CN102936004A - Preparation method for preparing cobalt diselenide-ethylenediamine micron-grade flowers through hydrothermal method - Google Patents
Preparation method for preparing cobalt diselenide-ethylenediamine micron-grade flowers through hydrothermal method Download PDFInfo
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Abstract
The invention belongs to the field of inorganic-organic micro-nano composite material synthesis, and relates to a method for synthesizing three-dimensional micron-grade flowers with relatively homogeneous morphology through a hydrothermal method. The invention especially relates to a method for preparing cobalt diselenide-ethylenediamine micron-grade flowers through the hydrothermal method. The method comprises the steps that: sodium selenite and cobalt chloride are subjected to hydrazine hydrate reduction through the hydrothermal method in an alkaline solution containing ethylenediamine, such that cobalt diselenide-ethylenediamine micron-grade flowers are prepared. The method provided by the invention has the advantages of simple process and good reproducibility. The adopted selenium and cobalt sources are inorganic compounds which have low prices and are easy to obtain. Therefore, the cost is low. Sodium selenite has good dissolubility, such that environment requirements are satisfied. The method provided by the invention does not require pretreatments such as high-temperature treatment and calcination, and preparation can be carried out under a relatively low temperature, such that energy consumption and reaction cost are reduced. Therefore, the method can be applied in industrialized batch productions.
Description
Technical field
The invention belongs to the synthetic field of inorganic-organic Micron-nano composites, relate to the synthetic method of utilizing hydrothermal method to prepare the three-dimensional micro-flowers of the relative homogeneous of pattern, particularly hydrothermal method prepares the method for two cobaltous selenides-quadrol micro-flowers.
Background technology
The nanometer selenium compound is the important semiconductor material of a class, good optics, electric property and nonlinear optical response performance are arranged, have widely in all many-sides such as luminescent material, solar cell material, optoelectron sensor, photoelectric conversion material, infrared electro detection, light detector, thermoelectric material, infrared window gate material, biomarker, laser apparatus and use.And in the last few years, controlling to affect material property by appearance structure becomes one of focus of nano materials research gradually.At present, the most researchs of people be to coat between the organic-inorganic and the problem of load, these results of study have embodied the characteristic that its inorganics and organism have concurrently.Along with expanding economy, people more and more receive people's concern for the research and development of new energy materials, reasonably for synthesizing inorganic-organically the research and development of intercalation configuration compound have day by day become the focus of people's research.
How the heat energy that produces in the daily life is reasonably used, realize rational Application and the conversion of the energy, also being subject to people's attention gradually.In these materials, two cobaltous selenides itself are exactly a kind of important IV-VI family semi-conductor, and stronger absorption is arranged in the near-infrared region; As a kind of rich content, environmental friendliness and chemically stable semiconductor material, two cobaltous selenides are that novel thermoelectricity is at one of candidate material.The intercalation configuration compound of inorganic-organic is compared with pure inorganics; tend to show a lot of different chemical property; and the commaterial of different-shape also usually can show different character, so the synthetic concern that day by day is subject to people of the inorganic-organic material of its multidimensional structure.So the preparation method who seeks technique polymorphic two cobaltous selenides simple, with low cost-organism (quadrol etc.) is very necessary, for becoming following thermoelectric material, it provides how potential scientific basis and technical support.
Summary of the invention
The object of the present invention is to provide that a kind of technique is simple, the preparation method of preparation two cobaltous selenides-quadrol micro-flowers under the lesser temps.
A kind of hydrothermal method prepares the method for two cobaltous selenides-quadrol micro-flowers, is with Sodium Selenite, and cobalt chloride utilizes hydrothermal method through the reduction of hydrazine hydrate in containing the basic solution of quadrol, is prepared into the micro-flowers of two cobaltous selenides-quadrol.
The method that hydrothermal method of the present invention prepares two cobaltous selenides-quadrol micro-flowers is to carry out according to following step:
Steps A, with Sodium Selenite, cobalt chloride, quadrol and deionized water according to Sodium Selenite: cobalt chloride: quadrol: the ratio of deionized water is the ratio short mix of 1～2mmol:1mmol:7～24mL:1～18mL and stirs, obtains finely dispersed precursor liquid;
Step B, in described precursor liquid, add the hydrazine hydrate of 5.0mL, stir it is uniformly dispersed;
Step C, the reaction system of step B gained is transferred in the teflon-lined reactor, constant temperature 12～24h under 140～180 ℃ of temperature, naturally cooling obtains hydrothermal product;
Step D, with the hydrothermal product centrifugation of step C gained, wash respectively three times with dehydrated alcohol and deionized water;
Step e, with the product after centrifugation at 60～80 ℃ of vacuum-drying 12～24h.
The Sodium Selenite that the present invention participates in reacting, cobalt chloride, quadrol are analytical pure, and described hydrazine hydrate weight percent is 85wt%.
In another preference of the present invention, reactant is according to Sodium Selenite in the steps A: cobalt chloride: quadrol: the ratio of deionized water is 2mmol:1mmol:22mL:3mL; And the temperature of reacting among the step C is 180 ℃, constant temperature time 24h.
According to the micro-flowers of two cobaltous selenides of the prepared one-tenth of method disclosed by the invention-quadrol, be by the about 40 ~ 60nm of thickness, the nanometer sheet self-assembly of length 1.5 ~ 2 μ m forms.
According to the micro-flowers of two cobaltous selenides of the prepared one-tenth of method disclosed by the invention-quadrol, the diameter of micro-flowers is 5 ~ 6 μ m.
The present invention adopts is that Liquid preparation methods goes out on the pattern relatively two cobaltous selenides of homogeneous-quadrol micro-flowers at a lower temperature.
Two cobaltous selenides among the present invention-quadrol (CoSe
2-EN) structure is determined by x-ray diffractometer, X-ray diffracting spectrum shows, is pure two cobaltous selenides-quadrol (CoSe by combine with the self-assembling technique product for preparing of liquid phase reaction
2-EN), there is other peak (using ◆ mark) to occur in the collection of illustrative plates, this has also just in time determined the intercalation configuration that synthesizes two cobaltous selenides-quadrol of success.
Field emission scanning electron microscope test shows, by liquid phase reaction two cobaltous selenides that the prepare-quadrol (CoSe that combines with self-assembling technique
2-EN) be to be about 40 ~ 60nm by thickness, the micro-flowers of 5 ~ 6 μ m that the nanometer sheet of about 1.5 ~ 2 μ m of length is self-assembled into.
Two cobaltous selenides among the present invention-quadrol (CoSe
2-EN) On Analysis of Chemical Species of Elements on the surface of micro-flowers adopts X-ray photoelectron spectroscopic analysis (XPS), at room temperature test.
Two cobaltous selenides of the relative homogeneous of pattern that is prepared by liquid phase method and self-assembling technique combined technology among the present invention-quadrol (CoSe
2-EN) micro-flowers, the contriver analyzes the valence state of the element on its product surface, 798.98 eV, these two strong peaks of 781.62 eV are corresponding CoSe respectively
2Co 2p1/2 among the-EN and Co 2p3/2; 56.18 eV is then corresponding to CoSe
2Se 3d3/2 among the-EN, these and block CoSe
2Numerical value be close; 399.24 eV is corresponding to CoSe
2N 1s among the-EN.Near the not appearance of other small peak main peak does not have oxidized phenomenon so show the surface of product in the XPS collection of illustrative plates.But by analysis, the contriver finds to have caused the absorption of its correlation energy certain skew to occur owing to there is organic micromolecular intercalation.Two cobaltous selenides that prepare by the present invention-quadrol (CoSe
2-EN) micro-flowers, performance is more stable, provides how potential scientific basis and technical support for it becomes following novel thermoelectric material.
Beneficial effect
The present invention adopts combine with self-assembling technique two cobaltous selenides-quadrol (CoSe of preparation of simple liquid phase reaction
2-EN), pattern is three-dimensional micro-flowers, this material has the advantages such as chemical stability is better.Technique of the present invention is simple, favorable reproducibility, and used selenium source, cobalt source are mineral compound, and cheap and easy to get, cost is low, the solubleness of Sodium Selenite is pretty good, meet environmental requirement, because this technique does not need the pre-treatment of high temperature, calcining and so on, can prepare at a lower temperature, thereby reduced energy consumption and reaction cost, be convenient to batch production.
Description of drawings
Accompanying drawing 1 two cobaltous selenides-quadrol (CoSe
2-EN) x-ray diffraction pattern (XRD).
Accompanying drawing 2 two cobaltous selenides-quadrol (CoSe
2-EN) scanning electron microscope (SEM) photograph (SEM): (a) low power (amplifying 2000 times); (b) high power (amplifying 10000 times).
Accompanying drawing 3 two cobaltous selenides-quadrol (CoSe
2-EN) at room temperature X-ray photoelectron spectroscopic analysis collection of illustrative plates (XPS): (a) Co; (b) Se; (c) N.
Embodiment
The present invention is described in detail below in conjunction with embodiment, so that those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
Embodiment 1
The preparation of two cobaltous selenides-quadrol micro-flowers:
Steps A, with Sodium Selenite, cobalt chloride, quadrol and deionized water according to Sodium Selenite: cobalt chloride: quadrol: the ratio of deionized water is the ratio short mix of 2mmol:1mmol:3mL:22mL and stirs, obtains finely dispersed precursor liquid;
Step B, add the hydrazine hydrate (85wt%) of 5.0mL again, stir it is uniformly dispersed;
Step C, reaction system is transferred in the teflon-lined reactor, constant temperature 24h under 180 ℃ of temperature, naturally cooling obtains hydrothermal product;
Step D, with above-mentioned hydrothermal product centrifugation, wash respectively three times with dehydrated alcohol and deionized water;
Step e, with the product after centrifugation at 80 ℃ of vacuum-drying 12h, can obtain the three-dimensional micro-flowers of two cobaltous selenides-quadrol.
Two cobaltous selenides among the present invention-quadrol (CoSe
2-EN) On Analysis of Chemical Species of Elements on the surface of micro-flowers adopts X-ray photoelectron spectroscopic analysis (XPS), at room temperature test.
In the accompanying drawing 1 position of each diffraction peak and relative intensity all with JCPDS(JCPDS) card (09-0234) matches, and shows that product is CoSe
2, there is other diffraction peak (using ◆ mark) to occur in the XRD figure spectrum, illustrated there is the organic molecule intercalation configuration in the product that what the present invention's proposition was described can prepare two cobaltous selenides-quadrol product by liquid phase-self-assembly method.
Can find out by combine with self-assembling technique two cobaltous selenides-quadrol (CoSe of preparation of liquid phase reaction from accompanying drawing 2
2-EN) be to be about 40～60nm by thickness, the micro-flowers of 5 ~ 6 μ m that the nanometer sheet of about 1.5 ~ 2 μ m of length is self-assembled into.
Can find out at 798.98 eV that from accompanying drawing 3 these two strong peaks of 781.62 eV are corresponding CoSe respectively
2Co 2p1/2 among the-EN and Co 2p3/2; 56.18 eV is then corresponding to CoSe
2Se 3d3/2 among the-EN, these and block CoSe
2Numerical value be close; 399.24 eV is corresponding to CoSe
2N 1s among the-EN.Near the not appearance of other small peak main peak does not have oxidized phenomenon so show the surface of product in the XPS collection of illustrative plates.The contriver finds it owing to there is organic micromolecular intercalation, has caused the absorption of its correlation energy certain skew to occur but by analysis.Two cobaltous selenides that prepare by the present invention-quadrol (CoSe
2-EN) micro-flowers, more stable, for becoming following novel thermoelectric material, it provides how potential scientific basis and technical support.
Embodiment 2
The preparation of two cobaltous selenides-quadrol micro-flowers:
Steps A, with Sodium Selenite, cobalt chloride, quadrol and deionized water according to Sodium Selenite: cobalt chloride: quadrol: the ratio of deionized water is the ratio short mix of 1mmol:1mmol:7mL:18mL and stirs, obtains finely dispersed precursor liquid;
Step B, add the hydrazine hydrate (85wt%) of 5.0mL again, stir it is uniformly dispersed;
Step C, reaction system is transferred in the teflon-lined reactor, constant temperature 12h under 140 ℃ of temperature, naturally cooling obtains hydrothermal product;
Step D, with above-mentioned hydrothermal product centrifugation, wash respectively three times with dehydrated alcohol and deionized water;
Step e, with the product after centrifugation at 60 ℃ of vacuum-drying 12h, can obtain the three-dimensional micro-flowers of two cobaltous selenides-quadrol.
Embodiment 3
The preparation of two cobaltous selenides-quadrol micro-flowers:
Steps A, with Sodium Selenite, cobalt chloride, quadrol and deionized water according to Sodium Selenite: cobalt chloride: quadrol: the ratio of deionized water is the ratio short mix of 2mmol:1mmol:7mL:18mL and stirs, obtains finely dispersed precursor liquid;
Step B, add the hydrazine hydrate (85wt%) of 5.0mL again, stir it is uniformly dispersed;
Step C, reaction system is transferred in the teflon-lined reactor, constant temperature 24h under 140 ℃ of temperature, naturally cooling obtains hydrothermal product;
Step D, with above-mentioned hydrothermal product centrifugation, wash respectively three times with dehydrated alcohol and deionized water;
Step e, with the product after centrifugation at 80 ℃ of vacuum-drying 24h, can obtain the three-dimensional micro-flowers of two cobaltous selenides-quadrol.
Embodiment 4
The preparation of two cobaltous selenides-quadrol micro-flowers:
Steps A, with Sodium Selenite, cobalt chloride, quadrol and deionized water according to Sodium Selenite: cobalt chloride: quadrol: the ratio of deionized water is the ratio short mix of 2mmol:1mmol:7mL:18mL and stirs, obtains finely dispersed precursor liquid;
Step B, add the hydrazine hydrate (85wt%) of 5.0mL again, stir it is uniformly dispersed;
Step C, reaction system is transferred in the teflon-lined reactor, constant temperature 24h under 180 ℃ of temperature, naturally cooling obtains hydrothermal product;
Step D, with above-mentioned hydrothermal product centrifugation, wash respectively three times with dehydrated alcohol and deionized water;
Step e, with the product after centrifugation at 80 ℃ of vacuum-drying 24h, can obtain the three-dimensional micro-flowers of two cobaltous selenides-quadrol.
Embodiment 5
The preparation of two cobaltous selenides-quadrol micro-flowers:
Steps A, Sodium Selenite, cobalt chloride, quadrol and deionized water are according to Sodium Selenite: cobalt chloride: quadrol: the ratio of deionized water is the ratio short mix of 2mmol:1mmol:24mL:1mL and stirs, obtains finely dispersed precursor liquid;
Step B, add the hydrazine hydrate (85wt%) of 5.0mL again, stir it is uniformly dispersed;
Step C, reaction system is transferred in the teflon-lined reactor, constant temperature 24h under 140 ℃ of temperature, naturally cooling obtains hydrothermal product;
Step D, with above-mentioned hydrothermal product centrifugation, wash respectively three times with dehydrated alcohol and deionized water;
Step e, with the product after centrifugation at 80 ℃ of vacuum-drying 24h, can obtain the three-dimensional micro-flowers of two cobaltous selenides-quadrol.
Embodiment 6
The preparation of two cobaltous selenides-quadrol micro-flowers:
Steps A, with Sodium Selenite, cobalt chloride, quadrol and deionized water according to Sodium Selenite: cobalt chloride: quadrol: the ratio of deionized water is the ratio short mix of 2mmol:1mmol:24mL:1mL and stirs, obtains finely dispersed precursor liquid;
Step B, add the hydrazine hydrate (85wt%) of 5.0mL again, stir it is uniformly dispersed;
Step C, reaction system is transferred in the teflon-lined reactor, constant temperature 24h under 180 ℃ of temperature, naturally cooling obtains hydrothermal product;
Step D, with above-mentioned hydrothermal product centrifugation, wash respectively three times with dehydrated alcohol and deionized water;
Step e, with the product after centrifugation at 80 ℃ of vacuum-drying 24h, can obtain the three-dimensional micro-flowers of two cobaltous selenides-quadrol.
Embodiment 7
The preparation of two cobaltous selenides-quadrol micro-flowers:
Steps A, with Sodium Selenite, cobalt chloride, quadrol and deionized water according to Sodium Selenite: cobalt chloride: quadrol: the ratio of deionized water is the ratio short mix of 2mmol:1mmol:18mL:7mL and stirs, obtains finely dispersed precursor liquid;
Step B, add the hydrazine hydrate (85wt%) of 5.0mL again, stir it is uniformly dispersed;
Step C, reaction system is transferred in the teflon-lined reactor, constant temperature 24h under 160 ℃ of temperature, naturally cooling obtains hydrothermal product;
Step D, with above-mentioned hydrothermal product centrifugation, wash respectively three times with dehydrated alcohol and deionized water;
Step e, with the product after centrifugation at 70 ℃ of vacuum-drying 18h, can obtain the three-dimensional micro-flowers of two cobaltous selenides-quadrol.
Claims (8)
1. a hydrothermal method prepares the method for two cobaltous selenides-quadrol micro-flowers, is with Sodium Selenite, and cobalt chloride utilizes hydrothermal method through the reduction of hydrazine hydrate in containing the basic solution of quadrol, is prepared into the micro-flowers of two cobaltous selenides-quadrol.
2. hydrothermal method according to claim 1 prepares the method for two cobaltous selenides-quadrol micro-flowers, it is characterized in that described method is to carry out according to following step:
Steps A, with Sodium Selenite, cobalt chloride, quadrol and deionized water according to Sodium Selenite: cobalt chloride: quadrol: the ratio of deionized water is the ratio short mix of 1～2mmol:1mmol:7～24mL:1～18mL and stirs, obtains finely dispersed precursor liquid;
Step B, in described precursor liquid, add the hydrazine hydrate of 5.0mL, stir it is uniformly dispersed;
Step C, the reaction system of step B gained is transferred in the teflon-lined reactor, constant temperature 12～24h under 140～180 ℃ of temperature, naturally cooling obtains hydrothermal product;
Step D, with the hydrothermal product centrifugation of step C gained, wash respectively three times with dehydrated alcohol and deionized water;
Step e, with the product after centrifugation at 60～80 ℃ of vacuum-drying 12～24h.
3. according to claim 1,2 described hydrothermal methods prepare the method for two cobaltous selenides-quadrol micro-flowers, it is characterized in that described Sodium Selenite, cobalt chloride, quadrol are analytical pure, described hydrazine hydrate weight percent is 85wt%.
4. hydrothermal method according to claim 2 prepares the method for two cobaltous selenides-quadrol micro-flowers, it is characterized in that, reactant is according to Sodium Selenite in the steps A: cobalt chloride: quadrol: the ratio of deionized water is 2mmol:1mmol:22mL:3mL.
5. hydrothermal method according to claim 2 prepares the method for two cobaltous selenides-quadrol micro-flowers, it is characterized in that, the temperature of reacting among the step C is 180 ℃, constant temperature time 24h.
6. the micro-flowers of two cobaltous selenides that are prepared into of described method-quadrol according to claim 1 ~ 5.
7. the micro-flowers of two cobaltous selenides according to claim 6-quadrol is characterized in that micro-flowers is by the about 40 ~ 60nm of thickness, and the nanometer sheet self-assembly of length 1.5 ~ 2 μ m forms.
8. the micro-flowers of two cobaltous selenides according to claim 6-quadrol, the diameter that it is characterized in that micro-flowers is 5 ~ 6 μ m.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104495760A (en) * | 2014-12-02 | 2015-04-08 | 复旦大学 | Cobalt diselenide material having micro/nano three-dimensional multilevel structure as well as preparation method and application thereof |
| CN108821247A (en) * | 2018-05-24 | 2018-11-16 | 北京科技大学 | A kind of kalium ion battery negative electrode material three-dimensional framework shape CoSe2The preparation method of electrode |
| CN113593918A (en) * | 2021-07-27 | 2021-11-02 | 陕西君普新航科技有限公司 | Lamellar CoxSelf-assembly preparation method of Se nanosheet array solar cell electrode |
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| CN101619034B (en) * | 2009-07-28 | 2012-07-25 | 辽宁大学 | Diselenide compound synthesis method |
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| CN108821247A (en) * | 2018-05-24 | 2018-11-16 | 北京科技大学 | A kind of kalium ion battery negative electrode material three-dimensional framework shape CoSe2The preparation method of electrode |
| CN113593918A (en) * | 2021-07-27 | 2021-11-02 | 陕西君普新航科技有限公司 | Lamellar CoxSelf-assembly preparation method of Se nanosheet array solar cell electrode |
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