CN109437298A - A kind of preparation method of Sodium thioantimonite nano material - Google Patents
A kind of preparation method of Sodium thioantimonite nano material Download PDFInfo
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Abstract
The invention discloses a kind of NaSbS2The preparation method of nano material, belongs to technical field of nanometer material preparation, the Na prepared using immersion method3SbS4·9H2O persursor material, safety hazard caused by being avoided using water as solvent because of organic solvent thermal evaporation and the influence to sample purity, feasibility is strong, reaction process is carried out in open-top receptacle, it without expensive autoclave, is not limited by reaction vessel volume, is a kind of mild condition, environmental-friendly, simple cheap process conditions, by heat treatment in argon atmosphere, NaSbS can be obtained in lower temperature2Nano-particle material, crystallinity is preferable, and purity is high, crystallinity is strong, is uniformly dispersed, and pattern is uniform.The raw material that the present invention reacts is easy to get, at low cost, and process equipment is simple, and low energy consumption, and the preparation of presoma is to carry out under normal pressure, and safety is good, and feasibility is strong, thus it is very economical, practical, there is good industrial prospect.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, are related to a kind of NaSbS2The preparation method of nano material, especially
It is related to a kind of using heat treatment assisted solution method preparation NaSbS2The method of nano material.
Background technique
Sodium thioantimonite (NaSbS2) it is a kind of potential p-type semiconductor thermoelectric material based on calculating sifting, it is proved to
It is a kind of very effective solar absorptive material, NaSbS2Energy band Eg=1.5~1.8eV, be slightly larger than solar absorption material
The best energy band (Eg=1.4eV) of material, there is the big absorption coefficient of light (α=10 in visible-range4~105cm-1), make
Use NaSbS2Nano particle obtains 3.18% efficiency in dye-sensitized solar cells, this with use organic metal halogen
The solar battery efficiency of early stage similar type made of compound perovskite is suitable.NaSbS simultaneously2Three kinds of elements used in material
At low cost, rich reserves, nontoxic, this makes NaSbS2As the potential environmentally friendly absorbing material of solar battery.
Nano structural material has quantum size effect, therefore the Semiconductor absorption agent of nanostructure is due to quantum size
Effect forms adjustable band structure, has biggish optical absorption coefficient, while a photon can produce multiple excitons；Separately
Outside, these special structures such as monodimension nanometer material such as nanometer rods, nanotube, nanobelt are in the side such as magnetics, electricity and optics
Face can generate the feature of some novelties.Therefore, the NaSbS of nanostructure is prepared2With very big application value.
The method for the preparation nano material reported at present mainly has sluggish precipitation [1], sol-gel method [2] and hydro-thermal
Method [3], wherein the crystallinity of sluggish precipitation products therefrom is relatively weak and the size of product is unevenly distributed；Sol-gel
Method is long reaction time, and products therefrom post-processing is comparatively laborious；Hydro-thermal method is easy to get, and strong to crystallinity, pattern is special, crystal grain is raw
Long controllable and even size distribution, good dispersion product, keeps reaction more abundant, but needs expensive autoclave, vulnerable to
The limitation of reaction vessel volume, is unfavorable for large-scale promotion.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of low in cost, simple process NaSbS2
The preparation method of nano material, by be heat-treated assisted solution method, be prepared purity is high, crystallinity is good, light absorption is active
NaSbS high, of uniform morphology2Nano particle.
This NaSbS provided by the invention2The preparation method of nano material, comprising the following steps:
(1) vulcanized sodium is dissolved in appropriate solvent, C is madeNaThe sodium sulfide solution of=0.6~1.0mol/L；
(2) sulphur source is added in sodium sulfide solution obtained by step (1) by predetermined ratio, is uniformly mixed, it is molten that mixing is made
Liquid；
(3) antimony source is added in mixed solution obtained by step (2) by setting ratio, is uniformly mixed, suspension is made；
(4) suspension obtained by step (3) is placed in 70~100 DEG C, persistently stirs 1~5h, form bronzing aaerosol solution,
It is stood in room temperature environment, product will be stood and successively washed, dried, Na is obtained3SbS4·9H2O forerunner's product；
(5) by Na3SbS4·9H2O forerunner's product is placed in vacuum tube furnace, is heat-treated 1 in 250~400 DEG C of argon atmospheres
~4h obtains the NaSbS2Nano material.
Preferably, in step (1), the solvent is one of deionized water, distilled water or ultrapure water.
Preferably, the sulphur source is thiocarbamide (CH4N2S), molar ratio n is controlledNa: nS=1:(1.2~1.8)；
The antimony source is Sb2O3Or Sb2S3, control molar ratio nNa: nSb=(2.90~3.15): 1.
Preferably, the sulphur source is thioacetamide (TAA), controls molar ratio nNa: nS=1:(1.1~1.5)；
The antimony source is Sb powder or Sb2S3, control molar ratio nNa: nSb=(2.9~3.3): 1.
Preferably, in step (4), bronzing aaerosol solution stands 8~12h at room temperature.
Preferably, in step (4), product will be stood with dehydrated alcohol centrifuge washing for several times, until the transparent clarification of centrifugate.
Preferably, in step (4), centrifugation product is placed in 50~100 DEG C of vacuum ovens dry 8~12h.
Compared with prior art, advantageous effects of the invention are as follows:
The present invention uses the NaSbS of immersion method preparation2Nano material is avoided using water as solvent because organic solvent heat is steamed
Safety hazard caused by sending out and the influence to sample purity, feasibility is strong, and reaction process is carried out in open-top receptacle, without high
Expensive autoclave, is not limited by reaction vessel volume, is a kind of mild condition, environmental-friendly, simple cheap technique
NaSbS can be obtained in lower temperature in an ar atmosphere by heat treatment in condition2Nano-particle material, crystallinity is preferable,
Purity is high, crystallinity is strong, is uniformly dispersed, and pattern is uniform.
NaSbS of the present invention2The raw material of the preparation method of nano material, the reaction is easy to get, at low cost, process equipment letter
Single, low energy consumption, and the preparation of presoma is to carry out under normal pressure, and safety is good, and feasibility is strong, so very economical, practical, tool
There is good industrial prospect.
Detailed description of the invention
Fig. 1 is Na prepared by the embodiment of the present invention 13SbS4·9H2The XRD diagram of O predecessor.
Fig. 2 is NaSbS prepared by the embodiment of the present invention 12The XRD diagram of nano structural material.
Fig. 3 is Na prepared by the embodiment of the present invention 23SbS4·9H2The XRD diagram of O predecessor.
Fig. 4 is NaSbS prepared by the embodiment of the present invention 22The XRD diagram of nano structural material.
Fig. 5 is NaSbS prepared by the embodiment of the present invention 22The SEM of nano structural material schemes.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, rather than whole embodiments, based on the embodiments of the present invention, ordinary skill
Personnel's every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
Unless otherwise specified, the chemical reagent used is to analyze pure to the present embodiment, is ordinary commercial products or passes through
Conventional means prepare, and the equipment of use is conventional equipment in the art, are the part of inventor in test below
Embodiment:
Embodiment 1
A kind of NaSbS of the embodiment of the present invention2The preparation method of nano material, comprising the following steps:
(1) by Na2S·9H2O is dissolved in appropriate amount of deionized water, and C is madeNaThe sodium sulfide solution of=0.6mol/L；
(2) n is pressedNa: nSThe molar ratio of=1:1.2 is by CH4N2S is added in sodium sulfide solution, is stirred continuously until CH4N2S
It is completely dissolved, mixed solution russet is made；
(3) n is pressedNa: nSbThe molar ratio of=2.9:1 is by Sb2O3It is added in mixed solution obtained by step (2), is uniformly mixed,
Suspension is made；
(4) suspension is placed in 70 DEG C, persistently stirs 1h, form bronzing aaerosol solution, stand 8h in room temperature environment, it will
Centrifugation product for several times, up to the transparent clarification of centrifugate, is placed in 50 DEG C of vacuum drying with dehydrated alcohol centrifuge washing by standing product
Dry 8h, obtains Na in case3SbS4·9H2O forerunner's product, Fig. 1 Na3SbS4·9H2The XRD diagram of O forerunner's product, Cong Tuzhong
As can be seen that forerunner's product is the Na of pure phase3SbS4·9H2O, good crystallinity；
(5) by Na3SbS4·9H2O forerunner's product is placed in vacuum tube furnace, is heat-treated 1h in 250 DEG C of argon atmospheres, obtains
To NaSbS2Nano material, Fig. 2 NaSbS2The XRD diagram of nano material, it can be seen from the figure that the product after heat treatment is pure
Phase NaSbS2, good crystallinity, no miscellaneous phase.
Embodiment 2
A kind of NaSbS of the embodiment of the present invention2The preparation method of nano material, comprising the following steps:
(1) by Na2S·9H2O is dissolved in appropriate amount of deionized water, and C is madeNaThe sodium sulfide solution of=0.8mol/L；
(2) n is pressedNa: nSTAA is added in sodium sulfide solution by the molar ratio of=1:1.3, is stirred continuously until that TAA is complete
Mixed solution is made in dissolution；
(3) n is pressedNa: nSbThe molar ratio of=3.1:1 is by Sb2S3It is added in mixed solution obtained by step (2), is uniformly mixed,
Suspension is made；
(4) suspension is placed in 80 DEG C, persistently stirs 3h, form bronzing aaerosol solution, stand 10h in room temperature environment,
For several times with dehydrated alcohol centrifuge washing by standing product, until the transparent clarification of centrifugate, is placed in 70 DEG C of vacuum for centrifugation product and does
Dry 10h, obtains Na in dry case3SbS4·9H2O forerunner's product, Fig. 3 Na3SbS4·9H2The XRD diagram of O forerunner's product, from figure
In as can be seen that forerunner's product be pure phase Na3SbS4·9H2O, good crystallinity；
(5) by Na3SbS4·9H2O forerunner's product is placed in vacuum tube furnace, is heat-treated 3h in 350 DEG C of argon atmospheres, obtains
To NaSbS2Nano material, Fig. 4 NaSbS2The XRD diagram of nano material, it can be seen from the figure that the product after heat treatment is
NaSbS2, good crystallinity；Fig. 5 is NaSbS prepared by the present invention2SEM spectrum, as can be seen from the figure be heat-treated after
NaSbS2Product is little particle reunion composition, and particle size is 50~70nm.
Embodiment 3
A kind of NaSbS of the embodiment of the present invention2The preparation method of nano material, comprising the following steps:
(1) by Na2S·9H2O is dissolved in appropriate amount of deionized water, and C is madeNaThe sodium sulfide solution of=0.6mol/L；
(2) n is pressedNa: nSTAA is added in sodium sulfide solution by the molar ratio of=1:1.1, is stirred continuously until that TAA is complete
Mixed solution is made in dissolution；
(3) n is pressedNa: nSbSb powder is added in mixed solution obtained by step (2) by the molar ratio of=2.9:1, is uniformly mixed,
Suspension is made；
(4) suspension is placed in 70 DEG C, persistently stirs 1h, form bronzing aaerosol solution, stand 8h in room temperature environment, it will
Centrifugation product for several times, up to the transparent clarification of centrifugate, is placed in 50 DEG C of vacuum drying with dehydrated alcohol centrifuge washing by standing product
Dry 8h, obtains Na in case3SbS4·9H2O forerunner's product；
(5) by Na3SbS4·9H2O forerunner's product is placed in vacuum tube furnace, is heat-treated 1h in 250 DEG C of argon atmospheres, obtains
To NaSbS2Nano material.
Embodiment 4
A kind of NaSbS of the embodiment of the present invention2The preparation method of nano material, comprising the following steps:
(1) by Na2S·9H2O is dissolved in appropriate amount of deionized water, and C is madeNaThe sodium sulfide solution of=1.0mol/L；
(2) n is pressedNa: nSTAA is added in sodium sulfide solution by the molar ratio of=1:1.5, is stirred continuously until that TAA is complete
Mixed solution is made in dissolution；
(3) n is pressedNa: nSbThe molar ratio of=3.3:1 is by Sb2S3It is added in mixed solution obtained by step (2), is uniformly mixed,
Suspension is made；
(4) suspension is placed in 100 DEG C, persistently stirs 5h, form bronzing aaerosol solution, stand 12h in room temperature environment,
For several times with dehydrated alcohol centrifuge washing by standing product, until the transparent clarification of centrifugate, is placed in 100 DEG C of vacuum for centrifugation product and does
Dry 12h, obtains Na in dry case3SbS4·9H2O forerunner's product；
(5) by Na3SbS4·9H2O forerunner's product is placed in vacuum tube furnace, is heat-treated 4h in 400 DEG C of argon atmospheres, obtains
To NaSbS2Nano material.
Embodiment 5
A kind of NaSbS of the embodiment of the present invention2The preparation method of nano material, comprising the following steps:
(1) by Na2S·9H2O is dissolved in appropriate distilled water, and C is madeNaThe sodium sulfide solution of=0.8mol/L；
(2) n is pressedNa: nSThe molar ratio of=1:1.6 is by CH4N2S is added in sodium sulfide solution, is stirred continuously until CH4N2S
It is completely dissolved, mixed solution russet is made；
(3) n is pressedNa: nSbThe molar ratio of=3.0:1 is by Sb2S3It is added in mixed solution obtained by step (2), is uniformly mixed,
Suspension is made；
(4) suspension is placed in 80 DEG C, persistently stirs 3h, form bronzing aaerosol solution, stand 10h in room temperature environment,
For several times with dehydrated alcohol centrifuge washing by standing product, until the transparent clarification of centrifugate, is placed in 70 DEG C of vacuum for centrifugation product and does
Dry 10h, obtains Na in dry case3SbS4·9H2O forerunner's product；
(5) by Na3SbS4·9H2O forerunner's product is placed in vacuum tube furnace, is heat-treated 2h in 300 DEG C of argon atmospheres, obtains
To NaSbS2Nano material.
Embodiment 6
A kind of NaSbS of the embodiment of the present invention2The preparation method of nano material, comprising the following steps:
(1) by Na2S·9H2O is dissolved in appropriate ultrapure water, and C is madeNaThe sodium sulfide solution of=1.0mol/L；
(2) n is pressedNa: nSThe molar ratio of=1:1.8 is by CH4N2S is added in sodium sulfide solution, is stirred continuously until CH4N2S
It is completely dissolved, mixed solution russet is made；
(3) n is pressedNa: nSbThe molar ratio of=3.15:1 is by Sb2S3It is added in mixed solution obtained by step (2), mixing is equal
It is even, suspension is made；
(4) suspension is placed in 100 DEG C, persistently stirs 5h, form bronzing aaerosol solution, stand 12h in room temperature environment,
For several times with dehydrated alcohol centrifuge washing by standing product, until the transparent clarification of centrifugate, is placed in 100 DEG C of vacuum for centrifugation product and does
Dry 12h, obtains Na in dry case3SbS4·9H2O forerunner's product；
(5) by Na3SbS4·9H2O forerunner's product is placed in vacuum tube furnace, is heat-treated 4h in 400 DEG C of argon atmospheres, obtains
To NaSbS2Nano material.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example.To those of ordinary skill in the art, obtained improvement and change in the case where not departing from the technology of the present invention concept thereof
It changes and also should be regarded as protection scope of the present invention.
Bibliography
[1]Wei Zhang,Shaoyi Jia,Studies of the magnetic field intensity on
the synthesis of chitosan-coated magnetite nanocomposites by co-precipitation
method[J],Materials Science and Engineering:C,2012,32(2):381-384.
[2]Mohammad Hossein Habibi,Bahareh Karimi,Preparation of
nanostructure CuO/ZnO mixed oxide by sol–gel thermal decomposition of a
CuCO3and ZnCO3:TG,DTG,XRD,FESEM and DRS investigations[J],Journal of
Industrial and Engineering Chemistry:2014,20(3):925-929.
[3]D.M.Fernandes,R.Silva,Synthesis and characterization of ZnO,CuO
and a mixed Zn and Cu oxide[J],Materials Chemistry and Physics:2009,115(1):
110-115。
Claims (7)
1. a kind of NaSbS2The preparation method of nano material, which comprises the following steps:
(1) vulcanized sodium is dissolved in appropriate solvent, C is madeNaThe sodium sulfide solution of=0.6~1.0mol/L；
(2) sulphur source is added in sodium sulfide solution obtained by step (1) by predetermined ratio, is uniformly mixed, mixed solution is made；
(3) antimony source is added in mixed solution obtained by step (2) by setting ratio, is uniformly mixed, suspension is made；
(4) suspension obtained by step (3) is placed in 70~100 DEG C, persistently stirs 1~5h, bronzing aaerosol solution is formed, in room
Warm environment is stood, and will be stood product and is successively washed, dried, obtains Na3SbS4·9H2O forerunner's product；
(5) by Na3SbS4·9H2O forerunner's product is placed in vacuum tube furnace, in 250~400 DEG C of argon atmospheres be heat-treated 1~
4h obtains the NaSbS2Nano material.
2. NaSbS according to claim 12The preparation method of nano material, which is characterized in that in step (1), the solvent
For one of deionized water, distilled water or ultrapure water.
3. NaSbS according to claim 12The preparation method of nano material, which is characterized in that the sulphur source is thiocarbamide, control
Molar ratio nNa: nS=1:(1.2~1.8)；
The antimony source is Sb2O3Or Sb2S3, control molar ratio nNa: nSb=(2.90~3.15): 1.
4. NaSbS according to claim 12The preparation method of nano material, which is characterized in that the sulphur source is thioacetyl
Amine controls molar ratio nNa: nS=1:(1.1~1.5)；
The antimony source is Sb powder or Sb2S3, control molar ratio nNa: nSb=(2.9~3.3): 1.
5. NaSbS according to claim 12The preparation method of nano material, which is characterized in that in step (4), bronzing is outstanding
Floating solution stands 8~12h at room temperature.
6. NaSbS according to claim 12The preparation method of nano material, which is characterized in that in step (4), produced standing
Object with dehydrated alcohol centrifuge washing for several times, until the transparent clarification of centrifugate.
7. NaSbS according to claim 12The preparation method of nano material, which is characterized in that in step (4), centrifugation is produced
Object is placed in 50~100 DEG C of vacuum ovens dry 8~12h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110155960A (en) * | 2019-06-04 | 2019-08-23 | 淮北师范大学 | A kind of convenient and efficient preparation NaSbS2Method |
| CN114715936A (en) * | 2022-04-18 | 2022-07-08 | 鸡西市唯大新材料科技有限公司 | Negative electrode NaSbS of lithium or sodium ion battery2Preparation method of @ C composite material |
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| CH605402A5 (en) * | 1974-10-28 | 1978-09-29 | Zellweger Uster Ag | Stable sulphide solns. prepn. using thiol complex |
| EP0806487A1 (en) * | 1996-05-06 | 1997-11-12 | ENGITEC S.p.A. | Extraction of antimony from sulfide ores by alkaline leaching, recovery of elemental sulfur and electrowinning antimony from fluoborate solution |
| CN105845976A (en) * | 2016-04-12 | 2016-08-10 | 燕山大学 | Tetragonal phase Na3SbS4 sodium fast ion conductor and preparation method thereof |
| CN108163890A (en) * | 2017-12-29 | 2018-06-15 | 广西生富锑业科技股份有限公司 | A kind of preparation method of nanometer sulfo antimony acid antimony |
| CN108455669A (en) * | 2018-04-23 | 2018-08-28 | 长沙烨星锑业有限公司 | A kind of preparation method of schlippe's salt |
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| CH605402A5 (en) * | 1974-10-28 | 1978-09-29 | Zellweger Uster Ag | Stable sulphide solns. prepn. using thiol complex |
| EP0806487A1 (en) * | 1996-05-06 | 1997-11-12 | ENGITEC S.p.A. | Extraction of antimony from sulfide ores by alkaline leaching, recovery of elemental sulfur and electrowinning antimony from fluoborate solution |
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| CN110155960A (en) * | 2019-06-04 | 2019-08-23 | 淮北师范大学 | A kind of convenient and efficient preparation NaSbS2Method |
| CN114715936A (en) * | 2022-04-18 | 2022-07-08 | 鸡西市唯大新材料科技有限公司 | Negative electrode NaSbS of lithium or sodium ion battery2Preparation method of @ C composite material |
| CN114715936B (en) * | 2022-04-18 | 2023-10-03 | 鸡西市唯大新材料科技有限公司 | Negative electrode NaSbS of lithium or sodium ion battery 2 Preparation method of @ C composite material |
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