CN108538618A - A kind of porous ZnO-C composite and its preparation method and application - Google Patents
A kind of porous ZnO-C composite and its preparation method and application Download PDFInfo
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- CN108538618A CN108538618A CN201810495908.2A CN201810495908A CN108538618A CN 108538618 A CN108538618 A CN 108538618A CN 201810495908 A CN201810495908 A CN 201810495908A CN 108538618 A CN108538618 A CN 108538618A
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- 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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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- 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
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- 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
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- 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 preparation methods of porous ZnO C composite electrode material for super capacitor, it uses solvent structure vanillic aldehyde to close Zn complex MOF materials first, is then calcined under high temperature anoxybiotic environment as persursor material and obtain porous ZnO C composite.Use the specific surface area of porous ZnO C made from preparation method of the present invention for 450~500m2/ g is 5A g in current density as electrode material‑1When maximum specific capacitance up to 550F g‑1, after carrying out 3000 cycle charge-discharges under high current density, the 92~97% of initial specific capacities can be kept, excellent chemical property and good stable circulation performance are can express out, be suitable for the electrode material etc. of ultracapacitor.
Description
Technical field
The invention belongs to supercapacitor technologies fields, and in particular to a kind of porous ZnO-C composite and its preparation side
Method and application.
Background technology
Since ultracapacitor can store high-energy in a short period of time and convey high power, the world is received
The concern of various countries researcher.So far, carbon material, transition metal oxide and conducting polymer are conventional Super capacitors
Electrode material, but due to the high-performance of ultracapacitor develop, application be restricted.Therefore, exploitation has high-performance
The new electrode materials of ultracapacitor are most important.
It grinds to make internal disorder or usurp and shows that ZnO is used as electrode material for super capacitor, because it is with higher capacitance, lower
It is cost, environmentally protective, and stable electrochemical property.But since the charge storage of ZnO is not sufficiently stable, operating voltage window
Stenostomia limits further application of the ZnO material in ultracapacitor field, and in order to solve this problem, scientists were once
Through attempting into ZnO electrode material to introduce carbon material, as graphene, graphene oxide, carbon nanotube, graphitic carbon nanofiber with
And carbon array etc..The introducing of carbon material increases the electric double layer capacitance value and window voltage range of composite material, however this does
The defect of method is that the binding ability between ZnO and carbon material is too poor, and electrode material is caused to be easily damaged in charge and discharge process, because
The stable circulation performance of this ultracapacitor is also poor.Therefore, design synthesis has good circulation stability and higher-energy
The ZnO complex carbon material electrodes of density are extremely urgent.
Invention content
The main purpose of the present invention is to provide a kind of porous ZnO-C composites, and Zn complex MOF is closed using vanillic aldehyde
Material carries out the calcining of high temperature anoxybiotic and obtains, and the specific surface area of gained porous ZnO-C is high, and the excellent bonding performance between ZnO and C,
It is used as electrode material for super capacitor, can express out higher energy density and good stable circulation performance, is suitble to push away
Wide application.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of porous ZnO-C composite, using vanillic aldehyde conjunction Zn complex MOF materials progress high temperature anoxybiotic calcining
At；Its specific surface area is 450~500m2/g。
In said program, the chemical formula that the vanillic aldehyde closes Zn complex is Zn (C8H7O3)2(H2O)2, molecular formula is
C16H18O8Zn is structurally characterized in that each central metallic ions Zn2+With the phenolic hydroxyl group oxygen and methoxyl group oxygen in 2 vanillic aldehyde bases
4 oxygen atoms and 2 hydrones in 2 oxygen atoms be coordinated, formed molecular complex, ligancy 6.
In said program, the preparation method that the vanillic aldehyde closes Zn complex includes the following steps：
1) zinc salt and organic base are dissolved in organic solvent, are uniformly mixed to obtain solution I；
2) vanillic aldehyde is dissolved in organic solvent, is uniformly mixed to obtain solution II；
3) step 1) acquired solution I and step 2) acquired solution II are uniformly mixed under stiring, obtain reaction solution, then will
Reaction solution carries out solvent thermal reaction, then through cooling, washing, drying, obtains vanillic aldehyde and close Zn complex MOF materials.
A kind of preparation method of above-mentioned porous ZnO-C composite, it includes the following steps：
1) zinc salt and organic base are dissolved in organic solvent, are uniformly mixed to obtain solution I；
2) vanillic aldehyde is dissolved in organic solvent, is uniformly mixed to obtain solution II；
3) step 1) acquired solution I and step 2) acquired solution II are uniformly mixed under stiring, obtain reaction solution, then will
Reaction solution carries out solvent thermal reaction, then through cooling, washing, drying, obtains vanillic aldehyde and close Zn complex MOF materials；
4) vanillic aldehyde is closed into Zn complex MOF materials and carries out anoxybiotic calcining, obtain porous ZnO-C composite materials.
In said program, zinc chloride, zinc nitrate etc. can be selected in the zinc salt.
In said program, absolute ethyl alcohol, methanol or isopropanol etc. can be selected in the organic solvent.
In said program, the organic base is secondary amine or primary amine.
In said program, dimethylamine, diethylamine or di-n-propylamine etc. can be selected in the secondary amine；Trimethylamine, three can be selected in tertiary amine
Ethamine or tripropyl amine (TPA) etc.；
Preferably, the secondary amine is diethylamine；Tertiary amine is triethylamine.
In said program, the molar ratio of the zinc salt and organic base is 1:(1-3).
In said program, the molar ratio of zinc salt and vanillic aldehyde is 1 in the reaction solution:(2-2.05).
In said program, a concentration of 0.05-0.10mol/L of zinc salt in the solution I；Vanillic aldehyde is a concentration of in solution II
0.03-0.05mol/L。
In said program, the solvent thermal reaction temperature is 160-200 DEG C, time 6-24h.
In said program, the solvent thermal reaction uses autoclave, compactedness 60-80%.
In said program, the anoxybiotic calcine technology is：First with the rate of 5-10 DEG C/min from room temperature to 100-
140 DEG C, 1-3h is kept the temperature, then continues to be warming up to 600-800 DEG C with the rate of 1-3 DEG C/min, keeps the temperature 3-9h, be cooled to room temperature.
Porous ZnO-C composite obtained by said program is used as electrode material for super capacitor, highest electric discharge specific capacitance
Amount is up to 550g-1(discharge current 5Ag-1), capacity attenuation very little after 3000 charge and discharge cycles can keep initial specific capacities
92~97%；Higher energy density and good circulation stability are can express out, existing ZnO/C composite materials can be effectively overcome
Deficiency.
It is multiple present invention firstly provides porous ZnO-C is prepared using vanillic aldehyde conjunction Zn complex MOF materials progress anoxybiotic calcining
Condensation material；Metal organic framework is to become three by series reaction in a suitable solvent by metal ion and organic ligand
Tie up mesh skeleton structure, large specific surface area, regulatable pore size, the advantages that porosity is high；As presoma into one
Step calcining prepares porous ZnO-C, can effectively promote the binding performance between gained composite material specific surface area and ZnO and C；By its
Applied to fields such as ultracapacitor batteries, high-energy density and good circulation stability are can express out, can effectively be broken through existing
Have ZnO/C composite materials applies bottleneck.
Compared with prior art, beneficial effects of the present invention are：
1) present invention firstly provides zinc salt, vanillic aldehyde is used as primary raw material, vanillic aldehyde is prepared by solvent-thermal method and closes zinc
Complex MOF materials, then calcining obtains porous ZnO-C composite, gained porous ZnO-C composite tool under anoxybiotic environment
There are higher specific surface area, pore passage structure to be evenly distributed, and the excellent bonding performance between ZnO and C；
2) preparation process of the present invention is simple, raw material is easy to get, is at low cost, efficient；
3) gained porous ZnO-C composite should be made into electrode material for super capacitor, can express out energy density height and
The advantages that stable circulation performance is good.
Specific implementation mode
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention
Content is not limited solely to the following examples.
In following embodiment, the ethyl alcohol used is absolute ethyl alcohol (AR).
Embodiment 1
A kind of porous ZnO-C composite, preparation method include the following steps：
1) 0.1633g (1mmol) ZnCl is weighed respectively2It is dissolved under stirring condition in 20ml ethyl alcohol, adds 0.0731g
(1mmol) diethylamine (C4H11N), stir evenly, obtain solution I；
2) 0.304g (2mmol) vanillic aldehyde is dissolved in 40ml ethyl alcohol, is uniformly mixed and is obtained solution II；
3) step 1) acquired solution I and step 2) acquired solution II are mixed under agitation, and stirs evenly instead
Liquid is answered, is then transferred in 100mL autoclaves and reacts 6h at 160 DEG C, then by reaction kettle cooled to room temperature, product
Washed through centrifugal filtration and with ethyl alcohol three times, after dry (80 DEG C drying 12 hours) vanillic aldehyde conjunction Zn complex MOF materials (Zn
(C8H7O3)2(H2O)2Powder)；
4) vanillic aldehyde is closed Zn complex MOF materials and is gradually heated up from room temperature with the heating rate of 10 DEG C/min in a vacuum furnace
To 120 DEG C, and 2h is kept at such a temperature, then continue to be warming up to 600 DEG C with the heating rate of 2 DEG C/min, and in the temperature
Lower maintenance 9h, cooling sample obtain porous ZnO-C composite materials to room temperature.
The present embodiment products therefrom is subjected to BET test analysis, the specific surface area of gained powder product is 500m2/g；It will
It is used as the electrode material of ultracapacitor, is 5Ag in current density-1When specific capacitance be 550F g-1, 3000 charge and discharges
After electricity cycle, specific capacity only reduces 3% compared to initial capacity.
Embodiment 2
A kind of porous ZnO-C composite, preparation method include the following steps：
1) 0.1633g (1mmol) ZnCl is weighed respectively2It is dissolved under stirring condition in 12ml ethyl alcohol, adds 0.2014g
(2mmol) triethylamine (C6H15N), stir evenly, obtain solution I；
2) 0.312g (2.02mmol) vanillic aldehyde is dissolved in 50ml ethyl alcohol, is uniformly mixed and is obtained solution II；
3) step 1) acquired solution I and step 2) acquired solution II are mixed under agitation, and stirs evenly instead
Liquid is answered, is then transferred in 100mL autoclaves and reacts 18h at 200 DEG C, then by reaction kettle cooled to room temperature, production
Object washs three times through centrifugal filtration and with ethyl alcohol, after dry (80 DEG C drying 12 hours) vanillic aldehyde conjunction Zn complex MOF materials
(Zn(C8H7O3)2(H2O)2Powder)；
4) vanillic aldehyde is closed Zn complex MOF materials and is gradually heated up from room temperature with the heating rate of 10 DEG C/min in a vacuum furnace
To 100 DEG C, and 3h is kept at such a temperature, then continue to be warming up to 700 DEG C with the heating rate of 3 DEG C/min, and in the temperature
Lower maintenance 7h, cooling sample obtain porous ZnO-C composite materials to room temperature.
The present embodiment products therefrom is subjected to BET test analysis, the specific surface area of gained powder product is 450m2/g；It will
It is used as the electrode material of ultracapacitor, is 5Ag in current density-1When specific capacitance be 527F g-1, 3000 charge and discharges
After electricity cycle, specific capacity only reduces 5% compared to initial capacity.
Embodiment 3
A kind of porous ZnO-C composite, preparation method include the following steps：
1) 163.3g (1mol) ZnCl is weighed respectively2It is dissolved under stirring condition in 10L ethyl alcohol, adds 219.3g (3mol)
C4H11N is stirred evenly, and obtains solution I；
2) 304.4g (2mol) vanillic aldehyde is dissolved in 60L ethyl alcohol, is uniformly mixed and is obtained solution II；
3) step 1) acquired solution I and step 2) acquired solution II are mixed under stiring, and stir evenly to obtain reaction solution,
Then be transferred in 100L autoclaves and reacted for 24 hours at 180 DEG C, then by reaction kettle cooled to room temperature, product pass through from
Heart filtering simultaneously wash three times with ethyl alcohol, and (80 DEG C drying 12 hours) obtain vanillic aldehyde and close Zn complex MOF materials (Zn after dry
(C8H7O3)2(H2O)2Powder)；
4) vanillic aldehyde is closed Zn complex MOF materials and is gradually heated up from room temperature with the heating rate of 10 DEG C/min in a vacuum furnace
To 140 DEG C, and 1h is kept at such a temperature, then continue to be warming up to 800 DEG C with the heating rate of 1 DEG C/min, and in the temperature
Lower maintenance 3h, cooling sample obtain porous ZnO-C composite materials to room temperature.
The present embodiment products therefrom is subjected to BET test analysis, the specific surface area of gained powder product is 471m2/g；It will
It is used as the electrode material of ultracapacitor, is 5Ag in current density-1When specific capacitance be 500F g-1, 3000 charge and discharges
After electricity cycle, specific capacity only reduces 4% compared to initial capacity.
Embodiment 4
A kind of porous ZnO-C composite, preparation method include the following steps：
1) 0.1633g (1mmol) ZnCl is weighed respectively2It is dissolved under stirring condition in 20mL ethyl alcohol, adds 0.2530g
(2.5mmol)C6H15N is stirred evenly, and obtains solution I；
2) 0.319g (2.05mol) vanillic aldehyde is dissolved in 60mL ethyl alcohol, is uniformly mixed and is obtained solution II；
3) step 1) acquired solution I and step 2) acquired solution II are mixed under agitation, and stirs evenly instead
Liquid is answered, is then transferred in 100mL autoclaves and reacts 20h at 170 DEG C, then by reaction kettle cooled to room temperature, production
Object washs three times through centrifugal filtration and with ethyl alcohol, after dry (80 DEG C drying 12 hours) vanillic aldehyde conjunction Zn complex MOF materials
(Zn(C8H7O3)2(H2O)2Powder)；
4) vanillic aldehyde is closed Zn complex MOF materials and is gradually heated up from room temperature with the heating rate of 10 DEG C/min in a vacuum furnace
To 130 DEG C, and 2.5h is kept at such a temperature, then continue to be warming up to 750 DEG C with the heating rate of 2 DEG C/min, and in the temperature
Degree is lower to maintain 5h, cooling sample to obtain porous ZnO-C composite materials to room temperature.
The present embodiment products therefrom is subjected to BET test analysis, the specific surface area of gained powder product is 483m2/g；It will
It is used as the electrode material of ultracapacitor, is 5Ag in current density-1When specific capacitance be 540F g-1, 3000 charge and discharges
After electricity cycle, specific capacity only reduces 8% compared to initial capacity.
Comparative example
A kind of ZnO-C composite materials, by glucose, the hydro-thermal reaction 10h at 180 DEG C obtains carbon ball for it, then by gained carbon ball
It is 1 with the compound molar ratios that obtain of ZnO:1 ZnO/ carbon balls nanocomposite (specific preparation process referring to：Yunnan University 2016
The pretty Master's thesis of Nian Hanbing " with chemical property grind by synthesis and its air-sensitive of the ZnO hollow balls with ZnO/ carbon ball nanocomposites
Study carefully ").
The specific surface area of gained ZnO/ carbon ball nanocomposites is 115.699m2/g；It is used as ultracapacitor
Electrode material is 5Ag in current density-1When specific capacitance be 459F g-1, after 1000 charge and discharge cycles, specific capacity is compared
Initial capacity reduces 18.6%.
The above results show that the specific surface area of gained porous ZnO-C of the invention is high, and the binding performance between ZnO and C
It is good, it is used as electrode material for super capacitor, can express out higher energy density and good stable circulation performance, can be had
Effect widens the suitable application area of ZnO-C composite materials.
Obviously, above-described embodiment be only intended to clearly illustrate made by example, and not limitation to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And the obvious variation or change therefore amplified
It moves within still in the protection domain of the invention.
Claims (10)
1. a kind of porous ZnO-C composite, which is characterized in that close Zn complex MOF materials progress anoxybiotic using vanillic aldehyde and forge
It burns；Its specific surface area is 450~500m2/g。
2. porous ZnO-C composite according to claim 1, which is characterized in that the vanillic aldehyde closes Zn complex MOF
The chemical formula of material is Zn (C8H7O3)2(H2O)2, molecular formula C16H18O8Zn is structurally characterized in that each central metallic ions
Zn2+It is sent out with 2 oxygen atoms in 4 oxygen atoms of phenolic hydroxyl group oxygen and methoxyl group oxygen in 2 vanillic aldehyde bases and 2 hydrones
Raw coordination, forms molecular complex, ligancy 6.
3. porous ZnO-C composite according to claim 1, which is characterized in that the vanillic aldehyde closes Zn complex
Preparation method includes the following steps：
1) zinc salt and organic base are dissolved in organic solvent, are uniformly mixed to obtain solution I；
2) vanillic aldehyde is dissolved in organic solvent, is uniformly mixed to obtain solution II；
3) step 1) acquired solution I and step 2) acquired solution II are uniformly mixed under stiring, obtain reaction solution, it then will reaction
Liquid carries out solvent thermal reaction, then through cooling, washing, drying, obtains vanillic aldehyde and close Zn complex MOF materials.
4. the preparation method of any one of claims 1 to 3 porous ZnO-C composite, which is characterized in that including walking as follows
Suddenly：
1) zinc salt and organic base are dissolved in organic solvent, are uniformly mixed to obtain solution I；
2) vanillic aldehyde is dissolved in organic solvent, is uniformly mixed to obtain solution II；
3) step 1) acquired solution I and step 2) acquired solution II are uniformly mixed under stiring, obtain reaction solution, it then will reaction
Liquid carries out solvent thermal reaction, then through cooling, washing, drying, obtains vanillic aldehyde and close Zn complex MOF materials；
4) vanillic aldehyde is closed into Zn complex MOF materials and carries out anoxybiotic calcining, obtain porous ZnO-C composite materials.
5. preparation method according to claim 4, which is characterized in that the organic base is secondary amine or primary amine.
6. preparation method according to claim 4, which is characterized in that the molar ratio of the zinc salt and organic base is 1:(1-
3)。
7. preparation method according to claim 4, which is characterized in that the molar ratio of zinc salt and vanillic aldehyde in the reaction solution
It is 1:(2-2.05).
8. preparation method according to claim 4, which is characterized in that the solvent thermal reaction temperature is 160-200 DEG C, when
Between be 6-24h.
9. preparation method according to claim 4, which is characterized in that the anoxybiotic calcine technology is：First with 5-10 DEG C/
The rate of min keeps the temperature 1-3h, then continues to be warming up to 600- with the rate of 1-3 DEG C/min from room temperature to 100-140 DEG C
800 DEG C, 3-9h is kept the temperature, is cooled to room temperature.
10. application of the porous ZnO-C composite in electrode material for super capacitor described in claim 1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109110745A (en) * | 2018-09-27 | 2019-01-01 | 北京长城华冠汽车科技股份有限公司 | A kind of preparation method of the hollow Nano carbon balls composite material of N doping multi-pore channel |
| CN112794359A (en) * | 2020-12-31 | 2021-05-14 | 浙江工业大学 | ZnO @ C composite material and preparation method and application thereof |
| CN113707467A (en) * | 2021-09-10 | 2021-11-26 | 安徽工业大学 | MOF-derived ZnO @ C cubic electrode material, and preparation method and application thereof |
| CN113871211A (en) * | 2021-09-15 | 2021-12-31 | 深圳市宏卓远电子科技有限公司 | High-energy-density super capacitor |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106784658A (en) * | 2016-12-01 | 2017-05-31 | 中南大学 | A kind of Morphological control method of lithium ion battery metal oxide/carbon negative pole material |
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2018
- 2018-05-22 CN CN201810495908.2A patent/CN108538618B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106784658A (en) * | 2016-12-01 | 2017-05-31 | 中南大学 | A kind of Morphological control method of lithium ion battery metal oxide/carbon negative pole material |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109110745A (en) * | 2018-09-27 | 2019-01-01 | 北京长城华冠汽车科技股份有限公司 | A kind of preparation method of the hollow Nano carbon balls composite material of N doping multi-pore channel |
| CN112794359A (en) * | 2020-12-31 | 2021-05-14 | 浙江工业大学 | ZnO @ C composite material and preparation method and application thereof |
| CN113707467A (en) * | 2021-09-10 | 2021-11-26 | 安徽工业大学 | MOF-derived ZnO @ C cubic electrode material, and preparation method and application thereof |
| CN113871211A (en) * | 2021-09-15 | 2021-12-31 | 深圳市宏卓远电子科技有限公司 | High-energy-density super capacitor |
| CN113871211B (en) * | 2021-09-15 | 2023-10-03 | 深圳市宏卓远电子科技有限公司 | Super capacitor with high energy density |
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