CN103447549B - Preparation method of cobalt nanosphere - Google Patents
Preparation method of cobalt nanosphere Download PDFInfo
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- CN103447549B CN103447549B CN201310415898.4A CN201310415898A CN103447549B CN 103447549 B CN103447549 B CN 103447549B CN 201310415898 A CN201310415898 A CN 201310415898A CN 103447549 B CN103447549 B CN 103447549B
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- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 56
- 239000010941 cobalt Substances 0.000 title claims abstract description 56
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000002077 nanosphere Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 13
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 239000004094 surface-active agent Substances 0.000 claims abstract description 12
- 239000013049 sediment Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 10
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 10
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 10
- 239000000376 reactant Substances 0.000 claims description 10
- 238000005119 centrifugation Methods 0.000 claims description 6
- 239000000428 dust Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 5
- 239000002086 nanomaterial Substances 0.000 abstract description 4
- 239000011358 absorbing material Substances 0.000 abstract description 3
- 239000000956 alloy Substances 0.000 abstract description 3
- 229910045601 alloy Inorganic materials 0.000 abstract description 3
- 239000011553 magnetic fluid Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract 8
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 239000000919 ceramic Substances 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 239000003643 water by type Substances 0.000 description 12
- 230000000694 effects Effects 0.000 description 6
- 238000004220 aggregation Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- -1 permanent magnet Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910021524 transition metal nanoparticle Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Abstract
The invention discloses a preparation method of cobalt nanospheres, which comprises the following steps: 1) dissolving cobalt chloride hexahydrate and a surfactant in a mixed solution of deionized water and absolute ethyl alcohol to prepare a solution A; dissolving sodium hydroxide in deionized water to prepare solution B; dissolving sodium borohydride in deionized water to prepare solution C; 2) mixing the solution A, the solution B and the solution C to obtain a reaction solution, transferring the reaction solution into a high-pressure kettle, and carrying out hydrothermal reaction to obtain cobalt nanospheres; the diameter of the cobalt nanospheres can be controlled to be 250-900 nm by controlling reaction conditions; the method has the characteristics of readily available raw materials, simple equipment, low cost, simple operation, high efficiency, rapidness and the like, and the prepared cobalt nanospheres have regular appearance, uniform particle size, good dispersibility, controllable size, high yield and good stability, and are suitable for large-scale industrial production; the cobalt nano-material prepared by the invention has wide application prospect in the fields of magnetic recording materials, magnetic fluids, permanent magnets, wave-absorbing materials, hard alloys, catalytic materials, ceramics, solar cells and the like.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, be specifically related to a kind of preparation method of cobalt nanosphere.
Background technology
Transition metal nanoparticles is owing to having skin effect, bulk effect, quantum size effect and macro quanta tunnel effect, and there are peculiar electrical, magnetic, optical property etc., be widely used in fields such as catalysis, luminescent material, magnetic material, semi-conducting material and nano-devices.Metallic cobalt nano-powder is a kind of important transition metal nano material, can be used as high-performance magnetism recording materials, magnetic fluid, absorbing material, activated sintering additive etc., be widely used in the fields such as carbide alloy, catalysis material, permanent magnet, pottery and solar cell, be subject to people to pay close attention to widely, become the focus of research.
The preparation method of current cobalt nano-powder material is a lot, as chemical precipitation method, microwave irradiation, high temperature solid-state reducing process, sol-gel process, microemulsion method, hydrothermal synthesis method, spray pyrolysis and ultrasonic etc.These methods Shortcomings to a certain extent, such as Product size, pattern are restive; Easy reunion; Productive rate is not high; Harsh or the preparation process more complicated of pyroreaction condition, cost are relatively high.Therefore, how to prepare high yield, high dispersive, size cobalt nano material that is controlled, regular appearance remain a crucial problem.
Summary of the invention
In view of this, the invention provides a kind of preparation method of cobalt nanosphere, the cobalt nanosphere regular appearance of preparation, uniform particle diameter, good dispersion, productive rate be high, good stability.
The preparation method of cobalt nanosphere of the present invention, comprises the following steps:
1) cobalt chloride hexahydrate and surfactant are dissolved in wiring solution-forming A in the mixed liquor of deionized water and absolute ethyl alcohol; NaOH is dissolved in wiring solution-forming B in deionized water; Sodium borohydride is dissolved in wiring solution-forming C in deionized water;
2) solution A, solution B and solution C three kinds of solution are mixed as reaction solution, transfer in autoclave, carry out hydro-thermal reaction, obtain cobalt nanosphere.
Further, in described solution A, the volume ratio of deionized water and absolute ethyl alcohol is 1:1 ~ 1:4;
Further, in described solution A, the molar concentration of cobalt chloride hexahydrate is 0.06 ~ 0.3 mol/L;
Further, described surfactant is polyvinylpyrrolidone;
Further, in described solution A, the consumption of surfactant is 0.3 ~ 0.6 g/100 ml;
Further, in described solution B, the molar concentration of NaOH is 2 ~ 4 mol/L;
Further, in described solution C, the molar concentration of sodium borohydride is 2 ~ 4 mol/L;
Further, in described reaction solution, the mol ratio of cobalt chloride hexahydrate and sodium borohydride is 1:5 ~ 1:20;
Further, in described reaction solution, the mol ratio of NaOH and sodium borohydride is 1:1 ~ 1:2;
Further, the temperature of described hydro-thermal reaction is 150 ~ 200 DEG C, and the reaction time is 15 ~ 20 hours;
Further, further comprising the steps of:
3) after water-bath, reactant liquor will be suspended and carry out centrifugation, then use deionized water and absolute ethanol washing sediment;
4) be placed on by sediment in vacuum drying chamber dry at 40 ~ 60 DEG C, drying time is 4 ~ 6 hours, finally obtains black cobalt dust.
Beneficial effect of the present invention is: the present invention with common cobalt chloride hexahydrate, NaOH and sodium borohydride for reaction raw materials, surfactant auxiliary under carry out hydro-thermal reaction, obtain cobalt nanosphere; By controlling reaction condition, the diameter of cobalt nanosphere can be controlled between 250 ~ 900 nm; Therefore, the features such as the present invention has that raw material is easy to get, device simple, with low cost, simple to operate, efficient quick, the cobalt nanosphere regular appearance of preparation, uniform particle diameter, good dispersion, productive rate are high, good stability, are applicable to large-scale industrial production; Cobalt nano material prepared by the present invention has broad application prospects in fields such as magnetic recording material, magnetic fluid, permanent magnet, absorbing material, carbide alloy, catalysis material, pottery and solar cells.
Accompanying drawing explanation
In order to make the object, technical solutions and advantages of the present invention clearly, below in conjunction with accompanying drawing, the present invention is described in further detail, wherein:
Fig. 1 is the scanning electron microscope (SEM) photograph of cobalt nanosphere prepared by the embodiment of the present invention 1;
Fig. 2 is the scanning electron microscope (SEM) photograph of cobalt nanosphere prepared by the embodiment of the present invention 2;
Fig. 3 is the scanning electron microscope (SEM) photograph of cobalt nanosphere prepared by the embodiment of the present invention 3;
Fig. 4 is the scanning electron microscope (SEM) photograph of cobalt nanosphere prepared by the embodiment of the present invention 4.
Detailed description of the invention
Hereinafter with reference to accompanying drawing, the preferred embodiments of the present invention are described in detail.
embodiment 1
The preparation method of the present embodiment cobalt nanosphere, comprises the following steps:
1) 0.25 g cobalt chloride hexahydrate is taken and 0.05 g polyvinylpyrrolidone is dissolved in wiring solution-forming A in the mixed liquor of 15 ml deionized waters and absolute ethyl alcohol; Take 0.4 g NaOH and be dissolved in wiring solution-forming B in 5 ml deionized waters; Take 0.4 g sodium borohydride again and be dissolved in wiring solution-forming C in 5 ml deionized waters;
2) 15 ml solution A, 5 ml solution B and 5 ml solution C mixed as reaction solution and transfer in autoclave, being placed in 160 DEG C of constant temperature blast drying ovens reactions 20 hours, obtaining cobalt nanosphere;
3) after hydro-thermal reaction, reactant liquor will be suspended and carry out centrifugation, then use deionized water and absolute ethanol washing sediment;
4) be placed on by sediment in vacuum drying chamber dry at 50 DEG C, drying time is 5 hours, finally obtains black cobalt dust.
In cobalt chloride hexahydrate solution, add a certain amount of surfactant polyvinylpyrrolidone, object is the pattern controlling product, also plays the effect preventing particle aggregation simultaneously; The object of step 3) and step 4) is separated from being suspended reactant liquor by the cobalt nanosphere of preparation; As shown in Figure 1, average diameter is about 350 nm to the scanning electron microscope (SEM) photograph of cobalt nanosphere prepared by the present embodiment.
embodiment 2
The preparation method of the present embodiment cobalt nanosphere, comprises the following steps:
1) 0.25 g cobalt chloride hexahydrate is taken and 0.06 g polyvinylpyrrolidone is dissolved in wiring solution-forming A in the mixed liquor of 15 ml deionized waters and absolute ethyl alcohol; Take 0.5 g NaOH and be dissolved in wiring solution-forming B in 5 ml deionized waters; Take 0.62 g sodium borohydride again and be dissolved in wiring solution-forming C in 5 ml deionized waters;
2) 15 ml solution A, 5 ml solution B and 5 ml solution C mixed as reaction solution and transfer in autoclave, being placed in 180 DEG C of constant temperature blast drying ovens reactions 15 hours, obtaining cobalt nanosphere;
3) after hydro-thermal reaction, reactant liquor will be suspended and carry out centrifugation, then use deionized water and absolute ethanol washing sediment;
4) be placed on by sediment in vacuum drying chamber dry at 50 DEG C, drying time is 5 hours, finally obtains black cobalt dust.
In cobalt chloride hexahydrate solution, add a certain amount of surfactant polyvinylpyrrolidone, object is the pattern controlling product, also plays the effect preventing particle aggregation simultaneously; The object of step 3) and step 4) is separated from being suspended reactant liquor by the cobalt nanosphere of preparation; As shown in Figure 2, average diameter is about 400 nm to the scanning electron microscope (SEM) photograph of cobalt nanosphere prepared by the present embodiment.
embodiment 3
The preparation method of the present embodiment cobalt nanosphere, comprises the following steps:
1) 0.25 g cobalt chloride hexahydrate is taken and 0.1 g polyvinylpyrrolidone is dissolved in wiring solution-forming A in the mixed liquor of 15 ml deionized waters and absolute ethyl alcohol; Take 0.48 g NaOH and be dissolved in wiring solution-forming B in 5 ml deionized waters; Take 0.55 g sodium borohydride again and be dissolved in wiring solution-forming C in 5 ml deionized waters;
2) 15 ml solution A, 5 ml solution B and 5 ml solution C mixed as reaction solution and transfer in autoclave, being placed in 180 DEG C of constant temperature blast drying ovens reactions 18 hours, obtaining cobalt nanosphere;
3) after hydro-thermal reaction, reactant liquor will be suspended and carry out centrifugation, then use deionized water and absolute ethanol washing sediment;
4) be placed on by sediment in vacuum drying chamber dry at 40 DEG C, drying time is 6 hours, finally obtains black cobalt dust.
In cobalt chloride hexahydrate solution, add a certain amount of surfactant polyvinylpyrrolidone, object is the pattern controlling product, also plays the effect preventing particle aggregation simultaneously; The object of step 3) and step 4) is separated from being suspended reactant liquor by the cobalt nanosphere of preparation; As shown in Figure 3, average diameter is about 250 nm to the scanning electron microscope (SEM) photograph of cobalt nanosphere prepared by the present embodiment.
embodiment 4
The preparation method of the present embodiment cobalt nanosphere, comprises the following steps:
1) 0.5 g cobalt chloride hexahydrate is taken and 0.08 g polyvinylpyrrolidone is dissolved in wiring solution-forming A in the mixed liquor of 15 ml deionized waters and absolute ethyl alcohol; Take 0.6 g NaOH and be dissolved in wiring solution-forming B in 5 ml deionized waters; Take 0.62 g sodium borohydride again and be dissolved in wiring solution-forming C in 5 ml deionized waters;
2) 15 ml solution A, 5 ml solution B and 5 ml solution C mixed as reaction solution and transfer in autoclave, being placed in 160 DEG C of constant temperature blast drying ovens reactions 20 hours, obtaining cobalt nanosphere;
3) after hydro-thermal reaction, reactant liquor will be suspended and carry out centrifugation, then use deionized water and absolute ethanol washing sediment;
4) be placed on by sediment in vacuum drying chamber dry at 40 DEG C, drying time is 6 hours, finally obtains black cobalt dust.
In cobalt chloride hexahydrate solution, add a certain amount of surfactant polyvinylpyrrolidone, object is the pattern controlling product, also plays the effect preventing particle aggregation simultaneously; The object of step 3) and step 4) is separated from being suspended reactant liquor by the cobalt nanosphere of preparation; As shown in Figure 4, average diameter is about 900 nm to the scanning electron microscope (SEM) photograph of cobalt nanosphere prepared by the present embodiment.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although by referring to the preferred embodiments of the present invention, invention has been described, but those of ordinary skill in the art is to be understood that, various change can be made to it in the form and details, and not depart from the spirit and scope of the present invention that appended claims limits.
Claims (10)
1. a preparation method for cobalt nanosphere, is characterized in that: comprise the following steps:
1) cobalt chloride hexahydrate and surfactant are dissolved in wiring solution-forming A in the mixed liquor of deionized water and absolute ethyl alcohol; NaOH is dissolved in wiring solution-forming B in deionized water; Sodium borohydride is dissolved in wiring solution-forming C in deionized water;
2) solution A, solution B and solution C three kinds of solution are mixed as reaction solution, transfer in autoclave, carry out hydro-thermal reaction, obtain cobalt nanosphere.
2. the preparation method of cobalt nanosphere according to claim 1, is characterized in that: in described solution A, and the volume ratio of deionized water and absolute ethyl alcohol is 1:1 ~ 1:4.
3. the preparation method of cobalt nanosphere according to claim 1, is characterized in that: in described solution A, and the molar concentration of cobalt chloride hexahydrate is 0.06 ~ 0.3 mol/L.
4. the preparation method of cobalt nanosphere according to claim 1, is characterized in that: in described solution A, surfactant is polyvinylpyrrolidone.
5. the preparation method of cobalt nanosphere according to claim 3, is characterized in that: in described solution A, and the concentration of surfactant is 0.3 ~ 0.6 g/100 ml.
6. the preparation method of cobalt nanosphere according to claim 1, is characterized in that: in described solution B, and the molar concentration of NaOH is 2 ~ 4 mol/L.
7. the preparation method of cobalt nanosphere according to claim 1, is characterized in that: in described solution C, and the molar concentration of sodium borohydride is 2 ~ 4 mol/L.
8. the preparation method of cobalt nanosphere according to claim 1, is characterized in that: in described reaction solution, and the mol ratio of cobalt chloride hexahydrate and sodium borohydride is 1:5 ~ 1:20.
9. the preparation method of cobalt nanosphere according to claim 1, is characterized in that: the temperature of described hydro-thermal reaction is 150 ~ 200 DEG C, and the reaction time is 15 ~ 20 hours.
10. the preparation method of the cobalt nanosphere according to claim 1 to 10 any one, is characterized in that: further comprising the steps of:
3) after hydro-thermal reaction, reactant liquor will be suspended and carry out centrifugation, then use deionized water and absolute ethanol washing sediment;
4) be placed on by sediment in vacuum drying chamber dry at 40 ~ 60 DEG C, drying time is 4 ~ 6 hours, finally obtains black cobalt dust.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104787807B (en) * | 2015-05-06 | 2016-10-12 | 厦门大学 | A kind of solvothermal preparation method of cobalt protoxide nanoparticle |
| CN105170991B (en) * | 2015-08-20 | 2017-11-17 | 河北工业大学 | A kind of preparation method of superfine metal cobalt powder |
| CN107900374B (en) * | 2015-12-28 | 2020-06-23 | 重庆文理学院 | Preparation method of cubic platinum nano material with good uniformity |
| CN106041113B (en) * | 2016-05-17 | 2018-09-04 | 国网重庆市电力公司电力科学研究院 | A kind of nano wave-absorbing material and preparation method |
| CN108380899A (en) * | 2018-04-04 | 2018-08-10 | 陕西理工大学 | A kind of preparation method of cobalt nano magnetic material |
| CN110518367A (en) * | 2019-09-03 | 2019-11-29 | 国网重庆市电力公司电力科学研究院 | A kind of super-branched absorbing material preparation method and absorbing material |
| CN111234248B (en) * | 2020-01-20 | 2021-12-21 | 安徽师范大学 | Method for synthesizing size-adjustable metal complex microspheres from Schiff base and metal complex microspheres |
| CN113664216A (en) * | 2021-08-13 | 2021-11-19 | 衢州华友钴新材料有限公司 | Preparation method of large-particle-size spherical cobalt powder |
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| CN102909391A (en) * | 2012-10-21 | 2013-02-06 | 吉林大学 | Method for preparing metal cobalt and nickel powder under room-temperature condition |
| CN103170606A (en) * | 2011-12-23 | 2013-06-26 | 北京有色金属研究总院 | Device for manufacturing metal paste in double forcing and homogenizing mode and machining forming method thereof |
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| US8962075B2 (en) * | 2011-06-17 | 2015-02-24 | National Tsing Hua University | Hollow metal sphere with mesoporous structure and method for manufacturing the same |
| EP2782693A4 (en) * | 2011-11-23 | 2015-08-19 | Momentive Performance Mat Inc | Functionalized metal-containing particles and methods of making the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103170606A (en) * | 2011-12-23 | 2013-06-26 | 北京有色金属研究总院 | Device for manufacturing metal paste in double forcing and homogenizing mode and machining forming method thereof |
| CN102909391A (en) * | 2012-10-21 | 2013-02-06 | 吉林大学 | Method for preparing metal cobalt and nickel powder under room-temperature condition |
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