CN105328202A - Preparing method of cobalt nanometer materials - Google Patents
Preparing method of cobalt nanometer materials Download PDFInfo
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- CN105328202A CN105328202A CN201410398839.5A CN201410398839A CN105328202A CN 105328202 A CN105328202 A CN 105328202A CN 201410398839 A CN201410398839 A CN 201410398839A CN 105328202 A CN105328202 A CN 105328202A
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Abstract
The invention discloses a preparing method of cobalt nanometer materials. The preparing method comprises the following steps that firstly, cobalt-nitrate hexahydrate, a complexing agent and a dispersing agent are sequentially added into 0.1 L of deionized water, magnetic stirring is carried out, and a mixed solution is obtained; secondly, the solution is placed in a drying box with the temperature of 150-200 DEG C to be dried till the loose porous state is achieved; and thirdly, a precursor is placed in a tubular furnace with the temperature of 300-500 DEG C to be roasted at the high temperature for 5-7 hours, and then the cobalt nanometer materials can be obtained. Cobalt nitrate containing six kinds of crystal water and several common carbohydrate are adopted as raw materials, the raw materials are cheap and easy to obtain, cost is low, and industrial production is greatly facilitated.
Description
Technical field
The present invention relates to the preparation of metal nano material, be specifically related to a kind of preparation method of cobalt nano material.
Background technology
Cobalt nano material, as a kind of nano functional metal material, has a series of special physics, chemical property, shows the performance of many excellences in the application in the fields such as carbide alloy, battery material, catalyst, magnetic material, absorbing material, pottery.Such as, make permanent magnetism recording materials with super-fine cobalt powder, the packing density of tape and soft or hard dish can be made to improve decades of times, and significantly can improve their fidelity performance.Simultaneously because super-fine cobalt powder is to electromagnetic special absorption, can be used as military high performance millimeter wave stealth material, visible ray-infrared ray stealth material and structural formula stealth material, mobile phone radiation shielding material.The super-fine cobalt powder used in carbide alloy is obtained for raising due to the cross-breaking strength of alloy, hardness and density, makes it have higher wearability and crack resistance.
The traditional preparation methods of cobalt nanometer particle is a lot, as hydrothermal synthesis method, Radiation Synthesis Method, plasma method, the precipitation method, microemulsion method etc.The Bawendi research group of the U.S. in 1993 has developed high temperature solution phase method, is synthesized semiconductor nanotube ME (M=Cd, Pd the earliest; E=Se, S, Te).In the later stage nineties 20th century, it is nanocrystalline that the Murray of IBM Corporation etc. utilize the method successfully to synthesize monodispersed Co.Shen Chengmin etc. utilize diphenyl ether to make solvent; using oleic acid and tri octyl phosphine as surfactant; adopt glycol reducing process to prepare the monodisperse magnetic Co nano particle with hcp phase under nitrogen protection, and Co self-assembly is become the orderly closelypacked single dispersing film of two dimension six side on copper mesh.They also use Co simultaneously
2(CO)
8the Co nano particle of self assembly is prepared in thermal decomposition, and is studied its magnetic property.But this method has individual shortcoming: carbonyl nickel is a kind of extremely toxic substance, hinders health, very large pollution is easily caused to environment.MaLixin etc. are cobalt source with cobaltous sulfate in alkaline environment, enough sodium potassium tartrate tetrahydrates are complexing agent, hydrazine hydrate is reducing agent, adopt chemical plating process in cobalt layers on sour barium coating surface of admiring.It is reducing agent with hydrazine hydrate that patent CN1923415 provides a kind of, and softex kw is the method that dispersant prepares sheet cobalt nano-particle, but reducing agent hydrazine hydrate toxicity used is comparatively large, unhealthful.University of Science & Technology, Beijing Wang Zhi is far away etc. reports with cobalt chloride hexahydrate is raw material, with NaBH
4for reducing agent, with triethanolamine and PVP for complexing agent, in absolute ethyl alcohol, synthesized the research of cobalt nano-particle, the cobalt nanometer particle average grain diameter that they obtain also is greater than 10nm, and easily produces the boride of cobalt, reducing agent NaBH
4toxicity is also comparatively large, and production cost is higher, and preparation process is also comparatively complicated.
Summary of the invention
The object of the invention is some defects overcoming prior art existence, the method preparing cobalt nano material that one is simple and convenient, with low cost, toxicity is few is provided.
In order to achieve the above object, technical scheme of the present invention is as follows:
1, first prepare cobalt nitrate solution, join in cobalt nitrate solution by complexing agent and dispersant, magnetic agitation is to settled solution;
2, above-mentioned mixed solution is placed in drying box dry, forms loose porous presoma;
3, precursor is put in Muffle furnace calcines, continue in tube furnace while calcining to pass into inert gas protection.
The molar concentration of the cobalt nitrate solution described in step 1 is 0.05-0.1mol/L.
Complexing agent described in step 1 is any one in citric acid, ascorbic acid, ethylenediamine tetra-acetic acid, glucose, starch or sucrose, and dispersant is polyvinylpyrrolidone (PVP).
The mol ratio of the cobalt nitrate described in step 1 and complexing agent is 1:0.5-1:2; The mol ratio of cobalt nitrate and dispersant is 1:2-1:4.
Baking temperature described in step 2 is 150-200 DEG C, and drying time is 10-15 hour.
Calcining heat described in step 3 is 300-500 DEG C, and calcination time is 5-7 hour, and heating rate is 5 DEG C/min.
Compared with the existing methods, the invention has the advantages that:
1. the present invention with the carbohydrate of common cabaltous nitrate hexahydrate and some cheapnesss for reaction raw materials, dispersant auxiliary under carry out coordination decomposition reaction, a small amount of complexing agent serves the effect triggering electroless plating reaction and carry out in order, ensure that the homogeneity of nanometer cobalt material particle size.
2. simply, raw material is easy to get for synthesis technique of the present invention and required production equipment, is applicable to suitability for industrialized production.
3. the grain size of cobalt nanometer particle that prepared by the present invention is 5-10nm, is uniformly dispersed, stable in properties.
Accompanying drawing explanation
Fig. 1 is the TEM figure of cobalt nano material in the embodiment of the present invention 1.
Fig. 2 is the XRD figure of cobalt nano material in the embodiment of the present invention 1.
Fig. 3 is the XRD figure of cobalt nano material in the embodiment of the present invention 2.
Fig. 4 is the XRD figure of cobalt nano material in the embodiment of the present invention 3.
Fig. 5 is the XRD figure of cobalt nano material in the embodiment of the present invention 4.
Fig. 6 is the XRD figure of cobalt nano material in the embodiment of the present invention 5.
Fig. 7 is the XRD figure of cobalt nano material in the embodiment of the present invention 6.
Detailed description of the invention
Below in conjunction with example and accompanying drawing, the present invention is described in detail.
Embodiment 1: 1.4699g cabaltous nitrate hexahydrate is dissolved in the deionized water of 0.1L, then taking 2.1123g citric acid adds in above-mentioned solution, magnetic agitation, treat that citric acid adds 2.2200g dispersant PVP after dissolving completely again in solution, continue to stir until PVP dissolves completely, mixed solution to be put in drying box at 150 DEG C dry 15 hours, obtain loose porous presoma, then presoma is put in Muffle furnace and calcines, continue in tube furnace in calcination process to pass into inert atmosphere protection, calcining heat is 300 DEG C, calcination time is 7 hours.Fig. 1 is the TEM figure of sample, and as can be seen from the figure the grain size of cobalt nano-particle is 5-10nm, and favorable dispersibility.Fig. 2 is the XRD figure of sample, three diffraction maximums are clearly had in figure, with (111), (200) and (220) crystal face of the corresponding centroid cubic crystal system cobalt of jade software analysis these angles of diffraction known difference, show the cobalt nano material for centroid cubic crystal system obtained.
Embodiment 2: 1.7638g cabaltous nitrate hexahydrate is dissolved in the deionized water of 0.1L, then taking 1.5899g ascorbic acid adds in above-mentioned solution, magnetic agitation, treat that ascorbic acid adds 2.6640g dispersant PVP after dissolving completely again in solution, continue to stir until PVP dissolves completely, mixed solution to be put in drying box at 160 DEG C dry 15 hours, obtain loose porous presoma, then presoma is put in Muffle furnace and calcines, continue in tube furnace in calcination process to pass into inert atmosphere protection, calcining heat is set to 300 DEG C and 500 DEG C respectively, calcination time is 6 hours.When calcining heat is 300 DEG C, (Fig. 3 a), the XRD figure of sample only has the diffraction maximum that very sharp-pointed, and analyzing known product is now face-centred cubic cobalt.But when calcining heat is elevated to 500 DEG C (Fig. 3 b), can see there are three diffraction maximums clearly from Fig. 3 b, analyze known product at this moment and remain face-centred cubic cobalt nano material, the decomposition product of cobalt and complexing agent generation is insufficient when the temperature is too low, and crystallization is not so good.
Embodiment 3: 2.0578g cabaltous nitrate hexahydrate is dissolved in the deionized water of 0.1L, then taking 2.0559g ethylenediamine tetra-acetic acid adds in above-mentioned solution, magnetic agitation, treat that ethylenediamine tetra-acetic acid adds 2.3310g dispersant PVP after dissolving completely again in solution, continue to stir until PVP dissolves completely, mixed solution to be put in drying box at 170 DEG C dry 10 hours, obtain loose porous presoma, then presoma is put in Muffle furnace and calcines, continue in tube furnace in calcination process to pass into inert atmosphere protection, calcining heat is 500 DEG C, calcination time is 6 hours.Fig. 4 is the XRD figure of sample, and have three diffraction maximums clearly in figure, analyzing known product is now face-centred cubic cobalt nano material.
Embodiment 4: 2.3518g cabaltous nitrate hexahydrate is dissolved in the deionized water of 0.1L, then taking 1.4268g glucose adds in above-mentioned solution, magnetic agitation, treat that glucose adds 2.6640g dispersant PVP after dissolving completely again in solution, continue to stir until PVP dissolves completely, mixed solution to be put in drying box at 180 DEG C dry 10 hours, obtain loose porous presoma, then presoma is put in Muffle furnace and calcines, continue in tube furnace in calcination process to pass into inert atmosphere protection, calcining heat is 400 DEG C, calcination time is 7 hours.Fig. 5 is the XRD figure of sample, and have three diffraction maximums clearly in figure, analyzing known product is now face-centred cubic cobalt nano material.
Embodiment 5: 2.6457g cabaltous nitrate hexahydrate is dissolved in the deionized water of 0.1L; then taking 1.2485g starch adds in above-mentioned solution; magnetic agitation; treat that starch adds 1.9980g dispersant PVP after dissolving completely again in solution; continue to stir until PVP dissolves completely; mixed solution to be put in drying box at 190 DEG C dry 15 hours; obtain loose porous presoma; then presoma is put in Muffle furnace and calcines; continue in tube furnace in calcination process to pass into inert atmosphere protection; calcining heat is 300 DEG C, and calcination time is 5 hours.Fig. 6 is the XRD figure of sample, and have three diffraction maximums clearly in figure, analyzing known product is now face-centred cubic cobalt nano material.
Embodiment 6: 2.9397g cabaltous nitrate hexahydrate is dissolved in the deionized water of 0.1L; then taking 1.7313g sucrose adds in above-mentioned solution; magnetic agitation; treat that sucrose adds 2.2200g dispersant PVP after dissolving completely again in solution; continue to stir until PVP dissolves completely; mixed solution to be put in drying box at 200 DEG C dry 10 hours; obtain loose porous presoma; then presoma is put in Muffle furnace and calcines; continue in tube furnace in calcination process to pass into inert atmosphere protection; calcining heat is 500 DEG C, and calcination time is 6 hours.Fig. 7 is the XRD figure of sample, and have three diffraction maximums clearly in figure, analyzing known product is now face-centred cubic cobalt nano material.
Claims (6)
1. a preparation method for cobalt nano material, is characterized in that, comprises the steps:
Step 1, first prepare cobalt nitrate solution, join in cobalt nitrate solution by complexing agent and dispersant, magnetic agitation is to settled solution;
Step 2, above-mentioned mixed solution to be placed in drying box dry, forms loose porous presoma;
Step 3, precursor is put in Muffle furnace and calcines, continue in tube furnace while calcining to pass into inert gas protection.
2. the preparation method of cobalt nano material according to claim 1, is characterized in that, the molar concentration of the cobalt nitrate solution described in step 1 is 0.05-0.1mol/L.
3. the preparation method of cobalt nano material according to claim 1, it is characterized in that, complexing agent described in step 1 is any one in citric acid, ascorbic acid, ethylenediamine tetra-acetic acid, glucose, starch or sucrose, and dispersant is polyvinylpyrrolidone.
4. the preparation method of cobalt nano material according to claim 1, is characterized in that, the mol ratio of the cobalt nitrate described in step 1 and complexing agent is 1:0.5-1:2; The mol ratio of cobalt nitrate and dispersant is 1:2-1:4.
5. the preparation method of cobalt nano material according to claim 1, is characterized in that, the baking temperature described in step 2 is 150-200 DEG C, and drying time is 10-15 hour.
6. the preparation method of cobalt nano material according to claim 1, is characterized in that, the calcining heat described in step 3 is 300-500 DEG C, and calcination time is 5-7 hour, and heating rate is 5 DEG C/min.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106082171A (en) * | 2016-06-17 | 2016-11-09 | 无锡英普林纳米科技有限公司 | A kind of preparation method of UV nano impression glue |
| CN107350480A (en) * | 2017-06-07 | 2017-11-17 | 常州瑞坦商贸有限公司 | A kind of preparation method of super-fine cobalt powder |
| CN108654640A (en) * | 2018-03-15 | 2018-10-16 | 安徽师范大学 | Cobalt hydroxide material of Ag doping and its preparation method and application |
| CN108788131A (en) * | 2018-07-04 | 2018-11-13 | 常州市金坛磁性材料有限公司 | A kind of soft magnetism cobalt micron bar material and preparation method thereof |
| CN109663930A (en) * | 2019-02-12 | 2019-04-23 | 闽江师范高等专科学校 | A kind of pyrophorisity micro-nano metal material and preparation method thereof |
| CN110899718A (en) * | 2018-09-14 | 2020-03-24 | 上海铁路通信有限公司 | Preparation method of large-particle-size cobalt particles with shell-core structures |
| CN113059179A (en) * | 2021-03-17 | 2021-07-02 | 电子科技大学 | Preparation method of magnetic cobalt particles |
| CN113798503A (en) * | 2021-09-18 | 2021-12-17 | 赣南医学院 | Method for preparing metal cobalt nanosheet |
| CN115026281A (en) * | 2022-05-05 | 2022-09-09 | 同济大学 | NiCo metallocene with NiCoPd ternary alloy embedded in situ and preparation method thereof |
| CN115304685A (en) * | 2022-08-11 | 2022-11-08 | 桂林理工大学 | Modified starch nanoparticles with water resistance, ultraviolet absorption and ammonia response color change functions as well as preparation method and application thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106082171A (en) * | 2016-06-17 | 2016-11-09 | 无锡英普林纳米科技有限公司 | A kind of preparation method of UV nano impression glue |
| CN107350480A (en) * | 2017-06-07 | 2017-11-17 | 常州瑞坦商贸有限公司 | A kind of preparation method of super-fine cobalt powder |
| CN108654640A (en) * | 2018-03-15 | 2018-10-16 | 安徽师范大学 | Cobalt hydroxide material of Ag doping and its preparation method and application |
| CN108788131A (en) * | 2018-07-04 | 2018-11-13 | 常州市金坛磁性材料有限公司 | A kind of soft magnetism cobalt micron bar material and preparation method thereof |
| CN110899718A (en) * | 2018-09-14 | 2020-03-24 | 上海铁路通信有限公司 | Preparation method of large-particle-size cobalt particles with shell-core structures |
| CN109663930A (en) * | 2019-02-12 | 2019-04-23 | 闽江师范高等专科学校 | A kind of pyrophorisity micro-nano metal material and preparation method thereof |
| CN113059179A (en) * | 2021-03-17 | 2021-07-02 | 电子科技大学 | Preparation method of magnetic cobalt particles |
| CN113059179B (en) * | 2021-03-17 | 2022-06-03 | 电子科技大学 | Preparation method of magnetic cobalt particles |
| CN113798503A (en) * | 2021-09-18 | 2021-12-17 | 赣南医学院 | Method for preparing metal cobalt nanosheet |
| CN115026281A (en) * | 2022-05-05 | 2022-09-09 | 同济大学 | NiCo metallocene with NiCoPd ternary alloy embedded in situ and preparation method thereof |
| CN115026281B (en) * | 2022-05-05 | 2023-03-14 | 同济大学 | NiCo metallocene with NiCoPd ternary alloy embedded in situ and preparation method thereof |
| CN115304685A (en) * | 2022-08-11 | 2022-11-08 | 桂林理工大学 | Modified starch nanoparticles with water resistance, ultraviolet absorption and ammonia response color change functions as well as preparation method and application thereof |
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