CN104900417B - One kind is based on Zn (OH)2/Co(OH)2Water system asymmetrical type ultracapacitor of anode composite and preparation method thereof - Google Patents
One kind is based on Zn (OH)2/Co(OH)2Water system asymmetrical type ultracapacitor of anode composite and preparation method thereof Download PDFInfo
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- CN104900417B CN104900417B CN201510274963.5A CN201510274963A CN104900417B CN 104900417 B CN104900417 B CN 104900417B CN 201510274963 A CN201510274963 A CN 201510274963A CN 104900417 B CN104900417 B CN 104900417B
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/13—Energy storage using capacitors
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Abstract
The invention discloses one kind to be based on Zn (OH)2/Co(OH)2Water system asymmetrical type ultracapacitor of anode composite and preparation method thereof, water system asymmetrical type ultracapacitor are by Zn (OH)2/Co(OH)2The button capacitor that anode composite, absorbent charcoal material negative pole, glass fibre ester barrier film, potassium hydroxide electrolyte and shell assemble；Water system asymmetrical type ultracapacitor voltage window is up to 1.5V, when power density is 6.2kW kg‑1Still there is high cyclical stability, 5000 circulations can keep more than the 99% of initial value, so as to have potential commercial application value；The preparation technology of water system asymmetrical type ultracapacitor is simple, safe to use, cost is low and environmentally friendly.
Description
Technical field
The present invention relates to one kind to be based on Zn (OH)2/Co(OH)2The water system asymmetrical type ultracapacitor of composite positive pole
And preparation method thereof, belong to supercapacitor technologies field.
Background technology
Ultracapacitor is a kind of new type of energy storage device for having traditional capacitor and battery advantage concurrently.Due to it possess it is high
Power density, quick discharge and recharge, stable cycle life and advantages of environment protection, have been obtained worldwide in recent years
Common concern.At present, commercialized ultracapacitor in water system energy density in 3~4Wh kg-1, its relatively low energy density
Limit further business application.Assembling asymmetric super-capacitor is a kind of effective method for improving energy density, its
Generally assembled by electric double layer carbon material as negative material, fake capacitance material as positive electrode.
Fake capacitance material mainly has metal oxide/hydroxide, conducting polymer with its compound etc..Wherein metal oxygen
Compound and hydroxide have higher theoretical specific capacity and are widely used.Co(OH)2Theoretical specific capacity be 3460F
g-1, and price is low, environment-friendly, is a kind of one of very promising electrode material.But substantial amounts of result of study shows
Co (OH)2Cyclical stability is relatively low, therefore improves its cycle performance, the circulation row particularly in asymmetric super-capacitor
To have important meaning for its further research in ultracapacitor.United States Patent (USP) (US3066178A) is prepared for Co
(OH)2With Ni (OH)2Composite, and show preferable chemical property.Tang etc. (Electrochim.Acta 2015,
161,279) Co (OH) for the different proportion being prepared2With Ni (OH)2Composite is shown in asymmetric super-capacitor
Higher energy density, but its cycle performance (being 84.4% after 1500 circulations) is not ideal enough.
The content of the invention
The defects of energy density is relatively low in water system be present for symmetric form ultracapacitor traditional in the prior art, and
Co(OH)2/Ni(OH)2Although composite shows higher energy density in asymmetric super-capacitor, circulation be present
The defects of poor performance, it is higher and have excellent cycling stability that the purpose of the present invention is to provide a kind of energy density
Containing Zn (OH)2/Co(OH)2The water system asymmetry type ultracapacitor of anode composite.
Another object of the present invention is to be to be based on Zn (OH) described in providing a kind of simple, low cost prepares2/Co(OH)2
The method of the water system asymmetrical type ultracapacitor of anode composite.
In order to realize the technical purpose of the present invention, the invention provides one kind to be based on Zn (OH)2/Co(OH)2Anode composite
Water system asymmetrical type ultracapacitor, is made up of positive pole, negative pole, barrier film, electrolyte and shell；
Described positive pole is by Zn (OH)2/Co(OH)2Composite positive pole and acetylene black and PVDF in mass ratio 70~80:
10~15:The composite of 10~15 compositions is coated in the Zn (OH) obtained in nickel foam2/Co(OH)2Anode composite；
Described Zn (OH)2/Co(OH)2Composite positive pole be using two identical cobalt pieces as positive and negative electrode, with
NaCl and Zn (CH3COO)2Mixed solution as electrolyte, be prepared by AC electrical method.
Preferable Zn (OH)2/Co(OH)2Zn (OH) in composite positive pole2With Co (OH)2Mol ratio be 0.1~1:
0.1~1.
Preferable NaCl and Zn (CH3COO)2Mixed solution in NaCl concentration range be 0.5~3.5mol/L, Zn
(CH3COO)2Concentration range be 0.005~1mol/L.
For the AC electrical method that the present invention uses preferably using power frequency for 50Hz, voltage is 3~30V alternating current.
Present invention also offers one kind to prepare based on Zn (OH)2/Co(OH)2The super electricity of water system asymmetrical type of anode composite
The method of container, this method comprise the following steps：
Step 1：Prepare Zn (OH)2/Co(OH)2Composite positive pole；
Using two identical cobalt pieces as positive and negative electrode, with NaCl and Zn (CH3COO)2Mixed solution as electrolysis
Liquid, it is 50Hz in frequency, is electrolysed 2~24h under the alternating current that voltage is 3~30V, obtains Zn (OH)2/Co(OH)2Anode composite material
Material；Described NaCl and Zn (CH3COO)2Mixed solution in NaCl concentration range be 0.5~3.5mol/L, Zn
(CH3COO)2Concentration range be 0.005~1mol/L；
Step 2：Prepare Zn (OH)2/Co(OH)2Anode composite
By gained Zn (OH)2/Co(OH)2Composite positive pole and acetylene black, PVDF in mass ratio 70~80:10~15:10
~15 mixing, add after NMP stirs, coated in nickel foam, vacuum drying, tabletting, produce Zn (OH)2/Co(OH)2
Anode composite；
Step 3：Prepare absorbent charcoal material negative pole
By absorbent charcoal material and acetylene black, PVDF in mass ratio 75~85:10~15:5~10 mixing, adds NMP
After stirring, coated in nickel foam, vacuum drying, tabletting, absorbent charcoal material negative pole is produced；
Step 4：Assemble water system asymmetrical type ultracapacitor
Using KOH solution as electrolyte, at mounted Zn (OH)2/Co(OH)2Anode composite and absorbent charcoal material negative pole
One layer of barrier film is set among assembling, is assembled into button-shaped water system asymmetrical type ultracapacitor.
Vacuum drying temperature in preferable preparation method in step 2 and three is 80~120 DEG C, and the pressure of tabletting is 2
~25MPa.
The present invention prepares the Zn (OH) of different mol ratio2/Co(OH)2The preparation method of composite positive pole, specifically include with
Lower step：
(1) using two identical cobalt pieces as two electrodes, with NaCl and Zn (CH3COO)2Mixed solution for electrolysis
Liquid, under alternating current (50Hz) effect, 2~24h is reacted, a period of time is stood after reaction；NaCl concentration range be 0.5~
3.5mol/L, Zn (CH3COO)2Concentration range be 0.005~1mol/L；
(2) product obtained by step (1) is centrifuged into (8000 turns/min), be washed with deionized, dried (at 80 DEG C
Dry 24h), produce Zn (OH)2/Co(OH)2Composite positive pole；
(3) Zn (CH are changed3COO)2Concentration (from 0.005mol/L to 1mol/L) in mixed liquor, can obtain difference and rubs
The Zn (OH) of your ratio2/Co(OH)2Composite.
The present invention uses Zn (OH)2/Co(OH)2Composite positive pole makes Zn (OH)2/Co(OH)2The method of anode composite
It is as follows：
By different proportion Zn (OH)2/Co(OH)2Composite positive pole, matter is pressed with acetylene black, polyvinylidene fluoride (PVDF)
Measure ratio 70~80:10~15:10~15 ratio mixing, adds a small amount of 1-METHYLPYRROLIDONE (NMP), is well mixed, then
Coated in nickel foam, 100 DEG C of dryings of vacuum, 20MPa lower sheetings, a series of Zn (OH) are made2/Co(OH)2Anode composite.
The method that the present invention makes negative pole using absorbent charcoal material is as follows：
By absorbent charcoal material and acetylene black, PVDF in mass ratio 75~85:10~15:5~10 ratio mixing, is added few
NMP is measured, is well mixed, is then coated with nickel foam, 80~120 DEG C of dryings of vacuum, 2~25MPa lower sheetings, activated carbon is made
Material negative pole.
Zn (OH) prepared by the present invention2/Co(OH)2Anode composite and absorbent charcoal material negative pole, KOH solution is used as electrolysis
Matter, glass fibre ester are barrier film, are assembled into button-shaped water system asymmetrical type ultracapacitor.
Compared with the prior art, beneficial effects of the present invention：The Zn (OH) prepared first with AC electrical method2/Co(OH)2It is compound
Water system asymmetrical type ultracapacitor prepared by positive electrode, its voltage window is up to 1.5V, when power density is 6.2kW kg-1
When still there is high cyclical stability, 5000 circulations can keep more than the 99% of initial value, so as to potential business
Application value.In addition, the preparation technology of water system asymmetrical type ultracapacitor is simple, safe to use, cost is low and environment-friendly.
Brief description of the drawings
【Fig. 1】It is Zn (OH) prepared by the embodiment of the present invention 32/Co(OH)2The X-ray diffractogram of composite；
【Fig. 2】It is Zn (OH) prepared by Example 1 and Example 2 of the present invention2/Co(OH)2The ESEM of composite
Figure, (a) and (b) is respectively that embodiment 1 and embodiment 2 are prepared；
【Fig. 3】It is the Zn (OH) that in the present invention prepared by embodiment 12/Co(OH)2Composite water system asymmetry super capacitor
The cyclic voltammetry curve of device is (sweep speed is 10mV s-1)；
【Fig. 4】It is that the water system asymmetric super-capacitor that in the present invention prepared by embodiment 2 in power density is 6.2kWkg-1
Cyclical stability figure.
Embodiment
Present invention is described further with reference to embodiments, rather than the protection model to the claims in the present invention
The limitation enclosed.
Embodiment 1
(1)Zn(OH)2/Co(OH)2Composite (mol ratio 0.2:1) preparation
A, using two essentially identical cobalt pieces as two electrodes, with NaCl and Zn (CH3COO)2Mixed solution for electricity
Solve liquid, Zn (CH3COO)2Concentration be 0.02mol/L, alternating current (50Hz) effect under, react 2~24h, stand one after reaction
The section time；
B, the product obtained by above-mentioned steps (1) is centrifuged into (8000 turns/min), be washed with deionized, dry (80
24h is dried at DEG C), produce Zn (OH)2/Co(OH)2Composite, its mol ratio are 0.2:1；
(2)Zn(OH)2/Co(OH)2Composite (mol ratio 0.2:1) preparation of electrode
The Zn (OH) that step (1) is obtained2/Co(OH)2Composite and acetylene black, PVDF in mass ratio 80:10:10
Ratio mixes, and adds a small amount of NMP, is well mixed, is then coated with nickel foam, 100 DEG C of dryings of vacuum, 20MPa lower sheetings, makes
Into the positive pole of asymmetric super-capacitor.
(3) preparation of absorbent charcoal material electrode
By absorbent charcoal material and acetylene black, PVDF in mass ratio 85:15:10 ratio mixing, adds a small amount of NMP, mixes
Uniformly, it is then coated with nickel foam, 100 DEG C of dryings of vacuum, 20MPa lower sheetings, the negative pole of asymmetric super-capacitor is made.
(4)Zn(OH)2/Co(OH)2Composite (mol ratio 0.2:1) assembling of water system asymmetric super-capacitor with
Zn(OH)2/Co(OH)2Composite (mol ratio 0.2:1) electrode is positive pole, and activated carbon electrodes are negative pole, 3mol/L KOH
For electrolyte, glass fibre ester is barrier film, is assembled into button-shaped asymmetric super-capacitor, and power density is 4.8kW kg-1When
Conservation rate is up to 98.7% after 5000 circulations.
Embodiment 2
(1)Zn(OH)2/Co(OH)2Composite (mol ratio 0.3:1) preparation
A uses two essentially identical cobalt pieces as two electrodes, with NaCl and Zn (CH3COO)2Mixed solution for electricity
Solve liquid, Zn (CH3COO)2Concentration be 0.035mol/L, alternating current (50Hz) effect under, react 2~24h, stood after reaction
For a period of time；
Product obtained by above-mentioned steps (1) is centrifuged (8000 turns/min) by B, is washed with deionized, and dries (80 DEG C
Lower dry 24h), produce Zn (OH)2/Co(OH)2Composite, its mol ratio are 0.3：1；
(2)Zn(OH)2/Co(OH)2Composite (mol ratio 0.3:1) preparation of electrode
The Zn (OH) that step (1) is obtained2/Co(OH)2Composite and acetylene black, PVDF in mass ratio 80:10:10
Ratio mixes, and adds a small amount of NMP, is well mixed, is then coated with nickel foam, 100 DEG C of dryings of vacuum, 20MPa lower sheetings, makes
Into the positive pole of asymmetric super-capacitor.
(3) preparation of absorbent charcoal material electrode
By absorbent charcoal material and acetylene black, PVDF in mass ratio 85:15:10 ratio mixing, adds a small amount of NMP, mixes
Uniformly, it is then coated with nickel foam, 100 DEG C of dryings of vacuum, 20MPa lower sheetings, the negative pole of asymmetric super-capacitor is made.
(4)Zn(OH)2/Co(OH)2Composite (mol ratio 0.3:1) assembling of water system asymmetric super-capacitor with
Zn(OH)2/Co(OH)2Composite (mol ratio 0.3:1) electrode is positive pole, and activated carbon electrodes are negative pole, 3mol/L KOH
For electrolyte, glass fibre ester is barrier film, is assembled into button-shaped asymmetric super-capacitor, and power density is 6.2kW kg-1When
Conservation rate is up to 99.1% after 5000 circulations.
Embodiment 3
(1)Zn(OH)2/Co(OH)2Composite (mol ratio 1.2:1) preparation
A uses two essentially identical cobalt pieces as two electrodes, with NaCl and Zn (CH3COO)2Mixed solution for electricity
Solve liquid, Zn (CH3COO)2Concentration be 0.1mol/L, alternating current (50Hz) effect under, react 2~24h, stand one after reaction
The section time；
Product obtained by above-mentioned steps (1) is centrifuged (8000 turns/min) by B, is washed with deionized, and dries (80 DEG C
Lower dry 24h), produce Zn (OH)2/Co(OH)2Composite, its mol ratio are 1.2：1；
(2)Zn(OH)2/Co(OH)2Composite (mol ratio 1.2:1) preparation of electrode
The Zn (OH) that step (1) is obtained2/Co(OH)2Composite and acetylene black, PVDF in mass ratio 80:10:10
Ratio mixes, and adds a small amount of NMP, is well mixed, is then coated with nickel foam, 100 DEG C of dryings of vacuum, 20MPa lower sheetings, makes
Into the positive pole of asymmetric super-capacitor.
(3) preparation of absorbent charcoal material electrode
By absorbent charcoal material and acetylene black, PVDF in mass ratio 85:15:10 ratio mixing, adds a small amount of NMP, mixes
Uniformly, it is then coated with nickel foam, 100 DEG C of dryings of vacuum, 20MPa lower sheetings, the negative pole of asymmetric super-capacitor is made.
(4)Zn(OH)2/Co(OH)2Composite (mol ratio 1.2:1) assembling of water system asymmetric super-capacitor with
Zn(OH)2/Co(OH)2Composite (mol ratio 1.2:1) electrode is positive pole, and activated carbon electrodes are negative pole, 3mol/L KOH
For electrolyte, glass fibre ester is barrier film, is assembled into button-shaped asymmetric super-capacitor, and power density is 2.3kW kg-1When
Conservation rate is up to 99.3% after 5000 circulations.
Claims (3)
1. one kind is based on Zn (OH)2/Co(OH)2The water system asymmetrical type ultracapacitor of anode composite, by positive pole, negative pole, every
Film, electrolyte and shell composition, it is characterised in that
Described positive pole is by Zn (OH)2/Co(OH)2Composite positive pole and acetylene black and PVDF in mass ratio 70~80:10~
15:The composite of 10~15 compositions is coated in the Zn (OH) obtained in nickel foam2/Co(OH)2Anode composite；
Described Zn (OH)2/Co(OH)2Composite positive pole is using two identical cobalt pieces as positive and negative electrode, with NaCl
With Zn (CH3COO)2Mixed solution as electrolyte, be prepared by AC electrical method；
Described Zn (OH)2/Co(OH)2Zn (OH) in composite positive pole2With Co (OH)2Mol ratio be 0.1~1:0.1~1；
Described NaCl and Zn (CH3COO)2Mixed solution in NaCl concentration range be 0.5~3.5mol/L, Zn
(CH3COO)2Concentration range be 0.005~1mol/L；The AC current frequency that described AC electrical method uses is 50Hz, voltage
For 3~30V.
2. preparation is based on Zn (OH)2/Co(OH)2The method of the water system asymmetrical type ultracapacitor of anode composite, its feature exist
In comprising the following steps：
Step 1：Prepare Zn (OH)2/Co(OH)2Composite positive pole；
Using two identical cobalt pieces as positive and negative electrode, with NaCl and Zn (CH3COO)2Mixed solution as electrolyte,
Frequency is 50Hz, is electrolysed 2~24h under the alternating current that voltage is 3~30V, obtains Zn (OH)2/Co(OH)2Composite positive pole；Institute
The NaCl and Zn (CH stated3COO)2Mixed solution in NaCl concentration range be 0.5~3.5mol/L, Zn (CH3COO)2It is dense
Degree scope is 0.005~1mol/L；
Step 2：Prepare Zn (OH)2/Co(OH)2Anode composite
By gained Zn (OH)2/Co(OH)2Composite positive pole and acetylene black, PVDF in mass ratio 70~80:10~15:10~15
Mixing, add after NMP stirs, coated in nickel foam, vacuum drying, tabletting, produce Zn (OH)2/Co(OH)2It is compound
Positive pole；
Step 3：Prepare active carbon material negative pole
By active carbon material and acetylene black, PVDF in mass ratio 75~85:10~15:5~10 mixing, add NMP stirrings
After uniformly, coated in nickel foam, vacuum drying, tabletting, active carbon material negative pole is produced；
Step 4：Assemble water system asymmetrical type ultracapacitor
Using KOH solution as electrolyte, at mounted Zn (OH)2/Co(OH)2Anode composite assembles with active carbon material negative pole
Centre sets one layer of barrier film, is assembled into button-shaped water system asymmetrical type ultracapacitor.
3. preparation method according to claim 2, it is characterised in that the vacuum drying temperature in step 2 and three is 80
~120 DEG C, the pressure of tabletting is 2~25MPa.
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| CN201510274963.5A CN104900417B (en) | 2015-05-26 | 2015-05-26 | One kind is based on Zn (OH)2/Co(OH)2Water system asymmetrical type ultracapacitor of anode composite and preparation method thereof |
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| CN201510274963.5A CN104900417B (en) | 2015-05-26 | 2015-05-26 | One kind is based on Zn (OH)2/Co(OH)2Water system asymmetrical type ultracapacitor of anode composite and preparation method thereof |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103341367A (en) * | 2013-07-15 | 2013-10-09 | 上海交通大学 | Method for synthesizing carbon-supported cobalt polypyrrole oxygen reduction catalyst by alternating current one-step method |
-
2015
- 2015-05-26 CN CN201510274963.5A patent/CN104900417B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103341367A (en) * | 2013-07-15 | 2013-10-09 | 上海交通大学 | Method for synthesizing carbon-supported cobalt polypyrrole oxygen reduction catalyst by alternating current one-step method |
Non-Patent Citations (3)
| Title |
|---|
| A simple and generic approach for synthesizing colloidal metal and metal oxide nanocrystals;Jacqueline E. Cloud等;《Nanoscale》;20130626;第5卷;第7368-7378页 * |
| Effect of Zn-substitution on cycling performance of α-Co(OH)2 nanosheet electrode for supercapacitors;Jun Tang等;《Journal of Materials Chemistry A》;20131120;第2卷;第2585-2591页 * |
| Electrochemically alternating voltage tuned Co2MnO4/Co hydroxide chloride for an asymmetric supercapacitor;Mingjun Jing等;《Electrochimica Acta》;20150307;第165卷;第198-205页 * |
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