CN109695042A - A kind of preparation method of micron order cobalt oxide cube - Google Patents
A kind of preparation method of micron order cobalt oxide cube Download PDFInfo
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- CN109695042A CN109695042A CN201811477445.3A CN201811477445A CN109695042A CN 109695042 A CN109695042 A CN 109695042A CN 201811477445 A CN201811477445 A CN 201811477445A CN 109695042 A CN109695042 A CN 109695042A
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- cobalt oxide
- micron order
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- order cobalt
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a kind of preparation methods of micron order cobalt oxide cube, specifically includes the following steps: configuration choline chloride and ethylene glycol eutectic solvent, sequentially add cobalt source and sodium hypophosphite, magnetic agitation forms uniform solution, potentiostatic electrodeposition is utilized in three-electrode system, the carrier for cleaning deposit cobalt oxide after deposition repeatedly with pure water, it is dry in baking oven, obtain micron order cobalt oxide cube.Present invention process is simple, and impurity content is low, prepares large-sized crystal grain to study the growth mechanism of crystal and provides model.
Description
Technical field
The invention belongs to materials and technical field, and in particular to a kind of preparation method of micron order cobalt oxide cube.
Background technique
Cobalt oxide has reversible redox reaction process, big specific surface area, high conductivity, the cycle life of length
And stability, thus it is used for electrode material, and catalyst, the technical fields such as gas sensor.Metal cobalt/cobalt oxide it is microcosmic
Structure, if crystallite dimension, distribution and crystal morphology are the key factors for influencing and determining its performance.Therefore, it explores suitable
When reaction and method prepare the cobalt/cobalt oxide of different-shape and size and study its performance and growth mechanism is of great significance.
People prepared the metal composite of various patterns and microstructure by distinct methods in recent years, including nanometer is micro-
Ball, nanometer sheet, nano wire, nanometer rods, nanotube, nano thin-film etc..Common preparation method has pyrolysismethod, hydro-thermal method, gas phase
Deposition, electrodeposition process etc..But the partial size for preparing these substances is smaller, is usually no more than 300nm.The present invention is with stable low total
Molten solvent is electrolyte, this electrolyte is stable during the deposition process, itself will not decompose, the shadow for being formed and being grown to nucleus
Sound can be ignored；By controlling sedimentation time, deposition voltage, it is successfully prepared micron order cobalt oxide cube.
Summary of the invention
The present invention changes the size and shape of metal composite by sedimentation potential and sedimentation time, prepares a kind of micron order
Cobalt oxide cube.Simple process, impurity content is low, and the large-size crystals particle of preparation provides to study the growth mechanism of crystal
Model.
The present invention can be achieved through the following technical solutions:
(1) 2:1 weighs the choline chloride and ethylene glycol of certain mass in molar ratio, heats in 80-100 DEG C of baking oven, is formed
Homogeneous and transparent mixed solution；
(2) sodium hypophosphite and cobalt chloride hexahydrate are sequentially added, magnetic agitation under room temperature is until sodium hypophosphite and six hydrations
Cobalt chloride is completely dissolved, and forms uniform solution；
(3) using above-mentioned solution as electrolyte, Ag/AgCl is reference electrode in three-electrode system, and Pt is to electrode, nickel foams
It is constant voltage deposition for carrier, deposition voltage is from -1.4 V-1.7 V (Vs. Ag/AgCl), sedimentation time 5min-
180min；
(4) after depositing, the nickel foam for being deposited with nanometer cobalt oxide is washed repeatedly with deionized water, is finally putting into 60 DEG C of bakings
Dry 12h in case.
Detailed description of the invention
Fig. 1 is the electronics surface sweeping figure of micron cube cobalt oxide prepared by the present invention.
Fig. 2 is the electronics surface sweeping figure of micron cube cobalt compound prepared by the present invention.
Specific embodiment
The following examples are intended to illustrate the invention, but does not limit the scope of the invention.
Embodiment 1:
(1) choline chloride for claiming 25g, takes 20 ml ethylene glycol, is placed in 80 DEG C of baking oven and forms homogeneous and transparent mixed solution；
(2) plus 0.4876g sodium hypophosphite and 1.0945g cobalt chloride hexahydrate, magnetic agitation 2h are molten up to forming uniform blue
Liquid；
(3) using above-mentioned solution as electrolyte, using nickel foam as carrier in three-electrode system (Ag/AgCl is reference electrode, Pt
For to electrode), -1.4 V constant voltages deposit 3 h；
(4) after depositing, the nickel foam for being deposited with cobalt compound is washed repeatedly with deionized water, is then placed in baking oven and does
Dry 12h.Obtained sample is cobalt oxide cube, and pattern is as shown in Figure 1.
Embodiment 2:
(1) choline chloride for claiming 25g, takes 20 ml ethylene glycol, is placed in 80 DEG C of baking oven and forms homogeneous and transparent mixed solution；
(2) plus 0.4876g sodium hypophosphite and 1.0945g cobalt chloride hexahydrate, magnetic agitation 2h are molten up to forming uniform blue
Liquid；
(3) using above-mentioned solution as electrolyte, using nickel foam as carrier in three-electrode system (Ag/AgCl is reference electrode, Pt
For to electrode), -1.4 V constant voltages deposit 1h；
(4) after depositing, the nickel foam for being deposited with cobalt compound is washed repeatedly with deionized water, is then placed in baking oven and does
Dry 12h.Cube cobalt compound is obtained, pattern is as shown in Figure 2.
Embodiment 3:
(1) choline chloride for claiming 25g, takes 20 ml ethylene glycol, is placed in 80 DEG C of baking oven and forms homogeneous and transparent mixed solution；
(2) add 0.4876g sodium hypophosphite and 1.3388g cobalt nitrate, magnetic agitation 2h is until form uniform blue solution；
(3) using above-mentioned solution as electrolyte, using nickel foam as carrier in three-electrode system (Ag/AgCl is reference electrode, Pt
For to electrode), -1.5 V constant voltages deposit 1h；
(4) after depositing, the nickel foam for being deposited with cobalt compound is washed repeatedly with deionized water, is then placed in baking oven and does
Dry 12h.
Claims (7)
1. a kind of preparation method of micron order cobalt oxide cube, it is characterised in that the following steps are included:
(1) 2:1 weighs the choline chloride and ethylene glycol of certain mass in molar ratio, heats in 80-100 DEG C of baking oven, is formed
Homogeneous and transparent mixed solution；
(2) phosphorus source and cobalt source are added by a certain percentage, room temperature magnetic agitation is until form uniform solution；
(3) using above-mentioned solution as electrolyte, using nickel foam as carrier, three-electrode system deposits 3h with constant potential -1.4V；
(4) substrate of sample is washed repeatedly with deionized water load after depositing, dry 12h, obtains in 60 DEG C of baking ovens
To micron order cobalt oxide cube.
2. a kind of preparation method of micron order cobalt oxide cube as described in claim 1, which is characterized in that the step
(1) electrolyte prepared is eutectic solvent system.
3. a kind of preparation method of micron order cobalt oxide cube as described in claim 1, which is characterized in that the step
(2) phosphorus source and cobalt source in are respectively a hydration sodium hypophosphite and cobalt chloride hexahydrate, nitrate, the solubilities such as acetate
Salt.
4. a kind of preparation method of micron order cobalt oxide cube as described in claim 1, which is characterized in that the micron
The partial size of grade cobalt oxide is more than or equal to 3 μm.
5. a kind of preparation method of micron order cobalt oxide cube as described in claim 1, which is characterized in that the micron
The pattern of grade cobalt oxide is cube.
6. a kind of preparation method of micron order cobalt oxide cube as described in claim 1, which is characterized in that three electricity
Polar body system potentiostatic electrodeposition, Ag/AgCl and Pt are respectively reference electrode and to electrode, and carrier is nickel foam and titanium foil, deposition
Voltage range is -1.4V-1.7V.
7. a kind of preparation method of micron order cobalt oxide cube as described in claim 1, which is characterized in that the deposition
Time is 5 ~ 180min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811477445.3A CN109695042A (en) | 2018-12-05 | 2018-12-05 | A kind of preparation method of micron order cobalt oxide cube |
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| CN201811477445.3A CN109695042A (en) | 2018-12-05 | 2018-12-05 | A kind of preparation method of micron order cobalt oxide cube |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114105219A (en) * | 2021-12-22 | 2022-03-01 | 昆明理工大学 | Method for preparing cobaltosic oxide material through eutectic ionic liquid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107653458A (en) * | 2017-09-29 | 2018-02-02 | 河北工业大学 | A kind of high-ratio surface phosphorus modifies Co3O4The preparation method of compound |
-
2018
- 2018-12-05 CN CN201811477445.3A patent/CN109695042A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107653458A (en) * | 2017-09-29 | 2018-02-02 | 河北工业大学 | A kind of high-ratio surface phosphorus modifies Co3O4The preparation method of compound |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114105219A (en) * | 2021-12-22 | 2022-03-01 | 昆明理工大学 | Method for preparing cobaltosic oxide material through eutectic ionic liquid |
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Application publication date: 20190430 |