CN106882846B - The preparation method of the controllable nickel cobalt hydroxide of crystal form - Google Patents
The preparation method of the controllable nickel cobalt hydroxide of crystal form Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of the controllable nickel cobalt hydroxide of crystal form.Include the following steps：Cobalt nitrate, nickel nitrate and six methines, four ammonium are dissolved in the water, stir to get dispersion liquid at room temperature by step 1；Step 2 is added solvent in the dispersion liquid obtained to step 1, stirs to get and wait for reaction solution；Step 3 waits for that reaction solution constant temperature, condensing reflux react by what step 2 obtained, obtains presoma；Step 4, it is the presoma centrifugation that step 3 is obtained, washing, dry to get to nickel cobalt hydroxide, wherein one timing of material concentration to be added, when product is α types, solvent described in step 2 is ethylene glycol, and when product is β types, the solvent is ethyl alcohol.This method that product form is controlled using solvent is easy to operate, can prepare the different nickel cobalt hydroxide of the crystal form with different electrochemical properties, be expected to obtain good application in energy storage field.
Description
Technical field
The present invention relates to a kind of preparation methods of the controllable nickel cobalt hydroxide of crystal form, belong to electrochemical material preparation field.
Background technology
Nickel cobalt hydroxide is a kind of extensive material studied and used, it has excellent chemical property.Due to it
Excellent properties can be applied to the fuel-cell catalyst of alternative noble metal.Meanwhile also having in terms of ultracapacitor
It and is widely applied, theoretical and practical specific capacitance is far above carbon material, can be as the electrode material of next-generation ultracapacitor
Material, and these potential application values also become the hot spot of investigation of materials.
In a series of application fields such as catalysis, electrochemistry, battery, the influence of the crystal form of material for performance is extensive
It proves.Research is concentrated mainly on for pattern control, and for material in terms of the electric property of nickel cobalt hydroxide materials at present
The research of crystal form and chemical property almost without.Specifically, for nickel cobalt hydroxide, α types have higher ratio
Capacitance and β types have better cyclical stability.
However, due to the diversity of nickel cobalt hydroxide crystal form, single crystal form nickel cobalt hydroxide is selectively prepared 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 form.
Invention content
The purpose of the present invention is to propose to a kind of systems of nickel cobalt hydroxide easy to operate, blanket crystal form is controllable
Preparation Method.
Realize that the technical solution of the object of the invention is：A kind of preparation method of the controllable nickel cobalt hydroxide of crystal form is led to
Change solvent is crossed, the controllable nickel cobalt hydroxide of crystal form is selectively prepared, includes the following steps：
Step 1：A certain amount of cobalt nitrate, nickel nitrate and six methines, four ammonium are dissolved in the water, stirring is equal at room temperature
It is even, so that it is fully dissolved, obtains dispersion liquid；
Step 2：Solvent is added in the dispersion liquid obtained to step 1, is dispersed with stirring at room temperature uniformly, obtains waiting reacting
Liquid, when nickel cobalt hydroxide is α types, the solvent is ethylene glycol, and when nickel cobalt hydroxide is β types, the solvent is
Ethyl alcohol；
Step 3：Reaction solution constant temperature and condensing reflux reaction are waited for by what step 2 obtained, obtain presoma；
Step 4：The presoma that step 3 is obtained is centrifuged, is washed, and is freeze-dried to obtain nickel cobalt hydroxide
Object.
Compared with prior art, the present invention has following remarkable advantage：1, preparation method is simple, mild condition, without special
The post-processing of equipment, product is easy, is highly suitable for large-scale industrial production；2, the product being prepared in different solvents is brilliant
Type is single, and crystal structure is preferable, and control effect is fine, and the preparation method of such controllable nickel cobalt hydroxide of crystal form still belongs to first
Secondary report；3, due to the control of synergistic effect and crystal form between nickel cobalt, resulting materials show excellent in electro-chemical test
Different chemical property so that its electrochemical field have boundless application prospect, also show this kind of method in addition to
Practical value outside novelty.
Invention is further described in detail with reference to the accompanying drawings and detailed description.
Description of the drawings
Fig. 1 is the preparation flow schematic diagram of the controllable nickel cobalt hydroxide of crystal form 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 nickel cobalt hydroxide sample obtained by 2 reaction condition of embodiment, wherein (a-c) α-
Ni0.5Co0.5 The TEM of sample different multiples schemes；(d-f) α-Ni0.5Co0.5 The SEM of sample different multiples schemes.
Fig. 4 is the electron microscope by nickel cobalt hydroxide sample obtained by embodiment 1 and 4 reaction conditions, wherein (a) α-Ni
(OH)2 The SEM of sample schemes；(b) α-Co(OH)2 The SEM of sample schemes；(c) α-Ni(OH)2 The TEM of sample schemes；(d) α-Co
(OH)2 The TEM of sample schemes.
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；(b) cyclic voltammetry curve of β types nickel cobalt hydroxide；(c) different nickel cobalt hydroxide
Constant current discharge curve；(d) the quality specific capacitance comparison diagram of different nickel cobalt hydroxide.
Specific implementation mode
Invention is further described in detail with reference to the accompanying drawings and detailed description.
The present invention achievees the purpose that control product form by using the different characteristics of different solvents.Specifically, make
With ethyl alcohol and water mixed solvent, the use of six methines, four ammonium is that alkali source, nickel cobalt nitrate are used as nickel and cobalt source, passes through change 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, other conditions not
Change solvent in the case of change, the ethyl alcohol of in the 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 respectively different electrochemical properties, is expected to obtain in energy storage field
To good application.
In conjunction with Fig. 1, the present invention selectively prepares the controllable nickel cobalt hydroxide of crystal form by change solvent, including
Following steps：
Step 1：A certain amount of cobalt nitrate and nickel nitrate and six methines, four ammonium are dissolved in the water, stirs, makes at room temperature
It is fully dissolved, and obtains dispersion liquid, and the wherein total ion concentration of nickel cobalt is 20 ~ 100 mmol/L, six methines, four ammonium and nickel cobalt
The molar ratio of element total amount is 2:1.
Step 2：Solvent is added in the dispersion liquid obtained to step 1, is dispersed with stirring at room temperature uniformly, obtains waiting reacting
Liquid, when nickel cobalt hydroxide is α types, the solvent is ethylene glycol, and when nickel cobalt hydroxide is β types, the solvent is
Ethyl alcohol, wherein the volume of solvent is identical as the volume of water in step 1；
Step 3：Wait for that reaction solution is transferred to round-bottomed flask by what step 2 obtained, constant temperature, condensing reflux certain time obtain
Presoma, wherein reaction temperature are 80 ~ 120oC, reaction time are 2 ~ 8 h；
Step 4：Presoma centrifugation, the washing that step 3 is obtained, and be freeze-dried, obtain the compound hydrogen-oxygen of nickel cobalt
Compound, wherein sublimation drying are 6 ~ 24 h.
With reference to embodiment and attached drawing, the present invention will be further described in detail：
Embodiment 1：
Step 1：Six methine four of 0.70 g (96 mmol/L) Nickelous nitrate hexahydrates and 0.67 g (192 mmol/L)
Ammonium is dissolved in 25 mL water, stirs at room temperature, it is made fully to dissolve, and obtains green dispersion liquid；
Step 2：25 mL solvents are added in the green dispersion liquid obtained to step 1, is stirred at room temperature and is uniformly dispersed,
It obtains waiting for reaction solution；
Step 3：Wait for that reaction solution is transferred to 100 mL round-bottomed flasks by what step 2 obtained, 80oCondensing reflux is anti-under C
Cooled to room temperature after 4 h is answered, presoma is obtained；
Step 4：The presoma that step 3 obtains is collected by centrifugation and is washed, and it is multiple to be freeze-dried to obtain nickel cobalt
Hydroxide is closed, wherein sublimation drying is 6 h.When the solvent described in the step 2 is ethylene glycol, α type hydrogen is obtained by the reaction
Nickel oxide is obtained by the reaction β type nickel hydroxides, is respectively labeled as α-Ni (OH) when the solvent is ethyl alcohol2 With β-Ni
(OH)2 。
It can verify that products therefrom is respectively α-Ni (OH) from Fig. 2 (a)2 (JCPDS No. 22-0444) and β-Ni (OH)2
(JCPDS No. 14-0117), Fig. 4 (a, c) is it can be seen that α-Ni (OH)2Pattern be very thin laminated structure.From Fig. 5 (a,
B) it can be found that being swept under speed identical（20 mV/s）, the β type nickel cobalt hydroxide redox peak position in Fig. 5 b corresponds to
It is essentially identical in the α type nickel cobalt hydroxide of identical nickel-to-cobalt ratio.However, the cyclic voltammetry curve face of β type nickel cobalt hydroxide
Product 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 1：By 0.35 g (24 mmol/L) Nickelous nitrate hexahydrate, 0.35 g (24 mmol/L) six nitric hydrates
Cobalt and 0.67 g (96 mmol/L) six methine, four ammonium are dissolved in 50 mL water, stir at room temperature, it is made fully to dissolve, obtain
To dirty-green dispersion liquid；
Step 2：50 mL solvents are added in the dirty-green dispersion liquid obtained to step 1, it is equal that dispersion is stirred at room temperature
It is even, it obtains waiting for reaction solution；
Step 3：Wait for that reaction solution is transferred to 150 mL round-bottomed flasks by what step 2 obtained, 100oCondensing reflux under C
Cooled to room temperature after 6 h is reacted, presoma is obtained；
Step 4：The presoma that step 3 obtains is collected by centrifugation and is washed, and it is multiple to be freeze-dried to obtain nickel cobalt
Hydroxide is closed, wherein sublimation drying is 12 h.When the solvent described in the step 2 is ethylene glycol, α type nickel is obtained by the reaction
Cobalt complex hydroxide（Nickel-to-cobalt ratio 1:1）, when the solvent is ethyl alcohol, β type nickel cobalt complex hydroxides are obtained by the reaction（Nickel
Cobalt is than 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 calculate lamella substantially is about 3 nm.From Fig. 5 (a, b) it can be found that being swept under speed identical（20 mV/
s）, the area for comparing cyclic voltammogram 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) is further verified 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 1：By 0.23 g (8 mmol/L) Nickelous nitrate hexahydrate, 0.47 g (16 mmol/L) cabaltous nitrate hexahydrate
It is dissolved in 100 mL water with 0.67 g (48 mmol/L) six methine, four ammonium, stirs at room temperature, it is made fully to dissolve, obtain
Powder grey dispersion liquid；
Step 2：100 mL solvents are added in the powder grey dispersion liquid obtained to step 1, it is equal that dispersion is stirred at room temperature
It is even, it obtains waiting for reaction solution；
Step 3：Wait for that reaction solution is transferred to 300 mL round-bottomed flasks by what step 2 obtained, 120oCondensing reflux under C
Cooled to room temperature after 2 h is reacted, presoma is obtained；
Step 4：The presoma that step 3 obtains is collected by centrifugation and is washed, and it is multiple to be freeze-dried to obtain nickel cobalt
Hydroxide is closed, wherein sublimation drying is 18 h.When the solvent described in the step 2 is ethylene glycol, α type nickel is obtained by the reaction
Cobalt complex hydroxide（Nickel-to-cobalt ratio 1:2）, when the solvent is ethyl alcohol, β type nickel cobalt complex hydroxides are obtained by the reaction（Nickel
Cobalt is than 1:2）, it is respectively labeled as α-Ni0.33Co0.67 With β-Ni0.33Co0.67 。
Embodiment 4：
Step 1：By 0.70 g (96 mmol/L) cabaltous nitrate hexahydrates and 0.67 g (192 mmol/L) six methines
Four ammoniums are dissolved in 25 mL water, stir at room temperature, it is made fully to dissolve, and obtain pink dispersion liquid；
Step 2：25 mL solvents are added in the pink dispersion liquid obtained to step 1, it is equal that dispersion is stirred at room temperature
It is even, it obtains waiting for reaction solution；
Step 3：Wait for that reaction solution is transferred to 100 mL round-bottomed flasks by what step 2 obtained, 110oCondensing reflux under C
Cooled to room temperature after 8 h is reacted, presoma is obtained；
Step 4：The presoma that step 3 obtains is collected by centrifugation and is washed, and it is multiple to be freeze-dried to obtain nickel cobalt
Hydroxide is closed, wherein sublimation drying is 24 h.When the solvent described in the step 2 is ethylene glycol, α type hydrogen is obtained by the reaction
Cobalt oxide is obtained by the reaction β type cobalt hydroxides, is respectively labeled as α-Co (OH) when the solvent is ethyl alcohol2 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 (4)
1. a kind of preparation method of the controllable nickel cobalt hydroxide of crystal form, which is characterized in that by changing solvent, selectively prepare
Go out the controllable nickel cobalt hydroxide of crystal form, includes the following steps：
Step 1：Cobalt nitrate, nickel nitrate and six methines, four ammonium are dissolved in the water, stirred evenly at room temperature, keeps it fully molten
Solution, obtains dispersion liquid；
Step 2：Solvent is added in the dispersion liquid obtained to step 1, is dispersed with stirring at room temperature uniformly, obtains waiting for reaction solution, when
When nickel cobalt hydroxide is α types, the solvent is ethylene glycol, and when nickel cobalt hydroxide is β types, the solvent is ethyl alcohol；
Step 3：Reaction solution constant temperature and condensing reflux reaction are waited for by what step 2 obtained, obtain presoma, reaction temperature is 80 ~
120 oC, reaction time are 2 ~ 8 h；
Step 4：The presoma that step 3 is obtained is centrifuged, is washed, and is freeze-dried to obtain nickel cobalt hydroxide.
2. preparation method as described in claim 1, which is characterized in that in step 1, the total ion concentration of nickel cobalt is 20 ~ 100
The molar ratio of mmol/L, six methines, four ammonium and nickel cobalt element total amount is 2:1.
3. preparation method as described in claim 1, which is characterized in that in step 2, water in the volume and step 1 of solvent
Volume is identical.
4. preparation method as described in claim 1, which is characterized in that sublimation drying is 6 ~ 24 h.
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| 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 |
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