CN106882846A - The preparation method of the controllable nickel cobalt hydroxide of crystal formation - Google Patents
The preparation method of the controllable nickel cobalt hydroxide of crystal formation Download PDFInfo
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- CN106882846A CN106882846A CN201710122754.8A CN201710122754A CN106882846A CN 106882846 A CN106882846 A CN 106882846A CN 201710122754 A CN201710122754 A CN 201710122754A CN 106882846 A CN106882846 A CN 106882846A
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- 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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- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
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Abstract
The invention discloses a kind of preparation method of the controllable nickel cobalt hydroxide of crystal formation.Comprise the following steps：Step one, cobalt nitrate, nickel nitrate and the ammonium of six methine four are dissolved in the water, and stirring at room temperature obtains dispersion liquid；Step 2, to solvent is added in the dispersion liquid that step one is obtained, stirring obtains question response liquid；Step 3, the question response liquid constant temperature that step 2 is obtained, condensing reflux reaction, obtains presoma；Step 4, the presoma that step 3 is obtained is centrifuged, washs, dries, that is, obtain nickel cobalt hydroxide, wherein, the timing of material concentration one is being added, when product is α types, solvent described in step 2 is ethylene glycol, and when product is β types, the solvent is ethanol.The method of this use solvent control product form is simple to operate, can prepare the different nickel cobalt hydroxide of the crystal formation with different electrochemical properties, is expected to obtain good application in energy storage field.
Description
Technical field
The present invention relates to a kind of preparation method of the controllable nickel cobalt hydroxide of crystal formation, belong to electrochemical material preparation field.
Background technology
Nickel cobalt hydroxide is material that is a kind of widely studied and using, and it possesses excellent chemical property.Due to it
Excellent properties, can be applied to the fuel-cell catalyst of alternative noble metal.Meanwhile, also have in terms of ultracapacitor
And be widely applied, its theoretical and actual specific capacitance is far above carbon material, can be as the electrode material of ultracapacitor of future generation
Material, and these potential application values also become the focus of investigation of materials.
In a series of application fields such as catalysis, electrochemistry, battery, the crystal formation of material is extensive for the influence of performance
Prove.The electric property aspect research of current nickel cobalt hydroxide materials is concentrated mainly on for pattern control, and for material
The research of crystal formation and chemical property does not almost have.Specifically, for nickel cobalt hydroxide, α types have ratio higher
Electric capacity and β types have more preferable cyclical stability.
However, due to the diversity of nickel cobalt hydroxide crystal formation, selectively preparing single crystal form nickel cobalt hydroxide always
It is a difficult point, this present situation causes the uncontrollable of material property.In order to control the performance and other properties of material, it is badly in need of development
The controllable nickel cobalt hydroxide preparation method of crystal formation.
The content of the invention
The purpose of the present invention is to propose to a kind of system simple to operate, the nickel cobalt hydroxide that blanket crystal formation is controllable
Preparation Method.
The technical solution for realizing the object of the invention is：A kind of preparation method of the controllable nickel cobalt hydroxide of crystal formation, leads to
Change solvent is crossed, the controllable nickel cobalt hydroxide of crystal formation is optionally prepared, comprised the following steps：
Step one：A certain amount of cobalt nitrate, nickel nitrate and the ammonium of six methine four are dissolved in the water, are stirred at room temperature, made
It fully dissolves, and obtains dispersion liquid；
Step 2：To solvent is added in the dispersion liquid that step one is obtained, dispersed with stirring is uniform at room temperature, obtains question response liquid, when
When nickel cobalt hydroxide is α types, the solvent is ethylene glycol, and when nickel cobalt hydroxide is β types, the solvent is ethanol；
Step 3：Question response liquid constant temperature and the condensing reflux reaction that step 2 is obtained, obtain presoma；
Step 4：Presoma centrifugation that step 3 is obtained, washing, and carry out freeze-drying and obtain nickel cobalt hydroxide.
Compared with prior art, the present invention has following remarkable advantage：1st, preparation method is simple, mild condition, without special
Equipment, the post processing of product is easy, is highly suitable for large-scale industrial production；2nd, the product for being prepared in different solvents is brilliant
Type is single, and crystal structure is preferably, and very well, the preparation method of this kind of controllable nickel cobalt hydroxide of crystal formation still belongs to first to control effect
Secondary report；3rd, due to the control of cooperative effect and crystal formation between nickel cobalt, resulting materials show excellent in electro-chemical test
Different chemical property so that it has boundless application prospect in electrochemical field, also show this kind of method except
Practical value outside novelty.
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
Brief description of the drawings
Fig. 1 is the preparation flow schematic diagram of the controllable nickel cobalt hydroxide of crystal formation of the present invention.
Fig. 2 is the XRD spectrum of nickel cobalt hydroxide sample in different embodiments, wherein, (a) α-Ni (OH)2 With β-Ni
(OH)2；(b) α-Ni0.5Co0.5 With β-Ni0.5Co0.5 ；(c) α-Ni0.33Co0.67 With β-Ni0.33Co0.67 ；(d) α-Co
(OH)2 With β-Co (OH)2 。
Fig. 3 is the electron microscope by the reaction condition of embodiment 2 gained nickel cobalt hydroxide sample, wherein, (a-c) α-
Ni0.5Co0.5 The TEM figures of sample different multiples；(d-f) α-Ni0.5Co0.5 The SEM figures of sample different multiples.
Fig. 4 is the electron microscope by the reaction condition of embodiment 1 and 4 gained nickel cobalt hydroxide sample, wherein, (a) α-Ni
(OH)2 The SEM figures of sample；(b) α-Co(OH)2 The SEM figures of sample；(c) α-Ni(OH)2 The TEM figures of sample；(d) α-Co
(OH)2 The TEM figures of sample.
Fig. 5 is the electro-chemical test figure of nickel cobalt hydroxide sample in different embodiments, wherein, (a) α type nickel cobalt hydrogen-oxygens
The cyclic voltammetry curve of compound；The cyclic voltammetry curve of (b) β type nickel cobalt hydroxide；(c) difference nickel cobalt hydroxide
Constant current discharge curve；The quality specific capacitance comparison diagram of (d) difference nickel cobalt hydroxide.
Specific embodiment
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
The present invention reaches the purpose of control product form by using the different qualities of different solvents.Specifically, make
With ethanol and water mixed solvent, using the ammonium of six methine four be alkali source, nickel cobalt nitrate as nickel and cobalt source, by changing nickel cobalt
Than a series of β types nickel cobalt complex hydroxides can be prepared.In addition, it is contemplated that the property of different solvents, in other conditions not
Change solvent in the case of change, the ethanol in mixed solvent is changed to ethylene glycol, a series of α types nickel cobalt hydrogen can be prepared
Oxide.The nickel cobalt hydroxide of prepared different crystal forms has each different electrochemical properties, is expected to be obtained in energy storage field
To good application.
With reference to Fig. 1, the present invention optionally prepares the controllable nickel cobalt hydroxide of crystal formation by changing solvent, including
Following steps：
Step one：A certain amount of cobalt nitrate and nickel nitrate and the ammonium of six methine four are dissolved in the water, are stirred at room temperature, fill it
Divide dissolving, obtain dispersion liquid, the wherein total ion concentration of nickel cobalt is 20 ~ 100 mmol/L, the ammonium of six methine four and nickel cobalt element
The mol ratio of total amount is 2:1.
Step 2：To solvent is added in the dispersion liquid that step one is obtained, dispersed with stirring is uniform at room temperature, obtains question response
Liquid, when nickel cobalt hydroxide is α types, the solvent is ethylene glycol, and when nickel cobalt hydroxide is β types, the solvent is
Ethanol, wherein, the volume of solvent is identical with the volume of step one reclaimed water；
Step 3：The question response liquid that step 2 is obtained is transferred to round-bottomed flask, and constant temperature, condensing reflux certain hour obtain forerunner
Body, wherein reaction temperature are 80 ~ 120oC, the reaction time is 2 ~ 8 h；
Step 4：Presoma centrifugation, the washing that step 3 is obtained, and freeze-drying is carried out, nickel cobalt complex hydroxide is obtained,
Wherein sublimation drying is 6 ~ 24 h.
With reference to embodiment and accompanying drawing, the present invention will be further described in detail：
Embodiment 1：
Step one：0.70 g (96 mmol/L) Nickelous nitrate hexahydrates and 0.67 g (192 mmol/L) ammonium of six methine four are molten
Solution is stirred at room temperature in 25 mL water, it is fully dissolved, and obtains green dispersion liquid；
Step 2：To 25 mL solvents are added in the green dispersion liquid that step one is obtained, it is stirred at room temperature and is uniformly dispersed, obtains
Question response liquid；
Step 3：The question response liquid that step 2 is obtained is transferred to 100 mL round-bottomed flasks, 80oCondensing reflux reaction 4 under C
Room temperature is naturally cooled to after h, presoma is obtained；
Step 4：The presoma that step 3 is obtained is collected by centrifugation and washed, and carries out freeze-drying and obtain the compound hydrogen of nickel cobalt
Oxide, wherein sublimation drying are 6 h.When the solvent described in the step 2 is ethylene glycol, reaction obtains α type hydroxides
Nickel, when the solvent is ethanol, reaction obtains β type nickel hydroxides, is respectively labeled as α-Ni (OH)2 With β-Ni (OH)2 。
Products therefrom respectively α-Ni (OH) are can verify that from Fig. 2 (a)2 (JCPDS No. 22-0444) and β-Ni (OH)2
(JCPDS No. 14-0117), Fig. 4 (a, c) are it can be seen that α-Ni (OH)2Pattern be very thin laminated structure.From Fig. 5 (a,
B) it can be found that in the case where identical sweeps speed（20 mV/s）, the β type nickel cobalt hydroxide redox peak position pair in Fig. 5 b
Should be essentially identical in the α type nickel cobalt hydroxide of identical nickel-to-cobalt ratio.However, the cyclic voltammetry curve of β type nickel cobalt hydroxide
Area is significantly less than α types, it is possible thereby to infer its specific capacitance performance much worse than α type nickel cobalt hydroxide.
Embodiment 2：
Step one：By 0.35 g (24 mmol/L) Nickelous nitrate hexahydrate, 0.35 g (24 mmol/L) cabaltous nitrate hexahydrates and
0.67 g (96 mmol/L) ammonium of six methine four is dissolved in 50 mL water, is stirred at room temperature, it is fully dissolved, and obtains dark
Green dispersion liquid；
Step 2：To 50 mL solvents are added in the dirty-green dispersion liquid that step one is obtained, it is stirred at room temperature and is uniformly dispersed, obtains
To question response liquid；
Step 3：The question response liquid that step 2 is obtained is transferred to 150 mL round-bottomed flasks, 100oCondensing reflux reaction 6 under C
Room temperature is naturally cooled to after h, presoma is obtained；
Step 4：The presoma that step 3 is obtained is collected by centrifugation and washed, and carries out freeze-drying and obtain the compound hydrogen of nickel cobalt
Oxide, wherein sublimation drying are 12 h.When the solvent described in the step 2 is ethylene glycol, reaction obtains α types nickel cobalt and answers
Close hydroxide（Nickel-to-cobalt ratio 1:1）, when the solvent is ethanol, reaction obtains β type nickel cobalt complex hydroxides（Nickel-to-cobalt ratio
1:1）, it is respectively labeled as α-Ni0.5Co0.5 With β-Ni0.5Co0.5 。
The pattern of material is very thin lamellar structure as can be seen from Figure 3, and lamella is larger.HRTEM from Fig. 3 c
The thickness that photo can substantially calculate lamella is about 3 nm.From Fig. 5 (a, b) it can be found that in the case where identical sweeps speed（20 mV/
s）, contrast cyclic voltammogram area can be seen that α and β type nickel cobalt hydroxide is Ni0.5Co0.5Area it is maximum, by
This can tentatively infer product Ni0.5Co0.5With highest electrochemical capacitor.Fig. 5 (c, d) further checkings simultaneously, identical
Under current density（1 A/g）, it can be seen that α-Ni0.5Co0.5 Quality specific capacitance it is maximum, material electrochemical performance is very excellent.
Embodiment 3：
Step one：By 0.23 g (8 mmol/L) Nickelous nitrate hexahydrate, 0.47 g (16 mmol/L) cabaltous nitrate hexahydrates and
0.67 g (48 mmol/L) ammonium of six methine four is dissolved in 100 mL water, is stirred at room temperature, it is fully dissolved, and obtains powder
Grey dispersion liquid；
Step 2：To 100 mL solvents are added in the powder grey dispersion liquid that step one is obtained, it is stirred at room temperature and is uniformly dispersed, obtains
To question response liquid；
Step 3：The question response liquid that step 2 is obtained is transferred to 300 mL round-bottomed flasks, 120oCondensing reflux reaction 2 under C
Room temperature is naturally cooled to after h, presoma is obtained；
Step 4：The presoma that step 3 is obtained is collected by centrifugation and washed, and carries out freeze-drying and obtain the compound hydrogen of nickel cobalt
Oxide, wherein sublimation drying are 18 h.When the solvent described in the step 2 is ethylene glycol, reaction obtains α types nickel cobalt and answers
Close hydroxide（Nickel-to-cobalt ratio 1:2）, when the solvent is ethanol, reaction obtains β type nickel cobalt complex hydroxides（Nickel-to-cobalt ratio
1:2）, it is respectively labeled as α-Ni0.33Co0.67 With β-Ni0.33Co0.67 。
Embodiment 4：
Step one：By 0.70 g (96 mmol/L) cabaltous nitrate hexahydrates and 0.67 g (192 mmol/L) ammonium of six methine four
It is dissolved in 25 mL water, stirs at room temperature, it is fully dissolved, obtains pink dispersion liquid；
Step 2：To 25 mL solvents are added in the pink dispersion liquid that step one is obtained, it is stirred at room temperature and is uniformly dispersed, obtains
To question response liquid；
Step 3：The question response liquid that step 2 is obtained is transferred to 100 mL round-bottomed flasks, 110oCondensing reflux reaction 8 under C
Room temperature is naturally cooled to after h, presoma is obtained；
Step 4：The presoma that step 3 is obtained is collected by centrifugation and washed, and carries out freeze-drying and obtain the compound hydrogen of nickel cobalt
Oxide, wherein sublimation drying are 24 h.When the solvent described in the step 2 is ethylene glycol, reaction obtains α type hydroxides
Cobalt, when the solvent is ethanol, reaction obtains β type cobalt hydroxides, is respectively labeled as α-Co (OH)2 With β-Co (OH)2 。
From Fig. 4 (b, d) it can be seen that α-Co (OH)2Pattern be very thin laminated structure.
Claims (5)
1. the preparation method of the controllable nickel cobalt hydroxide of a kind of crystal formation, it is characterised in that by changing solvent, optionally prepare
Go out the controllable nickel cobalt hydroxide of crystal formation, comprise the following steps：
Step one：Cobalt nitrate, nickel nitrate and the ammonium of six methine four are dissolved in the water, are stirred at room temperature, make it fully molten
Solution, obtains dispersion liquid；
Step 2：To solvent is added in the dispersion liquid that step one is obtained, dispersed with stirring is uniform at room temperature, obtains question response liquid, when
When nickel cobalt hydroxide is α types, the solvent is ethylene glycol, and when nickel cobalt hydroxide is β types, the solvent is ethanol；
Step 3：Question response liquid constant temperature and the condensing reflux reaction that step 2 is obtained, obtain presoma；
Step 4：Presoma centrifugation that step 3 is obtained, washing, and carry out freeze-drying and obtain nickel cobalt hydroxide.
2. preparation method as claimed in claim 1, it is characterised in that in step one, the total ion concentration of nickel cobalt is 20 ~ 100
Mmol/L, the ammonium of six methine four is 2 with the mol ratio of nickel cobalt element total amount:1.
3. preparation method as claimed in claim 1, it is characterised in that in step 2, volume and step one reclaimed water of solvent
Volume is identical.
4. preparation method as claimed in claim 1, it is characterised in that in step 3, reaction temperature is 80 ~ 120oC, during reaction
Between be 2 ~ 8 h.
5. preparation method as claimed in claim 1, it is characterised in that sublimation drying is 6 ~ 24 h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108609668A (en) * | 2018-06-12 | 2018-10-02 | 池州学院 | A kind of nanometer of α-Ni (OH)2Improvement synthetic method |
| CN114335448A (en) * | 2022-01-04 | 2022-04-12 | 湖北大学 | Nickel-cobalt hydroxide with multilayer nanosheet structure and preparation method and application thereof |
| CN116216796A (en) * | 2023-04-25 | 2023-06-06 | 荆门市格林美新材料有限公司 | Modified nickel-manganese binary precursor and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102509628A (en) * | 2011-09-29 | 2012-06-20 | 南开大学 | Nanometre Ni(OH)2 and Co(OH)2 composite material for super-capacitor and preparation method of nanometre Ni(OH)2 and Co(OH)2 composite material |
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2017
- 2017-03-03 CN CN201710122754.8A patent/CN106882846B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102509628A (en) * | 2011-09-29 | 2012-06-20 | 南开大学 | Nanometre Ni(OH)2 and Co(OH)2 composite material for super-capacitor and preparation method of nanometre Ni(OH)2 and Co(OH)2 composite material |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108609668A (en) * | 2018-06-12 | 2018-10-02 | 池州学院 | A kind of nanometer of α-Ni (OH)2Improvement synthetic method |
| CN114335448A (en) * | 2022-01-04 | 2022-04-12 | 湖北大学 | Nickel-cobalt hydroxide with multilayer nanosheet structure and preparation method and application thereof |
| CN114335448B (en) * | 2022-01-04 | 2023-10-31 | 湖北大学 | Nickel-cobalt hydroxide with multilayer nano-sheet structure, and preparation method and application thereof |
| CN116216796A (en) * | 2023-04-25 | 2023-06-06 | 荆门市格林美新材料有限公司 | Modified nickel-manganese binary precursor and preparation method and application thereof |
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