CN108373176A - A kind of nano-nickel oxide raw powder's production technology for ultracapacitor - Google Patents
A kind of nano-nickel oxide raw powder's production technology for ultracapacitor Download PDFInfo
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- CN108373176A CN108373176A CN201810337853.2A CN201810337853A CN108373176A CN 108373176 A CN108373176 A CN 108373176A CN 201810337853 A CN201810337853 A CN 201810337853A CN 108373176 A CN108373176 A CN 108373176A
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- ultracapacitor
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- 239000000843 powder Substances 0.000 title claims abstract description 28
- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 27
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000005516 engineering process Methods 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 19
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000725 suspension Substances 0.000 claims abstract description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 5
- 239000000706 filtrate Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000001914 filtration Methods 0.000 claims description 30
- 239000012153 distilled water Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 238000004140 cleaning Methods 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical compound NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 6
- 230000001629 suppression Effects 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 229910052593 corundum Inorganic materials 0.000 claims description 2
- 239000010431 corundum Substances 0.000 claims description 2
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000009826 distribution Methods 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- AMDUMQZTBRMNMG-UHFFFAOYSA-N nickel nitric acid Chemical compound [Ni].O[N+]([O-])=O AMDUMQZTBRMNMG-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- 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
- C01P2006/80—Compositional purity
-
- 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
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to technical field of nano material, and in particular to a kind of nano-nickel oxide raw powder's production technology for ultracapacitor.Technical scheme is as follows：A kind of nano-nickel oxide raw powder's production technology for ultracapacitor, prepare nickel nitrate solution, the pH of the nickel nitrate solution is adjusted with ammonium hydroxide, absinthe-green suspension is obtained after being synthesized to the nickel nitrate solution using hydrothermal synthesis method, the suspension is filtered and is cleaned, by obtained filtrate after drying, ball milling, is put into Muffle furnace and calcines, furnace cooling obtains nano-nickel oxide powder.Provided by the present invention for the nano-nickel oxide raw powder's production technology of ultracapacitor, the nano-nickel oxide powder that dispersibility is excellent, particle diameter distribution is narrow, purity is high can be obtained.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of nano-nickel oxide powder for ultracapacitor
Preparation method.
Background technology
With global economy and development in science and technology, the exhausted and environmental pollution of natural environment non-renewable resources is caused increasingly
Aggravation, it is desirable that development green and regenerative resource storage system.Ultracapacitor as a kind of novel large power energy storage device,
With very high power density and good cycle life.The electrode active material of ultracapacitor directly affects its battery
It is good and bad.Nano-nickel oxide powder is controllable due to having many advantages, such as environmental-friendly, at low cost, surface and structural behaviour, becomes a kind of
The ideal electrode active material of practical application can most be met.
Nano-nickel oxide raw powder's production technology has the precipitation method, sol-gel method, electrochemical process etc..But these types side
Method has that preparation purity is low, agglomeration is serious, specific capacitance is not high.
Invention content
The present invention provides a kind of nano-nickel oxide raw powder's production technology for ultracapacitor, can obtain dispersibility
Nano-nickel oxide powder excellent, particle diameter distribution is narrow, purity is high.
Technical scheme is as follows：
A kind of nano-nickel oxide raw powder's production technology for ultracapacitor prepares nickel nitrate solution, with ammonium hydroxide tune
The pH for saving the nickel nitrate solution obtains absinthe-green suspension after being synthesized to the nickel nitrate solution using hydrothermal synthesis method
The suspension is filtered and is cleaned, by obtained filtrate after drying, ball milling, is put into Muffle furnace and calcine, with furnace cooling by liquid
But, nano-nickel oxide powder is obtained.
The nano-nickel oxide raw powder's production technology for ultracapacitor, preferred embodiment are the nitric acid
Nickel solution is made of Nickelous nitrate hexahydrate, citric acid, carbonic acid amide and distilled water, Nickelous nitrate hexahydrate, citric acid, carbonic acid amide
It is 12~18 with the ratio between the mass fraction of distilled water：5~8：3~5：100.
The nano-nickel oxide raw powder's production technology for ultracapacitor, preferred embodiment are the suspension
Liquid filters the mode cleaned：Filtering → distilled water cleaning → filtering → washes of absolute alcohol → filtering → washes of absolute alcohol →
Filtering → distilled water cleaning → filtering → distilled water cleaning.
The nano-nickel oxide raw powder's production technology for ultracapacitor, specifically comprises the following steps：
1) take Nickelous nitrate hexahydrate, carbonic acid amide, carbonic acid amide and distilled water as raw material in proportion, after being mixed,
1h is stirred, nickel nitrate solution is made, the pH that nickel nitrate solution is adjusted with 0.01~0.5mol/L ammonium hydroxide is 6.2~6.8；
2) nickel nitrate solution is moved into polytetrafluoroethylene (PTFE) autoclave, hydrothermal synthesis reaction is carried out under the conditions of 162 DEG C
For 24 hours, absinthe-green suspension is obtained；
3) dry in 60 DEG C of baking ovens after cleaning up by the suspension centrifugal filtration, obtain green powder；
4) by the green powder after corundum ball grinder ball milling, it is put into the heating rate that 10 DEG C/min is used in Muffle furnace
150 DEG C are warming up to, 30~60min is kept the temperature, is then warming up to 550~650 DEG C with the heating rate of 5 DEG C/min, heat preservation 2~3 is small
Shi Hou, furnace cooling obtain nano-nickel oxide powder.
The nano-nickel oxide raw powder's production technology for ultracapacitor, preferred embodiment are the nanometer
The purity of nickel oxide powder is 99.92~99.99%, and particle size range is 10~30nm.
The nano-nickel oxide raw powder's production technology for ultracapacitor, preferred embodiment are the nanometer
Nickel oxide powder is added ultracapacitor, and the specific capacitance of ultracapacitor improves 30 relative to the specific capacitance of original capacitance device~
55%, after ultracapacitor circular flow 500 times 60~75% are slowed down under the specific capacitance of specific capacitance suppression ratio original capacitance device.
Beneficial effects of the present invention are：Nano-nickel oxide diameter of particle narrow distribution range prepared by the present invention, purity are high, full
The use demand of sufficient ultracapacitor.
Description of the drawings
Fig. 1 is that specific capacitance and its cycle life of the gained nano nickel oxide electrode for ultracapacitor are shown in embodiment 1
It is intended to.
Specific implementation mode
Invention is further explained for following examples, and the invention is not limited in the specific embodiments.In addition,
With without prejudice under the premise of technical solution of the present invention, easy to implement any of those of ordinary skill in the art that the present invention is done
Change or change are fallen within scope of the presently claimed invention.
Raw material in following embodiment is purchased in market.
Embodiment 1
By each raw material according to parts by weight：Nickelous nitrate hexahydrate is 12 parts, and citric acid is 5 parts, and carbonic acid amide is 3 parts, is steamed
Distilled water is 100 parts, and 1h is stirred after mixing, and nickel nitrate solution is made, and the pH that solution is adjusted with 0.01~0.5mol/L ammonium hydroxide is
6.2, hydrothermal temperature is 162 DEG C, in 24 hours reaction time, obtains absinthe-green suspension；
The suspension is cleaned using centrifugal filtration, which is filtering → distilled water cleaning → filtering → absolute ethyl alcohol
Cleaning → filtering → washes of absolute alcohol → filtering → distilled water cleaning filtering → distilled water cleaning, filtrate is in 60 DEG C of baking ovens
It is dry, it obtains green powder, after ball milling, is warming up to 150 DEG C according to the heating rate of 10 DEG C/min in Muffle furnace, heat preservation
30min is then warming up to 550 DEG C with the heating rate of 5 DEG C/min, air-cooled with stove after heat preservation 3 hours, obtain dispersibility it is excellent,
Grain size is the nano-nickel oxide powder of 10-13nm.Be prepared as nano nickel oxide electrode for ultracapacitor specific capacitance and its
Cycle life is as shown in Figure 1, be added the specific capacitance of ultracapacitor after Synthesized by Hydrothermal Method nickel oxide relative to original capacitance device
Specific capacitance improve 30%, slow down 65% under the original specific capacitance of specific capacitance suppression ratio after circular flow 500 times.
Embodiment 2
By each raw material according to parts by weight：Nickelous nitrate hexahydrate is 18 parts, and citric acid is 8 parts, and carbonic acid amide is 5 parts, is steamed
Distilled water is 100 parts, and 1h is stirred after mixing, and nickel nitrate solution is made, and the pH that solution is adjusted with 0.1mol/L NaOH is 6.8, hydro-thermal
Reaction temperature is 162 DEG C, after being mixed, stirs 1h, 24 hours reaction time obtained light green suspension；
The suspension is cleaned using centrifugal filtration, which is filtering → distilled water cleaning → filtering → absolute ethyl alcohol
Cleaning → filtering → washes of absolute alcohol → filtering → distilled water cleaning filtering → distilled water cleaning, it is dry in 60 DEG C of baking ovens,
It obtains green powder, after ball milling, 150 DEG C is warming up to according to the heating rate of 10 DEG C/min in Muffle furnace, keeps the temperature 30min, with
550 DEG C are warming up to the heating rate of 5 DEG C/min afterwards, it is air-cooled with stove after keeping the temperature 2 hours, obtain excellent, the grain size 10- of dispersibility
The nano-nickel oxide powder of 15nm, be added Synthesized by Hydrothermal Method nickel oxide after ultracapacitor specific capacitance relative to original capacitance
The specific capacitance of device improves 55%, and 75% is slowed down under the original specific capacitance of specific capacitance suppression ratio after circular flow 500 times.
Embodiment 3
By each raw material according to parts by weight：Nickelous nitrate hexahydrate is 12 parts, and citric acid is 5 parts, and carbonic acid amide is 3 parts, is steamed
Distilled water is 100 parts, and 1h is stirred after mixing, and nickel nitrate solution is made, and the pH that solution is adjusted with 0.01~0.5mol/L ammonium hydroxide is
6.8, hydrothermal temperature is 162 DEG C, in 24 hours reaction time, obtains absinthe-green suspension；
The suspension is cleaned using centrifugal filtration, which is filtering → distilled water cleaning → filtering → absolute ethyl alcohol
Cleaning → filtering → washes of absolute alcohol → filtering → distilled water cleaning filtering → distilled water cleaning, it is dry in 60 DEG C of baking ovens,
It obtains green powder, after ball milling, 150 DEG C is warming up to according to the heating rate of 10 DEG C/min in Muffle furnace, keeps the temperature 30min, with
550 DEG C are warming up to the heating rate of 5 DEG C/min afterwards, it is air-cooled with stove after keeping the temperature 3 hours, obtain excellent, the grain size 10- of dispersibility
The nano-nickel oxide powder of 14nm, be added Synthesized by Hydrothermal Method nickel oxide after ultracapacitor specific capacitance relative to original capacitance
The specific capacitance of device improves 40%, and 65% is slowed down under the original specific capacitance of specific capacitance suppression ratio after circular flow 500 times.
Claims (6)
1. a kind of nano-nickel oxide raw powder's production technology for ultracapacitor, which is characterized in that nickel nitrate solution is prepared,
The pH that the nickel nitrate solution is adjusted with ammonium hydroxide obtains pale green after being synthesized to the nickel nitrate solution using hydrothermal synthesis method
The suspension is filtered and is cleaned, by obtained filtrate after drying, ball milling, is put into Muffle furnace and forge by the suspension of color
It burns, furnace cooling obtains nano-nickel oxide powder.
2. the nano-nickel oxide raw powder's production technology according to claim 1 for ultracapacitor, which is characterized in that
The nickel nitrate solution is made of Nickelous nitrate hexahydrate, citric acid, carbonic acid amide and distilled water, Nickelous nitrate hexahydrate, citric acid,
The ratio between mass fraction of carbonic acid amide and distilled water is 12~18：5~8：3~5：100.
3. the nano-nickel oxide raw powder's production technology according to claim 1 for ultracapacitor, which is characterized in that
The suspension filters the mode cleaned：Filtering → distilled water cleaning → filtering → washes of absolute alcohol → filtering → anhydrous second
Alcohol cleaning → filtering → distilled water cleaning → filtering → distilled water cleaning.
4. the nano-nickel oxide raw powder's production technology for ultracapacitor according to one of claim 1-3, special
Sign is, specifically comprises the following steps：
1) take Nickelous nitrate hexahydrate, carbonic acid amide, carbonic acid amide and distilled water as raw material in proportion, after being mixed, stirring
Nickel nitrate solution is made in 1h, and the pH that nickel nitrate solution is adjusted with 0.01~0.5mol/L ammonium hydroxide is 6.2~6.8；
2) nickel nitrate solution is moved into polytetrafluoroethylene (PTFE) autoclave, hydrothermal synthesis reaction is carried out for 24 hours under the conditions of 162 DEG C,
Obtain absinthe-green suspension；
3) dry in 60 DEG C of baking ovens after cleaning up by the suspension centrifugal filtration, obtain green powder；
4) it by the green powder after corundum ball grinder ball milling, is put into the heating rate in Muffle furnace using 10 DEG C/min and heats up
To 150 DEG C, 30~60min is kept the temperature, is then warming up to 550~650 DEG C with the heating rate of 5 DEG C/min, after keeping the temperature 2~3 hours,
Furnace cooling obtains nano-nickel oxide powder.
5. the nano-nickel oxide raw powder's production technology according to claim 4 for ultracapacitor, which is characterized in that
The purity of the nano-nickel oxide powder is 99.92~99.99%, and particle size range is 10~30nm.
6. the nano-nickel oxide raw powder's production technology according to claim 4 for ultracapacitor, which is characterized in that
Ultracapacitor is added in the nano-nickel oxide powder, and the specific capacitance of ultracapacitor is carried relative to the specific capacitance of original capacitance device
It is high by 30~55%, slow down 60 after ultracapacitor circular flow 500 times under the specific capacitance of specific capacitance suppression ratio original capacitance device~
75%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810337853.2A CN108373176A (en) | 2018-04-16 | 2018-04-16 | A kind of nano-nickel oxide raw powder's production technology for ultracapacitor |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810337853.2A CN108373176A (en) | 2018-04-16 | 2018-04-16 | A kind of nano-nickel oxide raw powder's production technology for ultracapacitor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109530715A (en) * | 2018-12-13 | 2019-03-29 | 西安工程大学 | A kind of preparation method of ceramic capacitor Ni nanopowders |
| CN110540255A (en) * | 2019-09-23 | 2019-12-06 | 杨景帆 | Process for preparing nano nickel oxide by water-soluble salt isolation method |
| CN111634963A (en) * | 2020-07-03 | 2020-09-08 | 朱义奎 | Preparation method of iron-doped nano nickel oxide powder for super capacitor |
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| CN102863032A (en) * | 2012-09-11 | 2013-01-09 | 河北工业大学 | Preparation method of porous nano-nickel oxide material |
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| CN102863032A (en) * | 2012-09-11 | 2013-01-09 | 河北工业大学 | Preparation method of porous nano-nickel oxide material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109530715A (en) * | 2018-12-13 | 2019-03-29 | 西安工程大学 | A kind of preparation method of ceramic capacitor Ni nanopowders |
| CN110540255A (en) * | 2019-09-23 | 2019-12-06 | 杨景帆 | Process for preparing nano nickel oxide by water-soluble salt isolation method |
| CN110540255B (en) * | 2019-09-23 | 2021-12-21 | 杨景帆 | Process for preparing nano nickel oxide by water-soluble salt isolation method |
| CN111634963A (en) * | 2020-07-03 | 2020-09-08 | 朱义奎 | Preparation method of iron-doped nano nickel oxide powder for super capacitor |
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