CN109110822A - A kind of preparation method of quickly synthesizing porous cobalt acid zinc electrode material - Google Patents

A kind of preparation method of quickly synthesizing porous cobalt acid zinc electrode material Download PDF

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CN109110822A
CN109110822A CN201810998882.3A CN201810998882A CN109110822A CN 109110822 A CN109110822 A CN 109110822A CN 201810998882 A CN201810998882 A CN 201810998882A CN 109110822 A CN109110822 A CN 109110822A
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acid zinc
cobalt acid
room temperature
deionized water
porous
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徐春菊
孙家乐
王晋鹏
韩兴荣
陈慧玉
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North University of China
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00Compounds of cobalt
    • C01G51/40Cobaltates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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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    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
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    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/10Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/13Nanotubes
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    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/20Particle morphology extending in two dimensions, e.g. plate-like
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions
    • C01P2004/32Spheres
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    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer

Abstract

The invention discloses a kind of porous classification micro nano structure synthetic methods of cobalt acid zinc, include the following steps: the Zn (NO of 1, molar ratio 1:23)2•6H2O、Co(NO3)2•6H2O is dissolved in deionized water and ethylene glycol mixed solution under room temperature, obtains clear solution;2, it is dissolved in the resulting solution of step 1, is sufficiently stirred under urea room temperature;3, step 2 acquired solution is transferred in polytetrafluoroethyllining lining stainless steel cauldron, is sealed, 3 ~ 15h is reacted at 100 ~ 200 DEG C;4, after reaction, cooled to room temperature;Centrifugation, is respectively washed 3 times with deionized water and dehydrated alcohol, dry, and zinc cobalt-presoma can be obtained;5, step 4 gained powder is calcined in air;Calcination temperature is 350 ~ 600 DEG C, and calcination time is 2 ~ 10h, and heating rate is 1 ~ 15 DEG C of min‑1.The method of the present invention can synthesize to obtain the porous micro nano structure of different-shape cobalt acid zinc by simply regulation experiment parameter.

Description

A kind of preparation method of quickly synthesizing porous cobalt acid zinc electrode material
Technical field
The present invention relates to the preparation field of transition metal oxide cobalt acid zinc, specially a kind of porous classification microballoon and nanometer The preparation method of the transition metal oxide electrode material of chip architecture.
Background technique
In recent years, as energy requirement sustainable growth, energy consumption, environmental pollution increasingly aggravate, force people's exploitation can Sustainable development energy storage technology.Supercapacitor is with its large capacity, high power density (1 ~ 10kW kg-1), the long-life (100,000 times with On), fast charging and discharging, low cost, advantages of environment protection and be considered as extremely promising electrochemical energy storage device, cause The very big concern of researcher.
Currently, electrode material for super capacitor mainly has carbon-based material, transition metal oxide, conducting polymer.Ternary Oxide is capable of providing redox reaction abundant and by favor due to its changeable valent state.It is not only inherited The high specific capacitance of two-spot oxide, at the same it is bimetallic exist also improve the structural stability of material, electric conductivity, forthright again Energy, cyclical stability etc..The theoretical specific capacitance of spinel structure cobalt acid zinc is 2604F g-1, there is variable metal state, lead Electrically good, environmental-friendly, resourceful and at low cost advantage, it is considered to be one of most promising electrode material is answered extensively For fields such as supercapacitor and lithium ion batteries.
Summary of the invention
It is an object of the present invention to provide a kind of simple preparation methods of the porous classification microballoon and nanometer chip architecture of cobalt acid zinc, and The method of the present invention can synthesize to obtain the porous micro nano structure of different-shape cobalt acid zinc by simply regulation experiment parameter.
The present invention is achieved by the following technical solutions:
A kind of preparation method of quickly synthesizing porous cobalt acid zinc electrode material, comprising the following steps:
(1), a certain amount of Zn (NO is weighed3)2•6H2O、Co(NO3)2•6H2O, the two molar ratio are 1:2, are dissolved under room temperature In ionized water and ethylene glycol mixed solution, clear solution is obtained;
(2), a certain amount of urea is weighed, is dissolved in step (1) resulting solution, is sufficiently stirred under room temperature;
(3), step (2) acquired solution is transferred in polytetrafluoroethyllining lining stainless steel cauldron, is sealed, 100 DEG C ~ 200 3 ~ 15h is reacted at DEG C;
(4), after reaction, cooled to room temperature;Centrifugation, is respectively washed 3 times with deionized water and dehydrated alcohol, dry, Zinc cobalt-presoma can be obtained;
(5), powder obtained by step (4) is calcined in air;Calcination temperature is 350 DEG C ~ 600 DEG C, and calcination time is 2 ~ 10h, Heating rate is 1 ~ 15 DEG C of min-1
Further, amount of urea is 5 ~ 60a mol, and wherein a is equal to Zn (NO3)2•6H2The mole of O.
Compared with prior art, the present invention has the advantage that
1, it can synthesize to obtain the micro nano structure of different-shape cobalt acid zinc, especially cobalt acid zinc by simply regulating and controlling experiment parameter Porous classification microballoon and nanometer chip architecture.
2, product specific surface area is larger, electrochemical performance.
3, at low cost, energy fast low temperature synthesis.
4, preparation process is environmentally friendly, pollution-free.
The present invention has rational design, has good market application prospect and promotional value.
Detailed description of the invention
Fig. 1 shows X-ray diffraction (XRD) figures of the porous classification microballoon of cobalt acid zinc obtained by embodiment 1.
Fig. 2 indicates low power scanning electron microscope (SEM) photo of the porous classification microballoon of cobalt acid zinc obtained by embodiment 1.
Fig. 3 indicates the high power SEM photograph of the porous classification microballoon of cobalt acid zinc obtained by embodiment 1.
Fig. 4 indicates transmission electron microscope (TEM) photo of the porous classification microballoon of cobalt acid zinc obtained by embodiment 1.
Fig. 5 indicates cobalt acid zinc porous nano-sheet SEM photograph obtained by embodiment 2.
Fig. 6 indicates the porous micro nano structure SEM photograph of cobalt acid zinc obtained by embodiment 3.
Fig. 7 indicates the porous classification micro nano structure SEM photograph of cobalt acid zinc obtained by embodiment 4.
Fig. 8 shows the porous micro nano structure SEM photographs of cobalt acid zinc obtained by embodiment 5.
Fig. 9 indicates the porous micro nano structure SEM photograph of cobalt acid zinc obtained by embodiment 6.
Specific embodiment
Specific embodiments of the present invention are described in detail with reference to the accompanying drawing.
The present invention is that the porous micro-nano electrode material of cobalt acid zinc is prepared by a kind of simple solvent thermal method, anti-by controlling Between seasonable, the process conditions such as reaction temperature, solvent ratio, amount of urea, it is porous that the cobalt acid zinc with different-shape can be synthesized Micro Nano material.Specific embodiment is shown in the preparation method of the porous classification microballoon and nanometer chip architecture of following cobalt acid zinc.
Embodiment 1
A kind of synthetic method of the porous classification microballoon of cobalt acid zinc, comprising the following steps:
(1), 0.297g Zn (NO is weighed3)2•6H2O, 0.583g Co (NO3)2•6H2O is dissolved in 20mL deionized water under room temperature In 20mL ethylene glycol mixed solution, clear solution is obtained;
(2), 0.30g urea is weighed, is dissolved in step (1) resulting solution, is sufficiently stirred under room temperature;
(3), step (2) acquired solution is transferred in 50mL polytetrafluoroethyllining lining stainless steel cauldron, is sealed, at 120 DEG C Lower reaction 3h;
(4), after reaction, cooled to room temperature;Centrifugation, is respectively washed 3 times with deionized water and dehydrated alcohol, dry, Zinc cobalt-presoma can be obtained;
(5), by powder obtained by step (4), 400 DEG C of calcining 2h, heating rate are 5 DEG C of min in air-1
(6), sample is subjected to pattern, phase characterization, BET specific surface area analysis and electro-chemical test, final product XRD spectrum shows that all diffraction maximums correspond to the diffraction maximum of spinelle cubic phase cobalt acid zinc, illustrates that product purity is very high (see figure 1);High and low times of SEM photograph shows that cobalt acid zinc microballoon is made of a large amount of nanometer sheets interconnected, and microsphere diameter is about 5 ~ 6 μm (see Fig. 2,3);As can be seen that the nanometer sheet of composition cobalt acid zinc microballoon has porous character (see figure from the TEM photo of cobalt acid zinc 4);Nitrogen adsorption-desorption curve of cobalt acid zinc belongs to IV type, BET specific surface area 67.1m2∙g-1, average pore size 28.6nm. Excellent chemical property, 1A g are shown when the porous classification microballoon of cobalt acid zinc is as electrode material-1When have 689F g-1's High specific capacitance, and in 15A g-1There is down 81.3% capacity retention, illustrate that product has excellent high rate performance.In 5A g-1 Under current density, after 5000 circulations, specific capacitance still maintains 98.7%, and coulombic efficiency is about 98.5%, shows that electrode has There is fabulous cyclical stability.
Embodiment 2
A kind of synthetic method of cobalt acid zinc porous nano chip architecture, comprising the following steps:
(1), 0.297g Zn (NO is weighed3)2•6H2O, 0.583g Co (NO3)2•6H240mL deionized water is dissolved under O room temperature In, obtain clear solution;
(2), 0.90g urea is weighed, is dissolved in step (1) resulting solution, is sufficiently stirred under room temperature;
(3), step (2) acquired solution is transferred in 50mL polytetrafluoroethyllining lining stainless steel cauldron, is sealed, at 180 DEG C Lower reaction 3h;
(4), after reaction, cooled to room temperature;Centrifugation, is respectively washed 3 times with deionized water and dehydrated alcohol, dry, Zinc cobalt-presoma can be obtained;
(5), by powder obtained by step (4), 400 DEG C of calcining 2h, heating rate are 5 DEG C of min in air-1
(6), sample is subjected to morphology characterization, SEM shows that final product is cobalt acid zinc porous nano-sheet (see figure 5).
Embodiment 3
A kind of synthetic method of the porous micro nano structure of cobalt acid zinc, comprising the following steps:
(1), 0.297g Zn (NO is weighed3)2•6H2O, 0.583g Co (NO3)2•6H2It is dissolved under O room temperature in 40mL ethylene glycol, Obtain clear solution;
(2), 0.90g urea is weighed, is dissolved in step (1) resulting solution, is sufficiently stirred under room temperature;
(3), step (2) acquired solution is transferred in 50mL polytetrafluoroethyllining lining stainless steel cauldron, is sealed, at 180 DEG C Lower reaction 3h;
(4), after reaction, cooled to room temperature;Centrifugation, is respectively washed 3 times with deionized water and dehydrated alcohol, dry, Zinc cobalt-presoma can be obtained;
(5), by powder obtained by step (4), 400 DEG C of calcining 2h, heating rate are 5 DEG C of min in air-1
(6), sample is subjected to morphology characterization, SEM shows that products therefrom is cobalt acid zinc microballoon, and diameter is about 3 ~ 7 μm, surface Relatively rough, microballoon is made of nanoparticle;And there is the nano particle (see figure 6) being scattered on a small quantity.
Embodiment 4
A kind of synthetic method of the porous classification micro nano structure of cobalt acid zinc, comprising the following steps:
(1), 0.297g Zn (NO is weighed3)2•6H2O, 0.583g Co (NO3)2•6H2Be dissolved under O room temperature 20mL deionized water and In 20mL ethylene glycol, clear solution is obtained;
(2), 0.90g urea is weighed, is dissolved in step (1) resulting solution, is sufficiently stirred under room temperature;
(3), step (2) acquired solution is transferred in 50mL polytetrafluoroethyllining lining stainless steel cauldron, is sealed, at 120 DEG C Lower reaction 6h;
(4), after reaction, cooled to room temperature;Centrifugation, is respectively washed 3 times with deionized water and dehydrated alcohol, dry, Zinc cobalt-presoma can be obtained;
(5), by powder obtained by step (4), 400 DEG C of calcining 2h, heating rate are 5 DEG C of min in air-1
(6), sample is subjected to morphology characterization, the cobalt acid zinc that SEM shows that products therefrom is mainly made of porous nano needle is micro- Ball, diameter are about 2 ~ 4.5 μm;Also comprising a small amount of porous nano-sheet and the microballoon (see figure 7) being made of porous nano-sheet.
Embodiment 5
A kind of synthetic method of the porous micro nano structure of cobalt acid zinc, comprising the following steps:
(1), 0.297g Zn (NO is weighed3)2•6H2O, 0.583g Co (NO3)2•6H2Be dissolved under O room temperature 8mL deionized water and In 32mL ethylene glycol, clear solution is obtained;
(2), 0.30g urea is weighed, is dissolved in step (1) resulting solution, is sufficiently stirred under room temperature;
(3), step (2) acquired solution is transferred in 50mL polytetrafluoroethyllining lining stainless steel cauldron, is sealed, at 120 DEG C Lower reaction 3h;
(4), after reaction, cooled to room temperature;Centrifugation, is respectively washed 3 times with deionized water and dehydrated alcohol, dry, Zinc cobalt-presoma can be obtained;
(5), by powder obtained by step (4), 400 DEG C of calcining 2h, heating rate are 5 DEG C of min in air-1
(6), sample is subjected to morphology characterization, SEM shows that products therefrom is cobalt acid zinc nanoparticles, and has becoming for balling-up Gesture (see figure 8).
Embodiment 6
A kind of synthetic method of the porous classification micro nano structure of cobalt acid zinc, comprising the following steps:
(1), 0.297g Zn (NO is weighed3)2•6H2O, 0.583g Co (NO3)2•6H2Be dissolved under O room temperature 20mL deionized water and In 20mL ethylene glycol, clear solution is obtained;
(2), 3.60g urea is weighed, is dissolved in step (1) resulting solution, is sufficiently stirred under room temperature;
(3), step (2) acquired solution is transferred in 50mL polytetrafluoroethyllining lining stainless steel cauldron, is sealed, at 120 DEG C Lower reaction 3h;
(4), after reaction, cooled to room temperature;Centrifugation, is respectively washed 3 times with deionized water and dehydrated alcohol, dry, Zinc cobalt-presoma can be obtained;
(5), by powder obtained by step (4), 400 DEG C of calcining 2h, heating rate are 5 DEG C of min in air-1
(6), sample is subjected to morphology characterization, SEM shows that products therefrom is to be made of porous nano needle and porous nano-sheet Cobalt acid zinc microballoon, diameter is about 2.5 ~ 4.5 μm and minimal amount of porous nano-sheet (see figure 9).
It should be pointed out that for the those skilled in the art of the art, without departing from the principle of the present invention, Several improvement and application can also be made, these are improved and application is also considered as protection scope of the present invention.

Claims (4)

1. a kind of preparation method of quickly synthesizing porous cobalt acid zinc electrode material, characterized by the following steps:
(1), Zn (NO is weighed3)2•6H2O、Co(NO3)2•6H2O, the molar ratio of the two are 1:2, are dissolved in deionized water under room temperature In ethylene glycol mixed solution, clear solution is obtained;
(2), urea is weighed, is dissolved in step (1) resulting solution, is sufficiently stirred under room temperature;
(3), step (2) acquired solution is transferred in polytetrafluoroethyllining lining stainless steel cauldron, is sealed, 100 DEG C ~ 200 3 ~ 15h is reacted at DEG C;
(4), after reaction, cooled to room temperature;Centrifugation, is respectively washed 3 times with deionized water and dehydrated alcohol, dry, Zinc cobalt-presoma can be obtained;
(5), powder obtained by step (4) is calcined in air;Calcination temperature is 350 DEG C ~ 600 DEG C, and calcination time is 2 ~ 10h, Heating rate is 1 ~ 15 DEG C of min-1
2. a kind of preparation method of quickly synthesizing porous cobalt acid zinc electrode material according to claim 1, it is characterised in that: In step (1), the volume of deionized water and ethylene glycol is 1:0 ~ 0:1.
3. a kind of preparation method of quickly synthesizing porous cobalt acid zinc electrode material according to claim 1, it is characterised in that: In step (2), the amount of urea is 5 ~ 60a mol, and wherein a is equal to Zn (NO3)2•6H2The mole of O.
4. a kind of preparation method of quickly synthesizing porous cobalt acid zinc electrode material according to claim 1, it is characterised in that: In step (5), calcination temperature is 400 DEG C, calcination time 2h, and heating rate is 5 DEG C of min-1
CN201810998882.3A 2018-08-30 2018-08-30 A kind of preparation method of quickly synthesizing porous cobalt acid zinc electrode material Pending CN109110822A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110203976A (en) * 2019-05-16 2019-09-06 中北大学 Rapid synthesis flakes ZnCo2O4The preparation method of-ZnO compound electric grade material
CN110745872A (en) * 2019-11-29 2020-02-04 福州大学 Spherical porous high specific capacitance composite electrode material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110203976A (en) * 2019-05-16 2019-09-06 中北大学 Rapid synthesis flakes ZnCo2O4The preparation method of-ZnO compound electric grade material
CN110745872A (en) * 2019-11-29 2020-02-04 福州大学 Spherical porous high specific capacitance composite electrode material and preparation method thereof

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