CN106629869A - Co2O3 nanosheet and preparation method thereof - Google Patents
Co2O3 nanosheet and preparation method thereof Download PDFInfo
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- CN106629869A CN106629869A CN201611045944.6A CN201611045944A CN106629869A CN 106629869 A CN106629869 A CN 106629869A CN 201611045944 A CN201611045944 A CN 201611045944A CN 106629869 A CN106629869 A CN 106629869A
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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
- C01G51/04—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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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
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract
The invention discloses a Co2O3 nanosheet and a preparation method thereof. The preparation method comprises the following steps: dissolving cobalt sulfate, cobalt chloride, boric acid, trisodium citrate and o-sulfobenzimide in distilled water to obtain a plating solution while controlling the addition of cobalt sulfate to 100-200g, the addition of cobalt chloride to 80-120g, the addition of boric acid to 8-15g, the addition of trisodium citrate to 100-200g and the addition of o-sulfobenzimide to 0.2-0.8g in each liter of distilled water; adopting ITO conductive glass as a substrate, and electroplating the substrate with the plating solution to form a metal cobalt coating; and oxidizing the substrate containing the metal cobalt coating by an oxidation process to obtain a Co2O3 nanosheet. The Co2O3 nanosheet is prepared by the preparation method. In the invention, the raw material cost is low, and the preparation technology is easily industrialized and has relatively great practical value; and moreover, the obtained product has the advantages of high yield, high purity, uniform morphology, narrow size distribution and great length-diameter ratio.
Description
Technical field
The invention belongs to technical field prepared by new material, more particularly, is related to a kind of Co2O3Nanometer sheet and its preparation
Method.
Background technology
, used as a kind of important semiconductor-transition metal oxide, it is in catalysis, super capacitor, magnetic, lithium electricity for cobalt oxide
There is application in many fields such as pond.
The method that domestic and international report prepares nanometer cobalt oxide is few.Document " Self-supported hydrothermal
synthesized hollow Co3O4 nanowire arrays with high supercapacitor
capacitance,"Journal of Materials Chemistry,2011,21:9319-9325. " uses hydro-thermal
Method；Document " Shape-controlled synthesis and characterization of cobalt oxides
hollow spheres and octahedra,Dalton Transactions,2012,41:5981-5987. " is used
Thermal decomposition method；Document " Synthesis and optical properties of cubic Co3O4nanoparticles via
Thermal treatment of a trinuclear cobalt complex " use precursor process.These methods master
What is prepared is cobaltosic oxide, although and obtain nano level cobaltosic oxide, complex process and it is unfavorable for
Industrialization.
The content of the invention
In order to solve problems of the prior art, it is an object of the invention to provide a kind of product purity is high, technique letter
List and it is easy to the Co of industrialization2O3Nanometer sheet and preparation method thereof.
An aspect of of the present present invention provides Co2O3The preparation method of nanometer sheet, the preparation method is comprised the following steps：
A, cobaltous sulfate, cobalt chloride, boric acid, trisodium citrate and saccharin are dissolved in distilled water it are configured to
Plating solution, wherein, the addition for controlling cobaltous sulfate in every liter of distilled water be 100～200g, cobalt chloride addition be 80～120g,
It is that 100～200g, the addition of saccharin are that the addition of boric acid is 8～15g, the addition of trisodium citrate
0.2～0.8g；
B, using ITO electro-conductive glass as substrate, electroplated on substrate using the plating solution and form metallic cobalt coating；
C, the substrate containing metallic cobalt coating is aoxidized using oxidizing process, obtain Co2O3Nanometer sheet.
According to Co of the present invention2O3One embodiment of the preparation method of nanometer sheet, in stepb, successively with acetone, ethanol
It is with distilled water cleaning ITO electro-conductive glass and standby after drying up.
According to Co of the present invention2O3One embodiment of the preparation method of nanometer sheet, using the ITO electro-conductive glass after cleaning as
Negative electrode, using platinum electrode as anode, is electroplated in the plating solution.
According to Co of the present invention2O3One embodiment of the preparation method of nanometer sheet, plating is powered using D.C. regulated power supply,
The pH value for adjusting the plating solution using dilute sulfuric acid and diluted sodium hydroxide solution before being powered is 3.0～5.0 and controls the temperature of plating solution
For 20～60 DEG C, control electric current density is 10～200mA/cm after energization2, electromagnetic agitation plating solution is adopted in electroplating process and is controlled
Mixing speed processed is 50～150r/min, control conduction time for 5～120min, is powered containing metallic cobalt coating after terminating
Substrate take out and dry up after being cleaned with distilled water be put into it is standby in drying box.
According to Co of the present invention2O3One embodiment of the preparation method of nanometer sheet, in step C, using oxidation unit to containing
The substrate for having metallic cobalt coating is aoxidized, wherein,
Argon gas feed unit that the oxidation unit includes being sequentially connected by pipeline, ambient oxidation capacity adjustment unit,
Tube furnace and vavuum pump；
The argon gas feed unit includes argon bottle with the regulating valve and flowmeter that are arranged in the escaping pipe of argon bottle；
The ambient oxidation capacity adjustment unit includes Water Tank with Temp.-controlled and the sealing container being arranged in Water Tank with Temp.-controlled, described
Distilled water is housed, the escaping pipe of the argon gas feed unit is passed through in the distilled water of the sealing container in sealing container；
The porcelain dish for containing the substrate containing metallic cobalt coating is provided with the tube furnace, the air inlet pipe of the tube furnace is stretched
Enter in the sealing container and higher than the distilled water liquid level in the sealing container.
According to Co of the present invention2O3One embodiment of the preparation method of nanometer sheet, the substrate containing metallic cobalt coating is put into
In the tube furnace and discharge furnace air is vacuumized, with the flow of 20～100mL/min to ambient oxidation capacity adjustment unit
Sealing container in be passed through argon gas, control the ambient oxidation capacity adjustment unit Water Tank with Temp.-controlled temperature be 15～35 DEG C simultaneously
Make the argon gas carry water vapour to enter in tube furnace, lead to argon gas 20～30 minutes afterwards with the programming rate of 60～120 DEG C/h
Tube furnace is warming up into 900～1100 DEG C, stops heating and cooling to the furnace room temperature after 2～8h of insulation, obtain Co2O3Nanometer sheet.
Another aspect provides a kind of Co2O3Nanometer sheet, the Co2O3Nanometer sheet adopts above-mentioned Co2O3Nanometer
The preparation method of piece is prepared.
According to Co of the present invention2O3One embodiment of nanometer sheet, the Co2O3The length of nanometer sheet be 2～5 μm, width and
Thickness is 200～600nm.
The low raw-material cost of the present invention, preparation technology is easy to industrialization, there is larger practical value；Products therefrom yield
Height, purity height, homogeneous pattern, narrow size distribution and draw ratio are big, its as a kind of important semiconductor-transition metal oxide,
Can be applied in many fields such as catalysis, super capacitor, magnetic, lithium battery.
Description of the drawings
Fig. 1 shows the structural representation of the oxidation unit used in the present invention.
Fig. 2 shows the Co prepared in embodiment 12O3The SEM photograph of nanometer sheet.
Specific embodiment
All features disclosed in this specification, or disclosed all methods or during the step of, except mutually exclusive
Feature and/or step beyond, can combine by any way.
Any feature disclosed in this specification, unless specifically stated otherwise, can be equivalent or with similar purpose by other
Alternative features are replaced.I.e., unless specifically stated otherwise, each feature is an example in a series of equivalent or similar characteristics
.
Below first to Co of the present invention2O3The preparation method of nanometer sheet is described in detail.
Exemplary embodiment of the invention, the Co2O3The preparation method of nanometer sheet includes following multiple steps.
Step A：
Cobaltous sulfate, cobalt chloride, boric acid, trisodium citrate and saccharin are dissolved in distilled water and are configured to plating
Liquid, wherein, the addition for controlling cobaltous sulfate in every liter of distilled water be 100～200g, cobalt chloride addition be 80～120g, boron
It is that 100～200g, the addition of saccharin are that the addition of acid is 8～15g, the addition of trisodium citrate
0.2～0.8g.
It is to form metallic cobalt in substrate electroplated on top in follow-up plating step that this step prepares the plating solution for obtaining
Coating.Wherein, the effect of cobaltous sulfate and cobalt chloride is to provide cobalt source, and cobalt ions is reduced to cobalt atom shape in negative electrode deposition during plating
Effect into cobalt coating, boric acid and trisodium citrate has been the stable pH value of cushioning effect, and the effect of saccharin is
The crystal grain of cobalt in fining metal cobalt coating.
Step B：
Using ITO electro-conductive glass as substrate, the plating solution obtained using the preparation of step A is electroplated on substrate and forms metallic cobalt
Coating.
In this step, ITO electro-conductive glass is preferably cleaned with acetone, ethanol and distilled water successively and is drying up standby
With.
Using the ITO electro-conductive glass after cleaning as negative electrode, using platinum electrode as anode, electroplated in the plating solution.Tool
Body ground, plating is powered using D.C. regulated power supply, adjusts the pH value of plating solution before being powered using dilute sulfuric acid and diluted sodium hydroxide solution
For 3.0～5.0 and control plating solution temperature be 20～60 DEG C, after energization control electric current density be 10～200mA/cm2, in plating
During adopt electromagnetic agitation plating solution and control mixing speed for 50～150r/min, control conduction time for 5～120min, lead to
Electricity terminate after by the substrate containing metallic cobalt coating take out and dry up after being cleaned with distilled water be put into it is standby in drying box.
Step C：
The substrate containing metallic cobalt coating is aoxidized using oxidizing process, obtains Co2O3Nanometer sheet.
Preferably, the substrate containing metallic cobalt coating is aoxidized using specific oxidation unit.Fig. 1 shows this
The structural representation of the oxidation unit used in bright.
As shown in figure 1, the oxidation unit that the present invention is adopted includes the argon gas feed unit 10, gas being sequentially connected by pipeline
Atmosphere oxidability adjustment unit 20, tube furnace 30 and vavuum pump 40.Argon gas feed unit 10 includes argon bottle 11 and is arranged on argon
Regulating valve 13 and flowmeter 14 in the escaping pipe 12 of gas cylinder 11, ambient oxidation capacity adjustment unit 20 includes the He of Water Tank with Temp.-controlled 21
The sealing container 22 being arranged in Water Tank with Temp.-controlled 21, is equipped with distilled water, the escaping pipe of argon gas feed unit 10 in sealing container 22
12 are passed through in the distilled water of sealing container 22.The porcelain dish for containing the substrate 40 containing metallic cobalt coating is provided with tube furnace 30
31, tube furnace 30 can realize the controllable heating to substrate, and the air inlet pipe 41 of tube furnace 30 stretches into sealing container 22 and is higher than
Distilled water liquid level in sealing container 22.Tube furnace 30 is connected with vavuum pump 50, to be vacuumized to it by vavuum pump 50.
Additionally, evacuated tube 60 is additionally provided with tube furnace 30, to realize emptying after the completion of oxidation.
The oxidation step of the present invention is carried out preferably by the oxidation unit of said structure, but the invention is not restricted to this.
In this step, oxidizing process is concretely comprised the following steps：Substrate containing metallic cobalt coating is put into the tube furnace
And discharge furnace air is vacuumized, with the flow of 20～100mL/min in the sealing container of ambient oxidation capacity adjustment unit
Argon gas is passed through, the temperature for controlling the Water Tank with Temp.-controlled of the ambient oxidation capacity adjustment unit is 15～35 DEG C and takes the argon gas
Band water vapour is entered in tube furnace, and logical argon gas is afterwards heated up in tube furnace with the programming rate of 60～120 DEG C/h for 20～30 minutes
To 900～1100 DEG C, stop heating and cooling to the furnace room temperature after 2～8h of insulation, obtain Co2O3Nanometer sheet.
In this step, if directly aoxidized using air, due to content of oxygen in air it is too high, bad control oxygen
Change process, hardly results in the sheet cobalt oxide of this pattern of the invention.Therefore the present invention is creatively employed including atmosphere oxygen
Change capacity adjustment unit oxidation unit, the purpose that argon gas is first passed through the sealing container equipped with distilled water be by the use of argon gas as
Carrier is brought water vapour in tube furnace into, so as to carry out oxidized metal cobalt at high temperature using the water vapour with appropriate level oxygen
Obtain sheet cobalt oxide.Wherein, Water Tank with Temp.-controlled 21 can change the oxygen that water vapour brings by the vapour pressure of temperature controlled water
Press so as to change oxidizing condition.
The present invention additionally provides a kind of Co simultaneously2O3Nanometer sheet, the Co2O3Nanometer sheet adopts above-mentioned Co2O3The system of nanometer sheet
Preparation Method is prepared.According to the present invention, the Co2O3The length of nanometer sheet is 2～5 μm, width and thickness is 200～
600nm。
It should be understood that the above-mentioned embodiment and following examples of present invention detailed description are merely to illustrate the present invention rather than limit
The scope of the present invention processed, some nonessential improvement and tune that those skilled in the art's the above of the invention is made
It is whole to belong to protection scope of the present invention.
With reference to Co of the specific embodiment to the present invention2O3Nanometer sheet and preparation method thereof is described further.
Embodiment 1：
1) contain into 1L distilled water in the beaker of 1L capacity, sequentially add 150g cobaltous sulfates, 100g cobalt chlorides, 12g boric acid,
150g trisodium citrates and 0.5g saccharins, and be stirred continuously until all solids dissolve and obtain plating solution.
2) size is cleaned into removal surface and oil contaminant with acetone for the ITO electro-conductive glass of 20mm × 20mm × 1.1mm, then uses second
Alcohol is cleaned, stand-by after drying up finally with distilled water flushing.
3) using 2) step obtain ITO electro-conductive glass substrate as negative electrode, using platinum electrode as anode, in step 1) in
Electroplated in plating solution；Powered using D.C. regulated power supply, plating solution is adjusted using dilute sulfuric acid and diluted sodium hydroxide solution before being powered
PH is 4.0, and bath temperature is 55 DEG C；It is 80mA/cm that current density is arranged after energization2, electromagnetic agitation is adopted in electroplating process
Plating solution, mixing speed 100r/min；Conduction time 15min；Energization takes out the substrate containing metallic cobalt coating after terminating, with steaming
Distilled water cleaning after dry up be put into it is stand-by in drying box.
4) using the oxidation unit shown in Fig. 1, by step 3) in the substrate containing metallic cobalt coating that obtains be put into tubular type
In stove, exclusion furnace air is vacuumized, then argon gas is passed through with flow 50mL/min；Water Tank with Temp.-controlled temperature is controlled for 20 DEG C；It is logical
After entering argon gas half an hour, with the heating rate of 100 DEG C/h 1000 DEG C are warming up to tube furnace, are incubated 4h, then stop heating with
Stove is cooled to room temperature, takes out sample, and substrate surface metallic cobalt is oxidized, and obtains Co2O3Nanometer sheet.Wherein, gained Co2O3Nanometer
The pattern of piece as shown in the SEM photograph of Fig. 2, Co2O3The length of nanometer sheet is 2～5 μm, width and thickness my 200～600nm
Embodiment 2：
1) contain into 1L distilled water in the beaker of 1L capacity, sequentially add 120g cobaltous sulfates, 110g cobalt chlorides, 13g boric acid,
180g trisodium citrates and 0.6g saccharins, and be stirred continuously until all solids dissolve and obtain plating solution.
2) size is cleaned into removal surface and oil contaminant with acetone for the ITO electro-conductive glass of 20mm × 20mm × 1.1mm, then uses second
Alcohol is cleaned, stand-by after drying up finally with distilled water flushing.
3) using 2) step obtain ITO electro-conductive glass substrate as negative electrode, using platinum electrode as anode, in step 1) in
Electroplated in plating solution；Powered using D.C. regulated power supply, plating solution is adjusted using dilute sulfuric acid and diluted sodium hydroxide solution before being powered
PH is 4.0, and bath temperature is 55 DEG C；It is 10mA/cm that current density is arranged after energization2, electromagnetic agitation is adopted in electroplating process
Plating solution, mixing speed 100r/min；Conduction time 120min；Energization takes out the substrate containing metallic cobalt coating after terminating, and uses
Distilled water cleaning after dry up be put into it is stand-by in drying box.
4) using the oxidation unit shown in Fig. 1, by step 3) in the substrate containing metallic cobalt coating that obtains be put into tubular type
In stove, exclusion furnace air is vacuumized, then argon gas is passed through with flow 50mL/min；Water Tank with Temp.-controlled temperature is controlled for 20 DEG C；It is logical
After entering argon gas half an hour, 900 DEG C are warming up to tube furnace with the heating rate of 80 DEG C/h, are incubated 6h, then stop heating with stove
Room temperature is cooled to, sample is taken out, substrate surface metallic cobalt is oxidized, and obtains Co2O3Nanometer sheet.
Embodiment 3：
1) contain into 1L distilled water in the beaker of 1L capacity, sequentially add 200g cobaltous sulfates, 150g cobalt chlorides, 15g boric acid,
100g trisodium citrates and 0.3g saccharins, and be stirred continuously until all solids dissolve and obtain plating solution.
2) size is cleaned into removal surface and oil contaminant with acetone for the ITO electro-conductive glass of 20mm × 20mm × 1.1mm, then uses second
Alcohol is cleaned, stand-by after drying up finally with distilled water flushing.
3) using 2) step obtain ITO electro-conductive glass substrate as negative electrode, using platinum electrode as anode, in step 1) in
Electroplated in plating solution；Powered using D.C. regulated power supply, plating solution is adjusted using dilute sulfuric acid and diluted sodium hydroxide solution before being powered
PH is 3.5, and bath temperature is 40 DEG C；It is 40mA/cm that current density is arranged after energization2, electromagnetic agitation is adopted in electroplating process
Plating solution, mixing speed 100r/min；Conduction time 30min；Energization takes out the substrate containing metallic cobalt coating after terminating, with steaming
Distilled water cleaning after dry up be put into it is stand-by in drying box.
4) using the oxidation unit shown in Fig. 1, by step 3) in the substrate containing metallic cobalt coating that obtains be put into tubular type
In stove, exclusion furnace air is vacuumized, then argon gas is passed through with flow 30mL/min；Water Tank with Temp.-controlled temperature is controlled for 30 DEG C；It is logical
After entering argon gas half an hour, with the heating rate of 120 DEG C/h 1100 DEG C are warming up to tube furnace, are incubated 3h, then stop heating with
Stove is cooled to room temperature, takes out sample, and substrate surface metallic cobalt is oxidized, and obtains Co2O3Nanometer sheet.
Embodiment 4：
1) contain into 1L distilled water in the beaker of 1L capacity, sequentially add 110g cobaltous sulfates, 90g cobalt chlorides, 10g boric acid,
130g trisodium citrates and 0.6g saccharins, and be stirred continuously until all solids dissolve and obtain plating solution.
2) size is cleaned into removal surface and oil contaminant with acetone for the ITO electro-conductive glass of 20mm × 20mm × 1.1mm, then uses second
Alcohol is cleaned, stand-by after drying up finally with distilled water flushing.
3) using 2) step obtain ITO electro-conductive glass substrate as negative electrode, using platinum electrode as anode, in step 1) in
Electroplated in plating solution；Powered using D.C. regulated power supply, plating solution is adjusted using dilute sulfuric acid and diluted sodium hydroxide solution before being powered
PH is 4.5, and bath temperature is 20 DEG C；It is 60mA/cm that current density is arranged after energization2, electromagnetic agitation is adopted in electroplating process
Plating solution, mixing speed 100r/min；Conduction time 20min；Energization takes out the substrate containing metallic cobalt coating after terminating, with steaming
Distilled water cleaning after dry up be put into it is stand-by in drying box.
4) using the oxidation unit shown in Fig. 1, by step 3) in the substrate containing metallic cobalt coating that obtains be put into tubular type
In stove, exclusion furnace air is vacuumized, then argon gas is passed through with flow 80mL/min；Water Tank with Temp.-controlled temperature is controlled for 30 DEG C；It is logical
After entering argon gas half an hour, with the heating rate of 90 DEG C/h 1050 DEG C are warming up to tube furnace, are incubated 3.5h, then stop heating with
Stove is cooled to room temperature, takes out sample, and substrate surface metallic cobalt is oxidized, and obtains Co2O3Nanometer sheet.
In sum, low raw-material cost of the invention, preparation technology is easy to industrialization, there is larger practical value；Institute
Obtain Product yields height, purity height, homogeneous pattern, narrow size distribution and draw ratio is big, it is used as a kind of important semiconductor-transition
Metal oxide, can be applied in many fields such as catalysis, super capacitor, magnetic, lithium battery.
The invention is not limited in aforesaid specific embodiment.The present invention is expanded to and any in this manual disclosed
New feature or any new combination, and the arbitrary new method that discloses or the step of process or any new combination.
Claims (8)
1. a kind of Co2O3The preparation method of nanometer sheet, it is characterised in that the preparation method is comprised the following steps：
A, cobaltous sulfate, cobalt chloride, boric acid, trisodium citrate and saccharin are dissolved in distilled water be configured to plating
Liquid, wherein, the addition for controlling cobaltous sulfate in every liter of distilled water be 100～200g, cobalt chloride addition be 80～120g, boron
It is that 100～200g, the addition of saccharin are that the addition of acid is 8～15g, the addition of trisodium citrate
0.2～0.8g；
B, using ITO electro-conductive glass as substrate, electroplated on substrate using the plating solution and form metallic cobalt coating；
C, the substrate containing metallic cobalt coating is aoxidized using oxidizing process, obtain Co2O3Nanometer sheet.
2. Co according to claim 12O3The preparation method of nanometer sheet, it is characterised in that in stepb, successively with acetone,
Ethanol and distilled water cleaning ITO electro-conductive glass and standby after drying up.
3. Co according to claim 22O3The preparation method of nanometer sheet, it is characterised in that by the ITO electro-conductive glass after cleaning
As negative electrode, using platinum electrode as anode, electroplated in the plating solution.
4. Co according to claim 32O3The preparation method of nanometer sheet, it is characterised in that plating is supplied using D.C. regulated power supply
Electricity, the pH value for adjusting the plating solution using dilute sulfuric acid and diluted sodium hydroxide solution before being powered is 3.0～5.0 and controls the temperature of plating solution
Spend for 20～60 DEG C, control electric current density is 10～200mA/cm after energization2, in electroplating process using electromagnetic agitation plating solution simultaneously
Mixing speed is controlled for 50～150r/min, control conduction time for 5～120min, being powered will be containing metallic cobalt coating after terminating
Substrate take out and dry up after being cleaned with distilled water be put into it is standby in drying box.
5. Co according to claim 12O3The preparation method of nanometer sheet, it is characterised in that in step C, using oxidation unit
Substrate containing metallic cobalt coating is aoxidized, wherein,
The oxidation unit includes argon gas feed unit, ambient oxidation capacity adjustment unit, the tubular type being sequentially connected by pipeline
Stove and vavuum pump；
The argon gas feed unit includes argon bottle with the regulating valve and flowmeter that are arranged in the escaping pipe of argon bottle；
The ambient oxidation capacity adjustment unit includes Water Tank with Temp.-controlled and the sealing container being arranged in Water Tank with Temp.-controlled, the sealing
Distilled water is housed, the escaping pipe of the argon gas feed unit is passed through in the distilled water of the sealing container in container；
The porcelain dish for containing the substrate containing metallic cobalt coating is provided with the tube furnace, the air inlet pipe of the tube furnace stretches into institute
State in sealing container and higher than the distilled water liquid level in the sealing container.
6. Co according to claim 52O3The preparation method of nanometer sheet, it is characterised in that by the substrate containing metallic cobalt coating
Discharge furnace air is put into the tube furnace and vacuumizes, with the flow of 20～100mL/min to ambient oxidation capacity adjustment
Argon gas is passed through in the sealing container of unit, the temperature for controlling the Water Tank with Temp.-controlled of the ambient oxidation capacity adjustment unit is 15～35
DEG C and make the argon gas carry water vapour to enter in tube furnace, lead to argon gas 20～30 minutes afterwards with the intensification of 60～120 DEG C/h
Tube furnace is warming up to 900～1100 DEG C by speed, stops heating and cooling to the furnace room temperature after 2～8h of insulation, obtains Co2O3Receive
Rice piece.
7. a kind of Co2O3Nanometer sheet, it is characterised in that the Co2O3Nanometer sheet is using any one of claim 1 to 6
Co2O3The preparation method of nanometer sheet is prepared.
8. Co according to claim 12O3Nanometer sheet, it is characterised in that the Co2O3The length of nanometer sheet is 2～5 μm,
Width and thickness are 200～600nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108842169A (en) * | 2018-07-02 | 2018-11-20 | 西北师范大学 | A kind of metal oxide-loaded pucherite composite material and its preparation and application |
| CN109252196A (en) * | 2018-09-30 | 2019-01-22 | 四川理工学院 | A method of preparing MnCo2O4 micro nanometer fiber |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1515703A (en) * | 2003-01-08 | 2004-07-28 | 鞍钢集团机械制造公司风机电镀厂 | Method for electroforming nickel-cobalt alloy |
| CN1811017A (en) * | 2005-01-25 | 2006-08-02 | 来明工业(厦门)有限公司 | Decorating coating, electroplating solution and method to form the coating, and products with the coating |
| CN104445443A (en) * | 2014-12-24 | 2015-03-25 | 哈尔滨工业大学 | Method for preparing cobaltous oxide electrode with nanosheet structure |
| CN105401205A (en) * | 2015-11-26 | 2016-03-16 | 有研粉末新材料（北京）有限公司 | Foamed nickel and foamed nickel-based alloy plating device |
| CN106676592A (en) * | 2015-11-10 | 2017-05-17 | 天津瑞赛可新材料科技有限公司 | Nickel cobalt alloy plating solution |
-
2016
- 2016-11-22 CN CN201611045944.6A patent/CN106629869B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1515703A (en) * | 2003-01-08 | 2004-07-28 | 鞍钢集团机械制造公司风机电镀厂 | Method for electroforming nickel-cobalt alloy |
| CN1811017A (en) * | 2005-01-25 | 2006-08-02 | 来明工业(厦门)有限公司 | Decorating coating, electroplating solution and method to form the coating, and products with the coating |
| CN104445443A (en) * | 2014-12-24 | 2015-03-25 | 哈尔滨工业大学 | Method for preparing cobaltous oxide electrode with nanosheet structure |
| CN106676592A (en) * | 2015-11-10 | 2017-05-17 | 天津瑞赛可新材料科技有限公司 | Nickel cobalt alloy plating solution |
| CN105401205A (en) * | 2015-11-26 | 2016-03-16 | 有研粉末新材料（北京）有限公司 | Foamed nickel and foamed nickel-based alloy plating device |
Non-Patent Citations (2)
| Title |
|---|
| 付若鸿: "CoFe2O4薄膜的制备、表征和磁性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 杨瑞嵩等: "复合电镀与低氧分压法制备MnO–MnCr2O4 复合涂层", 《电镀与涂饰》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108842169A (en) * | 2018-07-02 | 2018-11-20 | 西北师范大学 | A kind of metal oxide-loaded pucherite composite material and its preparation and application |
| CN109252196A (en) * | 2018-09-30 | 2019-01-22 | 四川理工学院 | A method of preparing MnCo2O4 micro nanometer fiber |
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