CN106241891B - A kind of sheet CoV2O6Preparation method - Google Patents
A kind of sheet CoV2O6Preparation method Download PDFInfo
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- CN106241891B CN106241891B CN201610571630.3A CN201610571630A CN106241891B CN 106241891 B CN106241891 B CN 106241891B CN 201610571630 A CN201610571630 A CN 201610571630A CN 106241891 B CN106241891 B CN 106241891B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/17—Nanostrips, nanoribbons or nanobelts, i.e. solid nanofibres with two significantly differing dimensions between 1-100 nanometer
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Abstract
The present invention mainly introduces a kind of sheet CoV2O6Preparation method, belong to inorganic advanced technical field of nano-composite material preparation technology.By a certain amount of vanadium pentoxide powder and H2O2Stirred after mixing, add distilled water, be put into autoclave and carry out hydro-thermal reaction, then obtain after washing and drying ribbon V2O5；A certain amount of cobalt nitrate is distributed in deionized water, ribbon V is added under stirring2O5, resulting solution is carried out to the stirring of certain time, after centrifugation, washing, drying, obtained sample is placed in Muffle furnace under certain temperature and calcines certain time, you can sheet CoV is made2O6.The sheet CoV that the present invention is told about2O6Preparation method technique it is simple, yield is high, and cost is than relatively low, and obtained nano material has relatively thin lamella, and specific surface area is big, good product quality.
Description
Technical field
The invention belongs to the production field of nano material, in particular it relates to a kind of sheet CoV2O6Preparation
Method.
Background technology
Vanadic acid cobalt（CoV2O6）Structure and property it is more unique, its have photocatalytic activity, sensitivity characteristic, heat endurance,
Electric conductivity and good gas sensing property etc., there is extensive in terms of optical material, sorbing material, catalyst and chemical sensitisation
Using.
Due to the progress of science and technology and continuing to develop for all kinds of characterization methods, sheet nano material is added in each side
The special performance that face is showed, preparation, the research of lamellar structure nano material are increasingly paid close attention to application by all circles
With support.Unique interfacial effect, small-size effect, quantum size effect and macroscopic quantum tunneling effect that nano material has
Should, all there is embodiment well in sheet nano material.In addition, sheet nano material possess uniqueness electric property and
Larger specific surface area, makes it show distinguished physicochemical properties, such as planar conductivity, magnetic anisotropy, adjustable
Humorous band gap and surface-active.These characteristics cause them to be well suited for setting for making sensor, catalyst and energy storage
It is standby.Therefore for sheet CoV2O6Preparation and explore there is very profound significance.
At present on sheet CoV2O6Preparation had been reported that.Such as Chinese patent CN102730769A, entitled
" three-layer laminated CoV2O6The preparation method of micro nano powder ", three-layer laminated CoV is prepared using hydro-thermal method2O6Micro nano powder.But,
Its technology has the shortcomings that complex process, efficiency are low, it is difficult to be produced on a large scale.Therefore, other new methods are explored to close
Into sheet CoV2O6Be one still need to solution the problem of.
The content of the invention
The invention reside in provide a kind of sheet CoV2O6Preparation method.This method is with low cost, and technique is simple, yield
Height, obtained nano material has relatively thin lamella, and specific surface area is big, good product quality.
The technical scheme is that：By a certain amount of vanadium pentoxide powder and H2O2Stirred after mixing, add distillation
Water, is put into autoclave and carries out hydro-thermal reaction, then obtains after washing and drying ribbon V2O5；By a certain amount of cobalt nitrate
It is distributed in deionized water, ribbon V is added under stirring2O5, resulting solution is carried out to the stirring of certain time, passed through
After centrifugation, washing, drying, obtained sample is placed in Muffle furnace under certain temperature and calcines certain time, you can lamella is made
Shape CoV2O6.Specific embodiment is as follows：
（1）0.364 g vanadium pentoxide powders are weighed, are scattered in 30 mL deionized waters, 5 mL hydrogen peroxide are added, surpassed
Sound is scattered 30 minutes；Gained orange solution is moved in 50 mL hydrothermal reaction kettles, at a temperature of 190 DEG C, hydro-thermal reaction 72
Hour；Hydrothermal product obtains one-dimensional V through centrifuging, washing, dry2O5Nanoribbons；
（2）0.16-0.8 g cabaltous nitrate hexahydrates are weighed, the V that 0.1-0.5 g have been prepared is weighed2O5Sample, controls it to rub
You are than being 1：1, it is scattered in 10-50 mL deionized waters；Dipping is dried after 12 hours, obtains brown powder shape sample；
（3）Will（2）Obtained product is put into chamber type electric resistance furnace, is heat-treated 2 hours at 300-500 DEG C, after cooling i.e.
It can obtain the powder of compound.
The sheet CoV that the present invention is told about2O6Preparation method technique it is simple, reaction time is short, efficiency high, cost compared with
Low, obtained nano material has relatively thin lamella, and specific surface area is big, good product quality.
Brief description of the drawings
Fig. 1 is ribbon V in embodiment 12O5The FESEM pictures of nano material.
Fig. 2 is sheet CoV in embodiment 12O6SEM pictures.
Fig. 3 is sheet CoV in embodiment 12O6FESEM pictures.
Fig. 4 is sheet CoV in embodiment 12O6X ray diffracting spectrum.
The present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment
Embodiment 1
（1）0.364 g vanadium pentoxide powders are weighed, are scattered in 30 mL deionized waters, 5 mL hydrogen peroxide are added, surpassed
Sound is scattered 30 minutes；Gained orange solution is moved in 50 mL hydrothermal reaction kettles, at a temperature of 190 DEG C, hydro-thermal reaction 72
Hour；Hydrothermal product obtains one-dimensional V through centrifuging, washing, dry2O5Nanoribbons；
（2）0.16 g cabaltous nitrate hexahydrates are weighed, the V that 0.1 g has been prepared is weighed2O5Sample, it is 1 to control its mol ratio：
1, it is scattered in 10 mL deionized waters；Dipping is dried after 12 hours, obtains brown powder shape sample；
（3）Will（2）Obtained product is put into chamber type electric resistance furnace, is heat-treated 2 hours, can be obtained after cooling at 500 DEG C
To the powder of compound.
The ribbon V prepared with embodiment 12O5The FESEM collection of illustrative plates of nano material is as shown in Figure 1, it can be seen that obtained
Product is the homogeneous belt structure of pattern；Sheet CoV2O6SEM spectrum as shown in fig. 2, it can be seen that banded shape
State is not present, and the substitute is lamellar structure.
The sheet CoV prepared with embodiment 12O6FESEM collection of illustrative plates it is as shown in Figure 3, it can be seen that its lamellar structure is bright
It is aobvious；The sheet CoV prepared with embodiment 12O6X ray diffracting spectrum as shown in figure 4, using the present invention prepared by sample
The position of the diffraction maximum of the XRD spectrum of product is corresponding with international standard card PDF#38-0090, shows that obtained sample is
CoV2O6。
Embodiment 2
（1）0.364 g vanadium pentoxide powders are weighed, are scattered in 30 mL deionized waters, 5 mL hydrogen peroxide are added, surpassed
Sound is scattered 30 minutes；Gained orange solution is moved in 50 mL hydrothermal reaction kettles, at a temperature of 190 DEG C, hydro-thermal reaction 72
Hour；Hydrothermal product obtains one-dimensional V through centrifuging, washing, dry2O5Nanoribbons；
（2）0.2 g cabaltous nitrate hexahydrates are weighed, the V that 0.32 g has been prepared is weighed2O5Sample, it is 1 to control its mol ratio：
1, it is scattered in 15 mL deionized waters；Dipping is dried after 12 hours, obtains brown powder shape sample；
（3）Will（2）Obtained product is put into chamber type electric resistance furnace, is heat-treated 2 hours, can be obtained after cooling at 300 DEG C
To the powder of compound.
Embodiment 3
（1）0.364 g vanadium pentoxide powders are weighed, are scattered in 30 mL deionized waters, 5 mL hydrogen peroxide are added, surpassed
Sound is scattered 30 minutes；Gained orange solution is moved in 50 mL hydrothermal reaction kettles, at a temperature of 190 DEG C, hydro-thermal reaction 72
Hour；Hydrothermal product obtains one-dimensional V through centrifuging, washing, dry2O5Nanoribbons；
（2）0.3 g cabaltous nitrate hexahydrates are weighed, the V that 0.48 g has been prepared is weighed2O5Sample, it is 1 to control its mol ratio：
1, it is scattered in 20 mL deionized waters；Dipping is dried after 12 hours, obtains brown powder shape sample；
（3）Will（2）Obtained product is put into chamber type electric resistance furnace, is heat-treated 2 hours, can be obtained after cooling at 400 DEG C
To the powder of compound.
Embodiment 4
（1）0.364 g vanadium pentoxide powders are weighed, are scattered in 30 mL deionized waters, 5 mL hydrogen peroxide are added, surpassed
Sound is scattered 30 minutes；Gained orange solution is moved in 50 mL hydrothermal reaction kettles, at a temperature of 190 DEG C, hydro-thermal reaction 72
Hour；Hydrothermal product obtains one-dimensional V through centrifuging, washing, dry2O5Nanoribbons；
（2）0.3 g cabaltous nitrate hexahydrates are weighed, the V that 0.48 g has been prepared is weighed2O5Sample, it is 1 to control its mol ratio：
1, it is scattered in 50 mL deionized waters；Dipping is dried after 12 hours, obtains brown powder shape sample；
（3）Will（2）Obtained product is put into chamber type electric resistance furnace, is heat-treated 2 hours, can be obtained after cooling at 450 DEG C
To the powder of compound.
Claims (1)
1. a kind of sheet CoV2O6Preparation method, it is characterised in that：
（1）0.364 g vanadium pentoxide powders are weighed, are scattered in 30 mL deionized waters, 5 mL hydrogen peroxide, ultrasound point are added
Dissipate 30 minutes；Gained orange solution is moved in 50 mL hydrothermal reaction kettles, at a temperature of 190 DEG C, hydro-thermal reaction 72 hours；
Hydrothermal product obtains one-dimensional V through centrifuging, washing, dry2O5Nanoribbons；
（2）0.16-0.8 g cabaltous nitrate hexahydrates are weighed, the V that 0.1-0.5 g have been prepared is weighed2O5Sample, controls its mol ratio
For 1：1, it is scattered in 10-50 mL deionized waters；Dipping is dried after 12 hours, obtains brown powder shape sample；
（3）Will（2）Obtained product is put into chamber type electric resistance furnace, is heat-treated 2 hours, can be obtained after cooling at 300-500 DEG C
To the powder of compound.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610571630.3A CN106241891B (en) | 2016-07-20 | 2016-07-20 | A kind of sheet CoV2O6Preparation method |
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| CN109585186B (en) * | 2018-11-29 | 2020-12-29 | 电子科技大学 | Supercapacitor electrode material CoV2O6Preparation method of (1) |
| CN113149085B (en) * | 2021-02-23 | 2022-09-30 | 北京科技大学 | Positioning synthesis method and application of mixed metal vanadate with two-dimensional structure |
| CN114634202B (en) * | 2021-12-13 | 2023-10-24 | 东南大学 | Method for preparing layered vanadate electrode material based on electrostatic self-assembly method and application |
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| CN105140509B (en) * | 2015-09-08 | 2017-06-13 | 武汉理工大学 | Porous C oV2O6Nanometer sheet electrode material and its preparation method and application |
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