CN108994313A - A kind of preparation method of Ni nano wire - Google Patents
A kind of preparation method of Ni nano wire Download PDFInfo
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- CN108994313A CN108994313A CN201810610765.5A CN201810610765A CN108994313A CN 108994313 A CN108994313 A CN 108994313A CN 201810610765 A CN201810610765 A CN 201810610765A CN 108994313 A CN108994313 A CN 108994313A
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- nano wire
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
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- 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
Abstract
The invention belongs to material chemistry technical fields, it is related to a kind of preparation method of Ni nano wire, it is characterized by comprising following steps: (1) ingredient: divalent Ni salt is added in the beaker for filling deionized water, sequentially add alkali, complexing agent and template, stirring dissolves it sufficiently, then reducing agent is added, stops stirring after completely dissolution；(2) isothermal reaction；(3) it washs；(4) it is dried in vacuum drying oven.Raw material of the present invention is cheap, and synthetic method is full liquid-phase chemical reaction process, carries out at normal temperature, and yield is high, is suitable for industrialized production.
Description
Technical field
The invention belongs to material chemistry technical fields, are related to a kind of preparation method of Ni nano wire.
Background technique
Ni metal nano material conductivity with higher and preferable antioxygenic property, can be used for electrocondution slurry and thermoelectricity
The conducting function component of slurry.Ni nano wire is as one-dimensional electric nano material, usage amount low in electrocondution slurry percolation threshold
Few, conductivity is higher.One-dimensional Ni metal nano material preparation method is varied, is broadly divided into two major classes: gas phase and liquid phase method.
Vapor phase method yield is relatively low, and liquid phase method is usually using the templates such as AAO, using carrying out under electrochemical means or higher temperature.
Summary of the invention
For prior art defect, the purpose of the present invention is to provide a kind of quick cheap full chemistry method synthesis Ni to receive
The preparation method of rice noodles, it is characterised in that include the following steps:
(1) ingredient: divalent Ni salt is added in the beaker for filling deionized water, alkali, complexing agent and template are sequentially added
Agent, stirring dissolve it sufficiently, reducing agent are then added, and stop stirring after completely dissolution；Divalent Ni salt include Nickel Chloride and
One of nickel sulfate or combinations thereof, concentration are 0.01mol/L~0.08mol/L；
(2) isothermal reaction；
(3) wash: for obtained nano-powder, be washed with deionized, using centrifuge precipitating or pumping and filtering device into
Row filtering, filtration product are dispersed in deionized water again, and repeated filtration is 7 until filtrate pH value, are finally washed with dehydrated alcohol
It washs with convenient and dry；
(4) dry: to be dried in vacuum drying oven, vacuum drying condition is vacuum degree < 133Pa.
The alkali is one of sodium hydroxide, potassium hydroxide, rubidium hydroxide or combinations thereof, alkali concentration 0.1mol/L
~0.5mol/L；The complexing agent is thioacetic acid, mercaptopropionic acid, ethylenediamine tetra-acetic acid, citric acid, one in sodium citrate
Kind or combinations thereof, the mole that complexing agent is added is 1~3 times of Ni atomic mol in reaction system；Template is α-naphthalene sulphur
One of acid, beta-naphthalenesulfonic-acid, 1,5-, bis- naphthalene sulfonic acids, 2,4- dinitro naphthols -7- sulfonic acid or combinations thereof, concentration is after addition
0.02mol/L~0.1mol/L.
The reducing agent is one of potassium borohydride, sodium borohydride or combinations thereof；Be added reducing agent mole be
3~8 times of Ni atomic mol in reaction system.
The isothermal reaction temperature is room temperature~70 DEG C；The time of the isothermal reaction is 12~24 hours；Heat preservation
Equipment is the water-bath or oil bath pan of energy temperature control.
Raw material of the present invention is cheap, and synthetic method is full liquid-phase chemical reaction process, is carried out at normal temperature, and yield is higher, fits
Together in industrialized production.
The contents of the present invention and feature have revealed that as above, however the present invention that describes of front only briefly or pertains only to this
The specific part of invention, feature of the invention may be more than what content disclosed herein was related to.Therefore, protection model of the invention
The revealed content of embodiment should be not limited to by enclosing, and should include the combination of all the elements embodied in different piece, with
And it is various without departing substantially from replacement and modification of the invention, and covered by claims of the present invention.
Detailed description of the invention
Fig. 1 is the stereoscan photograph using (embodiment 1) of the invention synthesis Ni nano wire.
Specific embodiment
Embodiment 1
0.001mol dichloride nickel salt is added in the beaker for filling 100mL deionized water, 0.01mol hydrogen is sequentially added
Sodium oxide molybdena, 0.001mol thioacetic acid and 0.002mol α-naphthalenesulfonicacid, stirring dissolve it sufficiently, and 0.003mol boron is then added
Hydrofining stops stirring after completely dissolution；Isothermal reaction 24 hours at room temperature；Precipitating deionized water and ethyl alcohol are alternately washed
It washs, is filtered each time after washing using centrifuge precipitating or pumping and filtering device, filtration product is again in deionized water or ethyl alcohol
Dispersion, repeated filtration are that drying obtains Ni nano wire powder, SEM photograph such as Fig. 1 in 7,50 DEG C of vacuum drying ovens until filtrate pH value
It is shown.
Embodiment 2
0.008mol sulfuric acid nickel salt is added in the beaker for filling 100mL deionized water, 0.05mol hydrogen-oxygen is sequentially added
Change sodium, 0.001mol mercaptopropionic acid and 0.002mol beta-naphthalenesulfonic-acid, stirring dissolves it sufficiently, and 0.03mol boron hydrogen is then added
Change sodium, stops stirring after completely dissolution；Isothermal reaction 24 hours at 70 DEG C；Precipitating deionized water and ethyl alcohol are alternately washed,
It is filtered each time after washing using centrifuge precipitating or pumping and filtering device, filtration product is divided in deionized water or ethyl alcohol again
It dissipates, repeated filtration is that drying obtains Ni nano wire powder in 7,50 DEG C of vacuum drying ovens until filtrate pH value.
Embodiment 3
0.001mol dichloride nickel salt is added in the beaker for filling 100mL deionized water, 0.01mol hydrogen is sequentially added
Bis- naphthalene sulfonic acids of potassium oxide, 0.001mol ethylenediamine tetra-acetic acid and 0.01mol1,5-, stirring are dissolved it sufficiently, are then added
0.003mol sodium borohydride stops stirring after completely dissolution；Isothermal reaction 12 hours at 50 DEG C；By precipitating deionized water and second
Alcohol alternately washs, and is filtered each time after washing using centrifuge precipitating or pumping and filtering device, filtration product is again in deionized water
Or disperse in ethyl alcohol, repeated filtration is that drying obtains Ni nano wire powder in 7,50 DEG C of vacuum drying ovens until filtrate pH value.
Embodiment 4
0.001mol sulfuric acid nickel salt is added in the beaker for filling 100mL deionized water, 0.01mol hydrogen-oxygen is sequentially added
Change potassium, 0.001mol sodium citrate and 0.002mol α-naphthalenesulfonicacid, stirring dissolves it sufficiently, and 0.008mol boron hydrogen is then added
Change potassium, stops stirring after completely dissolution；Isothermal reaction 18 hours at room temperature；Precipitating deionized water and ethyl alcohol are alternately washed,
It is filtered each time after washing using centrifuge precipitating or pumping and filtering device, filtration product is divided in deionized water or ethyl alcohol again
It dissipates, repeated filtration is that drying obtains Ni nano wire powder in 7,50 DEG C of vacuum drying ovens until filtrate pH value.
Embodiment 5
0.001mol dichloride nickel salt is added in the beaker for filling 100mL deionized water, 0.01mol hydrogen is sequentially added
Sodium oxide molybdena, 0.001mol citric acid and 0.005mol2,4- dinitro naphthols -7- sulfonic acid, stirring dissolve it sufficiently, then plus
Enter 0.003mol potassium borohydride, stops stirring after completely dissolution；Isothermal reaction 24 hours at room temperature；By precipitating deionized water and
Ethyl alcohol alternately washs, and is filtered each time after washing using centrifuge precipitating or pumping and filtering device, filtration product is again in deionization
Disperse in water or ethyl alcohol, repeated filtration is that drying obtains Ni nano wire powder in 7,50 DEG C of vacuum drying ovens until filtrate pH value.
Claims (5)
1. a kind of preparation method of Ni nano wire, it is characterised in that include the following steps:
(1) ingredient: divalent Ni salt is added in the beaker for filling deionized water, alkali, complexing agent and template is sequentially added, stirs
Mixing dissolves it sufficiently, and reducing agent is then added, and stops stirring after completely dissolution；Divalent Ni salt includes Nickel Chloride and nickel sulfate
One of or combinations thereof, concentration is 0.01mol/L~0.08mol/L；
(2) isothermal reaction；
(3) it washs: for obtained nano-powder, being washed with deionized, carried out using centrifuge precipitating or pumping and filtering device
Filter, filtration product disperses in deionized water again, and repeated filtration is 7 until filtrate pH value, finally with dehydrated alcohol wash with
Convenient and dry；
(4) dry: to be dried in vacuum drying oven, vacuum drying condition is vacuum degree < 133Pa.
2. the preparation method of Ni nano wire according to claim 1, it is characterised in that: the alkali is sodium hydroxide, hydrogen-oxygen
Change one of potassium, rubidium hydroxide or combinations thereof, alkali concentration is 0.1mol/L~0.5mol/L；The complexing agent is sulfydryl second
One of acid, mercaptopropionic acid, ethylenediamine tetra-acetic acid, citric acid, sodium citrate or combinations thereof, the mole that complexing agent is added are
1~3 times of Ni atomic mol in reaction system；Template is α-naphthalenesulfonicacid, beta-naphthalenesulfonic-acid, 1,5-, bis- naphthalene sulfonic acids, 2,4- bis-
One of nitronaphthol -7- sulfonic acid or combinations thereof, concentration is 0.02mol/L~0.1mol/L after addition.
3. the preparation method of Ni nano wire according to claim 1, it is characterised in that: the reducing agent be potassium borohydride,
One of sodium borohydride or combinations thereof；The mole that reducing agent is added is 3~8 times of Ni atomic mol in reaction system.
4. the preparation method of Ni nano wire according to claim 1, it is characterised in that: the isothermal reaction temperature is room temperature
~70 DEG C；The time of the isothermal reaction is 12~24 hours；Heat-preserving equipment is the water-bath or oil bath pan of energy temperature control.
5. Ni nano wire prepared by a kind of preparation method of Ni nano wire as described in Claims 1 to 4 any one.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810610765.5A CN108994313A (en) | 2018-06-07 | 2018-06-07 | A kind of preparation method of Ni nano wire |
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| CN201810610765.5A CN108994313A (en) | 2018-06-07 | 2018-06-07 | A kind of preparation method of Ni nano wire |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109904000A (en) * | 2019-04-10 | 2019-06-18 | 蚌埠学院 | A kind of preparation method and applications of the Ni-based complex electrode material of nanometer of threadiness |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486102A (en) * | 2009-01-05 | 2009-07-22 | 江苏科技大学 | Method for preparing metallic nickel nano-wire |
| CN103352132A (en) * | 2013-07-05 | 2013-10-16 | 浙江大学 | Copper-nickel nanowire and preparation method thereof |
| CN103774232A (en) * | 2012-10-18 | 2014-05-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of Ag2E nano wire |
| CN103962570A (en) * | 2013-02-03 | 2014-08-06 | 宇辰新能源材料科技无锡有限公司 | Preparation method of nickel nanopowder |
| CN103978227A (en) * | 2014-05-22 | 2014-08-13 | 冷劲松 | Method for preparing controllable nickel nanowires conveniently at low cost |
| JP2015160977A (en) * | 2014-02-26 | 2015-09-07 | 公立大学法人 滋賀県立大学 | Cu-Ni NANOWIRE AND PRODUCTION METHOD THEREOF |
| US20170066049A1 (en) * | 2015-06-13 | 2017-03-09 | Board Of Regents, The University Of Texas System | Nanowire-based magnets and methods of making same |
-
2018
- 2018-06-07 CN CN201810610765.5A patent/CN108994313A/en not_active Withdrawn
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486102A (en) * | 2009-01-05 | 2009-07-22 | 江苏科技大学 | Method for preparing metallic nickel nano-wire |
| CN103774232A (en) * | 2012-10-18 | 2014-05-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of Ag2E nano wire |
| CN103962570A (en) * | 2013-02-03 | 2014-08-06 | 宇辰新能源材料科技无锡有限公司 | Preparation method of nickel nanopowder |
| CN103352132A (en) * | 2013-07-05 | 2013-10-16 | 浙江大学 | Copper-nickel nanowire and preparation method thereof |
| JP2015160977A (en) * | 2014-02-26 | 2015-09-07 | 公立大学法人 滋賀県立大学 | Cu-Ni NANOWIRE AND PRODUCTION METHOD THEREOF |
| CN103978227A (en) * | 2014-05-22 | 2014-08-13 | 冷劲松 | Method for preparing controllable nickel nanowires conveniently at low cost |
| US20170066049A1 (en) * | 2015-06-13 | 2017-03-09 | Board Of Regents, The University Of Texas System | Nanowire-based magnets and methods of making same |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109904000A (en) * | 2019-04-10 | 2019-06-18 | 蚌埠学院 | A kind of preparation method and applications of the Ni-based complex electrode material of nanometer of threadiness |
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Application publication date: 20181214 |