CN109133194A - A kind of preparation method of the flower-shaped cobalt hydroxide of high electrocatalytic active three-dimension curved surface - Google Patents
A kind of preparation method of the flower-shaped cobalt hydroxide of high electrocatalytic active three-dimension curved surface Download PDFInfo
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- CN109133194A CN109133194A CN201810962666.3A CN201810962666A CN109133194A CN 109133194 A CN109133194 A CN 109133194A CN 201810962666 A CN201810962666 A CN 201810962666A CN 109133194 A CN109133194 A CN 109133194A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
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- 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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
- C01P2004/50—Agglomerated particles
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Abstract
The invention discloses a kind of preparation methods of flower-shaped cobalt hydroxide of high electrocatalytic active three-dimension curved surface, specifically comprise the following steps: step 1, by 1mmol~1mol CoSO4·7H2O is dissolved in deionized water as the source Co, after being completely dissolved, obtains solution A；Step 2,0.5mmol~2mol hydrazine hydrate N is added into the resulting solution A of step 12H4·H2O, is stirred at room temperature 1~10h, stands centrifugation, with deionized water centrifuge washing 3~6 times, it is dry to get.The technique that the present invention overcomes traditional preparation methods to need high temperature, heats or needs template requires, and greatly reduces preparation cost and the requirement to equipment, volume production easy to accomplish.
Description
Technical field
The invention belongs to the preparation technical fields of cobalt hydroxide, and in particular to a kind of high electrocatalytic active three-dimension curved surface is flower-shaped
The preparation method of cobalt hydroxide.
Background technique
Hydrogen Energy is considered as one of 21 century most promising clean energy resource, and water electrolysis hydrogen production is obtained because of its simple process
Hydrogen purity it is high, have received widespread attention.However, water electrolysis hydrogen production includes that evolving hydrogen reaction and oxygen evolution reaction two and half are anti-
It answers, wherein oxygen evolution reaction is related to four electronic transfer process, so the serious W-response rate for having influenced entire reaction,
Moreover, in many energy converters, such as: metal-air battery in regeneratable fuel cell, can be related to oxygen evolution reaction.
Therefore exploitation prepares development of nontoxic, inexpensive, high activity the oxygen evolution reaction elctro-catalyst to clean energy resource and energy converter
All have very important significance.
Co sill is regarded as ideal electrolysis water catalysis material a long time ago, because of its cheap and reserves
Abundant, the potentiality in terms of large-scale application are substantially better than IrO2、RuO2Equal metal oxide containing precious metals elctro-catalyst, and in alkalinity
There is excellent electrocatalysis characteristic in electrolyte.Cobalt oxide, cobalt sulfide, the Co sill such as cobalt hydroxide and phosphatization cobalt are extensive
Be applied to electro-catalysis water oxygen.Generally, the preparation of Co base catalyst includes two steps, first synthesis Co ion forerunner
Then body carries out the treatment processes such as hydro-thermal, high temperature or phosphatization to obtain product.Reaction process is complicated and consumes energy larger, has
Reaction even relates to template, and neither economical rationality is also not suitable for producing in enormous quantities.Therefore, development is quick and easy and low energy consumption
Co substrate preparation method for material is that the following water electrolysis hydrogen production moves towards the key technical problem urgently to be resolved using words.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of flower-shaped cobalt hydroxide of high electrocatalytic active three-dimension curved surface, the party
Method overcomes that traditional preparation methods need high temperature, the technique that heats or need template requires, greatly reduce preparation cost and
Requirement to equipment, volume production easy to accomplish.
The technical scheme adopted by the invention is that a kind of preparation side of the flower-shaped cobalt hydroxide of high electrocatalytic active three-dimension curved surface
Method specifically comprises the following steps:
Step 1, by 1mmol~1mol CoSO4·7H2O is dissolved in deionized water as the source Co, after being completely dissolved, is obtained molten
Liquid A；
Step 2,0.5mmol~2mol hydrazine hydrate N is added into the resulting solution A of step 12H4·H2O is stirred at room temperature
Mix 1~10h, stand centrifugation, with deionized water centrifuge washing 3~6 times, it is dry to get.
The features of the present invention also characterized in that
Hydrazine hydrate provides alkaline environment as Morphological control agent, hydrolysis.
In step 2 drying temperature be 60~80 DEG C, drying time be 12~for 24 hours.
The invention has the advantages that the present invention is used by the three-dimensional flower-shaped cobalt hydroxide of simple one-step synthesis method
The flower-shaped cobalt hydroxide of this method preparation is assembled by curved sheet, has very excellent electro-catalysis oxygen evolution activity.
Detailed description of the invention
Fig. 1 is that a kind of preparation method embodiment 2 of the flower-shaped cobalt hydroxide of high electrocatalytic active three-dimension curved surface of the present invention is made
Three-dimensional flower-shaped α-Co (OH)2Scanning electron microscope (SEM) photograph；
Fig. 2 is that a kind of preparation method embodiment 2 of the flower-shaped cobalt hydroxide of high electrocatalytic active three-dimension curved surface of the present invention is made
Three-dimensional flower-shaped α-Co (OH)2Transmission electron microscope picture；
Fig. 3 is that a kind of preparation method embodiment 2 of the flower-shaped cobalt hydroxide of high electrocatalytic active three-dimension curved surface of the present invention is made
Three-dimensional flower-shaped α-Co (OH)2XRD spectrum；
Fig. 4 is that a kind of preparation method embodiment 2 of the flower-shaped cobalt hydroxide of high electrocatalytic active three-dimension curved surface of the present invention is made
Three-dimensional flower-shaped α-Co (OH)2Linear surface sweeping volt-ampere curve.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of preparation method of the flower-shaped cobalt hydroxide of high electrocatalytic active three-dimension curved surface of the present invention, specifically includes mistake as follows
Journey:
Step 1, the CoSO of 1mmol~1mol is weighed4·7H2O (as the source Co) is dissolved in deionized water (50~200ml),
After being completely dissolved, solution A is obtained；
Step 2, the hydrazine hydrate (N of 0.5mmol~2mol is added into the resulting solution A of step 12H4·H2O), wherein water
Hydrazine is closed as Morphological control agent, and offer alkaline environment is provided, in 25 DEG C of 1~10h of stirring, after having stirred, centrifugation is stood, spends
Ionized water centrifuge washing 3~6 times, 60~80 DEG C at a temperature of it is dry 12~for 24 hours to get.
Embodiment 1
It is that 0.5mol:0.5mmol weighs CoSO according to molar ratio4·7H2O and N2H4·H2O, by CoSO4·7H2O is dissolved in
In 50ml deionized water, after being completely dissolved, solution A is obtained, by the N of measurement2H4·H2O is slowly added dropwise into solution A, in room temperature
Under (25 DEG C) stirring 1h, after having stirred, stand centrifugation, be washed with deionized 4 times, the dry 12h at 60 DEG C.
Embodiment 2
It is that 1.0mmol:1.0mmol weighs CoSO according to molar ratio4·7H2O and N2H4·H2O, by CoSO4·7H2O is dissolved in
In 60ml deionized water, after being completely dissolved, solution A is obtained, by the N of measurement2H4·H2O is slowly added dropwise into solution A, in room temperature
Under (25 DEG C) stirring 10h, after having stirred, stand centrifugation, be washed with deionized 3 times, at 80 DEG C it is dry for 24 hours.
There is three-dimensional flower-shaped structure, as depicted in figs. 1 and 2, Mei Geju according to the material that the preparation method of embodiment 2 obtains
Collective is formed by curved flake-assembly mode, and by Fig. 3, XRD result is it is found that the material of preparation is α-Co (OH)2.As shown in figure 4, should
Product has excellent electro-catalysis oxygen evolution activity, with good application prospect.
Embodiment 3
It is that 1.0mol:1.5mol weighs CoSO according to molar ratio4·7H2O and N2H4·H2O, by CoSO4·7H2O is dissolved in
In 100ml deionized water, after being completely dissolved, solution A is obtained, by the N of measurement2H4·H2O is slowly added dropwise into solution A, in room temperature
Under (25 DEG C) stirring 5h, after having stirred, stand centrifugation, be washed with deionized 5 times, the dry 18h at 70 DEG C.
Embodiment 4
It is that 0.8mol:2.0mol weighs CoSO according to molar ratio4·7H2O and N2H4·H2O, by CoSO4·7H2O is dissolved in
In 200ml deionized water, after being completely dissolved, solution A is obtained, by the N of measurement2H4·H2O is slowly added dropwise into solution A, in room temperature
Under (25 DEG C) stirring 10h, after having stirred, stand centrifugation, be washed with deionized 6 times, at 80 DEG C it is dry for 24 hours.
Claims (3)
1. a kind of preparation method of the flower-shaped cobalt hydroxide of high electrocatalytic active three-dimension curved surface, it is characterised in that: specifically include as follows
Step:
Step 1, by 1mmol~1mol CoSO4·7H2O is dissolved in deionized water as the source Co, after being completely dissolved, obtains solution A；
Step 2,0.5mmol~2mol hydrazine hydrate N is added into the resulting solution A of step 12H4·H2O, it is stirred at room temperature 1~
10h stands centrifugation, with deionized water centrifuge washing 3~6 times, it is dry to get.
2. a kind of preparation method of flower-shaped cobalt hydroxide of high electrocatalytic active three-dimension curved surface according to claim 1, special
Sign is: the hydrazine hydrate provides alkaline environment as Morphological control agent, hydrolysis.
3. a kind of preparation method of flower-shaped cobalt hydroxide of high electrocatalytic active three-dimension curved surface according to claim 1, special
Sign is: in the step 2 drying temperature be 60~80 DEG C, drying time be 12~for 24 hours.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101544408A (en) * | 2009-04-17 | 2009-09-30 | 中国科学院上海硅酸盐研究所 | Method for preparing laminated Co(OH)2 or Co3O4 nano-rod by hydro-thermal method |
| CN103224258A (en) * | 2013-04-26 | 2013-07-31 | 吉林化工学院 | Simple method for preparing Co3O4 nano-spheres and beta-Co(OH)2 micron-flowers |
| CN104261489A (en) * | 2014-09-25 | 2015-01-07 | 安徽师范大学 | Hexagonal beta-cobalt hydroxide nanosheet and preparation method thereof as well as super capacitor and electrode thereof |
| CN105329954A (en) * | 2014-08-11 | 2016-02-17 | 荆门市格林美新材料有限公司 | Large-particle size cobalt hydroxide and preparation method thereof |
| CN106219615A (en) * | 2016-08-23 | 2016-12-14 | 肖洋 | The preparation method of flower-shaped cobalt hydroxide microsphere |
| CN106563450A (en) * | 2016-11-05 | 2017-04-19 | 北京理工大学 | Preparation method of alpha phase cobaltous hydroxide nanosheet for oxygen evolution reaction |
| CN107308958A (en) * | 2017-06-12 | 2017-11-03 | 首都师范大学 | A kind of oxygen evolution reaction electrochemical catalyst and its preparation and application |
-
2018
- 2018-08-22 CN CN201810962666.3A patent/CN109133194A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101544408A (en) * | 2009-04-17 | 2009-09-30 | 中国科学院上海硅酸盐研究所 | Method for preparing laminated Co(OH)2 or Co3O4 nano-rod by hydro-thermal method |
| CN103224258A (en) * | 2013-04-26 | 2013-07-31 | 吉林化工学院 | Simple method for preparing Co3O4 nano-spheres and beta-Co(OH)2 micron-flowers |
| CN105329954A (en) * | 2014-08-11 | 2016-02-17 | 荆门市格林美新材料有限公司 | Large-particle size cobalt hydroxide and preparation method thereof |
| CN104261489A (en) * | 2014-09-25 | 2015-01-07 | 安徽师范大学 | Hexagonal beta-cobalt hydroxide nanosheet and preparation method thereof as well as super capacitor and electrode thereof |
| CN106219615A (en) * | 2016-08-23 | 2016-12-14 | 肖洋 | The preparation method of flower-shaped cobalt hydroxide microsphere |
| CN106563450A (en) * | 2016-11-05 | 2017-04-19 | 北京理工大学 | Preparation method of alpha phase cobaltous hydroxide nanosheet for oxygen evolution reaction |
| CN107308958A (en) * | 2017-06-12 | 2017-11-03 | 首都师范大学 | A kind of oxygen evolution reaction electrochemical catalyst and its preparation and application |
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