CN101823769A - Method for preparing ternary FexCo1-xS2 powder - Google Patents
Method for preparing ternary FexCo1-xS2 powder Download PDFInfo
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- CN101823769A CN101823769A CN201010168154A CN201010168154A CN101823769A CN 101823769 A CN101823769 A CN 101823769A CN 201010168154 A CN201010168154 A CN 201010168154A CN 201010168154 A CN201010168154 A CN 201010168154A CN 101823769 A CN101823769 A CN 101823769A
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Abstract
The invention discloses a method for preparing ternary FexCo1-xS2 powder through hydrothermal synthesis. The method is realized through the following technological processes that: analytically pure FeCl2.4H2O, CoCl2.6H2O and Na2S2O3.5H2O are dissolved in 35ml of deionized water according to molar ratio of 1:19:40 to 3:17:40, and the obtained mixture is agitated for 15min in a magneton agitator to enable reactants to be fully dissolved and evenly mixed; the mixed solution is transferred to a reaction kettle with capacity of 50ml, the reaction kettle is closed and is placed in an incubator with temperature of 140 DEG C for reaction, the reaction duration is 24h and the reaction kettle is taken out and is naturally cooled to room temperature; sediments at the bottom of the reaction kettle are filtered, absolute ethyl alcohol (CH3CH2OH) and deionized water are used for washing the obtained product for times, carbon disulfide (CS2) is used for washing S impurities in the product and finally the product is vacuum-dried for 6 hours at 60 DEG C. The ternary FexCo1-xS2 powder prepared through the method is formed by micron particles with pyrite structures. The invention has the advantages that the method is simple, the cost is low, the pollution is low and the industrialized mass production can be realized.
Description
Technical field
The invention belongs to the synthetic field of material, is a kind of hydrothermal growth ternary Fe
xCo
1-xS
2The method of powder.
Background technology
Pyrite type CoS
2Have higher photoabsorption coefficient, semi-metal ferromegnetism, high spin polarization(SP), have important application prospects in fields such as catalysis, photovoltaic, electronics.Pyrite type FeS
2Also because of its suitable energy gap (E
g≈ 0.95eV) and higher photoabsorption coefficient (during λ＜700nm, α ≈ 105cm
-1), cause the extensive concern of Chinese scholars in novel solar battery material application facet.The a few thing group is attempted preparation ternary Fe
xCo
1-xS
2Crystal is in the hope of obtaining the material that physico-chemical property is better than Fe, Co binary compound.As S.W.Lehner group with the vapor transportation method adulterated pyrite type of the Co FeS that grown
2Film, the result shows that the gained film is the n N-type semiconductorN, has less impedance and bigger carrier concentration, consults J.Cryst.Growth2006 the 286th phase 306-317 page or leaf.A.M.Abd E1 Halim group is with Co
2-Galvanic deposit is to FeS
2(100) CoS that grown on the substrate
2, obtain Co in the two-phase intersection
xFe
1-xS
2, consult Electrochim.Acta the 47th phase of calendar year 2001 2615-2623 page or leaf.P.D í az-Chao group at first on glass-based hot evaporation obtain Fe/Co double-level-metal film, then Fe/Co double-level-metal film is placed the hot sulfurization of vitreosil Glass tubing, prepared Co Doped n-type FeS
2Film is consulted 2008 the 516th phase 7116-7119 pages or leaves of Thin Solid Films.
Preparation ternary compound Fe
xCo
1-xS
2Report actually rare.The ternary compound for preparing in the above-mentioned report is Co doping pyrite FeS
2, the lower and skewness of the concentration of Co.The present invention is at next step synthetic Fe of thermal and hydric environment
xCo
1-xS
2The method of powder.Do not prepare ternary compound Fe at present in this way
xCo
1-xS
2Relevant report.Present method is simple relatively, and cost is low, pollutes and lacks, and controllable parameter is many, has certain value in the industrial production application facet.
Summary of the invention
The object of the present invention is to provide a kind of hydrothermal growth Fe
xCo
1-xS
2The method of powder.
The present invention realizes by following technological process:
With mol ratio is 1: 19: 40-3: dissolve in the 35ml deionized water in 17: 40 source of iron, cobalt source and sulphur source, stirs 15min through the magneton agitator and make reactant fully dissolve and uniform mixing.Mixed solution is moved in the 50ml reactor, and closed reactor is placed in 140 ℃ of thermostat containers, and the reaction times is 24h, naturally cools to room temperature behind the taking-up reactor.Leach throw out at the bottom of the still, with dehydrated alcohol (CH
3CH
2OH) and washed with de-ionized water for several times, and with dithiocarbonic anhydride (CS
2) S impurity in the flush away product, 60 ℃ of following vacuum-dryings 6 hours, gained black sample was Fe at last
xCo
1-xS
2Powder.
Described source of iron is Iron dichloride tetrahydrate (FeCl
24H
2O), the cobalt source is cobalt chloride hexahydrate (CoCl
26H
2O), the sulphur source is Sodium Thiosulfate Pentahydrate (Na
2S
2O
35H
2O), used reagent is analytical pure in the building-up process.
Described reactor overcoat is the flange plate type kettle that the stainless material of high strength, low creep is made, and liner is made by the tetrafluoroethylene of acid and alkali-resistance, high temperature high voltage resistant, and thermostat container is the adjustable process furnace of resistance-type temperature.
The Fe that the present invention prepares
xCo
1-xS
2Powder is the pyrite structure, and its thing mutually as shown in Figure 1.Fig. 2 is the variation broken line graphs of peak position angular deflection amount Δ 2 θ at (211) peak and (210) peak in the XRD diffraction peak of product with source of iron concentration ratio a in the initial reactant, a be in the initial reactant on the source of iron concentration ratio source of iron and cobalt source concentration with, promptly
Fig. 3 is the shape appearance figure of 1: 19: 40 products obtained therefrom for source of iron, cobalt source and sulphur source mol ratio in the initial reactant.
Description of drawings
Fig. 1 embodiment 1,2,3 product F e
xCo
1-xS
2XRD figure spectrum and standard C oS
2Diffraction peak.
Fig. 2 embodiment 1,2,3 product F e
xCo
1-xS
2The XRD diffraction peak in peak position angular deflection amount Δ 2 θ at (210) peak and (211) peak with the variation broken line graph of source of iron mol ratio a in the initial reactant.
Fig. 3 embodiment 1 product F e
xCo
1-xS
2The scanning electron microscope picture.
Embodiment
Embodiment 1
Be in molar ratio 1: 19: 40 with analytically pure FeCl
24H
2O, CoCl
26H
2O and Na
2S
2O
35H
2O dissolves in the 35ml deionized water, stirs 15min through the magneton agitator and makes reactant fully dissolve and uniform mixing.Mixed solution is moved in the 50ml reactor, and closed reactor is placed in 140 ℃ of thermostat containers, and the reaction times is 24h, naturally cools to room temperature behind the taking-up reactor.Leach throw out at the bottom of the still, with dehydrated alcohol (CH
3CH
2OH) and washed with de-ionized water for several times, and with dithiocarbonic anhydride (CS
2) S impurity in the flush away product, at last 60 ℃ of following vacuum-dryings 6 hours.Products obtained therefrom is a black powder, and Fig. 1 a is its XRD spectra.Spectrogram shows, product tool pyrite structure, and each diffraction peak peak position is with respect to standard C oS
2The peak is offset to high angular direction.The skew of diffraction peak is because the Fe atomic radius is less, when its alternative Co atom enters CoS
2When lattice participated in into key, due to lattice dwindled, this had proved that product is ternary pyrite Fe
xCo
1-xS
2Fig. 2 shows that (210) peak in the diffraction peak of product is respectively 0.105 degree and 0.19 degree with peak position angular deflection amount Δ 2 θ at (211) peak.The pattern of product is the micron particle of reuniting mutually as shown in Figure 3, and particle diameter is 1-2 μ m.
Embodiment 2
Be in molar ratio 2: 18: 40 with analytically pure FeCl
24H
2O, CoCl
26H
2O and Na
2S
2O
35H
2O dissolves in the 35ml deionized water, stirs 15min through the magneton agitator and makes reactant fully dissolve and uniform mixing.Mixed solution is moved in the 50ml reactor, and closed reactor is placed in 140 ℃ of thermostat containers, and the reaction times is 24h, naturally cools to room temperature behind the taking-up reactor.Leach throw out at the bottom of the still, with dehydrated alcohol (CH
3CH
2OH) and washed with de-ionized water for several times, and with dithiocarbonic anhydride (CS
2) S impurity in the flush away product, at last 60 ℃ of following vacuum-dryings 6 hours.Products obtained therefrom is a black powder, and Fig. 1 b is its XRD spectra.Spectrogram shows, product tool pyrite structure, and each diffraction peak peak position is with respect to standard C oS
2The peak is offset to high angular direction, and visible product is ternary pyrite Fe
xCo
1-xS
2Fig. 2 shows that (210) peak in the XRD diffraction peak of product is respectively 0.164 degree and 0.253 degree with peak position angular deflection amount Δ 2 θ at (211) peak.Product pattern and embodiment 1 product are similar, and its shape appearance figure slightly.
Embodiment 3
Be in molar ratio 3: 17: 40 with analytically pure FeCl
24H
2O, CoCl
26H
2O and Na
2S
2O
35H
2O dissolves in the 35ml deionized water, stirs 15min through the magneton agitator and makes reactant fully dissolve and uniform mixing.Mixed solution is moved in the 50ml reactor, and closed reactor is placed in 140 ℃ of thermostat containers, and the reaction times is 24h, naturally cools to room temperature behind the taking-up reactor.Leach throw out at the bottom of the still, with dehydrated alcohol (CH
3CH
2OH) and washed with de-ionized water for several times, and with dithiocarbonic anhydride (CS
2) S impurity in the flush away product, at last 60 ℃ of following vacuum-dryings 6 hours.Products obtained therefrom is a black powder, and Fig. 1 c is its XRD spectra.Spectrogram shows, product tool pyrite structure, and each diffraction peak peak position is with respect to standard C oS
2The peak is offset to high angular direction, and visible product is ternary pyrite Fe
xCo
1-xS
2Fig. 2 shows that (210) peak in the XRD diffraction peak of product is respectively 0.224 degree and 0.294 degree with peak position angular deflection amount Δ 2 θ at (211) peak.Product pattern and embodiment 1 product are similar, and its shape appearance figure slightly.
Claims (4)
1. hydrothermal growth ternary Fe
xCo
1-xS
2The method of powder, it is characterized in that realizing: be 1: 19 in molar ratio: 40-1: analytically pure source of iron, cobalt source and sulphur source dissolved in the 35ml deionized water in 19: 40, stir 15min through the magneton agitator and make reactant fully dissolve and uniform mixing by following technological process.Mixed solution is moved in the 50ml reactor, and closed reactor is placed in 140 ℃ of thermostat containers, and the reaction times is 24h, naturally cools to room temperature behind the taking-up reactor.Leach throw out at the bottom of the still, with dehydrated alcohol (CH
3CH
2OH) and washed with de-ionized water for several times, and with dithiocarbonic anhydride (CS
2) S impurity in the flush away product, at last 60 ℃ of following vacuum-dryings 6 hours.
2. the method for claim 1 is characterized in that, used growing apparatus is a reactor.
3. the method for claim 1 is characterized in that, described source of iron is FeCl
24H
2O, the cobalt source is CoCl
26H
2O, the sulphur source is Na
2S
2O
35H
2O.
4. the method for claim 1 is characterized in that, described thermostat container is for adding the adjustable process furnace of resistance-type temperature.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103938265A (en) * | 2014-05-13 | 2014-07-23 | 东北大学 | Method for preparing strawberry-shaped pyrite crystal under hydrothermal condition |
| EP2897202A1 (en) * | 2014-01-17 | 2015-07-22 | Greatbatch Ltd. | New high capacity cathode material with improved rate capability performance |
| CN107026256A (en) * | 2016-08-12 | 2017-08-08 | 中国科学院过程工程研究所 | A kind of thermal cell positive electrode FexCo1‑xS2Powder and preparation method thereof |
| CN107857305A (en) * | 2017-12-20 | 2018-03-30 | 南京隆信达新材料科技有限公司 | Ternary FexCo1‑xS2The synthetic method of powder |
| CN108069461A (en) * | 2017-12-20 | 2018-05-25 | 南京隆信达新材料科技有限公司 | The synthetic method of cobalt disulfide powder |
| CN109052486A (en) * | 2018-07-02 | 2018-12-21 | 中南大学 | A kind of thermal cell single-phase positive electrode and preparation method thereof, application |
| CN109659147A (en) * | 2018-12-19 | 2019-04-19 | 哈尔滨师范大学 | One kind preparing FeCo based on foam nickel base2S4The method of nano-chip arrays |
| US10581075B2 (en) | 2014-01-17 | 2020-03-03 | Greatbatch Ltd. | Method for providing a high capacity cathode material with improved rate capability performance |
-
2010
- 2010-05-11 CN CN201010168154A patent/CN101823769A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2897202A1 (en) * | 2014-01-17 | 2015-07-22 | Greatbatch Ltd. | New high capacity cathode material with improved rate capability performance |
| US10581075B2 (en) | 2014-01-17 | 2020-03-03 | Greatbatch Ltd. | Method for providing a high capacity cathode material with improved rate capability performance |
| CN103938265A (en) * | 2014-05-13 | 2014-07-23 | 东北大学 | Method for preparing strawberry-shaped pyrite crystal under hydrothermal condition |
| CN107026256A (en) * | 2016-08-12 | 2017-08-08 | 中国科学院过程工程研究所 | A kind of thermal cell positive electrode FexCo1‑xS2Powder and preparation method thereof |
| CN107026256B (en) * | 2016-08-12 | 2020-07-07 | 中国科学院过程工程研究所 | Thermal battery anode material FexCo1-xS2Powder and preparation method thereof |
| CN107857305A (en) * | 2017-12-20 | 2018-03-30 | 南京隆信达新材料科技有限公司 | Ternary FexCo1‑xS2The synthetic method of powder |
| CN108069461A (en) * | 2017-12-20 | 2018-05-25 | 南京隆信达新材料科技有限公司 | The synthetic method of cobalt disulfide powder |
| CN109052486A (en) * | 2018-07-02 | 2018-12-21 | 中南大学 | A kind of thermal cell single-phase positive electrode and preparation method thereof, application |
| CN109052486B (en) * | 2018-07-02 | 2019-08-09 | 中南大学 | A kind of thermal cell single-phase positive electrode and preparation method thereof, application |
| CN109659147A (en) * | 2018-12-19 | 2019-04-19 | 哈尔滨师范大学 | One kind preparing FeCo based on foam nickel base2S4The method of nano-chip arrays |
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Application publication date: 20100908 |