CN106531466A - Preparation method for three-element oxide composite material and application - Google Patents
Preparation method for three-element oxide composite material and application Download PDFInfo
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- CN106531466A CN106531466A CN201611016452.4A CN201611016452A CN106531466A CN 106531466 A CN106531466 A CN 106531466A CN 201611016452 A CN201611016452 A CN 201611016452A CN 106531466 A CN106531466 A CN 106531466A
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- oxide composite
- ternary oxide
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- potassium permanganate
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- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000003990 capacitor Substances 0.000 claims abstract description 9
- 229910000521 B alloy Inorganic materials 0.000 claims abstract description 8
- 238000006479 redox reaction Methods 0.000 claims abstract description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 40
- 239000012279 sodium borohydride Substances 0.000 claims description 16
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 11
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 7
- 230000005611 electricity Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000956 alloy Substances 0.000 abstract 2
- 229910045601 alloy Inorganic materials 0.000 abstract 1
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 abstract 1
- 238000003860 storage Methods 0.000 abstract 1
- 230000002195 synergetic effect Effects 0.000 abstract 1
- 239000007772 electrode material Substances 0.000 description 6
- 229910000314 transition metal oxide Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 150000002927 oxygen compounds Chemical class 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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 preparation method for a three-element oxide composite material and an application in the field of super capacitors. According to the method, an in-situ chemical reduction method is employed to prepare a Co-Ni-B alloy material in solution, then the alloy and potassium permanganate realize oxidation reduction reaction to acquire a Co3O4-Ni3O4-MnO2 ternary oxide. Through the method, strong reductibility of the Co-Ni-B alloy and strong oxidizability of the potassium permanganate are utilized to realize oxidation reduction reaction of the two, the Co-Ni-B is oxidized to be Co3O4-Ni3O4, the potassium permanganate is reduced to be MnO2, the method is simple, an application scope is wide, and manufacturing cost is low; the three oxides are composed together, under the synergistic effect among the materials, excellent electricity storage property is realized, the three-element oxide composite material can be applied to the super capacitors, excellent electrical performance is realized, moreover, the method is applicable to mass-scale production, and the application effect is good.
Description
Technical field
The present invention relates to supercapacitor technologies field, more particularly to a kind of Co3O4-Ni3O4-MnO2Ternary oxide is combined
The preparation method of material and its application in ultracapacitor field.
Background technology
Ultracapacitor has the advantages that power density is high, has extended cycle life, energy density is big, in recent years by people's
Extensive concern.The research of the electrode material of ultracapacitor at present is concentrated mainly on carbon-based material, polymeric material, transition metal
On the materials such as oxide.Wherein the quality of performance directly determines the size of condenser capacity, and affects ultracapacitor most
For one of crucial factor.Transition metal oxide is not only cheap, wide material sources, and has various electron valence states, excellent
Good energy storage characteristic and receive much concern.Therefore, metal-oxide becomes the most widely used electrode material in ultracapacitor field
One of, its Faraday pseudo-capacitance energy storage for mainly being formed using the change of oxide valence state.But transition metal oxide is generally adopted
With hydro-thermal method, vapour deposition process, Physical etc., preparation method is complicated, and the time of needs is longer, and can not large batch of life
Produce, therefore develop the preparation method of new transition metal oxide and seem extremely important.
The content of the invention
The invention aims to provide a kind of Co3O4-Ni3O4-MnO2The preparation method of ternary oxide composite and
Its application in ultracapacitor.
The present invention is adopted the following technical scheme that：
Co of the present invention3O4-Ni3O4-MnO2The preparation method of ternary oxide composite, comprises the following steps that：
（1）Take a certain amount of CoSO4、NiSO4It is soluble in water；
（2）Weigh a certain amount of NaBH4, it is then added in water, obtains NaBH4Aqueous solution；
（3）By step（2）NaBH4Aqueous solution is slowly dropped to step（1）Aqueous solution in；
（4）After being added dropwise to complete, then allow solution reaction 2 hours, filter, washing, dry powder；
（5）By step（4）Resulting powder is reacted in being added to certain density potassium permanganate solution, is filtered, washs, is done
It is dry, obtain Co3O4-Ni3O4-MnO2Ternary oxide composite.
Step（1）The CoSO4、NiSO4Weight with water is：CoSO4NiSO4Water=5 1 100.
Step（2）Described NaBH4Concentration of aqueous solution is 1g 20-100ml.
Step（5）Described potassium permanganate solution concentration is 0.1 g 20-100ml
Step（3）In, using NaBH4The slaine of chemical Co, Ni prepares Co-Ni-B alloys, wherein precursor CoSO4NiSO4
Weight be 51.
Step（5）In, ternary oxide is prepared using the redox reaction between Co-Ni-B and potassium permanganate multiple
Condensation material.
The Co prepared using the method for the present invention3O4-Ni3O4-MnO2Ternary oxide composite can be used for super electricity
Container electrode material.
The concrete grammar for being applied to electrode of super capacitor is as follows：
（A）Weigh 0.008 g Co3O4-Ni3O4-MnO2Ternary oxide composite, 0.001 g acetylene blacks（Is produced from Tianjin,
90%）With 0.001 g ptfe micropowders（Is produced from Tianjin, and 90%）, it is placed in little Achatess and grinds in alms bowl, adds a few drop ethanol（Is produced from Tianjin,
AR）It is ground；
（B）Will with the pressure of 10 kPa（A）In the thick foamed nickel current collector compacting of composite and 1 mm, in atmosphere, room
The lower drying of temperature, cuts into 2 cm × 3 cm, electrode of super capacitor is obtained.
Co of the present invention3O4-Ni3O4-MnO2Ternary oxide composite supercapacitor electrode, can be in -0.25-0.3V
In the range of discharge and recharge, discharge current density be 1 A/g when, its specific capacitance can reach 1600 F/g, be much better than similar oxygen
Compound electrode material.
The present invention operation principle be：
Co, Ni metal ion in the presence of borohydride reduction agent is reduced out, obtains Co-Ni-B alloys, due to Co-
Ni-B alloys have strong reproducibility, and potassium permanganate solution has strong oxidisability, after the two mixing, Co-Ni-B alloys
The oxide of Co, Ni is oxidized to, while potassium permanganate is reduced to MnO2, therefore while obtain Co3O4、Ni3O4、MnO2Ternary
Oxide composite.And the Co for preparing3O4-Ni3O4-MnO2Ternary oxide composite has good electrochemistry special again
Property, thus the electrode material for ultracapacitor shows good performance.
The positive effect of the present invention is as follows：
1. Co is synthesized3O4-Ni3O4-MnO2Ternary oxide composite：The present invention is prepared for Co-Ni-B conjunctions using electronation
Gold, is prepared for Co using the superpower oxidisability of the superpower reproducibility of Co-Ni-B alloys and potassium permanganate3O4-Ni3O4-MnO2Three
First oxide composite, method are simple, with low cost, take short, suitable production in enormous quantities；
2. application effect is good：Synthesis Co3O4-Ni3O4-MnO2Ternary oxide composite is than simple MnO2, Co3O4-Ni3O4
Alloyed oxide specific capacitance improves nearly 5 times, and the storing up electricity performance of Co, Ni oxide than being prepared using conventional method is improved very
It is many；
3. preparation process is simple, properties of product are stable：Prepared compound preparation is simple, is adapted to large batch of preparation, Er Qiehou
Handling process is simple.
Description of the drawings
Fig. 1 is Co prepared by the embodiment of the present invention 13O4-Ni3O4-MnO2The scanning electron microscope of ternary oxide composite
Figure；
Fig. 2 is Co prepared by the embodiment of the present invention 13O4-Ni3O4-MnO2Ternary oxide composite and Co3O4-Ni3O4, MnO2
The comparison diagram of the discharge curve of alloyed oxide.
Specific embodiment
Present invention is further described with reference to embodiment and accompanying drawing, but is not limitation of the invention.
Embodiment 1：
Prepare Co3O4-Ni3O4-MnO2Ternary oxide composite：
（1）Take 50 g CoSO4、5 g NiSO4It is dissolved in 100 mL water；
（2）Weigh 2 g NaBH4, it is then added in water, obtains NaBH4Aqueous solution；
（3）By step（2）NaBH4Aqueous solution is slowly dropped to step（1）Aqueous solution in；
（4）After being added dropwise to complete, then allow solution reaction 2 hours, filter, washing, dry powder；
（5）By step（4）Resulting powder is reacted in being added to the potassium permanganate solution of 1 g/L；Filter, wash, be dried,
Obtain Co3O4-Ni3O4-MnO2Ternary oxide composite；
（6）Weigh 0.008 g Co-Ni-W alloyed oxides-graphene composite material, 0.001 g acetylene blacks（Is produced from Tianjin, and 90%）
With 0.001 g ptfe micropowders（Is produced from Tianjin, and 90%）, it is placed in little Achatess and grinds in alms bowl, adds a few drop ethanol（Is produced from Tianjin, AR）
It is ground；
（7）Will with the pressure of 10 kPa（A）In the thick foamed nickel current collector compacting of composite and 1 mm, in atmosphere, room
The lower drying of temperature, cuts into 2 cm × 3 cm, electrode of super capacitor is obtained, its specific capacitance is tested.
With reference to Co prepared by Fig. 1, embodiment 13O4-Ni3O4-MnO2The scanning electron microscope (SEM) photograph of ternary oxide composite.
It can be seen that the nano-particle of three kinds of oxide material formation cluster-shapeds, is combined with each other well.
With reference to Co prepared by Fig. 2, embodiment 13O4-Ni3O4-MnO2Ternary oxide composite and Co3O4-Ni3O4,
MnO2The comparison diagram of the discharge curve of alloyed oxide.From Fig. 2 as can be seen that under same current density, Co3O4-Ni3O4-
MnO2The discharge time of ternary oxide composite is apparently higher than Co3O4-Ni3O4, MnO2Oxide electrode material, during its electric discharge
Between improve more than 5 times.
Embodiment 2：
Prepare Co3O4-Ni3O4-MnO2Ternary oxide composite：
（1）Take 50 g CoSO4、5 g NiSO4It is dissolved in 100 mL water；
（2）Weigh 1 g NaBH4, it is then added in water, obtains NaBH4Aqueous solution；
（3）By step（2）NaBH4Aqueous solution is slowly dropped to step（1）Aqueous solution in；
（4）After being added dropwise to complete, then allow solution reaction 2 hours, filter, washing, dry powder；
（5）By step（4）Resulting powder is reacted in being added to the potassium permanganate solution of 3 g/L, is filtered, washs, is dried,
Obtain Co3O4-Ni3O4-MnO2Ternary oxide composite；
（6）Weigh 0.008 g Co-Ni-W alloyed oxides-graphene composite material, 0.001 g acetylene blacks（Is produced from Tianjin, and 90%）
With 0.001 g ptfe micropowders（Is produced from Tianjin, and 90%）, it is placed in little Achatess and grinds in alms bowl, adds a few drop ethanol（Is produced from Tianjin, AR）
It is ground；
（7）Will with the pressure of 10 kPa（A）In the thick foamed nickel current collector compacting of composite and 1 mm, in atmosphere, room
The lower drying of temperature, cuts into 2 cm × 3 cm, electrode of super capacitor is obtained, its specific capacitance is tested.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding can carry out various changes, modification, replacement to these embodiments without departing from the principles and spirit of the present invention
And modification, the scope of the present invention be defined by the appended.
Claims (6)
1. a kind of preparation method of ternary oxide composite, it is characterised in that：Methods described is comprised the following steps that：
（1）Take a certain amount of CoSO4、NiSO4It is soluble in water；
（2）Weigh a certain amount of NaBH4, it is then added in water, obtains NaBH4Aqueous solution；
（3）By step（2）NaBH4Aqueous solution is slowly dropped to step（1）Aqueous solution in；
（4）After being added dropwise to complete, then allow solution reaction 2 hours, filter, washing, dry powder；
（5）By step（4）Resulting powder is reacted in being added to certain density potassium permanganate solution, is filtered, washs, is done
It is dry, obtain Co3O4-Ni3O4-MnO2Ternary oxide composite.
2. the preparation method of ternary oxide composite according to claim 1, it is characterised in that：
Step（1）The CoSO4、NiSO4Weight with water is：CoSO4NiSO4Water=5 1 100；
Step（2）Described NaBH4Concentration of aqueous solution is 1g 20-100ml；
Step（5）Described potassium permanganate solution concentration is 0.1 g 20-100ml.
3. ternary oxide composite material and preparation method thereof according to claim 1, it is characterised in that：
Step（3）In, using NaBH4The slaine of chemical Co, Ni prepares Co-Ni-B alloys, wherein precursor CoSO4NiSO4
Weight be 51.
4. ternary oxide composite material and preparation method thereof according to claim 1, it is characterised in that：Step（5）In, adopt
Redox reaction between Co-Ni-B and potassium permanganate is preparing ternary oxide composite.
5. the ternary oxide composite that prepared by the method according to any one of claim 1 ~ 4 is in electrode of super capacitor
In application.
6. the application according to right wants 5, it is characterised in that：The concrete grammar for being applied to electrode of super capacitor is such as
Under：
（A）Weigh 0.08 g Co3O4-Ni3O4-MnO2Ternary oxide composite, 0.01 g, 90% acetylene blacks and 0.01 g
90% ptfe micropowder is placed in little Achatess and grinds in alms bowl, adds a few drop ethanol AR to be ground
（B）Will with the pressure of 10 kPa（A）In the thick foamed nickel current collector compacting of composite and 1 mm, in atmosphere, room
The lower drying of temperature, cuts into 2 cm × 3 cm, electrode of super capacitor is obtained.
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| CN201611016452.4A CN106531466B (en) | 2016-11-18 | 2016-11-18 | A kind of preparation and application of ternary oxide composite material |
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| CN201611016452.4A CN106531466B (en) | 2016-11-18 | 2016-11-18 | A kind of preparation and application of ternary oxide composite material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107221446A (en) * | 2017-06-08 | 2017-09-29 | 桂林电子科技大学 | A kind of three-dimensional manometer sheet Co Ni Mn oxide composites and its preparation method and application |
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|---|---|---|---|---|
| CN1971786A (en) * | 2005-11-25 | 2007-05-30 | 中国科学院金属研究所 | An electrochemical capacitor electrode material and its preparing method |
| US20140072836A1 (en) * | 2011-04-05 | 2014-03-13 | Blacklight Power, Inc. | H2o-based electrochemical hydrogen-catalyst power system |
| CN104148085A (en) * | 2014-07-22 | 2014-11-19 | 桂林电子科技大学 | Nanoporous quaternary alloy catalyst and preparation method thereof |
| CN105390706A (en) * | 2015-10-29 | 2016-03-09 | 武汉理工大学 | Preparation method of cobalt-manganese-oxide catalyst |
-
2016
- 2016-11-18 CN CN201611016452.4A patent/CN106531466B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1971786A (en) * | 2005-11-25 | 2007-05-30 | 中国科学院金属研究所 | An electrochemical capacitor electrode material and its preparing method |
| US20140072836A1 (en) * | 2011-04-05 | 2014-03-13 | Blacklight Power, Inc. | H2o-based electrochemical hydrogen-catalyst power system |
| CN104148085A (en) * | 2014-07-22 | 2014-11-19 | 桂林电子科技大学 | Nanoporous quaternary alloy catalyst and preparation method thereof |
| CN105390706A (en) * | 2015-10-29 | 2016-03-09 | 武汉理工大学 | Preparation method of cobalt-manganese-oxide catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107221446A (en) * | 2017-06-08 | 2017-09-29 | 桂林电子科技大学 | A kind of three-dimensional manometer sheet Co Ni Mn oxide composites and its preparation method and application |
| CN107221446B (en) * | 2017-06-08 | 2019-04-12 | 桂林电子科技大学 | A kind of Co-Ni-Mn oxide composite and its preparation method and application |
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Application publication date: 20170322 Assignee: Guangxi Yifang Environmental Protection Technology Co.,Ltd. Assignor: GUILIN University OF ELECTRONIC TECHNOLOGY Contract record no.: X2023980045358 Denomination of invention: Preparation and application of a ternary oxide composite material Granted publication date: 20181019 License type: Common License Record date: 20231101 |