CN110203976A - Rapid synthesis flakes ZnCo2O4The preparation method of-ZnO compound electric grade material - Google Patents

Rapid synthesis flakes ZnCo2O4The preparation method of-ZnO compound electric grade material Download PDF

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CN110203976A
CN110203976A CN201910407662.3A CN201910407662A CN110203976A CN 110203976 A CN110203976 A CN 110203976A CN 201910407662 A CN201910407662 A CN 201910407662A CN 110203976 A CN110203976 A CN 110203976A
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znco
flakes
zno
coo
preparation
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陈慧玉
杜旭明
吴润泽
韩兴荣
徐春菊
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North University of China
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/40—Cobaltates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/02—Oxides; Hydroxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/46—Metal oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/16—Pore diameter
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13—Energy storage using capacitors

Abstract

The invention discloses a kind of porous flakes ZnCo2O4The micro nano structure synthetic method of/ZnO combination electrode material includes the following steps: (1), weighs Zn (CH3COO)2·2H2O and Co (CH3COO)2·4H2O；(2), urea is weighed to be dissolved in step (1) acquired solution；(3), NH is weighed4F is dissolved in step (2) acquired solution；(4), acquired solution is transferred in reaction kettle, 1 ~ 12h is reacted at 100 ~ 200 DEG C；(5), after reaction, cooling eccentric cleaning is dry to get presoma；(6), gained powder is calcined, 350 ~ 800 DEG C of calcination temperature, 2 ~ 10h of calcination time, 1 ~ 15 DEG C of min of heating rate‑1.The method of the present invention can synthesize to obtain the porous ZnCo of flakes pattern by simply regulation experiment parameter2O4/ ZnO combination electrode material micro nano structure.

Description

Rapid synthesis flakes ZnCo2O4The preparation method of-ZnO compound electric grade material
Technical field
The present invention relates to the preparation fields of transition metal combination electrode material, specially a kind of to have porous flakes multistage The transition metal oxide ZnCo of structure2O4The preparation method of/ZnO combination electrode material.
Background technique
Supercapacitor is because of its large capacity, high power density, excellent stable circulation performance, fast charging and discharging ability, low Cost, advantages of environment protection are in hybrid vehicle, industrial electrical, portable device, national defence troops' use and storage system etc. Various fields have huge potential using value.
Relative to carbon material specific capacitance with higher, facing conductive polymer is with higher to follow transition metal oxide Ring stability, so that become one kind has potential electrode material for super capacitor very much.Spinel structure ZnCo2O4Due to it The advantages that element compounds valence state abundant, good electric conductivity, environmental-friendly, extensive raw material sources and low cost, is in electrode material Material aspect causes many research interests.Since electrode material usually can participate in the real area of faraday's redox reaction Very limited, the more difficult effective use of electrode interior material leads to ZnCo2O4Practical specific capacitance far below its theoretical capacitor (2604F g-1).By ZnCo2O4The compound synergistic effect for playing two kinds of materials is carried out with other metal oxides, to be expected to Improve its chemical property.
Summary of the invention
It is an object of the present invention to provide a kind of ZnCo of porous flakes multilevel structure2O4/ ZnO combination electrode material is simply made Preparation Method, the ZnCo synthesized using one step hydro thermal method2O4/ ZnO composite material has many advantages, such as easy to operate, at low cost, passes through letter Single control experiment parameter can get the ZnCo of different flakes morphology and sizes2O4/ ZnO micro nano structure, and can obtain different Chemical property can be applied to supercapacitor field.
The present invention is achieved by the following technical scheme:
A kind of rapid synthesis flakes ZnCo2O4The preparation method of-ZnO compound electric grade material, includes the following steps:
(1), Zn (CH is weighed3COO)2·2H2O、Co(CH3COO)2·4H2O, the molar ratio of the two are 1:2, are dissolved under room temperature In deionized water, clear solution is obtained；
(2), urea is weighed, is dissolved in step (1) resulting solution, is sufficiently stirred under room temperature；
(3), NH is weighed4F is dissolved in step (2) resulting solution under room temperature, is sufficiently stirred；
(4), step (3) acquired solution is transferred in polytetrafluoroethyllining lining stainless steel cauldron, is sealed, 100 DEG C ~ 200 1 ~ 12h is reacted at DEG C；
(5), after reaction, cooled to room temperature；Centrifugation, is respectively washed 3 times with deionized water and dehydrated alcohol, dry, Presoma can be obtained；
(6), precursor powder obtained by step (5) is calcined in air；Calcination temperature is 350 DEG C ~ 800 DEG C, calcination time 2 ~ 10h, heating rate are 1 ~ 15 DEG C of min-1, i.e. acquisition flakes ZnCo2O4- ZnO compound electric grade material.
Further, in step (2), the amount of urea is 5 ~ 25amol, and wherein a is equal to Zn (CH3COO)2·2H2O's Mole.
Further, in step (3), the NH4F dosage is 2.5 ~ 15amol, and wherein a is equal to Zn (CH3COO)2·2H2O Mole.
Compared with prior art, the present invention has the advantage that
1, ZnCo is quickly and easily synthesized by one step hydro thermal method2O4/ ZnO micro nano structure combination electrode material.
2, it can synthesize to obtain the ZnCo of different-shape and size by simply regulating and controlling experiment parameter2O4The micro-nano knot of/ZnO Structure, especially porous flakes multilevel structure；Reaction process is simple, the reaction time is short；Device simple, preparation process be simple, nothing Need surfactant and template, at low cost；Product preparation process is easy to control, is reproducible, can be mass-produced；Preparation process In do not generate harmful toxic matter, no pollution to the environment；Obtained flakes ZnCo2O4/ ZnO multilevel structure size uniformity, dispersibility It is good.
3, the porous flakes ZnCo that the method for the present invention is prepared2O4/ ZnO combination electrode material, specific surface area reach 32.3m2g-1, average pore size 16.4nm.The combination electrode material has very high specific capacitance and high rate performance, in current density For 1Ag-1When specific capacitance be 827Fg-1；Current density increases to 15Ag-1, high rate performance 69.6%；The structure has good Electrochemical stability, 5Ag-1By 5000 circulations under current density, specific capacitance conservation rate is 68.7%, and coulombic efficiency 99.3%.The above result shows that porous flakes ZnCo2O4/ ZnO composite material is a kind of excellent electrode material for super capacitor.
The present invention has rational design, has the application of good market and promotional value.
Detailed description of the invention
Fig. 1 shows the porous flakes ZnCo of the preparation gained of embodiment 12O4The X-ray diffraction of/ZnO combination electrode material (XRD) figure.
Fig. 2 indicates the porous flakes ZnCo of the preparation gained of embodiment 12O4The scanning electron microscopy of/ZnO combination electrode material Mirror (SEM) photo.
Fig. 3 indicates the porous flakes ZnCo of the preparation gained of embodiment 12O4The transmission electron microscopy of/ZnO combination electrode material Mirror (TEM) photo.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.
The embodiment of the present invention is to prepare ZnCo by simple one step hydro thermal method2O4The micro-nano combination electrode material of/ZnO, By process conditions such as control reaction time, reaction temperature, ammonium fluoride dosage, amount of urea, can synthesize with flakes The porous ZnCo of pattern2O4The micro-nano combination electrode material of/ZnO.
Embodiment 1
A kind of rapid synthesis flakes ZnCo2O4The preparation method of-ZnO compound electric grade material, includes the following steps:
(1), 1mmol Zn (CH is weighed3COO)2·2H2O, 2mmol Co (CH3COO)2·4H2O is dissolved in 40mL under room temperature In ionized water, clear solution is obtained；
(2), 5mmol urea is weighed, is dissolved in step (1) resulting solution, is sufficiently stirred under room temperature；
(3), 2.7mmol NH is weighed4F is dissolved in step (2) resulting solution under room temperature, is sufficiently stirred；
(4), step (3) acquired solution is transferred in 50mL polytetrafluoroethyllining lining stainless steel cauldron, is sealed, at 120 DEG C Lower reaction 1h；
(5), after reaction, cooled to room temperature；Centrifugation, is respectively washed 3 times with deionized water and dehydrated alcohol, dry, Presoma can be obtained；
(6), by powder obtained by step (5), 450 DEG C of calcining 4h, heating rate are 2 DEG C of min in air-1, obtain ZnCo2O4/ ZnO solid combination electrode material.
(7), 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 respectively correspond ZnCo2O4With the diffraction maximum of ZnO, illustrate that product is by ZnCo2O4It is formed with ZnO (see figure 1)；SEM photograph shows that product is by flakes ZnCo2O4/ ZnO composition, having a size of 4 μm；And single snowflake structure be by Six symmetrical petals that length is 1.5 μm form (see figure 2)；From ZnCo2O4It can be seen that in the TEM photo of/ZnO composite material Flakes ZnCo2O4/ ZnO material has porous character (see figure 3)；ZnCo2O4Nitrogen adsorption-desorption curve of/ZnO belongs to IV Type, BET specific surface area 32.3m2∙g-1, average pore size 16.4nm.By electro-chemical test, which shows excellent Different chemical property, in 1A g-1When have 827F g-1High specific capacitance；In 15A g-1There is down 69.6% capacity retention, Illustrate that product has excellent high rate performance；In 5A g-1It is lower that specific capacitance still keeps initial 68.7% after 5000 circulations, Coulombic efficiency is about 99.3%, shows preferable cyclical stability.
Embodiment 2
A kind of rapid synthesis flakes ZnCo2O4The preparation method of-ZnO compound electric grade material, includes the following steps:
(1), 1mmol Zn (CH is weighed3COO)2·2H2O, 2mmol Co (CH3COO)2·4H2O is dissolved in 40mL under room temperature In ionized water, clear solution is obtained；
(2), 10mmol urea is weighed, is dissolved in step (1) resulting solution, is sufficiently stirred under room temperature；
(3), 2.7mmol NH is weighed4F is dissolved in step (2) resulting solution under room temperature, is sufficiently stirred；
(4), step (3) acquired solution is transferred in 50mL polytetrafluoroethyllining lining stainless steel cauldron, is sealed, at 165 DEG C Lower reaction 1h；
(5), after reaction, cooled to room temperature；Centrifugation, is respectively washed 3 times with deionized water and dehydrated alcohol, dry, Presoma can be obtained；
(6), by powder obtained by step (5), 600 DEG C of calcining 2h, heating rate are 5 DEG C of min in air-1, obtain ZnCo2O4/ ZnO solid combination electrode material.
Embodiment 3
A kind of rapid synthesis flakes ZnCo2O4The preparation method of-ZnO compound electric grade material, includes the following steps:
(1), 1mmol Zn (CH is weighed3COO)2·2H2O, 2mmol Co (CH3COO)2·4H2O is dissolved in 40mL under room temperature In ionized water, clear solution is obtained；
(2), 20mmol urea is weighed, is dissolved in step (1) resulting solution, is sufficiently stirred under room temperature；
(3), 13.5mmol NH is weighed4F is dissolved in step (2) resulting solution under room temperature, is sufficiently stirred；
(4), step (3) acquired solution is transferred in 50mL polytetrafluoroethyllining lining stainless steel cauldron, is sealed, at 180 DEG C Lower reaction 5h；
(5), after reaction, cooled to room temperature；Centrifugation, is respectively washed 3 times with deionized water and dehydrated alcohol, dry, Presoma can be obtained；
(6), by powder obtained by step (5), 800 DEG C of calcining 4h, heating rate are 2 DEG C of min in air-1, obtain ZnCo2O4/ ZnO solid combination electrode material.
Embodiment 4
A kind of rapid synthesis flakes ZnCo2O4The preparation method of-ZnO compound electric grade material, includes the following steps:
(1), 1mmol Zn (CH is weighed3COO)2·2H2O, 2mmol Co (CH3COO)2·4H2O is dissolved in 40mL under room temperature In ionized water, clear solution is obtained；
(2), 10mmol urea is weighed, is dissolved in step (1) resulting solution, is sufficiently stirred under room temperature；
(3), 8.1mmol NH is weighed4F is dissolved in step (2) resulting solution under room temperature, is sufficiently stirred；
(4), step (3) acquired solution is transferred in 50mL polytetrafluoroethyllining lining stainless steel cauldron, is sealed, at 150 DEG C Lower reaction 8h；
(5), after reaction, cooled to room temperature；Centrifugation, is respectively washed 3 times with deionized water and dehydrated alcohol, dry, Presoma can be obtained；
(6), by powder obtained by step (5), 450 DEG C of calcining 7h, heating rate are 10 DEG C of min in air-1, obtain ZnCo2O4/ ZnO solid combination electrode material.
Above embodiments are only to illustrate the present invention rather than limit, it will be appreciated by those skilled in the art that in the present invention Appearance is modified or replaced equivalently, without departure from range described in the claims in the present invention.

Claims (3)

1. a kind of rapid synthesis flakes ZnCo2O4The preparation method of-ZnO compound electric grade material, it is characterised in that: including as follows Step:
(1), Zn (CH is weighed3COO)2·2H2O、Co(CH3COO)2·4H2O, the molar ratio of the two are 1:2, are dissolved under room temperature In deionized water, clear solution is obtained；
(2), urea is weighed, is dissolved in step (1) resulting solution, is sufficiently stirred under room temperature；
(3), NH is weighed4F is dissolved in step (2) resulting solution under room temperature, is sufficiently stirred；
(4), step (3) acquired solution is transferred in polytetrafluoroethyllining lining stainless steel cauldron, is sealed, 100 DEG C ~ 200 1 ~ 12h is reacted at DEG C；
(5), after reaction, cooled to room temperature；Centrifugation, is respectively washed 3 times with deionized water and dehydrated alcohol, dry, Presoma can be obtained；
(6), precursor powder obtained by step (5) is calcined in air；Calcination temperature is 350 DEG C ~ 800 DEG C, calcination time 2 ~ 10h, heating rate are 1 ~ 15 DEG C of min-1。
2. rapid synthesis flakes ZnCo according to claim 12O4The preparation method of/ZnO combination electrode material, it is special Sign is: in step (2), the amount of urea is 5 ~ 25amol, and wherein a is equal to Zn (CH3COO)2·2H2The mole of O.
3. rapid synthesis flakes ZnCo according to claim 12O4The preparation method of/ZnO combination electrode material, it is special Sign is: in step (3), the NH4F dosage is 2.5 ~ 15amol, and wherein a is equal to Zn (CH3COO)2·2H2The mole of O.
CN201910407662.3A 2019-05-16 2019-05-16 Rapid synthesis flakes ZnCo2O4The preparation method of-ZnO compound electric grade material Pending CN110203976A (en)

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CN110988053A (en) * 2019-12-31 2020-04-10 吉林大学 Formaldehyde sensor based on zinc oxide/zinc cobaltate composite material and preparation method thereof
CN112038106A (en) * 2020-09-02 2020-12-04 广东工业大学 Electrode material, preparation method thereof and supercapacitor electrode
CN113948687A (en) * 2021-09-28 2022-01-18 江苏理工学院 MOF-based ZnO/ZnCo2O4Preparation method and application of/C composite material

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CN110563049A (en) * 2019-09-30 2019-12-13 淮阴师范学院 cobalt zinc sulfide nano material and preparation method and application thereof
CN110563049B (en) * 2019-09-30 2021-11-02 淮阴师范学院 Cobalt zinc sulfide nano material and preparation method and application thereof
CN110988053A (en) * 2019-12-31 2020-04-10 吉林大学 Formaldehyde sensor based on zinc oxide/zinc cobaltate composite material and preparation method thereof
CN110988053B (en) * 2019-12-31 2021-03-30 吉林大学 Formaldehyde sensor based on zinc oxide/zinc cobaltate composite material and preparation method thereof
CN112038106A (en) * 2020-09-02 2020-12-04 广东工业大学 Electrode material, preparation method thereof and supercapacitor electrode
CN113948687A (en) * 2021-09-28 2022-01-18 江苏理工学院 MOF-based ZnO/ZnCo2O4Preparation method and application of/C composite material
CN113948687B (en) * 2021-09-28 2023-11-03 江苏理工学院 MOF-based ZnO/ZnCo 2 O 4 Preparation method and application of/C composite material

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