CN102140691A - Method for synthesizing vanadium acid zinc micro/nanowire material by adopting hydrothermal method - Google Patents
Method for synthesizing vanadium acid zinc micro/nanowire material by adopting hydrothermal method Download PDFInfo
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Abstract
The invention discloses a method for synthesizing a vanadium acid zinc micro/nanowire material by adopting a hydrothermal method. In the method, ammonium metavanadate and zinc nitrate are used as reaction materials, distilled water is used as a solvent, a surfactant is used for controlling a microstructure, and the vanadium acid zinc micro/nanowire material with a regular appearance can be prepared under a hydro-thermal condition. The technology has the advantages of simplicity in operation, feasibility, controllable experimental condition, good repeatability, suitability for mass production and the like; and the synthesized material can play an important and positive role in multiple fields such as electrode material, photoluminescence, gas sensing and the like.
Description
Technical field
Patent of the present invention relates to the synthetic technology of inorganic functional micro Nano material, particularly a kind of method that adopts the synthetic vanadic acid zinc micro-/ nano wire material of hydrothermal method.
Technical background
The vanadium metal hydrochlorate can be used as the key core material in the fields such as electrode materials, photoluminescence, gas sensing, permanent magnet material, biological medicine material because of its unique crystalline structure.Be small-size effect and the quantum effect of giving full play to material, micro-nanoization of vanadium metal hydrochlorate become one of the research focus in materials chemistry field (C.C.Yu, C.X.Li, et al, Crystal Growth ﹠amp in recent years; Design.2009,9,783; L.W.Qian, J.Zhu, et al, Chem.Eur.J.2009,15,1233; J.F.Liu, Y.D.Li, Adv.Mater.2007,19,1118; J.F.Liu, Y.D.Li, J.Mater.Chem.2007,17,1797; Y.P.Fang, A.W.Xu, et al, Adv.Funct.Mater.2003,13.955; A.W.Xu, Y.P.Fang, et al.J.Am.Chem.Soc.2003,125,1494.).Vanadic acid Zinc material after micro-nanoization has been given the functionalization characteristic again on the basis of its original traditional character; More it is worth noting, by the optimization of material microstructure, of great advantage to the application of material.
With regard to material was synthetic, the traditional method of existing this vanadic acid zinc of preparation mainly was high-temperature solid phase reaction method (D.J.Lloyd, J.Galy, Cryst.Struct.Comm.1973,2,209.; M.Saux, J.Galy, C.R.Acad.Sci.1973,276, C81.).But also there is certain technical difficulty in existing synthesizing mean to the microscopic appearance control of vanadic acid zinc micro-/ nano material, and especially, less document relates to the report of micro-nano filamentary material; Patent of the present invention is intended to go out by Hydrothermal Preparation the vanadic acid zinc micro-/ nano wire material of size homogeneous, by adjusting the committed step condition, has realized the regulation and control to the product microtexture, for the good technique basis is established in applied research in the material building-up process.
Summary of the invention
The purpose of patent of the present invention is to provide a kind of method that adopts the synthetic vanadic acid zinc micro-/ nano wire material of hydrothermal method, its advantage is the adjusting by major influence factors parameter in the hydrothermal system under the supercritical state, finish the microcosmic regulation and control of product nucleation and process of growth, thereby prepare the micro-nano filamentary material of vanadic acid zinc that pattern is regular, be fit to carry out applied research.This method has advantages such as technology is simple, good reproducibility, product crystallinity excellence.
The technical scheme of patent of the present invention:
A kind of method that adopts the synthetic vanadic acid zinc micro-/ nano wire material of hydrothermal method, using tensio-active agent to be structure directing agent in reaction system, is raw material with zinc nitrate, ammonium meta-vanadate, is solvent with distilled water, utilize Hydrothermal Preparation vanadic acid zinc micro-/ nano filamentary material, may further comprise the steps:
The one, at room temperature with zinc nitrate solid or zinc nitrate and surfactant mixtures, adds the solution that distilled water makes certain zinc nitrate volumetric molar concentration, and violent stirring is 10 minutes then, makes solution a;
The ammonium meta-vanadate solid of 2 times of zinc nitrate mole numbers in the 2nd, weighing first step, the hot distilled water that adds 60～75 ℃, stir and dissolved fully to ammonium meta-vanadate in 5 minutes, make the homogeneous settled solution, dropwise join then among the solution a that first step prepares, violent stirring 10 minutes makes solution b;
The 3rd. the reaction precursor liquid solution that solution b is obtained is transferred in the hydrothermal reaction kettle, and insulation is 12 hours in 140 degree thermostat containers, just prepares superfine powdery material.Product after the X-ray diffraction analysis revealed is handled is ZnV
3O
8Vanadic acid zinc micro-/ nano wire material, corresponding JCPDS card number is 24-1481.Wherein, the outer courage of hydrothermal reaction kettle is made of high-intensity 304 material stainless steel work-pieces, inner bag is that the polytetrafluoroethylene (PTFE) material processes, and the hydro-thermal reaction system that constitutes after inside and outside courage closely cooperates can be used to prepare this class vanadic acid zinc micro-/ nano filamentary material.
The mol ratio of described zinc nitrate and tensio-active agent is 10: 1～10.
Described zinc nitrate volumetric molar concentration is 0.00125～0.01mol/L.
Described and the mixed uniformly tensio-active agent of zinc nitrate mainly plays the effect of structure directing, and tensio-active agent is a kind of, two or more the arbitrary combination in ethylenediamine tetraacetic acid (EDTA), cetyl trimethylammonium bromide (CTAB), Sodium dodecylbenzene sulfonate (SDBS), the polyoxyethylene glycol (PEG) 6000 in this system.
Advantage of the present invention and effect:
The present invention adopts hydrothermal method to synthesize vanadic acid zinc micro-/ nano wire material, with ammonium meta-vanadate, zinc nitrate is reaction raw materials, distilled water is solvent, and tensio-active agent is used for the regulation and control of microtexture, can prepare the regular vanadic acid zinc micro-/ nano filamentary material of pattern under hydrothermal reaction condition.Advantages such as this technology has not only that operation is simple, experiment condition is controlled, good reproducibility and suitable batch production; In addition, the material that synthesizes also can be brought into play important active effect at numerous areas such as electrode materials, photoluminescence, gas sensings.
Description of drawings
Fig. 1 is the SEM sem photograph of vanadic acid zinc overlong nanowire
Fig. 2 is the SEM sem photograph of vanadic acid zinc nano wire
Fig. 3 is the SEM sem photograph of vanadic acid zinc nano wire and nanometer sheet coexistence pattern
Fig. 4 is the SEM sem photograph of vanadic acid zinc nano wire
Fig. 5 is the SEM sem photograph of the nano wire of vanadic acid zinc reunion
Fig. 6 is the SEM sem photograph of vanadic acid zinc micro wire and nano wire coexistence pattern
Fig. 7 is the SEM sem photograph of vanadic acid zinc agglomeration nano line
Fig. 8 is the SEM sem photograph of vanadic acid zinc overlong nanowire
Embodiment:
Embodiment 1:
At room temperature, the zinc nitrate aqueous solution of configuration 0.00125mol/L, weighing ammonium meta-vanadate solid mole number is the twice of zinc nitrate mole number, distilled water to the ammonium meta-vanadate that adds 60～75 ℃ dissolves fully, dropwise be added drop-wise in the zinc nitrate aqueous solution then, mixed solution is moved in the hydrothermal reaction kettle, and insulation is 12 hours in 140 degree thermostat containers, just prepares the vanadic acid zinc micro-/ nano material of pure phase.Product shows that through SEM scanning electron microscope (Fig. 1) product is the uniform overlong nanowire of diameter, and its diameter is 80～120 nanometers, and length can reach 3～10 microns, and smooth surface, and many nano wires are woven into a mesh structure mutually, and agglomeration is arranged slightly.
Embodiment 2:
At room temperature, the zinc nitrate aqueous solution of configuration 0.00750mol/L, weighing ammonium meta-vanadate solid mole number is the twice of zinc nitrate mole number, distilled water to the ammonium meta-vanadate that adds 60～75 ℃ dissolves fully, dropwise be added drop-wise in the zinc nitrate aqueous solution then, mixed solution is moved in the hydrothermal reaction kettle, and insulation is 12 hours in 140 degree thermostat containers, just prepares the vanadic acid zinc micro-/ nano material of pure phase.Product shows that through SEM scanning electron microscope (Fig. 2) product is the nano wire of length and diameter homogeneous, and its diameter only is 20～100 nanometers, and length can reach 1～10 micron.
Embodiment 3:
At room temperature, the zinc nitrate aqueous solution of configuration 0.00875mol/L, weighing ammonium meta-vanadate solid mole number is the twice of zinc nitrate mole number, distilled water to the ammonium meta-vanadate that adds 60～75 ℃ dissolves fully, dropwise be added drop-wise in the zinc nitrate aqueous solution then, mixed solution is moved in the hydrothermal reaction kettle, and insulation is 12 hours in 140 degree thermostat containers, just prepares the vanadic acid zinc micro-/ nano material of pure phase.Product shows that through SEM scanning electron microscope (Fig. 3) product is relatively large nano wire and a small amount of nanometer sheet; Wherein, dispersed well nano wire has the diameter and the length of homogeneous, and diameter is that 50～100 nanometers, length are 2～4 microns.
Embodiment 4:
At room temperature, the zinc nitrate aqueous solution of configuration 0.0100mol/L, weighing ammonium meta-vanadate solid mole number is the twice of zinc nitrate mole number, distilled water to the ammonium meta-vanadate that adds 60～75 ℃ dissolves fully, dropwise be added drop-wise in the zinc nitrate aqueous solution then, mixed solution is moved in the hydrothermal reaction kettle, and insulation is 12 hours in 140 degree thermostat containers, just makes the vanadic acid zinc micro-/ nano material of pure phase.Product shows that through SEM scanning electron microscope (Fig. 4) product is made of filamentary material, and wherein the diameter of the nano wire that length-to-diameter ratio is bigger only is 200～500 nanometers, and length can reach several microns.
Embodiment 5:
At room temperature, the zinc nitrate aqueous solution of configuration 0.0100mol/L adds ethylenediamine tetraacetic acid (EDTA) in solution, and the mol ratio that makes zinc nitrate and tensio-active agent ethylenediamine tetraacetic acid (EDTA) is 10: 1, violent stirring 10 minutes; Weighing ammonium meta-vanadate solid mole number is the twice of zinc nitrate mole number, distilled water to the ammonium meta-vanadate that adds 60～75 ℃ dissolves fully, dropwise be added drop-wise in the zinc nitrate aqueous solution then, mixed solution is moved in the hydrothermal reaction kettle, insulation is 12 hours in 140 degree thermostat containers, just prepares the vanadic acid zinc micro-/ nano material of pure phase.Product is through the nano wire of main body pattern for reuniting together that SEM scanning electron microscope (Fig. 5) shows product, and the diameter of being not difficult to tell nano wire is between 100～250 nanometers, length can reach several microns; Less because of material diameter, length-to-diameter ratio is bigger, presents tangible agglomeration.
Embodiment 6:
At room temperature, the zinc nitrate aqueous solution of configuration 0.00125mol/L adds CTAB in solution, and the mol ratio that makes zinc nitrate and Surfactant CTAB is 10: 5, violent stirring 10 minutes; Weighing ammonium meta-vanadate solid mole number is the twice of zinc nitrate mole number, distilled water to the ammonium meta-vanadate that adds 60～75 ℃ dissolves fully, dropwise be added drop-wise in the zinc nitrate aqueous solution then, mixed solution is transferred in the hydrothermal reaction kettle, insulation is 12 hours in 140 degree thermostat containers, just prepares the vanadic acid zinc micro-/ nano material of pure phase.Product shows that through SEM scanning electron microscope (Fig. 6) product is the plates that micro wire and nano wire are gathered into, can find out clearly that from figure the corner angle of micro-nano rice noodles are clearly demarcated, the less nanowire diameter of diameter is 150～220 nanometers, large-size be 500 nanometers, length all can reach several microns.
Embodiment 7:
At room temperature, the zinc nitrate aqueous solution of configuration 0.0025mol/L adds SDBS in solution, and the mol ratio that makes zinc nitrate and tensio-active agent SDBS is 10: 2, violent stirring 10 minutes; Weighing ammonium meta-vanadate solid mole number is the twice of zinc nitrate mole number, distilled water to the ammonium meta-vanadate that adds 60～75 ℃ dissolves fully, dropwise be added drop-wise in the zinc nitrate aqueous solution then, mixed solution is moved in the hydrothermal reaction kettle, insulation is 12 hours in 140 degree thermostat containers, just prepares the vanadic acid zinc micro-/ nano material of pure phase.Product shows that through SEM scanning electron microscope (Fig. 7) product is together the nano-material of reuniting, wherein the diameter of nano wire be 100～250 nanometers, length between 1～5 micron, nano wire is arranged regular, tight.
Embodiment 8:
At room temperature, the zinc nitrate aqueous solution of configuration 0.00125mol/L adds PEG in solution, and the mol ratio that makes zinc nitrate and Surfactant PEG is 10: 10, violent stirring 10 minutes; Weighing ammonium meta-vanadate solid mole number is the twice of zinc nitrate mole number, distilled water to the ammonium meta-vanadate that adds 60～75 ℃ dissolves fully, dropwise be added drop-wise in the zinc nitrate aqueous solution then, mixed solution is transferred in the hydrothermal reaction kettle, in hydrothermal reaction kettle, be incubated 12 hours in the 140 degree thermostat containers, just prepare the vanadic acid zinc micro-/ nano material of pure phase.Mixed solution is poured in the tetrafluoroethylene hydrothermal reaction kettle, places 180 ℃ of baking ovens reaction 12 hours that mixed solution is moved to hydrothermal reaction kettle, and insulation is 12 hours in 140 degree thermostat containers, just prepares the vanadic acid zinc micro-/ nano material of pure phase.Product shows that through SEM scanning electron microscope (Fig. 8) product is an overlong nanowire, diameter evenly, be distributed between 100～150 nanometers, length is 10～15 microns.
Claims (5)
1. method that adopts the synthetic vanadic acid zinc micro-/ nano wire material of hydrothermal method, using tensio-active agent to be structure directing agent in reaction system, is raw material with zinc nitrate, ammonium meta-vanadate, is solvent with distilled water, utilize Hydrothermal Preparation vanadic acid zinc micro-/ nano filamentary material, may further comprise the steps:
The one, at room temperature with zinc nitrate solid or zinc nitrate and surfactant mixtures, adds the solution that distilled water makes certain zinc nitrate volumetric molar concentration, and violent stirring is 10 minutes then, makes solution a;
The ammonium meta-vanadate solid of 2 times of zinc nitrate mole numbers in the 2nd, weighing first step, the hot distilled water that adds 60～75 ℃, stir and dissolved fully to ammonium meta-vanadate in 5 minutes, make the homogeneous settled solution, dropwise join then among the solution a that first step prepares, violent stirring 10 minutes makes solution b;
The 3rd. the reaction precursor liquid solution that solution b is obtained is transferred in the hydrothermal reaction kettle, and insulation is 12 hours in 140 degree thermostat containers, just prepares superfine powdery material.X-ray diffraction analysis revealed product is ZnV
30
8Vanadic acid zinc micro-/ nano wire material.
2. the method for synthesizing vanadic acid zinc micro-/ nano wire material according to the described employing hydrothermal method of claim 1, it is characterized in that described and zinc nitrate blended tensio-active agent mainly plays the effect of structure directing, tensio-active agent is a kind of, two or more the arbitrary combination in ethylenediamine tetraacetic acid (EDTA), cetyl trimethylammonium bromide (CTAB), Sodium dodecylbenzene sulfonate (SDBS), the polyoxyethylene glycol (PEG) 6000 in this system.
3. according to the method for the synthetic vanadic acid zinc micro-/ nano wire material of the described employing hydrothermal method of claim 1, it is characterized in that: the mol ratio of described zinc nitrate and tensio-active agent is 10: 1～10.
4. the method for synthesizing vanadic acid zinc micro-/ nano wire material according to the described employing hydrothermal method of claim 1, it is characterized in that: described with zinc nitrate solid or zinc nitrate and surfactant mixtures, the solution that adding distilled water makes certain zinc nitrate volumetric molar concentration is 0.00125～0.0100mol/L.
5. according to the method for the synthetic vanadic acid zinc micro-/ nano wire material of the described employing hydrothermal method of claim 1, it is characterized in that: the mole ratio of zinc nitrate and ammonium meta-vanadate is 1: 2.
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| CN107720823A (en) * | 2017-11-13 | 2018-02-23 | 攀钢集团攀枝花钢铁研究院有限公司 | The preparation method of nanoscale Zinc vanadate |
| CN108933046A (en) * | 2018-07-11 | 2018-12-04 | 青岛科技大学 | A kind of preparation of the Zinc vanadate of porous level structure and its application in supercapacitor |
| CN111426647A (en) * | 2020-05-13 | 2020-07-17 | 福州大学 | Hydrothermal synthesis method of zinc vanadate microspheres for glucose colorimetric method detection |
| CN111426647B (en) * | 2020-05-13 | 2021-12-21 | 福州大学 | Hydrothermal synthesis method of zinc vanadate microspheres for glucose colorimetric method detection |
| CN111952578A (en) * | 2020-08-28 | 2020-11-17 | 天津工业大学 | Preparation method of heterojunction structure nanowire for anode of water-based zinc ion battery |
| CN113611846A (en) * | 2021-07-29 | 2021-11-05 | 中汽创智科技有限公司 | Electrode material of lithium battery and preparation method and application thereof |
| CN115010175A (en) * | 2022-07-25 | 2022-09-06 | 西安交通大学苏州研究院 | Preparation method of nano ammonium metavanadate |
| CN115010175B (en) * | 2022-07-25 | 2023-04-14 | 西安交通大学苏州研究院 | Preparation method of nano ammonium metavanadate |
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