydrotalcite-like compound and cleaning preparation method thereof | |
| CN104030348B (en) | A kind of preparation method of titanium dioxide nano-belts |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | 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 | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150513 Termination date: 20160228 |