CN107758750A - A kind of method that hydro-thermal method prepares the nickel hydroxide nano piece of different-shape - Google Patents

A kind of method that hydro-thermal method prepares the nickel hydroxide nano piece of different-shape Download PDF

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CN107758750A
CN107758750A CN201710976753.XA CN201710976753A CN107758750A CN 107758750 A CN107758750 A CN 107758750A CN 201710976753 A CN201710976753 A CN 201710976753A CN 107758750 A CN107758750 A CN 107758750A
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foam substrate
nickel
hydro
nickel foam
nano piece
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王硕
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Zhengzhou Bak Battery Co Ltd
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Zhengzhou Bak Battery Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00Compounds of nickel
    • C01G53/04Oxides; Hydroxides
    • 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
    • H01G11/30Electrodes characterised by their material
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/20Particle morphology extending in two dimensions, e.g. plate-like
    • 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)
  • Organic Chemistry (AREA)
  • Power Engineering (AREA)
  • Nanotechnology (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
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Abstract

A kind of method that the nickel hydroxide nano piece of different-shape is prepared the invention provides hydro-thermal method, comprises the following steps:(1)Handle nickel foam substrate:Nickel foam substrate is put into hydrochloric acid, is subsequently placed into ultrasonic cleaner and cleans 5min, the nickel foam substrate after ultrasonic cleaner is handled, which is put into drying baker, to be dried for standby;(2)Prepare mixed aqueous solution:By Ni (NO3)2∙6H2O、NH4F、H3BO3, CTAB be successively scattered in by a certain percentage in deionized water, be stirred obtained A mixed solutions;(3)Hydro-thermal method synthesizes nickel hydroxide nano piece:By step(1)In treat nickel foam substrate be put into A mixed solutions, be then placed in the h of hydro-thermal reaction 12 in the reactor of 100 DEG C of constant temperature, you can obtain nickel hydroxide nano piece.It is an advantage of the invention that change the pattern of nanometer sheet, increasing specific surface area and chemical property by changing the concentration of nickel ion in the solution, so as to obtain higher specific capacity, good cycle performance.

Description

A kind of method that hydro-thermal method prepares the nickel hydroxide nano piece of different-shape
Technical field
The present invention relates to electrode material for super capacitor technical field, more particularly to a kind of hydro-thermal method to prepare different-shape Nickel hydroxide nano piece method.
Background technology
With the progress in epoch, global economy is fast-developing, and fossil energy constantly consumes, environmental pollution getting worse, The energy conversion and storage system for studying a kind of efficient, overcast have seemed more and more important, and ultracapacitor is due to tool There is the advantages that power density is high, and the charging interval is short, service life is long, be widely used in electric automobile, military affairs, mobile communication are set The field such as standby, so as to trigger the extensive concern of vast researcher.
To the demand of the energy, vast researcher by sight put into cleaning and regenerative resource energy storage and In conversion, ultracapacitor is also referred to as electrochemical capacitor, including non-faraday double layer capacitor(Double layer capacitor), its The electric charge of storage is stored in the interface between electrode and electrolyte;And fake capacitance, its store by electrode material and electrolyte it Between quickly through electric charge caused by faraday's reaction.In ultracapacitor, fake capacitance can provide more than double layer capacitor High energy density, an attractive candidate include conducting polymer and some metal oxides, including RuO2、MnO2、 Fe2O3、Co3O4With Ni (OH)2It is studied personnel's research, wherein RuO extensively2Higher specific capacity is shown than other materials, But because cost is high, its business application is limited, therefore we need to find suitable substitute, the present invention is with Ni (NO3)2∙6H2O is raw material, and the nickel hydroxide nano piece of different-shape is obtained by hydro-thermal method, wherein in hydrothermal reaction process, is led to The content of control nickel ion is crossed, so as to control the growth course of nickel hydroxide, changes nickel hydroxide nano piece pattern to reach, from And higher specific capacity is obtained, good cycle performance.
The content of the invention
A kind of method that the nickel hydroxide nano piece of different-shape is prepared it is an object of the invention to provide hydro-thermal method, passes through water Hot method synthesizes nickel hydroxide nano piece in nickel foam substrate, and changes nanometer sheet by changing the concentration of nickel ion in the solution Pattern, so as to obtain higher specific capacity, good cycle performance.
The technical solution adopted by the present invention is as follows:
A kind of method that hydro-thermal method prepares the nickel hydroxide nano piece of different-shape, comprises the following steps:
(1)Handle nickel foam substrate:Nickel foam substrate is put into hydrochloric acid, then put the nickel foam substrate being immersed in hydrochloric acid Enter and 5min cleaned in ultrasonic cleaner, the nickel foam substrate after ultrasonic cleaner is handled be put into drying baker dry it is standby With;
(2)Prepare mixed aqueous solution:By Ni (NO3) 2 6H2O, NH4F, H3BO3, CTAB be successively scattered in by a certain percentage from In sub- water, obtained A mixed solutions are stirred;
(3)Hydro-thermal method synthesizes nickel hydroxide nano piece:By step(1)In treat nickel foam substrate be put into A mixed solutions, Then the A mixed solutions for being placed with nickel foam substrate are put into the h of hydro-thermal reaction 12 in the reactor of 100 DEG C of constant temperature, you can obtain hydrogen Nickel oxide nano piece.
Preferably, the step(1)In, the temperature dried in baking oven is 60 DEG C.
Preferably, the step(2)In, mixing time is 8-12 h.
Preferably, the step(2)In, Ni (NO3)2∙6H2O addition is 0.5-5mM, NH4F addition is 4mM, H3BO3Addition be 9.1mM, CTAB addition is 0.685mmol, and the addition of deionized water is 50ml.
Preferably, the step(3)In, reacted nickel foam substrate is successively respectively washed 3 times with deionized water, ethanol, Then the nickel foam substrate after washing is put into drying baker and dried, wherein, drying temperature is 60 DEG C.
The advantage of the invention is that:
(1)This method is with Ni (NO3)2∙6H2O is raw material, reduces cost, and preparation method is simple, and green, obtained difference The nickel hydroxide nano piece of pattern can obtain larger specific surface area and more preferable chemical property.
(2)Nickel hydroxide nano piece made from this method be used to showing during electrode material for super capacitor specific capacity it is high, The features such as good cycling stability, low internal resistance.
Brief description of the drawings
Fig. 1 is the SEM image of nickel hydroxide nano piece prepared by embodiment 3 in the present invention.
Fig. 2 is the XRD picture of nickel hydroxide nano piece prepared by embodiment 3 in the present invention.
Fig. 3 is the TEM image of nickel hydroxide nano piece prepared by embodiment 3 in the present invention.
Fig. 4 is the HRTEM images of nickel hydroxide nano piece prepared by embodiment 3 in the present invention.
Fig. 5 is the cycle-index test that the nickel hydroxide nano piece that in the present invention prepared by embodiment 3 is used for ultracapacitor Figure.
Embodiment
The method work for preparing the nickel hydroxide nano piece of different-shape to a kind of hydro-thermal method of the present invention below is further detailed Description.
Embodiment 1
(1)Handle nickel foam substrate:Nickel foam substrate is put into hydrochloric acid, then put the nickel foam substrate being immersed in hydrochloric acid Enter 5min in ultrasonic cleaner, the cleaned nickel foam substrate of ultrasonic wave is put into drying baker and is dried for standby, wherein, The temperature dried in baking oven is 60 DEG C;
(2)Prepare mixed aqueous solution:Weigh 0.5mM Ni (NO3)2∙6H2O, 4mM NH4F, 9.1mM H3BO3With 0.685mmol CTAB is successively scattered in 50ml deionized water, is stirred obtained A mixed solutions, wherein mixing time 8h;
(3)Hydro-thermal method synthesizes nickel hydroxide nano piece:By step(1)In treat nickel foam substrate be put into A mixed solutions, Then the A mixed solutions for being put into nickel foam substrate are put into the h of hydro-thermal reaction 12 in the reactor of 100 DEG C of constant temperature, you can obtain hydrogen Nickel oxide nano piece;
(4)By step(3)In, reacted nickel foam substrate is successively respectively washed 3 times with deionized water, ethanol, then will washing Nickel foam substrate afterwards, which is put into drying baker, dries, wherein, drying temperature is set to 60 DEG C.
Embodiment 2
(1)Handle nickel foam substrate:Nickel foam substrate is put into hydrochloric acid, then put the nickel foam substrate being immersed in hydrochloric acid Enter 5min in ultrasonic cleaner, the cleaned nickel foam substrate of ultrasonic wave is put into drying baker and is dried for standby, wherein, The temperature dried in baking oven is 60 DEG C;
(2)Prepare mixed aqueous solution:Weigh 1mM Ni (NO3)2∙6H2O, 4mM NH4F, 9.1mM H3BO3And 0.685mmol CTAB successively be scattered in 50ml deionized water, be stirred obtained A mixed solutions, wherein mixing time 9h;
(3)Hydro-thermal method synthesizes nickel hydroxide nano piece:By step(1)In treat nickel foam substrate be put into A mixed solutions, Then the A mixed solutions for being put into nickel foam substrate are put into the h of hydro-thermal reaction 12 in the reactor of 100 DEG C of constant temperature, you can obtain hydrogen Nickel oxide nano piece;
(4)By step(3)In, reacted nickel foam substrate is successively respectively washed 3 times with deionized water, ethanol, then will washing Nickel foam substrate afterwards, which is put into drying baker, dries, wherein, drying temperature is set to 60 DEG C.
Embodiment 3
(1)Handle nickel foam substrate:Nickel foam substrate is put into hydrochloric acid, then put the nickel foam substrate being immersed in hydrochloric acid Enter 5min in ultrasonic cleaner, the nickel foam substrate after ultrasonication is put into drying baker and is dried for standby, wherein, baking oven The temperature of middle drying is 60 DEG C;
(2)Prepare mixed aqueous solution:Weigh 3mM Ni (NO3)2∙6H2O, 4mM NH4F, 9.1mM H3BO3And 0.685mmol CTAB successively be scattered in 50ml deionized water, be stirred obtained A mixed solutions, wherein mixing time 10h;
(3)Hydro-thermal method synthesizes nickel hydroxide nano piece:By step(1)In treat nickel foam substrate be put into A mixed solutions, Then the A mixed solutions for being put into nickel foam substrate are put into the h of hydro-thermal reaction 12 in the reactor of 100 DEG C of constant temperature, you can obtain hydrogen Nickel oxide nano piece;
(4)By step(3)In, reacted nickel foam substrate is successively respectively washed 3 times with deionized water, ethanol, then will washing Nickel foam substrate afterwards, which is put into drying baker, dries, wherein, drying temperature is set to 60 DEG C.
Embodiment 4
(1)Handle nickel foam substrate:Nickel foam substrate is put into hydrochloric acid, then put the nickel foam substrate being immersed in hydrochloric acid Enter 5min in ultrasonic cleaner, the cleaned nickel foam substrate of ultrasonic wave is put into drying baker and is dried for standby, wherein, The temperature dried in baking oven is 60 DEG C;
(2)Prepare mixed aqueous solution:5mM Ni (NO3)2∙6H2O, 4mM NH4F, 9.1mM H3BO3With 0.685mmol's CTAB is successively scattered in 50ml deionized water, is stirred obtained A mixed solutions, wherein mixing time 12h;
(3)Hydro-thermal method synthesizes nickel hydroxide nano piece:By step(1)In treat nickel foam substrate be put into A mixed solutions, Then the A mixed solutions for being put into nickel foam substrate are put into the h of hydro-thermal reaction 12 in the reactor of 100 DEG C of constant temperature, you can obtain hydrogen Nickel oxide nano piece;
(4)By step(3)In, reacted nickel foam substrate is successively respectively washed 3 times with deionized water, ethanol, then will washing Nickel foam substrate afterwards, which is put into drying baker, dries, wherein, drying temperature is set to 60 DEG C.
Experimental result:Obtained nickel hydroxide nano piece in embodiment 3 therein is chosen to be tested, can from Fig. 2 Go out and successfully prepare nickel hydroxide;Nickel hydroxide nano piece is perpendicular to the growth of nickel foam substrate as can be seen from Figure 1, and structure causes Close uniform, specific surface area is high, can improve chemical property, it is vertical life that Fig. 3, Fig. 4, which further demonstrate nickel hydroxide nano piece, Long;It can be seen that capacity stills remain in more than 90% after circulating 2000 times, significantly improves following for ultracapacitor in Fig. 5 The ring life-span.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention All any modification, equivalent and improvement made within refreshing and principle etc., all should be included within protection scope of the present invention.

Claims (5)

1. a kind of method that hydro-thermal method prepares the nickel hydroxide nano piece of different-shape, it is characterised in that:Comprise the following steps:
Handle nickel foam substrate:Nickel foam substrate is put into hydrochloric acid, is then put into the nickel foam substrate being immersed in hydrochloric acid 5min is cleaned in ultrasonic cleaner, the nickel foam substrate after ultrasonic cleaner is handled, which is put into drying baker, to be dried for standby;
Prepare mixed aqueous solution:By Ni (NO3)2∙6H2O、NH4F、H3BO3, CTAB be successively scattered in deionized water by a certain percentage In, it is stirred obtained A mixed solutions;
Hydro-thermal method synthesizes nickel hydroxide nano piece:By step(1)In treat nickel foam substrate be put into A mixed solutions, so The A mixed solutions for being placed with nickel foam substrate are put into the h of hydro-thermal reaction 12 in the reactor of 100 DEG C of constant temperature afterwards, you can obtain hydrogen-oxygen Change nickel nano film.
2. a kind of hydro-thermal method according to claim 1 prepares the method for the nickel hydroxide nano piece of different-shape, its feature It is:The step(1)In, the temperature dried in baking oven is 60 DEG C.
3. a kind of hydro-thermal method according to claim 1 prepares the method for the nickel hydroxide nano piece of different-shape, its feature It is:The step(2)In, mixing time is 8-12 h.
4. a kind of hydro-thermal method according to claim 1 prepares the method for the nickel hydroxide nano piece of different-shape, its feature It is:The step(2)In, Ni (NO3)2∙6H2O addition is 0.5-5mM, NH4F addition is 4mM, H3BO3Addition Measure as 9.1mM, CTAB addition is 0.685mmol, and the addition of deionized water is 50ml.
5. a kind of hydro-thermal method according to claim 1 prepares the method for the nickel hydroxide nano piece of different-shape, its feature It is:The step(3)In, reacted nickel foam substrate is successively respectively washed 3 times with deionized water, ethanol, then will washing Nickel foam substrate afterwards, which is put into drying baker, dries, wherein, drying temperature is 60 DEG C.
CN201710976753.XA 2017-10-19 2017-10-19 A kind of method that hydro-thermal method prepares the nickel hydroxide nano piece of different-shape Pending CN107758750A (en)

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Cited By (8)

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Publication number Priority date Publication date Assignee Title
CN109273291A (en) * 2018-11-23 2019-01-25 海南大学 A kind of synthetic method of sulphur cobalt nickel composite material
CN109809482A (en) * 2019-04-08 2019-05-28 西安工业大学 A kind of preparation method of monodisperse, multiform looks Zirconium powder
CN109830380A (en) * 2019-02-18 2019-05-31 南阳理工学院 A kind of electrode material for super capacitor, preparation method and application
CN110040792A (en) * 2019-03-04 2019-07-23 天津大学 Preparation method of nickel hydroxide nanosheet array material growing on surface of foamed nickel
CN110911657A (en) * 2018-12-28 2020-03-24 云南铑熠金属材料有限公司 Preparation method and application of nano flaky nickel-hydroxide composite cobalt-ruthenium oxide
CN111195518A (en) * 2020-01-10 2020-05-26 兰州大学 NiO/Co3O4Preparation method and application thereof
CN111943286A (en) * 2020-08-18 2020-11-17 中国人民解放军空军预警学院雷达士官学校 Nickel-nickel hydroxide composite film electrode and preparation method and application thereof
CN115161646A (en) * 2022-07-07 2022-10-11 宁波江丰电子材料股份有限公司 Method for removing oxide on surface of electrolytic nickel

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CN106298285A (en) * 2016-09-26 2017-01-04 安徽师范大学 A kind of nickel hydroxide@manganese dioxide nucleocapsid heterogeneous structural nano chip arrays material of growth, preparation method and applications on carbon cloth

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109273291A (en) * 2018-11-23 2019-01-25 海南大学 A kind of synthetic method of sulphur cobalt nickel composite material
CN110911657A (en) * 2018-12-28 2020-03-24 云南铑熠金属材料有限公司 Preparation method and application of nano flaky nickel-hydroxide composite cobalt-ruthenium oxide
CN109830380A (en) * 2019-02-18 2019-05-31 南阳理工学院 A kind of electrode material for super capacitor, preparation method and application
CN110040792A (en) * 2019-03-04 2019-07-23 天津大学 Preparation method of nickel hydroxide nanosheet array material growing on surface of foamed nickel
CN110040792B (en) * 2019-03-04 2021-08-27 天津大学 Preparation method of nickel hydroxide nanosheet array material growing on surface of foamed nickel
CN109809482A (en) * 2019-04-08 2019-05-28 西安工业大学 A kind of preparation method of monodisperse, multiform looks Zirconium powder
CN109809482B (en) * 2019-04-08 2021-03-30 西安工业大学 Preparation method of monodisperse multi-morphology zirconia powder
CN111195518A (en) * 2020-01-10 2020-05-26 兰州大学 NiO/Co3O4Preparation method and application thereof
CN111195518B (en) * 2020-01-10 2022-11-25 兰州大学 NiO/Co 3 O 4 Preparation method and application thereof
CN111943286A (en) * 2020-08-18 2020-11-17 中国人民解放军空军预警学院雷达士官学校 Nickel-nickel hydroxide composite film electrode and preparation method and application thereof
CN115161646A (en) * 2022-07-07 2022-10-11 宁波江丰电子材料股份有限公司 Method for removing oxide on surface of electrolytic nickel

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