CN103147128B - Manganese vanadate nanoneedle structure and synthesis method thereof - Google Patents
Manganese vanadate nanoneedle structure and synthesis method thereof Download PDFInfo
- Publication number
- CN103147128B CN103147128B CN201310074998.5A CN201310074998A CN103147128B CN 103147128 B CN103147128 B CN 103147128B CN 201310074998 A CN201310074998 A CN 201310074998A CN 103147128 B CN103147128 B CN 103147128B
- Authority
- CN
- China
- Prior art keywords
- nanoneedle
- sds
- vanadate
- manganese
- water
- 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.)
- Expired - Fee Related
Links
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
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 technical field of nanometer material preparation, be specifically related to a kind of Manganese vanadate nanoneedle structure and synthetic method thereof.
Background technology:
Manganese vanadate is a kind of important inorganic vanadium hydrochlorate, has laminate structure, causes the research interest of people, has a good application prospect in optics, electrochemical sensor and field of lithium ion battery.The manganese vanadate powder of random form can be prepared by high temperature solid-state method.The inorganic nano material with certain dimension there will be novel functionalization characteristic on the basis of conventional blocks material physical properties, it is the important tectonic element of following nanocomposite optical device, electron device, in the fundamental and applied research of inorganic materials, there is good development potentiality, therefore, the form of manganese vanadate nanostructure is to its performance important.Also the manganese vanadate nanostructure about specific form is had at present, the such as report of manganese vanadate nanometer rod and manganese vanadate nano belt.
Compared with the manganese vanadate nanometer rod of uniform diameter and nano belt, Manganese vanadate nanoneedle structure has the conical needle-shaped nano-structure that one end size is large, the other end is small-sized, some specific area can be applied to, such as it can be used as the tip member of various detection analysis probe, the spatial resolution of equipment can be improved, simultaneously also much smaller to the destructiveness of test material.But, up to the present, not yet there is the report about Manganese vanadate nanoneedle structure.Compared with the manganese vanadate nanometer rod of uniform diameter and nano belt, this Manganese vanadate nanoneedle structure is difficult to synthesis.
Summary of the invention:
The object of this invention is to provide a kind of Manganese vanadate nanoneedle structure and synthetic method thereof.
Manganese vanadate nanoneedle structure provided by the present invention is by MnV
2o
5crystalline phase is formed, and length about 10 μm, nanoneedle tip diameter is about 50nm, and described manganese vanadate nanoneedle is oblique square structure.
The synthetic method of Manganese vanadate nanoneedle structure provided by the present invention, adopt Manganous chloride tetrahydrate, vanadic acid sodium to be raw material, sodium laurylsulfonate (SDS) is as structure directing agent, in encloses container, low-temperature heat is incubated for some time synthesis Manganese vanadate nanoneedle structure, and synthetic method is specific as follows:
With Manganous chloride tetrahydrate, vanadic acid sodium for 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 and water Homogeneous phase mixing being placed in reaction vessel and sealing, in temperature 120-180 DEG C, soaking time 6-24h, the amount that the amount of described Manganous chloride tetrahydrate and vanadic acid sodium is not more than 10%, SDS of water weight is not more than 10% of water weight.Finally can obtain brown fluffy solid, be Manganese vanadate nanoneedle structure.
Manganous chloride tetrahydrate of the present invention and vanadic acid sodium account for that 8%, SDS of water weight accounts for water weight 5%.
Manganous chloride tetrahydrate of the present invention and vanadic acid sodium account for that 5%, SDS of water weight accounts for water weight 3%.
The present invention preferably synthesis condition is 150-180 DEG C, insulation 12-18h.
The present invention adopts above-mentioned building-up process, Manganous chloride tetrahydrate, vanadic acid sodium are dissolved in the water, in sealed vessel, under certain temperature, reaction generates manganese vanadate, manganese vanadate reaches degree of supersaturation and separates out in water, form manganese vanadate nucleus, surfactant SDS is adsorbed in manganese vanadate core surface, as the formation of structure directing agent induction of Manganese vanadate nanoneedle structure, has oblique side MnV so can be synthesized in a large number by this kind of method
2o
5the Manganese vanadate nanoneedle structure of crystalline phase.Because building-up process is simple, synthesis temperature is low, so the cost of gained Manganese vanadate nanoneedle structure is low, for the practical application of Manganese vanadate nanoneedle structure provides condition.The invention provides a kind of method that Manganese vanadate nanoneedle structure of novelty and cryochemistry process synthesize Manganese vanadate nanoneedle structure in a large number, new approaches have been opened up in this research being novel inorganic nano-functional material, and have more important Research Significance for the formation and process of growth 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 synthesis of Manganese vanadate nanoneedle structure.
Accompanying drawing illustrates:
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the Manganese vanadate nanoneedle structure that the present invention synthesizes.
According to JCPDS PDF card (JCPDS card, PDF51-0203), gained germanic acid manganese nano whiskers structure can be retrieved by MnV
2o
5crystalline phase is formed, and is oblique square structure.
Fig. 2 is the SDS that the present invention adds 5wt.%, in 180 DEG C, scanning electronic microscope (SEM) image of Manganese vanadate nanoneedle structure synthesized by insulation 24h.
As can be seen from the figure can synthesize the uniform Manganese vanadate nanoneedle structure of form by the present invention, mix in together without other nanostructures.Add the SDS of 5wt.%, in 180 DEG C, the length about 10 μm of insulation 24h gained germanium Manganese vanadate nanoneedle structure, nanoneedle reduces gradually from large-sized one end, smooth surface, larger-size one end diameter about 1 μm, and the tip diameter of acicular structure is about 50nm.
Fig. 3 is the SDS that the present invention adds 3wt.%, in 180 DEG C, the SEM image of Manganese vanadate nanoneedle structure synthesized by insulation 24h.
As can be seen from the figure the SDS of 3wt.% is added, in 180 DEG C, the length about 10 μm of insulation 24h gained germanium Manganese vanadate nanoneedle structure, nanoneedle smooth surface, larger-size one end diameter about 1 μm, and the tip diameter of acicular structure is approximately 50nm.
Fig. 4 is the SDS that the present invention adds 5wt.%, in 180 DEG C, the SEM image of Manganese vanadate nanoneedle structure synthesized by insulation 6h.
As can be seen from the figure the SDS of 5wt.% is added, in 180 DEG C, the length about 10 μm of insulation 6h gained germanium Manganese vanadate nanoneedle structure, nanoneedle smooth surface, larger-size one end diameter about 1 μm, and the tip diameter of acicular structure is approximately 50nm.
Embodiment:
Embodiment 1: inserting after Manganous chloride tetrahydrate, vanadic acid sodium, SDS and water Homogeneous phase mixing in reaction vessel and seal, wherein the mol ratio of Manganous chloride tetrahydrate and vanadic acid sodium is 1: 2, Manganous chloride tetrahydrate, vanadic acid sodium account for that 10%, SDS of water solvent weight accounts for water solvent weight 8%.Then at temperature 180 DEG C, be incubated 24h, finally obtain length about 10 μm, the velvet-like tan product of Manganese vanadate nanoneedle structure that nanoneedle tip diameter is about 50nm.
Embodiment 2: inserting after Manganous chloride tetrahydrate, vanadic acid sodium, SDS and water Homogeneous phase mixing in reaction vessel and seal, wherein the mol ratio of Manganous chloride tetrahydrate and vanadic acid sodium is 1: 2, Manganous chloride tetrahydrate, vanadic acid sodium account for that 5%, SDS of water solvent weight accounts for water solvent weight 5%.Then at temperature 180 DEG C, be incubated 24h, finally obtain length about 10 μm, the velvet-like tan product of Manganese vanadate nanoneedle structure that nanoneedle tip diameter is about 50nm.
Embodiment 3: inserting after Manganous chloride tetrahydrate, vanadic acid sodium, SDS and water Homogeneous phase mixing in reaction vessel and seal, wherein the mol ratio of Manganous chloride tetrahydrate and vanadic acid sodium is 1: 2, Manganous chloride tetrahydrate, vanadic acid sodium account for that 10%, SDS of water solvent weight accounts for water solvent weight 8%.Then at temperature 180 DEG C, be incubated 18h, finally obtain length about 10 μm, the velvet-like tan product of Manganese vanadate nanoneedle structure that nanoneedle tip diameter is about 50nm.
Embodiment 4: inserting after Manganous chloride tetrahydrate, vanadic acid sodium, SDS and water Homogeneous phase mixing in reaction vessel and seal, wherein the mol ratio of Manganous chloride tetrahydrate and vanadic acid sodium is 1: 2, Manganous chloride tetrahydrate, vanadic acid sodium account for that 10%, SDS of water solvent weight accounts for water solvent weight 8%.Then at temperature 180 DEG C, be incubated 12h, finally obtain length about 10 μm, the velvet-like tan product of Manganese vanadate nanoneedle structure that nanoneedle tip diameter is about 50nm.
Embodiment 5: inserting after Manganous chloride tetrahydrate, vanadic acid sodium, SDS and water Homogeneous phase mixing in reaction vessel and seal, wherein the mol ratio of Manganous chloride tetrahydrate and vanadic acid sodium is 1: 2, Manganous chloride tetrahydrate, vanadic acid sodium account for that 10%, SDS of water solvent weight accounts for water solvent weight 3%.Then at temperature 150 DEG C, be incubated 6h, finally obtain length about 10 μm, the velvet-like tan product of Manganese vanadate nanoneedle structure that nanoneedle tip diameter is about 50nm.
Embodiment 6: inserting after Manganous chloride tetrahydrate, vanadic acid sodium, SDS and water Homogeneous phase mixing in reaction vessel and seal, wherein the mol ratio of Manganous chloride tetrahydrate and vanadic acid sodium is 1: 2, Manganous chloride tetrahydrate, vanadic acid sodium account for that 10%, SDS of water solvent weight accounts for water solvent weight 3%.Then at temperature 120 DEG C, be incubated 12h, finally obtain length about 10 μm, the velvet-like tan product of Manganese vanadate nanoneedle structure that nanoneedle tip diameter is about 50nm.
Embodiment 7: inserting after Manganous chloride tetrahydrate, vanadic acid sodium, SDS and water Homogeneous phase mixing in reaction vessel and seal, wherein the mol ratio of Manganous chloride tetrahydrate and vanadic acid sodium is 1: 2, Manganous chloride tetrahydrate, vanadic acid sodium account for that 3%, SDS of water solvent weight accounts for water solvent weight 5%.Then at temperature 180 DEG C, be incubated 6h, finally obtain length about 10 μm, the velvet-like tan product of Manganese vanadate nanoneedle structure that nanoneedle tip diameter is about 50nm.
Embodiment 8: inserting after Manganous chloride tetrahydrate, vanadic acid sodium, SDS and water Homogeneous phase mixing in reaction vessel and seal, wherein the mol ratio of Manganous chloride tetrahydrate and vanadic acid sodium is 1: 2, Manganous chloride tetrahydrate, vanadic acid sodium account for that 8%, SDS of water solvent weight accounts for water solvent weight 3%.Then at temperature 150 DEG C, be incubated 24h, finally obtain length about 10 μm, the velvet-like tan product of Manganese vanadate nanoneedle structure that nanoneedle tip diameter is about 50nm.
Claims (5)
1. a Manganese vanadate nanoneedle structure, is characterized in that this Manganese vanadate nanoneedle structure is by MnV
2o
5crystalline phase is formed, and length about 10 μm, nanoneedle tip diameter is about 50nm, and described manganese vanadate nanoneedle is oblique square structure.
2. a synthetic method for Manganese vanadate nanoneedle structure as claimed in claim 1, is characterized in that this synthetic method is as follows:
With Manganous chloride tetrahydrate, vanadic acid sodium for 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 and water Homogeneous phase mixing to be placed in reaction vessel and to seal, in temperature 120-180 DEG C, soaking time 6-24h, the amount that the amount of described Manganous chloride tetrahydrate and vanadic acid sodium is not more than 10%, SDS of water weight is not more than 10% of water weight.
3. synthetic method according to claim 2, is characterized in that: Manganous chloride tetrahydrate and vanadic acid sodium account for that 8%, SDS of water weight accounts for water weight 5%.
4. synthetic method according to claim 2, is characterized in that: Manganous chloride tetrahydrate and vanadic acid sodium account for that 5%, SDS of water weight accounts for water weight 3%.
5. synthetic method according to claim 2, is characterized in that: described temperature is 150-180 DEG C, 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 CN103147128A (en) | 2013-06-12 |
| CN103147128B true 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) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104528830B (en) * | 2014-12-03 | 2016-10-05 | 石家庄学院 | A kind of method synthesizing manganese vanadate nano-micrometre material |
| 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 |
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 |
|---|
| Hydrothermal synthesis and electrochemistry of a manganese vanadium oxide,γ-MnV2O5;Fan Zhang,et.al;《Electrochemistry Communications》;19991101;第1卷;第564-567页 * |
| Hydrothermal synthesis and electrochemistry of δ-type manganese vanadium oxide;Fan Zhang, et.al;《Electrochemistry Communications》;20000101;第2卷;第69-71页 * |
| Synthesis and characterization of a pipe-structure manganese vanadium oxide by hydrothermal reaction;Fan Zhang,et.al;《Journal of materials chemistry》;19990101;第9卷;第3137-3140页 * |
| Synthesis and characterization of manganese vanadate nanorods as glassy carbon electrode modified materials for the determination of L-cysteine;L. Z. Pei,et.al;《CrystEngComm》;20121219;第15卷;第1729-1738页 * |
| 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》.2010,第27卷第374-378页. * |
| 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》.2005,第29卷第194-199页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103147128A (en) | 2013-06-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Wu et al. | High-performance nanogenerators based on flexible cellulose nanofibril/MoS2 nanosheet composite piezoelectric films for energy harvesting | |
| CN103147128B (en) | Manganese vanadate nanoneedle structure and synthesis method thereof | |
| CN1333474C (en) | Preparation method of spinel lithium titanate nano tube/wire for lithium battery and capacitor | |
| CN103193273B (en) | Preparation method of extra-long manganese dioxide nanowires | |
| CN102965105B (en) | Graphene-CuInS2 quantum dot compound and preparation method thereof | |
| CN102259929B (en) | Method for preparing porous nano or submicron rod-like manganese oxide | |
| CN103482712B (en) | Method for preparing beta-Ni(OH)2 flower-like microsphere | |
| Kong et al. | Fabrication of flower-like Ni3 (NO3) 2 (OH) 4 and their electrochemical properties evaluation | |
| CN107123555B (en) | Empty nanotube and its preparation method and application in a kind of metal hydroxides | |
| Rezaie et al. | Effect of calcination on structural and supercapacitance properties of hydrothermally synthesized plate-like SrFe12O19 hexaferrite nanoparticles | |
| CN103130277B (en) | Method for preparing zinc vanadate nanorod | |
| 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 | |
| CN106986387A (en) | A kind of three-dimensional molybdenum disulfide bouquet and preparation method thereof | |
| Yan et al. | Photo-responsive shape memory polymer composites enabled by doping with biomass-derived carbon nanomaterials | |
| Li et al. | SnO 2/C composites fabricated by a biotemplating method from cotton and their electrochemical performances | |
| Xu et al. | Green synthesis of Bi 2 Se 3 hierarchical nanostructure and its electrochemical properties | |
| Hamedani et al. | Electrochemical performance of 3D porous PANI/Gr/MIL-100 (Fe) nanocomposite as a novel smart supercapacitor electrode material | |
| CN101993115B (en) | Preparation method of ferroferric oxide magnetic nanoparticles | |
| WO2008007752A1 (en) | Lithium composite metal oxide | |
| CN108101123B (en) | Square prism vanadic acid nickel nano material and preparation method thereof | |
| 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 | |
| CN101973573B (en) | Method for preparing zinc oxide nano microspheres | |
| CN103466693B (en) | Copper titanate nanoneedle and preparation method thereof |
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 |
Granted publication date: 20150513 Termination date: 20160228 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |