CN102941355A - Solvothermal preparation method of cobalt nano-fibers - Google Patents
Solvothermal preparation method of cobalt nano-fibers Download PDFInfo
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- CN102941355A CN102941355A CN2012105169591A CN201210516959A CN102941355A CN 102941355 A CN102941355 A CN 102941355A CN 2012105169591 A CN2012105169591 A CN 2012105169591A CN 201210516959 A CN201210516959 A CN 201210516959A CN 102941355 A CN102941355 A CN 102941355A
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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 the metal material technical field, be specifically related to a kind of solvothermal preparation method of cobalt nanofiber.
Background technology
The cobalt nano material has unique photoelectromagnetic and catalysis characteristics, has broad application prospects at aspects such as single-electron device, Ultrahigh-Density Data Storage, magnetic fluid, catalyst and biological anticancer medicines.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.Preparation diameter cobalt nanofiber even, that compliance is good is to realize its practical basis.
According to " Rare Metal Materials and Engineering " 2012,41(9): 1527 ~ 1530 reports take the oxalic acid hydrate cobalt nanorod as presoma, under 360 ℃, can prepare the nano metal cobalt fiber by thermal decomposition process in Ar atmosphere.Yet can find out that from its ESEM product is ribbon, and stacking adhesion is more serious between the band.
The molecular self-assembling method is to utilize the interaction between the molecule to be assembled into orderly nanostructured." Nano Letter " 2004,4 (11): 2299 ~ 2302 reported that fluorocarbon is at Co
3C or Co particle surface be catalytic decomposition lentamente, forms CNT, simultaneously, and Co
3C or Co particle are connected to the inner Co of formation of carbon pipe nano wire by orientation.It is inner that yet this method is grown in the carbon pipe with cobalt nanowire, although can prevent its oxidation, is disadvantageous to its magnetic property, and this microreaction process and complicated difficult control thereof.
Soft template method is the hole phase that adopts in the surfactant, is template with the rod-shaped micelle microemulsion namely, the growth of guiding nano material in its duct.According to " high chemical journal " 2003,24(6): 986 ~ 988 reports, microemulsion technology is combined with the solvent heat technology, the transformation behavior that utilizes lysotropic liquid crystal to vary with temperature and occur, the cobalt nanofiber that can prepare multilevel hierarchy, yet transmission electron microscope photo shows, the cobalt nanofiber of the method preparation is to be coalescent the forming of nano particle of 5nm by average grain diameter, has the shortcomings such as diameter is inhomogeneous, compliance is poor, easy fracture.Application number provides a kind of chemical preparation process of metal cobalt nanowire for the patent of invention of CN 101698234B, 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 μ m.But can find that from its scanned photograph this nano wire also is to be combined by nano level cobalt ball, and the particle diameter of cobalt nanosphere exists between larger difference, the adjacent cobalt nanosphere in conjunction with weak.
In sum, all there is certain defective in the preparation method of existing cobalt nanofiber, is difficult to prepare the cobalt nanofiber that diameter is even, compliance is good.
Summary of the invention
The solvothermal preparation method that the purpose of this invention is to provide a kind of cobalt nanofiber overcomes the defective that compliance is poor, diameter is inhomogeneous 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, in solution cobalt salt 0.05 ~ 0.2mol/L, ethylenediamine 2 ~ 4mol/L, NaOH 0.5 ~ 1mol/L, polyvinylpyrrolidone 5 ~ 10g/L, the preparation of polyoxyethylene laurel ether Brij30 1 ~ 5ml/L ratio, magnetic agitation 50 ~ 70 minutes.
Described cobalt salt is any among cobalt acetate, hydrochloric acid cobalt, cobalt nitrate, the cobaltous sulfate.
Described NaOH joins in the reaction solution in the mode of deionized water solution.
2, cobalt nanofiber preparation
The solution for preparing is as stated above moved in the reactor, and compactedness is 50% ~ 70%, the lid of reactor is screwed to be placed on be heated to 180 ~ 190 ℃ in the heating furnace, react generation cobalt nanofiber 20 ~ 40 hours.The cobalt nanofiber that generates is used absolute ethanol washing 2 ~ 3 times after centrifugation, the dry collection.
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 the reduction cobalt is grown to serve as the cobalt nanofiber that diameter is even, compliance is good along (001) direction line style; Simple, the with low cost and suitable suitability for industrialized production of this preparation method's technique.
Description of drawings
Fig. 1 is the SEM photo figure of the cobalt nanofiber of embodiment 1 preparation.
Fig. 2 is the TEM photo figure of the cobalt nanofiber of embodiment 1 preparation.
Fig. 3 is the SEM photo figure of the cobalt nanofiber of embodiment 2 preparations.
Fig. 4 is the X-ray diffraction spectrogram of the cobalt nanofiber of embodiment 2 preparations.
The specific embodiment
Be described in detail the specific embodiment of the present invention below in conjunction with technical scheme and accompanying drawing.
Embodiment one:
1, the preparation of reaction solution
The preparation precursor liquid take ethylene glycol as solvent, each reactant concentration is as follows:
2, the preparation of cobalt nanofiber
Mentioned solution is moved in the reactor, and compactedness is 50%, the lid of reactor is screwed to be placed on be heated to 180 ℃ in the heating furnace, be incubated 36 hours, the question response still is opened after cooling off fully, after the black precipitate centrifugation that generates, with absolute ethanol washing 3 times, then 50 ℃ of oven dry 24 hours.The SEM photo of products therefrom as shown in Figure 1, the TEM photo is as shown in Figure 2.
Embodiment two:
1, the preparation of reaction solution
The preparation precursor liquid take ethylene glycol as solvent, each reactant concentration is as follows:
2, the preparation of cobalt nanofiber
Mentioned solution is moved in the reactor, and compactedness is 70%, the lid of reactor is screwed to be placed on be heated to 190 ℃ in the heating furnace, be incubated 24 hours, the question response still is opened after cooling off fully, after the black precipitate centrifugation that generates, with absolute ethanol washing 3 times, then 50 ℃ of oven dry 24 hours.The SEM picture of products therefrom as shown in Figure 3, the X-ray diffraction spectrogram is as shown in Figure 4.
Claims (4)
1. the solvothermal preparation method of a cobalt nanofiber is characterized in that, concrete steps are as follows:
1) preparation of reaction solution
Take ethylene glycol as solvent, in solution cobalt salt 0.05 ~ 0.2mol/L, ethylenediamine 2 ~ 4mol/L, NaOH 0.5 ~ 1mol/L, polyvinylpyrrolidone 5 ~ 10g/L, the preparation of polyoxyethylene laurel ether Brij30 1 ~ 5ml/L ratio, magnetic agitation 50 ~ 70 minutes;
2) preparation of cobalt nanofiber
The solution for preparing is as stated above moved in the reactor, and compactedness is 50% ~ 70%, the lid of reactor is screwed to be placed on be heated to 180 ~ 190 ℃ in the heating furnace, react generation cobalt nanofiber 20 ~ 40 hours.
2. the solvothermal preparation method of a kind of cobalt nanofiber according to claim 1 is characterized in that, described cobalt salt is any among cobalt acetate, hydrochloric acid cobalt, cobalt nitrate, the cobaltous sulfate.
3. the solvothermal preparation method of a kind of cobalt nanofiber according to claim 1 is characterized in that, described NaOH joins in the reaction solution in the mode of deionized water solution.
4. the solvothermal preparation method of a kind of cobalt nanofiber according to claim 1 is characterized in that, the cobalt nanofiber of generation is used absolute ethanol washing 2 ~ 3 times after centrifugation, the dry collection.
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| CN201210516959.1A CN102941355B (en) | 2012-12-05 | 2012-12-05 | Solvothermal preparation method of cobalt nano-fibers |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109261981A (en) * | 2018-08-20 | 2019-01-25 | 浙江师范大学 | Bimetallic cobalt-based core-shell material and the preparation method and application thereof |
| 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 |
Citations (4)
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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 |
| WO2012071117A1 (en) * | 2010-11-23 | 2012-05-31 | Carestream Health, Inc. | Nanowire preparation methods, compositions, and articles |
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2012
- 2012-12-05 CN CN201210516959.1A patent/CN102941355B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| WO2012071117A1 (en) * | 2010-11-23 | 2012-05-31 | Carestream Health, Inc. | Nanowire preparation methods, compositions, and articles |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109261981A (en) * | 2018-08-20 | 2019-01-25 | 浙江师范大学 | Bimetallic cobalt-based core-shell material and the preparation method and application thereof |
| 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 |
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| CN102941355B (en) | 2014-12-24 |
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