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CN111634963A - Preparation method of iron-doped nano nickel oxide powder for super capacitor - Google Patents

Preparation method of iron-doped nano nickel oxide powder for super capacitor Download PDF

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Publication number
CN111634963A
CN111634963A CN202010629963.3A CN202010629963A CN111634963A CN 111634963 A CN111634963 A CN 111634963A CN 202010629963 A CN202010629963 A CN 202010629963A CN 111634963 A CN111634963 A CN 111634963A
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iron
oxide powder
nickel oxide
doped nano
nano nickel
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朱义奎
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00Compounds of nickel
    • C01G53/04Oxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/24Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/46Metal oxides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/40Electric properties
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Power Engineering (AREA)
  • Nanotechnology (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Organic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of iron-doped nano nickel oxide powder for a super capacitor. The technical scheme of the invention is as follows: a preparation method of iron-doped nano nickel oxide powder for a super capacitor comprises the steps of preparing a mixed solution of nickel nitrate and ferric nitrate according to a proportion, adding a certain amount of polyacrylamide, uniformly stirring, transferring the solution into a polytetrafluoroethylene reaction kettle, synthesizing a brownish red prepolymer suspension by adopting a hydrothermal method, filtering, cleaning, drying, ball-milling, sintering in a muffle furnace, and cooling along with the furnace to obtain the iron-doped nano nickel oxide powder. The preparation method of the iron-doped nano nickel oxide powder for the super capacitor can obtain the nano nickel oxide powder with excellent dispersibility, narrow particle size distribution, high specific capacitance and small internal resistance.

Description

Preparation method of iron-doped nano nickel oxide powder for super capacitor
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of iron-doped nano nickel oxide powder for a super capacitor.
Background
The rapid increase of global economy is not away from the rapid development of industry, but the promotion of economic growth by means of industrial development consumes a large amount of fossil energy, causes the gradual exhaustion of natural resources, and leads to the great increase of carbon dioxide emission. Therefore, renewable energy and clean energy are required to be searched as soon as possible.
As a novel energy storage element, the super capacitor has excellent characteristics of high power density, rapid charging, wide temperature range of use, long service life and the like, and is an important support technology for energy reformation and draws more and more attention.
The activity of the electrode material directly influences the performance of the super capacitor, and the nano nickel oxide powder has the advantages of controllable structural performance, environmental friendliness, low cost and the like, so that the nano nickel oxide powder is widely applied.
However, the existing nano nickel oxide powder has the problems of serious agglomeration phenomenon, low specific capacitance and large internal resistance.
Disclosure of Invention
The invention provides a preparation method of iron-doped nano nickel oxide powder for a super capacitor, which is characterized in that nickel nitrate hexahydrate, ferric nitrate, polyacrylamide, ammonia water and deionized water are used as main raw materials, a prepolymer is prepared by a hydrothermal method, and then the doped nano nickel oxide powder with excellent dispersibility, large specific capacitance and small internal resistance is prepared by the processes of filtering, cleaning, drying, ball milling, sintering and the like.
The technical scheme of the invention is as follows:
a preparation method of iron-doped nano nickel oxide powder for a super capacitor comprises the steps of preparing a mixed solution of nickel nitrate and ferric nitrate according to a proportion, adding a certain amount of polyacrylamide, uniformly stirring, transferring the solution into a polytetrafluoroethylene reaction kettle, synthesizing a brownish red prepolymer suspension by adopting a hydrothermal method, filtering, cleaning, drying, ball-milling, sintering in a muffle furnace, and cooling along with the furnace to obtain the iron-doped nano nickel oxide powder.
The preferable scheme of the preparation method of the iron-doped nano nickel oxide powder for the super capacitor is that the raw materials for preparing the iron-doped nano nickel oxide powder comprise the following components in parts by weight: 25-40 parts of nickel nitrate hexahydrate, 8-15 parts of ferric nitrate nonahydrate, 3-8 parts of polyacrylamide, 2-4 parts of 0.05mol/L ammonia water and 100 parts of deionized water.
The preparation method of the iron-doped nano nickel oxide powder for the super capacitor specifically comprises the following steps:
1) taking nickel nitrate hexahydrate, ferric nitrate nonahydrate and deionized water according to a certain proportion, mixing, uniformly stirring, adding polyacrylamide, and continuously uniformly stirring to obtain a yellow mixed solution A;
2) adding 0.05mol/L ammonia water into the solution A to adjust the pH value of the nickel nitrate solution to 7.1-7.5 to obtain a solution B;
3) transferring the solution B into a polytetrafluoroethylene reaction kettle to enable the filling degree of the reaction kettle to be 75%, carrying out hydration reaction for 2-5 hours at the temperature of 150 ℃, and cooling to obtain a dark yellow suspension C;
4) carrying out suction filtration on the suspension C, sequentially washing the suspension C with deionized water and absolute ethyl alcohol, washing the suspension C for three times in this way, carrying out suction filtration after each washing, and drying the suspension C in a 75 ℃ drying oven after the suspension C is washed clean to obtain brownish red powder D;
5) and (3) performing ball milling on the brownish red powder D in a corundum ball milling tank, sintering for 2 hours in a muffle furnace at 350-450 ℃, and cooling along with the furnace to obtain the iron-doped nano nickel oxide powder.
The preferable scheme of the preparation method of the iron-doped nano nickel oxide powder for the super capacitor is that the average particle size of the iron-doped nano nickel oxide powder is 25-50 nm.
The preferable scheme of the preparation method of the iron-doped nano nickel oxide powder for the super capacitor is that the iron-doped nano nickel oxide powder is filled on porous nickel to prepare an electrode, and the electrode is prepared at 5-12 mA/cm2The specific capacitance of the porous nickel electrode is improved by 35.6-52.3% compared with that of a single porous nickel electrode under the current density of (2).
The preferable scheme of the preparation method of the iron-doped nano nickel oxide powder for the super capacitor is that the iron-doped nano nickel oxide powder is filled on porous nickel to prepare an electrode, and when the iron-doped nano nickel oxide powder is used as the super capacitor, the internal resistance is 0.36-0.41 m omega, which is reduced by 60.2-65.0% compared with the internal resistance of a super capacitor with a single porous nickel electrode.
The invention has the beneficial effects that:
(1) the ammonia water used in the invention is used for adjusting the pH value of the solution.
(2) The polyacrylamide used in the invention is used as a reinforcing agent and a dispersing agent, and the prepolymer nickel hydroxide and the ferric hydroxide can be connected together, so that the sintered iron element is uniformly doped in the nickel oxide powder.
(3) The iron-doped nano nickel oxide powder prepared by the invention has good dispersibility, narrow particle size distribution range, high specific capacitance and small internal resistance, and meets the use requirement of a super capacitor.
Detailed Description
The technical solutions of the present application will be described in detail below with reference to specific embodiments of the present application, but the present invention is not limited to the specific embodiments. In addition, any modification or change that can be easily made by a person having ordinary skill in the art without departing from the technical solution of the present invention will fall within the scope of the claims of the present invention.
The starting materials in the following examples are all commercially available.
Example 1
1) In the preparation method of the iron-doped nano nickel oxide powder for the super capacitor, the raw materials and the parts by mass are as follows: 25 parts of nickel nitrate hexahydrate, 8 parts of ferric nitrate nonahydrate and 100 parts of deionized water, mixing, uniformly stirring, adding 3 parts of polyacrylamide, and continuously uniformly stirring to obtain a yellow mixed solution A;
2) adding 2 parts of 0.05mol/L ammonia water into the solution A, and adjusting the pH value of the nickel nitrate solution to 7.1 to obtain a solution B;
3) transferring the solution B into a polytetrafluoroethylene reaction kettle, enabling the filling degree of the reaction kettle to be 75%, reacting for 2 hours at the temperature of 150 ℃, and cooling to obtain a dark yellow suspension C;
4) carrying out suction filtration on the suspension C, sequentially washing the suspension C with deionized water and absolute ethyl alcohol, washing the suspension C for three times in this way, carrying out suction filtration after each washing, and drying the suspension C in a 75 ℃ drying oven after the suspension C is washed clean to obtain brownish red powder D;
5) ball-milling the brownish red powder D in a corundum ball-milling tank, sintering for 2 hours at 350 ℃ in a muffle furnace, cooling along with the furnace to obtain iron-doped nano nickel oxide powder with the average particle size of 28nm, filling the iron-doped nano nickel oxide powder on porous nickel to prepare an electrode, and performing ball milling at 5mA/cm2Specific capacitance of the porous nickel electrode than that of a single porous nickel electrode at a current density ofThe internal resistance of the electrode is improved by 38.1 percent, and when the electrode is used as a super capacitor, the internal resistance is 0.39m omega, which is reduced by 62.1 percent compared with the internal resistance of a super capacitor with a single porous nickel electrode.
Example 2
1) In the preparation method of the iron-doped nano nickel oxide powder for the super capacitor, the raw materials and the parts by mass are as follows: 35 parts of nickel nitrate hexahydrate, 15 parts of ferric nitrate nonahydrate and 100 parts of deionized water, mixing, uniformly stirring, adding 5 parts of polyacrylamide, and continuously uniformly stirring to obtain a yellow mixed solution A;
2) adding 4 parts of 0.05mol/L ammonia water into the solution A, and adjusting the pH value of the nickel nitrate solution to 7.4 to obtain a solution B;
3) transferring the solution B into a polytetrafluoroethylene reaction kettle to enable the filling degree of the reaction kettle to be 75%, carrying out hydration reaction for 5 hours at the temperature of 150 ℃, and cooling to obtain a dark yellow suspension C;
4) carrying out suction filtration on the suspension C, sequentially washing the suspension C with deionized water and absolute ethyl alcohol, washing the suspension C for three times in this way, carrying out suction filtration after each washing, and drying the suspension C in a 75 ℃ drying oven after the suspension C is washed clean to obtain brownish red powder D;
5) ball-milling the brownish red powder D in a corundum ball-milling tank, sintering for 2 hours in a muffle furnace at the temperature of 420 ℃, cooling along with the furnace to obtain iron-doped nano nickel oxide powder with the average particle size of 46nm, filling the iron-doped nano nickel oxide powder on porous nickel to prepare an electrode, and performing ball-milling at the temperature of 10mA/cm2The specific capacitance of the electrode is improved by 49.6 percent compared with the specific capacitance of a single porous nickel electrode, and when the electrode is used as a super capacitor, the internal resistance is 0.37m omega, which is reduced by 64.1 percent compared with the internal resistance of the super capacitor with the single porous nickel electrode.
Example 3
1) In the preparation method of the iron-doped nano nickel oxide powder for the super capacitor, the raw materials and the parts by mass are as follows: 40 parts of nickel nitrate hexahydrate, 12 parts of ferric nitrate nonahydrate and 100 parts of deionized water, uniformly stirring after mixing, adding 8 parts of polyacrylamide, and continuously uniformly stirring to obtain a yellow mixed solution A;
2) adding 3 parts of 0.05mol/L ammonia water into the solution A, and adjusting the pH value of the nickel nitrate solution to 7.3 to obtain a solution B;
3) transferring the solution B into a polytetrafluoroethylene reaction kettle, enabling the filling degree of the reaction kettle to be 75%, reacting for 3 hours at the temperature of 150 ℃, and cooling to obtain a dark yellow suspension C;
4) carrying out suction filtration on the suspension C, sequentially washing the suspension C with deionized water and absolute ethyl alcohol, washing the suspension C for three times in this way, carrying out suction filtration after each washing, and drying the suspension C in a 75 ℃ drying oven after the suspension C is washed clean to obtain brownish red powder D;
5) ball-milling the brownish red powder D in a corundum ball-milling tank, sintering for 2 hours at 450 ℃ in a muffle furnace, cooling along with the furnace to obtain iron-doped nano nickel oxide powder with the average particle size of 42nm, filling the iron-doped nano nickel oxide powder on porous nickel to prepare an electrode, and performing ball milling at 5mA/cm2The specific capacitance of the electrode is improved by 47.3 percent compared with that of a single porous nickel electrode, and when the electrode is used as a super capacitor, the internal resistance is 0.40m omega and is reduced by 61.2 percent compared with that of the super capacitor with the single porous nickel electrode.

Claims (6)

1. A preparation method of iron-doped nano nickel oxide powder for a super capacitor is characterized by preparing a mixed solution of nickel nitrate and ferric nitrate according to a proportion, adding a certain amount of polyacrylamide, uniformly stirring, transferring the solution into a polytetrafluoroethylene reaction kettle, synthesizing a brownish red prepolymer suspension by adopting a hydrothermal method, filtering, cleaning, drying and ball-milling the suspension, then putting the suspension into a muffle furnace for sintering, and cooling along with the furnace to obtain the iron-doped nano nickel oxide powder.
2. The method for preparing the iron-doped nano nickel oxide powder for the supercapacitor according to claim 1, wherein the iron-doped nano nickel oxide powder is prepared from the following raw materials in parts by mass: 25-40 parts of nickel nitrate hexahydrate, 8-15 parts of ferric nitrate nonahydrate, 3-8 parts of polyacrylamide, 2-4 parts of 0.05mol/L ammonia water and 100 parts of deionized water.
3. The preparation method of the iron-doped nano nickel oxide powder for the supercapacitor according to claims 1 to 2, which is characterized by comprising the following steps:
1) taking nickel nitrate hexahydrate, ferric nitrate nonahydrate and deionized water according to a certain proportion, mixing, uniformly stirring, adding polyacrylamide, and continuously uniformly stirring to obtain a yellow mixed solution A;
2) adding 0.05mol/L ammonia water into the solution A to adjust the pH value of the nickel nitrate solution to 7.1-7.5 to obtain a solution B;
3) transferring the solution B into a polytetrafluoroethylene reaction kettle to enable the filling degree of the reaction kettle to be 75%, carrying out hydration reaction for 2-5 hours at the temperature of 150 ℃, and cooling to obtain a dark yellow suspension C;
4) carrying out suction filtration on the suspension C, sequentially washing the suspension C with deionized water and absolute ethyl alcohol, washing the suspension C for three times in this way, carrying out suction filtration after each washing, and drying the suspension C in a 75 ℃ drying oven after the suspension C is washed clean to obtain brownish red powder D;
5) and ball-milling the brownish red powder D in a corundum ball-milling tank, sintering for 2 hours in a muffle furnace at 350-450 ℃, and cooling along with the furnace to obtain the iron-doped nano nickel oxide powder.
4. The method for preparing the iron-doped nano nickel oxide powder for the supercapacitor according to claim 1, wherein the average particle size of the iron-doped nano nickel oxide powder is 25-50 nm.
5. The method for preparing the iron-doped nano nickel oxide powder for the supercapacitor according to claim 1, wherein the iron-doped nano nickel oxide powder is filled on porous nickel to form an electrode, and the electrode is prepared at 5-12 mA/cm2The specific capacitance of the porous nickel electrode is improved by 35.6-52.3% compared with that of a single porous nickel electrode under the current density of (2).
6. The method for preparing the iron-doped nano nickel oxide powder for the supercapacitor according to claim 1, wherein the iron-doped nano nickel oxide powder is filled on porous nickel to form an electrode, and when the iron-doped nano nickel oxide powder is used as the supercapacitor, the internal resistance is 0.36-0.41 m Ω, which is 60.2-65.0% lower than that of a supercapacitor with a single porous nickel electrode.
CN202010629963.3A 2020-07-03 2020-07-03 Preparation method of iron-doped nano nickel oxide powder for super capacitor Pending CN111634963A (en)

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Publication number Priority date Publication date Assignee Title
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