CN101830522A - Nickel oxide microspheres with ferromagnetism and excellent electrochemical performance and synthetic method thereof - Google Patents
Nickel oxide microspheres with ferromagnetism and excellent electrochemical performance and synthetic method thereof Download PDFInfo
- Publication number
- CN101830522A CN101830522A CN200910111238A CN200910111238A CN101830522A CN 101830522 A CN101830522 A CN 101830522A CN 200910111238 A CN200910111238 A CN 200910111238A CN 200910111238 A CN200910111238 A CN 200910111238A CN 101830522 A CN101830522 A CN 101830522A
- Authority
- CN
- China
- Prior art keywords
- nickel oxide
- micron
- temperature
- microspheres
- spherical
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
- Y02E60/10—Energy storage using batteries
Landscapes
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to nickel oxide microspheres with ferromagnetism and excellent electrochemical performance and a synthetic method thereof. The preparation method comprises the following steps of: preparing alpha-Ni(OH)2 spherical precursors in a hydrothermal environment in the absence of template agent and alkali, and then sintering the precursors at the temperature of above 300 DEG C to form pure-phase nickel oxide microspheres. The size of the nickel oxide microspheres is 1 to 5 microns, each microsphere is assembled by 10 to 100 nanometers, the microspheres have obvious room temperature ferromagnetism, the coercive force of the microspheres can reach 500Oe, the obtained nickel oxide microspheres serve as an electrode material for a lithium ion battery, and the primary discharge capacity of the nickel oxide microspheres is 918mAh/g.
Description
Technical field
The present invention relates to technical field of nano material, is development high-performance nano magneticsubstance, the important directions of battery electrode material.Especially a kind of important method that develops the nano material self-assembly.
Background technology
In industry, nickel oxide is important material and functional materials, and is main as the powder stock of producing battery electrode, catalyzer, magneticsubstance, semi-conductor (as pressure-sensitive, thermistor), nickel-zinc ferrite, glass and ceramic coloring material.The performance of these materials is decided by the size and the pattern of nickel oxide to a great extent, so people adopt the template aid preparation to go out the nickel oxide particle of various patterns. directly do not using under the situation of template, yet it is found that the ammonia that ammoniacal liquor discharges can be used as the nickel oxide that soft template is synthesized various hollow structures equally in heat-processed. neither using organic formwork agent, do not use under the situation of ammoniacal liquor or urea again, prepare spherical nickel oxide and do not appear in the newspapers yet and lead.
Industrial nickel oxide powder commonly used is the near-spherical particle of several micron dimensions, because bigger particle can improve the tap density of powder body material, for example in magneticsubstance, higher tap density can improve magnetic energy product density; In lithium ion and electrode material for nickel-hydrogen cell, higher tap density can improve its unit volume energy density.On the other hand, less during to nano-scale when particle size, dimensional effect and side effect will be more and more important, for example in magneticsubstance, the micron order nickel oxide has antiferromagnetic ground state, but the side effect of nano-scale particle can make the antiferromagnetism nickel oxide become ferromagnetic substance; In lithium ion battery material, nano particle can improve its specific storage and high rate performance, but nano particle is easy to come off in ionogen, thereby and penetrates barrier film and reduce its cycle performance.Therefore want to obtain simultaneously the feature that higher tap density and nano material are brought, prepare that a kind of to assemble the micron order second particle by nanoparticle obviously extremely important.
The present invention proposes by control precursor α-Ni (OH)
2, prepare the method for the micron level spherical nickel oxide that assembles by nano particle. and the micron level spherical nickel oxide that is obtained has ferromegnetism and excellent electrochemical properties.
Summary of the invention
The present invention proposes a kind of micron level spherical nickel oxide and synthetic method thereof that assembles by nano particle, purpose is to improve its tap density, utilize simultaneously the dimensional effect of nano material to greatest extent, magneticsubstance that development and application has a extensive future and electrode materials.
The present invention relates to the preparation method of the micron level spherical nickel oxide that nano particle assembles, detailed process is as follows: (1) is at first at preparation precursor α-Ni (OH) 2 micron order balls.With Ni (NO
3)
26H
2O is dissolved in the ethanol, after fully stirring, changes the reactor constant temperature reaction over to, and thermostat temperature is 120 ℃-250 ℃, and constant temperature time is 2-48h.After reaction finishes, cool to room temperature, centrifugal, washing, drying is collected and is obtained micron level spherical α-Ni (OH) of being made up of nano particle
2(2) with the micron level spherical α-Ni (OH) that obtains
2Put into temperature and be 300-900 ℃ stove and heat-treat, promptly obtain micron order nickel oxide spherical particle.
We are of a size of the 1-5 micron by the nickel oxide microballoon of above method preparation, and each microballoon assembles by 10-100nm.This micron ball has tangible room-temperature ferromagnetic, and its coercive force can reach 500Oe.The nickel oxide microballoon that obtains is a lithium ion battery electrode material, its first loading capacity be 918mAh/g, far above the capacity of block nickel oxide and commercial graphite (less than 400mAh/g).
The technology of preparing of nickel oxide spheroidal material of the present invention is simple, equipment requirements is not high, with low cost, and entire reaction course has only been used Ni (NO
3)
26H
2O and ethanol reagent do not produce other harmful liquid or tensio-active agent, and synthetic is environmental protection.Because sample is the powder state, be easy to and other material mixing processing, therefore have great application prospect in fields such as lithium ion battery, nickel metal hydride battery, nano magnetic materials.
Description of drawings
Fig. 1 is the α-Ni (OH) of Hydrothermal Preparation
2The X-ray diffraction of precursor and the nickel oxide microballoon after 400 ℃ and 700 ℃ of sintering processes is composed.
Fig. 2 is α-Ni (OH)
2Precursor (a, b) and the surface sweeping electromicroscopic photograph of the nickel oxide that obtains after 400 ℃ (c) and 700 ℃ of (d) sintering processes.α-Ni (OH)
2All be spherical with nickel oxide, and assemble (d) by small nano particle.
Fig. 3 is the M-H curve of the nickel oxide powder that obtains through 400 ℃ of thermal treatments.Sample presents ferromegnetism, and coercive force is about 500Oe.Fig. 4 is the first charge-discharge curve of the nickel oxide that obtains of 400 ℃ of thermal treatments as lithium ion cell positive.
Embodiment
Example 1:
α-Ni (OH)
2Preparation: the Ni (NO that gets 29.8g
3)
26 (H
2O) be dissolved in a certain amount of dehydrated alcohol, obtaining cation concn is the solution of 1mol/L, and in the reactor of immigration 100ml (compactedness is 70%), reaction is 3 hours in 160 ℃ of baking ovens, the reaction postcooling with distilled water suction filtration and oven dry, promptly obtains required green powder sample to room temperature.Products therefrom is globular-Ni (OH)
2
Example 2:
The preparation of spherical nickel oxide: get gained α-Ni (OH) in the example 1
2Sintering is 2 hours in retort furnace, and temperature of reaction is 400 degree, obtains the nickel oxide of black.This micron ball is that the small-particle of 15.6 nanometers assembles by granularity.
Example 3:
The preparation of spherical nickel oxide: get gained α-Ni (OH) in the example 1
2Sintering is 2 hours in retort furnace, and temperature of reaction is 700 degree, obtains the nickel oxide of black.This micron ball is that the small-particle of 47 nanometers assembles by granularity.
Example 4:
Get nickel oxide microballoon in the example 2, carry out the magnetic test, find that sample is ferromegnetism, the saturation magnetization that coercive force is about the ferromagnetic component of 500Oe. is 0.12emu/g.
Example 5:
Nickel oxide microballoon powder graphitized carbon black in the example 2 and tackiness agent (PVDF) are mixed and add an amount of N-alkyl pyrrolidone (PVDF) at 8: 1: 1 stir and be coated on the metal copper film by mass ratio, obtain the positive pole of lithium cell then 100 ℃ of vacuum-dryings.With the metal lithium sheet is negative pole, the LiPF of 1M concentration
6Be ionogen, EC: DC: EMC=1: 1: 1 (volume ratio) is electrolytic solution, and polypropylene is a barrier film.In the glove box that is full of Ar gas, assemble button cell.The loading capacity first that records is 918mAh/g.
Claims (3)
1. nickel oxide micron ball with ferromegnetism and excellent electrochemical performance, it is characterized in that: this nickel oxide micron ball is of a size of the 1-5 micron, each microballoon assembles by 10-100nm, this micron ball has tangible room-temperature ferromagnetic, its coercive force can reach 500Oe, the nickel oxide microballoon that obtains is a lithium ion battery electrode material, its first loading capacity be 918mAh/g.
2. the preparation method of the described micron level spherical nickel oxide of claim 1, detailed process is as follows:
(1) at first at preparation precursor α-Ni (OH) 2 micron order ball, with Ni (NO
3)
26H
2O is dissolved in the ethanol, after fully stirring, changes the reactor constant temperature reaction over to, and thermostat temperature is 120 ℃-250 ℃, constant temperature time is 2-48h, after reaction finishes, and cool to room temperature, centrifugal, washing, drying is collected and to be obtained micron level spherical α-Ni (OH) of being made up of nano particle
2
(2) with the micron level spherical α-Ni (OH) that obtains
2Put into temperature and be 300-900 ℃ stove and heat-treat, promptly obtain micron order nickel oxide spherical particle.
3. the described micron level spherical nickel oxide of claim 1 is as lithium ion battery electrode material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910111238A CN101830522A (en) | 2009-03-13 | 2009-03-13 | Nickel oxide microspheres with ferromagnetism and excellent electrochemical performance and synthetic method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910111238A CN101830522A (en) | 2009-03-13 | 2009-03-13 | Nickel oxide microspheres with ferromagnetism and excellent electrochemical performance and synthetic method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101830522A true CN101830522A (en) | 2010-09-15 |
Family
ID=42714768
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910111238A Pending CN101830522A (en) | 2009-03-13 | 2009-03-13 | Nickel oxide microspheres with ferromagnetism and excellent electrochemical performance and synthetic method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101830522A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103746104A (en) * | 2013-12-09 | 2014-04-23 | 中国科学院福建物质结构研究所 | Manganese cobalt oxide self-assembled micro-spheres, and preparation and applications thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1274335A (en) * | 1998-05-21 | 2000-11-22 | 堺化学工业株式会社 | Method for producing fine spherical particles of carbonate or hydroxide of nickel, cobalt or copper |
| CN101143734A (en) * | 2007-09-13 | 2008-03-19 | 河南科技大学 | Method for preparing lithium ionic cell nano-crystal nickel oxide anode material |
| CN101357780A (en) * | 2007-07-30 | 2009-02-04 | 湖南科力远新能源股份有限公司 | Spherical shape nickel hydroxide for high-temperature nickle electric cell |
-
2009
- 2009-03-13 CN CN200910111238A patent/CN101830522A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1274335A (en) * | 1998-05-21 | 2000-11-22 | 堺化学工业株式会社 | Method for producing fine spherical particles of carbonate or hydroxide of nickel, cobalt or copper |
| CN101357780A (en) * | 2007-07-30 | 2009-02-04 | 湖南科力远新能源股份有限公司 | Spherical shape nickel hydroxide for high-temperature nickle electric cell |
| CN101143734A (en) * | 2007-09-13 | 2008-03-19 | 河南科技大学 | Method for preparing lithium ionic cell nano-crystal nickel oxide anode material |
Non-Patent Citations (2)
| Title |
|---|
| SHEN XIANG-QIAN ET AL.: "Formation of microstructures for spherical Ni(OH) 2 particles", 《功能材料》 * |
| 宋彩霞 等: "Ni(OH)2和NiO空心球壳的纳米构筑", 《青岛科技大学学报( 自然科学版)》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103746104A (en) * | 2013-12-09 | 2014-04-23 | 中国科学院福建物质结构研究所 | Manganese cobalt oxide self-assembled micro-spheres, and preparation and applications thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102130334B (en) | Graphene-based nano iron oxide composite material and preparation method thereof | |
| CN102790217B (en) | Carbon cladded ferriferrous oxide negative electrode material of lithium ion battery and preparation method thereof | |
| CN109244427B (en) | Preparation method of carbon-coated zinc sulfide loaded graphene as potassium ion battery cathode | |
| CN103094558A (en) | Zinc-ferrite-based nanometer composite as well as preparation method and application thereof | |
| CN103123968A (en) | High-performance lithium iron phosphate cathode material and preparation method of lithium iron phosphate cathode material | |
| CN101826617B (en) | Preparation method of lithium iron phosphate | |
| CN109461926A (en) | A kind of anode material for lithium-ion batteries and preparation method thereof, anode and lithium ion battery | |
| CN102745675A (en) | Preparation method of spinel-type magnetic MFe2O4/graphene composite material | |
| CN104505508A (en) | Preparation method of nickel cobalt oxide electrode material | |
| CN104003368A (en) | Porous phosphor-nitrogen-codoped carbon material and preparation method thereof | |
| CN103236519B (en) | Porous carbon base monolith composite material for lithium ion battery, and preparation method thereof | |
| CN103247793B (en) | High-performance compound spherical lithium ion secondary battery positive electrode and preparation method | |
| CN102779994A (en) | Iron-based complex oxide/graphene composite and preparation method and application thereof | |
| CN106252090B (en) | A kind of high fold grapheme material and preparation method thereof | |
| TWI577640B (en) | Nickel-lithium metal composite oxide powder and method for producing same,positive electrode active material for lithium ion battery, positive electrode for lithium ion battery and lithium ion battery | |
| CN103450843A (en) | Preparation method of reduced graphene oxide/ferroferric oxide composite wave-absorbing hydrogel with three-dimensional structure | |
| CN105958063B (en) | A kind of preparation method of lithium ion battery nickel cobalt aluminium positive electrode | |
| CN106971855B (en) | A kind of nickel ferrite based magnetic loaded nanoparticle electrode material and preparation method and purposes | |
| CN104900420A (en) | NiCo2O4@MOx material of hollow core-shell structure and preparation and application methods thereof | |
| CN104701527A (en) | Preparation method for lithium ion battery anode material Li(Ni1-x-yCoxAly)O2 | |
| CN109775762A (en) | A kind of Fe of hollow graded structure2O3And Fe2O3The preparation method of/CNT composite material | |
| CN105826551A (en) | Preparation method of dumbbell type NiCo2O4 lithium ion battery anode material | |
| CN105514365B (en) | A kind of hydro-thermal method prepares lithium ion battery negative material MnFe2O4The technique of/rGO | |
| Lv et al. | Hexamethylenetetramine-induced synthesis of hierarchical NiO nanostructures on nickel foam and their electrochemical properties | |
| Li et al. | Microwave-assisted synthesis of the sandwich-like porous Al2O3/RGO nanosheets anchoring NiO nanocomposite as anode materials for lithium-ion batteries |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20100915 |