CN101525162A - Method for synthesizing beta-phase nickel hydroxide nano structure - Google Patents
Method for synthesizing beta-phase nickel hydroxide nano structure Download PDFInfo
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- CN101525162A CN101525162A CN200910080646A CN200910080646A CN101525162A CN 101525162 A CN101525162 A CN 101525162A CN 200910080646 A CN200910080646 A CN 200910080646A CN 200910080646 A CN200910080646 A CN 200910080646A CN 101525162 A CN101525162 A CN 101525162A
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- Prior art keywords
- nickel hydroxide
- arginine
- beta
- nano structure
- phase
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- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 title claims abstract description 36
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 10
- 230000002194 synthesizing effect Effects 0.000 title abstract 3
- ODKSFYDXXFIFQN-BYPYZUCNSA-N L-arginine Chemical compound OC(=O)[C@@H](N)CCCN=C(N)N ODKSFYDXXFIFQN-BYPYZUCNSA-N 0.000 claims abstract description 25
- 229930064664 L-arginine Natural products 0.000 claims abstract description 25
- 235000014852 L-arginine Nutrition 0.000 claims abstract description 25
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 8
- 239000010935 stainless steel Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 7
- 230000004087 circulation Effects 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000010189 synthetic method Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 239000007774 positive electrode material Substances 0.000 abstract description 2
- 238000011160 research Methods 0.000 abstract description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 abstract 2
- 239000007788 liquid Substances 0.000 abstract 2
- 239000003513 alkali Substances 0.000 abstract 1
- 230000002596 correlated effect Effects 0.000 abstract 1
- -1 polytetrafluoroethylene Polymers 0.000 abstract 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract 1
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract 1
- 238000001000 micrograph Methods 0.000 description 12
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 238000010276 construction Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000002131 composite material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011149 active material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
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- 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
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- Battery Electrode And Active Subsutance (AREA)
Abstract
A method for synthesizing beta-phase nickel hydroxide nano structure relates to a preparation technology of positive electrode active material of alkali storage battery. The method takes nickel chloride (NiC2.6H2O) and L-Arginine (C6H14N4O2) as the raw materials to prepare aqueous solution including nickel chloride and L-Arginine under the room temperature to be used as the reaction starting liquid. The reaction starting liquid is placed in a stainless steel reactor with polytetrafluoroethylene lining and heated for 5 to 15 hours within the temperature range of 200 to 250 DEG C so as to obtain the beta-phase nickel hydroxide with a flower-like complex nano structure which takes the flaky shape as the secondary structure. Property, dimension, shape and reaction system of the nano material are highly correlated. The beta-phase nickel hydroxide nano structure synthesized by the method utilizes the biomolecule L-Arginine as one of the raw materials in the reaction and provides a new synthesizing method and a new material for studying the property and practical usage of nickel hydroxide, which is of significance no matter in academic research or in application.
Description
Technical field
The present invention relates to a kind of synthetic method of β-beta-phase nickel hydroxide nano structure, belong to the nickel hydroxide of complicated nanostructure, particularly the positive electrode active materials technical field of β-beta-phase nickel hydroxide Edison battery.
Background technology
Nano material provides important new technical means for the research and development of new forms of energy.Characteristics such as nano material is big owing to specific surface area, surface energy height make it to provide novel material for the new energy materials exploitation.Nickel hydroxide is a material of alkaline battery, and obviously, behind the active material nanometer as electrode, surface-area increases, and current density can reduce, and polarization reduces, and causes electrical capacity to increase, thereby has better electrochemical activity.No matter the complicated nanostructure of synthetic β-beta-phase nickel hydroxide is in academic research or in application facet, all significant.
By retrieval, there are 2 in the prior art about β phase-nickel hydroxide patent report:
(1) " process for preparing nm-class beta-phase spherical nickel hydroxide " (applicant: Kehai Maidi Bio-Technology Co., Ltd, Beijing, contriver: Li Daohuo; Zhang Hongbing; Magnify just; Xu Junli; Application number: 01109695.0), a kind of process for preparing nm-class beta-phase spherical nickel hydroxide of this invention report, promptly by controlling the coefficient of surface tension of reaction solution, improve the stability of nanometer small-particle in the supersaturation reaction solution, it is good to prepare dispersity, the nano-sized nickel hydroxide powder about mean particle size 10 nanometers.It is characterized in that selecting suitable dispersion agent.
(2) " technology of preparing nm-class beta-plase composite nickel hydroxide " (applicant: Kehai Maidi Bio-Technology Co., Ltd, Beijing, contriver: Li Daohuo; Zhang Hongbing; Magnify just; Xu Junli, application number: 01109693.4), the technology of a kind of preparing nm-class beta-plase composite nickel hydroxide of this invention report, it is even in certain mass ratio and certain size mixed with micron ball-type nickel hydroxide to be about to finely disseminated nm-class beta-phase spherical or needle-like nickel hydroxide, be mixed with the preparing nm-class beta-plase composite nickel hydroxide electrode materials, with the moulding of uninterrupted post forming method.It is characterized in that the nanometer beta phase nickel hydroxide is a ball-type or acicular, and the micron nickel hydroxide is a ball-type, nano powder is pressed certain mass than preparing with certain particle diameter ratio with micropowder; Feature of the present invention also is the post forming method.
The character of nano material and its size, shape and reaction system have much relations, a kind of β-beta-phase nickel hydroxide nano structure that we synthesize is to utilize biomolecules---the L-arginine is that one of raw material participates in reaction, and this provides new synthetic method and novel material for studying its character and practical application.
Summary of the invention
The object of the present invention is to provide a kind of hydrothermal synthesis method of easy preparation β-beta-phase nickel hydroxide nano structure.Raw materials used being easy to get in the synthetic method of the present invention, technology is easy.
The synthetic method of a kind of β-beta-phase nickel hydroxide nano structure provided by the invention is characterized in that, this method is carried out as follows:
(1) with nickelous chloride (NiCl
26H
2O), L-arginine (L-Arginine, C
6H
14N
4O
2) be raw material, at room temperature, preparation comprises that with nickelous chloride, the arginic aqueous solution of L-wherein the arginic concentration range of nickelous chloride and L-is 1～2 mmole/40 milliliter, L-arginine concentration range is 2～4 mmoles/40 milliliter;
(2) described mixing solutions is positioned in the teflon-lined stainless steel cauldron, 200～250 ℃ of temperature range heating 5～15 hours;
(3) throw out that obtains after will reacting is with deionized water and alternately washing of dehydrated alcohol, and three circulations are washed in centrifugation, put into loft drier then and carry out drying 3 hours, promptly obtain the nanostructure of nickel hydroxide.
Description of drawings
Fig. 1: (a) be the electron scanning micrograph of embodiment 1,
Fig. 1: (b) be the x-ray diffraction pattern of embodiment 1.
Fig. 2: (a) be the electron scanning micrograph of embodiment 2,
Fig. 2: (b) be the field emission scanning electron microscope photo of embodiment 2,
Fig. 2: (c) microphotograph is the x-ray diffraction pattern of embodiment 2.
Fig. 3: (a) be the electron scanning micrograph of embodiment 3,
Fig. 3: (b) be the field emission scanning electron microscope photo of embodiment 3,
Fig. 3: (c) microphotograph is the x-ray diffraction pattern of embodiment 3.
Fig. 4: be the electron scanning micrograph of embodiment 4.
Fig. 5: (a) be the electron scanning micrograph of embodiment 5,
Fig. 5: (b) be the x-ray diffraction pattern of embodiment 5.
Embodiment
Below by specific embodiment the present invention further is illustrated.
Embodiment 1:
---with nickelous chloride (NiCl
26H
2O), L-arginine (L-Arginine, C
6H
14N
4O
2) be raw material, at room temperature, preparation comprises that with nickelous chloride, the arginic aqueous solution of L-wherein the arginic concentration of nickelous chloride and L-is 1 mmole/40 milliliter, L-arginine concentration is 2 mmoles/40 milliliter.
---described mixing solutions is positioned in the teflon-lined stainless steel cauldron, 200 ℃ of temperature range heating 5 hours.
---the throw out that will obtain after will reacting alternately washs with deionized water and dehydrated alcohol, and three circulations are washed in centrifugation, put into loft drier (80 ℃) then and carry out drying 3 hours, promptly obtain the nanostructure of nickel hydroxide.Fig. 1 (a) is the electron scanning micrograph of embodiment 1, and it is the complex construction of the flower-like structure of secondary structure composition for sheet structure as seen from the figure, and Fig. 1 (b) is an x-ray diffraction pattern, determines that product is β-beta-phase nickel hydroxide.
Embodiment 2:
---with nickelous chloride (NiCl
26H
2O), L-arginine (L-Arginine, C
6H
14N
4O
2) be raw material, at room temperature, preparation comprises that with nickelous chloride, the arginic aqueous solution of L-wherein the arginic concentration of nickelous chloride and L-is 1 mmole/40 milliliter, L-arginine concentration is 2 mmoles/40 milliliter.
---described mixing solutions is positioned in the teflon-lined stainless steel cauldron, 200 ℃ of temperature range heating 10 hours.
---the throw out that will obtain after will reacting alternately washs with deionized water and dehydrated alcohol, and three circulations are washed in centrifugation, put into loft drier (80 ℃) then and carry out drying 3 hours, promptly obtain the nanostructure of nickel hydroxide.Fig. 2 (a) is the electron scanning micrograph of embodiment 2, it is the complex construction of the flower-like structure of secondary structure composition for sheet structure as seen from the figure, Fig. 2 (b) is the field emission scanning electron microscope photo of embodiment 2, the slice, thin piece thickness that shows flower is about 17 nanometers, Fig. 2 (c) is an x-ray diffraction pattern, determines that product is β-beta-phase nickel hydroxide.
Embodiment 3:
---with nickelous chloride (NiCl
26H
2O), L-arginine (L-Arginine, C
6H
14N
4O
2) be raw material, at room temperature, preparation comprises that with nickelous chloride, the arginic aqueous solution of L-wherein the arginic concentration of nickelous chloride and L-is 1 mmole/40 milliliter, L-arginine concentration is 2 mmoles/40 milliliter.
---described mixing solutions is positioned in the teflon-lined stainless steel cauldron, 200 ℃ of temperature range heating 15 hours.
---the throw out that will obtain after will reacting alternately washs with deionized water and dehydrated alcohol, and three circulations are washed in centrifugation, put into loft drier (80 ℃) then and carry out drying 3 hours, promptly obtain the nanostructure of nickel hydroxide.Fig. 3 (a) is the electron scanning micrograph of embodiment 3, it is the complex construction of the flower-like structure of secondary structure composition for sheet structure as seen from the figure, Fig. 3 (b) is the field emission scanning electron microscope photo of embodiment 3, the slice, thin piece thickness that shows flower is about 20 nanometers, Fig. 3 (c) is an x-ray diffraction pattern, determines that product is β-beta-phase nickel hydroxide.
Embodiment 4:
---with nickelous chloride (NiCl
26H
2O), L-arginine (L-Arginine, C
6H
14N
4O
2) be raw material, at room temperature, preparation comprises that with nickelous chloride, the arginic aqueous solution of L-wherein the arginic concentration of nickelous chloride and L-is 2 mmoles/40 milliliter, L-arginine concentration is 4 mmoles/40 milliliter.
---described mixing solutions is positioned in the teflon-lined stainless steel cauldron, 200 ℃ of temperature range heating 10 hours.
---the throw out that will obtain after will reacting alternately washs with deionized water and dehydrated alcohol, and three circulations are washed in centrifugation, put into loft drier (80 ℃) then and carry out drying 3 hours, promptly obtain the nanostructure of nickel hydroxide.Fig. 4 is the electron scanning micrograph of embodiment 4, and it is the complex construction of the flower-like structure of secondary structure composition for sheet structure as seen from the figure.
Embodiment 5:
---with nickelous chloride (NiCl
26H
2O), L-arginine (L-Arginine, C
6H
14N
4O
2) be raw material, at room temperature, preparation comprises that with nickelous chloride, the arginic aqueous solution of L-wherein the arginic concentration of nickelous chloride and L-is 1 mmole/40 milliliter, L-arginine concentration is 2 Bo mole/40 milliliter.
---described mixing solutions is positioned in the teflon-lined stainless steel cauldron, 250 ℃ of temperature range heating 10 hours.
---the throw out that will obtain after will reacting alternately washs with deionized water and dehydrated alcohol, and three circulations are washed in centrifugation, put into loft drier (80 ℃) then and carry out drying 3 hours, promptly obtain the nanostructure of nickel hydroxide.Fig. 5 (a) is the electron scanning micrograph of embodiment 5, and it is the complex construction of the flower-like structure of secondary structure composition for sheet structure as seen from the figure, and Fig. 5 (b) is an x-ray diffraction pattern, determines that product is β-beta-phase nickel hydroxide.
Claims (1)
1, a kind of synthetic method of β-beta-phase nickel hydroxide nano structure is characterized in that, this method is carried out as follows:
(1) with nickelous chloride (NiCl
26H
2O), L-arginine (L-Arginine, C
6H
14N
4O
2) be raw material, at room temperature, preparation comprises that with nickelous chloride, the arginic aqueous solution of L-wherein the arginic concentration range of nickelous chloride and L-is 1～2 mmole/40 milliliter, L-arginine concentration range is 2～4 mmoles/40 milliliter;
(2) described mixing solutions is positioned in the teflon-lined stainless steel cauldron, 200～250 ℃ of temperature range heating 5～15 hours;
(3) throw out that obtains after will reacting is with deionized water and alternately washing of dehydrated alcohol, and three circulations are washed in centrifugation, put into loft drier then and carry out drying 3 hours, promptly obtain the nanostructure of nickel hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910080646A CN101525162A (en) | 2009-03-20 | 2009-03-20 | Method for synthesizing beta-phase nickel hydroxide nano structure |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910080646A CN101525162A (en) | 2009-03-20 | 2009-03-20 | Method for synthesizing beta-phase nickel hydroxide nano structure |
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|---|---|
| CN101525162A true CN101525162A (en) | 2009-09-09 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271445A (en) * | 2015-11-13 | 2016-01-27 | 无锡清杨机械制造有限公司 | Spherical cobalt-doped nickel hydroxide continuous preparation method |
| CN108123124A (en) * | 2017-12-19 | 2018-06-05 | 宁波高新区锦众信息科技有限公司 | A kind of preparation method of alkaline secondary cell β-nickel hydroxide composite material |
| CN112362713A (en) * | 2020-11-24 | 2021-02-12 | 吉林大学 | Sensitive electrode material for direct electrochemical detection of ammonia nitrogen in water and preparation method thereof |
-
2009
- 2009-03-20 CN CN200910080646A patent/CN101525162A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271445A (en) * | 2015-11-13 | 2016-01-27 | 无锡清杨机械制造有限公司 | Spherical cobalt-doped nickel hydroxide continuous preparation method |
| CN108123124A (en) * | 2017-12-19 | 2018-06-05 | 宁波高新区锦众信息科技有限公司 | A kind of preparation method of alkaline secondary cell β-nickel hydroxide composite material |
| CN112362713A (en) * | 2020-11-24 | 2021-02-12 | 吉林大学 | Sensitive electrode material for direct electrochemical detection of ammonia nitrogen in water and preparation method thereof |
| CN112362713B (en) * | 2020-11-24 | 2021-12-07 | 吉林大学 | Sensitive electrode material for direct electrochemical detection of ammonia nitrogen in water and preparation method thereof |
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Open date: 20090909 |