CN102941355B - Solvothermal preparation method of cobalt nano-fibers - Google Patents
Solvothermal preparation method of cobalt nano-fibers Download PDFInfo
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- CN102941355B CN102941355B CN201210516959.1A CN201210516959A CN102941355B CN 102941355 B CN102941355 B CN 102941355B CN 201210516959 A CN201210516959 A CN 201210516959A CN 102941355 B CN102941355 B CN 102941355B
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Abstract
The invention discloses a solvothermal preparation method of cobalt nano-fibers, which belongs to the technical field of metal materials. The solvothermal preparation method is characterized by adopting a solvothermal method, taking glycol as a solvent and ethidene diamine as a reducing agent and reducing cobalt salt to the cobalt nano-fibers with the help of surfactants including polyvinylpyrrolidone and polyethylene glycol monooleyl ether. The generated cobalt nano-fibers are subjected to centrifugal separation, washed twice or three times by absolute ethyl alcohol, dried and collected. The cobalt nano-fibers range from fifty to one hundred nanometers in diameter and ten to dozens of micrometers in length, the length-diameter ratio of the cobalt nano-fibers is very large, and the cobalt nano-fibers grow in a bundle form. The solvothermal preparation method has the effects and benefits that under the combined action of the two surfactants and the ethidene diamine, reduced cobalt grows linearly in a direction (001) to form the cobalt nano-fibers with even diameters and good flexibility; and the solvothermal preparation method has the advantages of simple process and low cost.
Description
Technical field
The invention belongs to technical field of metal, be specifically related to a kind of solvothermal preparation method of cobalt nanofiber.
Background technology
Cobalt nano material has unique photoelectromagnetic and catalysis characteristics, has broad application prospects in single-electron device, Ultrahigh-Density Data Storage, magnetic fluid, catalyst and biological anticancer medicine etc.One dimension cobalt nanofiber has unique Quantum Teleportation effect, superpower mechanical strength, higher luminous efficiency and significant pyroelectric effect, is one of study hotspot of field of nanometer material technology.Prepare uniform diameter, cobalt nanofiber that compliance is good realizes its practical basis.
According to " Rare Metal Materials and Engineering " 2012,41(9): 1527 ~ 1530 reports, with oxalic acid hydrate cobalt nanorod for presoma, in an ar atmosphere at 360 DEG C, nano metal cobalt fiber can be prepared by thermal decomposition process.But can find out that product is ribbon from its ESEM, and between band, stacking adhesion is more serious.
Molecular self-assembling method utilizes the interaction between molecule to be assembled into orderly nanostructured." Nano Letter " 2004,4 (11): 2299 ~ 2302 report fluorocarbon at Co
3c or Co particle surface catalytic decomposition lentamente, forms CNT, meanwhile, and Co
3c or Co particle is connected to carbon pipe inside by orientation and forms Co nano wire.But this method is by inner at carbon pipe for cobalt nanowire growth, although it can be prevented to be oxidized, is disadvantageous to its magnetic property, and this microreaction process and complicated difficult control thereof.
Soft template method adopts the hole phase in surfactant, is namely the growth of template, the nano material that leads in its duct with rod-shaped micelle microemulsion.According to " advanced chemical journal " 2003,24(6): 986 ~ 988 reports, microemulsion technology is combined with solvent heat technology, lysotropic liquid crystal is utilized to vary with temperature and the transformation behavior occurred, the cobalt nanofiber of multilevel hierarchy can be prepared, but transmission electron microscope photo shows, cobalt nanofiber prepared by the method is that the nano particle of 5nm is coalescent by average grain diameter, there is the shortcomings such as diameter is uneven, compliance is poor, easy fracture.Application number is the chemical preparation process that the patent of invention of CN 101698234B provides a kind of metal cobalt nanowire, the method forms soft template jointly with ethylene glycol and surfactant, take hydrazine hydrate as reducing agent, can prepare diameter is 100 ~ 800nm, and length reaches the cobalt nanowire of 2.0 ~ 10.0 μm.But can find that from its scanned photograph this nano wire is also combined by nano level cobalt ball, and there is combination weakness between larger difference, adjacent cobalt nanosphere in the particle diameter of cobalt nanosphere.
In sum, all there is certain defect in the preparation method of existing cobalt nanofiber, is difficult to prepare uniform diameter, cobalt nanofiber that compliance is good.
Summary of the invention
The object of this invention is to provide a kind of solvothermal preparation method of cobalt nanofiber, overcome the defect that compliance is poor, diameter is uneven that existing cobalt nanofiber preparation method exists.
Technical scheme of the present invention is as follows:
1, the preparation of reaction solution
Take ethylene glycol as solvent, by solution cobalt salt 0.05 ~ 0.2mol/L, ethylenediamine 2 ~ 4mol/L, NaOH 0.5 ~ 1mol/L, polyvinylpyrrolidone 5 ~ 10g/L, polyoxyethylene laurel ether Brij30 1 ~ 5ml/L proportions, magnetic agitation 50 ~ 70 minutes.
Described cobalt salt is any one among cobalt acetate, hydrochloric acid cobalt, cobalt nitrate, cobaltous sulfate.
Described NaOH joins in reaction solution in the mode of deionized water solution.
2, cobalt nanofiber preparation
Moved in reactor by the solution prepared as stated above, compactedness is 50% ~ 70%, is screwed to be placed in heating furnace by the lid of reactor to be heated to 180 ~ 190 DEG C, reacts 20 ~ 40 hours, generates cobalt nanofiber.The cobalt nanofiber generated, after centrifugation, with absolute ethanol washing 2 ~ 3 times, dryly to be collected.
Effect of the present invention and benefit are under two kinds of surfactants (polyvinylpyrrolidone PVP and polyoxyethylene laurel ether Brij30) and ethylenediamine acting in conjunction, and reduction cobalt is grown to serve as uniform diameter, cobalt nanofiber that compliance is good along (001) direction line style; Simple, the with low cost and applicable suitability for industrialized production of this preparation method's technique.
Accompanying drawing explanation
Fig. 1 is the SEM photo figure of cobalt nanofiber prepared by embodiment 1.
Fig. 2 is the TEM photo figure of cobalt nanofiber prepared by embodiment 1.
Fig. 3 is the SEM photo figure of cobalt nanofiber prepared by embodiment 2.
Fig. 4 is the X-ray diffraction spectrogram of cobalt nanofiber prepared by embodiment 2.
Detailed description of the invention
The specific embodiment of the present invention is described in detail below in conjunction with technical scheme and accompanying drawing.
Embodiment one:
1, the preparation of reaction solution
Be that precursor liquid prepared by solvent with ethylene glycol, each reactant concentration is as follows:
2, the preparation of cobalt nanofiber
Moved in reactor by above-mentioned solution, compactedness is 50%, is screwed to be placed in heating furnace by the lid of reactor to be heated to 180 DEG C, be incubated 36 hours, open after question response still cools completely, after the black precipitate centrifugation of generation, with absolute ethanol washing 3 times, then dry 24 hours at 50 DEG C.As shown in Figure 1, TEM photo as shown in Figure 2 for the SEM photo of products therefrom.
Embodiment two:
1, the preparation of reaction solution
Be that precursor liquid prepared by solvent with ethylene glycol, each reactant concentration is as follows:
2, the preparation of cobalt nanofiber
Moved in reactor by above-mentioned solution, compactedness is 70%, is screwed to be placed in heating furnace by the lid of reactor to be heated to 190 DEG C, be incubated 24 hours, open after question response still cools completely, after the black precipitate centrifugation of generation, with absolute ethanol washing 3 times, then dry 24 hours at 50 DEG C.As shown in Figure 3, X-ray diffraction spectrogram as shown in Figure 4 for the SEM picture of products therefrom.
Claims (3)
1. a solvothermal preparation method for cobalt nanofiber, is characterized in that, concrete steps are as follows:
1) preparation of reaction solution
Take ethylene glycol as solvent, by solution cobalt salt 0.05 ~ 0.2mol/L, ethylenediamine 2 ~ 4mol/L, NaOH0.5 ~ 1mol/L, polyvinylpyrrolidone 5 ~ 10g/L, polyoxyethylene laurel ether Brij301 ~ 5ml/L proportions, magnetic agitation 50 ~ 70 minutes;
2) preparation of cobalt nanofiber
Moved in reactor by the solution prepared as stated above, compactedness is 50% ~ 70%, is screwed to be placed in heating furnace by the lid of reactor to be heated to 180 ~ 190 DEG C, reacts 20 ~ 40 hours, generates cobalt nanofiber.
2. the solvothermal preparation method of a kind of cobalt nanofiber according to claim 1, is characterized in that, described cobalt salt is any one among cobalt acetate, hydrochloric acid cobalt, cobalt nitrate, cobaltous sulfate.
3. the solvothermal preparation method of a kind of cobalt nanofiber according to claim 1, is characterized in that, the cobalt nanofiber of generation, after centrifugation, with absolute ethanol washing 2 ~ 3 times, dryly to be collected.
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| CN104117377A (en) * | 2014-06-26 | 2014-10-29 | 童东革 | Co-B-N-H nanowire catalyst as well as preparation method and catalytic method of catalyst |
| CN106115801A (en) * | 2016-06-24 | 2016-11-16 | 北京农学院 | A kind of Cobalto-cobaltic oxide and preparation method thereof, application |
| CN110653379A (en) * | 2018-06-28 | 2020-01-07 | 宁波山功新材料科技有限公司 | Preparation method of degradable metal nanowires |
| CN109261981B (en) * | 2018-08-20 | 2022-02-15 | 浙江师范大学 | Bimetal cobalt-based core-shell material and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2009120867A (en) * | 2007-11-12 | 2009-06-04 | Konica Minolta Holdings Inc | Metal nanowire, manufacturing method of metal nanowire, and transparent electric conductor including metal nanowire |
| CN101698234A (en) * | 2009-10-21 | 2010-04-28 | 北京科技大学 | Chemical preparation method of metal cobalt nanowire |
| CN101898251A (en) * | 2010-08-17 | 2010-12-01 | 上海交通大学 | Template-free method for realizing preparation of metalliccobalt nanowire |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2009120867A (en) * | 2007-11-12 | 2009-06-04 | Konica Minolta Holdings Inc | Metal nanowire, manufacturing method of metal nanowire, and transparent electric conductor including metal nanowire |
| CN101698234A (en) * | 2009-10-21 | 2010-04-28 | 北京科技大学 | Chemical preparation method of metal cobalt nanowire |
| CN101898251A (en) * | 2010-08-17 | 2010-12-01 | 上海交通大学 | Template-free method for realizing preparation of metalliccobalt nanowire |
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