CN101643938B - Method for preparing submicron grade square pipe-shaped Sb2Se3 - Google Patents
Method for preparing submicron grade square pipe-shaped Sb2Se3 Download PDFInfo
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- CN101643938B CN101643938B CN2009100347711A CN200910034771A CN101643938B CN 101643938 B CN101643938 B CN 101643938B CN 2009100347711 A CN2009100347711 A CN 2009100347711A CN 200910034771 A CN200910034771 A CN 200910034771A CN 101643938 B CN101643938 B CN 101643938B
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- Prior art keywords
- pipe
- square pipe
- submicron grade
- shaped
- submicron
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- 238000000034 method Methods 0.000 title abstract description 12
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000001291 vacuum drying Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000013019 agitation Methods 0.000 claims description 7
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 229910003424 Na2SeO3 Inorganic materials 0.000 abstract 1
- FAPDDOBMIUGHIN-UHFFFAOYSA-K antimony trichloride Chemical compound Cl[Sb](Cl)Cl FAPDDOBMIUGHIN-UHFFFAOYSA-K 0.000 abstract 1
- 235000011187 glycerol Nutrition 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 235000015921 sodium selenite Nutrition 0.000 abstract 1
- 239000011781 sodium selenite Substances 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- -1 nanometer rod Substances 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- 239000002070 nanowire Substances 0.000 description 2
- 230000000243 photosynthetic effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000004098 selected area electron diffraction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
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Abstract
The invention relates to a method for preparing submicron grade square pipe-shaped Sb2Se3. The method comprises the following steps: adding SbCl3 and Na2SeO3 with the substance amount ratio of 2:3 at room temperature into glycerin liquid, magnetically stirring for 0.5-2 hours and placing the mixture into a microwave reaction vessel to be heated for 8-10 min; cooling and then alternately washing the product by alcohol and water repeatedly; drying in a vacuum drying oven and then acquiring a submicron grade Sb2Se3 square pipe. The acquired Sb2Se3 is the submicron grade square pipe, has the pipe length of 10-20 microns, the pipe opening width of 0.5-1 micron and the pipe wall thickness of 100-200 nm and grows along the (001) direction. The method for preparing the Sb2Se3 submicron grade square pipe is simple and convenient, has simple used equipment and short time consumption, can realize large-scale preparation in short time and is convenient for industrialized production.
Description
Technical field
The invention belongs to the synthetic field of inorganic nano material, be specifically related to submicron order Sb2Se3 semiconductor material of a kind of square pipe-shaped pattern and preparation method thereof.
Background technology
Sb
2Se
3Be a kind of direct band-gap semicondictor material, have laminate structure, belong to rhombic system.Because it has excellent photoelectric properties, high thermoelectric transformation efficiency, and transition effects are subjected to increasing attention, and are widely used in light selectivity and decorative coating, thermoelectric refrigeration and photochemistry device, and field such as initial storage transfer equipment.Traditionally, Sb
2Se
3Be under hot conditions, to react synthetic by simple substance Sb and Se.Now, many wet chemical methods are applied to synthetic Sb
2Se
3Nanocrystalline, as methods such as hydro-thermal, solvent thermal.Many one dimension Sb
2Se
3Nanocrystalline nano wire, nanometer rod, nano belt, the micron tube of comprising has been successfully synthesized.Because have outstanding mechanical property and unique electron motion characteristic, nano tubular structure is subjected to scientific circles and pays close attention to widely.Other one-dimentional structures are because nanotube has unique cavernous structure, more difficult synthetic relatively.Former study shows, the material that can synthesize tubular structure need have and is similar to the same laminate structure of graphite.Though Sb
2Se
3Also have laminate structure, but few people successfully synthesize tubulose Sb so far
2Se
32002, people such as the Xie Yi Sb that reported for work
2Se
3Microtubule.They adopt solvent-thermal method, with SbCl
3With the Se powder be raw material, in ethanolic soln, 180 ℃ of down reactions 7 days successfully synthesize Sb
2Se
3Tubular structure (Xiuwen Zheng, Yi Xie, Liying Zhu, Xuchuan Jiang, Yunbo Jia, Wenhai Song, and Yuping Sun.Inorg.Chem.2002,41 (3), 455-461.).The synthetic Sb of institute
2Se
3Pipe is a micron order four directions pipe, pipe range 5-10mm, the wide 10-20 μ of mouth of pipe m, thick 5-10 μ m.Because institute's synthetic micron order four directions pipe is oversize, can not present the excellent properties of nanotube, its application is subjected to certain limitation.Simultaneously because the reaction times is long, output is low excessively, has also influenced its industrialization greatly.The present invention adopts microwave-assisted poly-hydroxy method, with SbCl
3And Na
2SeO
3Being raw material, is solvent and reductive agent with the glycerol, and microwave heating 8-10min successfully synthesizes submicron grade square tubular construction Sb
2Se
3The synthetic Sb of institute
2Se
3Pipe, pipe range 10-20 μ m, the wide 0.5-1 μ of mouth of pipe m, thickness of pipe 100-200nm is along the growth of (001) direction.Size is near nano level, much smaller than bibliographical information.This method is simple, consuming time extremely short, is convenient to suitability for industrialized production.
Summary of the invention
Technical problem to be solved by this invention provides a kind of submicron grade square pipe-shaped Sb
2Se
3Pipe, and simple fast synthetic this submicron grade square pipe-shaped Sb
2Se
3The method of pipe.
Submicron grade square pipe-shaped Sb of the present invention
2Se
3, the monocrystalline of genus rhombic system, unit cell parameters is a=11.633
B=11.78
C=3.985
Its structure is the submicron grade square structure, pipe range 10-20 μ m, and the wide 0.5-1 μ of mouth of pipe m, thickness of pipe 100-200nm is along the growth of (001) direction.
Prepare this Sb
2Se
3The method of pipe is: at first, at room temperature be 2: 3 SbCl with weight ratio
3And Na
2SeO
3Join in the glycerol, magnetic agitation 0.5-2 hour, put into microwave reactor and heat 8-10min; After the cooling, product is alternately cleaned repeatedly with the second alcohol and water, in vacuum drying oven, promptly got submicron order Sb after the drying
2Se
3The four directions pipe.
As above-mentioned preparation method's further improvement, the operating frequency of microwave reactor is preferably 2.45GHz, power is 800W.And microwave reactor preferably adopts 40s work, the circulation heating mode that 60s stops.
Utilize measurement of ultraviolet-visible spectrophotometer gained Sb
2Se
3The energy gap of submicron four directions pipe is 1.161eV, with Sb in the document
2Se
3The energy gap numerical value of nanostructure such as nanometer rod, nano wire is consistent.The Sb of this explanation present method gained
2Se
3The submicron grade square pipe can show the performance of certain nano structural material too.
The invention has the beneficial effects as follows:
(1) Sb of the present invention
2Se
3Regular, the big or small homogeneous of submicron grade square tubular construction, size is reported in document near nano level;
(2) the energy gap measured value is 1.161eV, can show the performance of certain nano structural material;
(3) Sb of the present invention's proposition
2Se
3The preparation method of submicron grade square pipe is easy, and equipment used is simple, and is consuming time extremely short, can realize a large amount of preparations in the short period of time, is convenient to suitability for industrialized production.
Description of drawings
Fig. 1 is by being synthesized Sb
2Se
3XRD figure spectrum.
Fig. 2 is the synthetic Sb of microwave heating 8min institute
2Se
3The stereoscan photograph of submicron grade square pipe.
Fig. 3 is the synthetic Sb of microwave heating 10min institute
2Se
3The stereoscan photograph of submicron grade square pipe.
Fig. 4 is Sb
2Se
3The transmission electron microscope photo of submicron grade square pipe.
Fig. 5 is Sb
2Se
3The selected area electron diffraction photo of submicron grade square pipe.
Fig. 6 is Sb
2Se
3The diffuse-reflectance collection of illustrative plates of submicron grade square pipe.
Fig. 7 for calculate by the diffuse scattering collection of illustrative plates the collection of illustrative plates of calculating energy gap.
Embodiment
Further specify the present invention below in conjunction with drawings and Examples, wherein the part preparation condition only is the explanation as typical case, is not limitation of the invention.
Embodiment 1
Under the room temperature, with load weighted 0.5mmol SbCl
3With 0.75mmol Na
2SeO
3, adding fills in the container of 15mL glycerol liquid, and magnetic agitation is after 0.5 hour, and putting into operating frequency is that 2.45GHz, power are the microwave reactor of 800W, and reactor adopts 40s work, the circulation heating mode that 60s stops, microwave heating 8min.After the cooling, alternately clean dry 12h under 60 ℃ in the vacuum drying oven repeatedly with the second alcohol and water.
Fig. 1 is by being synthesized Sb
2Se
3XRD figure spectrum.All diffraction peaks and lattice parameter are a=11.633
B=11.780
And=3.985
Rhombic system Sb
2Se
3The diffraction peak unanimity.The synthetic Sb of institute of the present invention is described
2Se
3Be pure phase.
Fig. 2 is microwave heating 8min synthetic Sb
2Se
3The field emission scanning electron microscope photo of submicron grade square pipe.From the photo synthetic Sb of institute as can be seen
2Se
3Pipe is tetragonal, pipe range 10-20 μ m, the wide 0.5-1 μ of mouth of pipe m, thickness of pipe 100-200nm.
Fig. 4 is Sb
2Se
3The transmission electron microscope photo of submicron grade square pipe.Can confirm synthetic Sb of the present invention from photo
2Se
3Be tubular structure, and present tetragonal.
Fig. 5 is Sb
2Se
3The constituency electronics long drive photo of submicron grade square pipe.Diffraction pattern presents regular point diffraction to be arranged, and the synthetic Sb of institute is described
2Se
3The submicron grade square pipe is a monocrystalline.Demarcate diffraction pattern, find that crystal is along the growth of (001) direction.
Fig. 6 is Sb
2Se
3The diffuse-reflectance collection of illustrative plates of submicron grade square pipe.Collection of illustrative plates is extrapolated Fig. 7 thus, by the slope of Fig. 7 cut-off line part, synthesize Sb
2Se
3The energy gap of pipe is 1.161eV.
Under the room temperature, with load weighted 0.5mmol SbCl
3With 0.75mmol Na
2SeO
3, adding fills in the container of 15mL glycerol solution, and magnetic agitation is after 1 hour, and putting into operating frequency is that 2.45GHz, power are the microwave reactor of 800W, and reactor adopts 40s work, the circulation heating mode that 60s stops, microwave heating 10min.After the cooling, alternately clean dry 12h under 60 ℃ in the vacuum drying oven repeatedly with the second alcohol and water.
Fig. 3 is microwave heating 10min synthetic Sb
2Se
3The field emission scanning electron microscope photo of submicron grade square pipe.From the photo synthetic Sb of institute as can be seen
2Se
3Pipe size dimension and the synthetic Sb of microwave heating 8min institute
2Se
3Pipe is consistent, but has cracked slightly.
Embodiment 3
Under the room temperature, with load weighted 0.5mmol SbCl
3With 0.75mmol Na
2SeO
3, adding fills in the container of 15mL glycerol solution, and magnetic agitation is after 1 hour, and putting into operating frequency is that 2.45GHz, power are the microwave reactor of 800W, and reactor adopts 40s work, the circulation heating mode that 60s stops, microwave heating 9min.After the cooling, alternately clean repeatedly with the second alcohol and water, dry 12h under 60 ℃ promptly obtains Sb in the vacuum drying oven
2Se
3The submicron grade square pipe.
Under the room temperature, with load weighted 0.5mmol SbCl
3With 0.75mmol Na
2SeO
3, adding fills in the container of 20mL glycerol solution, and magnetic agitation is after 1 hour, and putting into operating frequency is that 2.45GHz, power are the microwave reactor of 800W, and reactor adopts 40s work, the circulation heating mode that 60s stops, microwave heating 10min.After the cooling, alternately clean repeatedly with the second alcohol and water, dry 12h under 60 ℃ promptly obtains Sb in the vacuum drying oven
2Se
3The submicron grade square pipe.
Embodiment 5
Under the room temperature, with load weighted 0.2mmol SbCl
3With 0.3mmol Na
2SeO
3, adding fills in the container of 20mL glycerol solution, and magnetic agitation is after 1 hour, and putting into operating frequency is that 2.45GHz, power are the microwave reactor of 800W, and reactor adopts 40s work, the circulation heating mode that 60s stops, microwave heating 10min.After the cooling, alternately clean repeatedly with the second alcohol and water, dry 12h under 60 ℃ promptly obtains Sb in the vacuum drying oven
2Se
3The submicron grade square pipe.
Claims (3)
1. submicron grade square pipe-shaped Sb
2Se
3The preparation method, this submicron grade square pipe-shaped Sb
2Se
3Belong to the monocrystalline of rhombic system, unit cell parameters is a=11.633
B=11.78
C=3.985
Its structure is the submicron grade square structure, pipe range 10-20 μ m, and the wide 0.5-1 μ of mouth of pipe m, thickness of pipe 100-200nm along the growth of (001) direction, is characterized in that this submicron grade square pipe-shaped Sb of preparation
2Se
3May further comprise the steps: at first, at room temperature be 2: 3 SbCl the amount of substance ratio
3And Na
2SeO
3Join in the glycerol liquid, magnetic agitation 0.5-2 hour, put into microwave reactor and heat 8-10min; After the cooling, product is alternately cleaned repeatedly with the second alcohol and water, in vacuum drying oven, promptly got submicron order Sb after the drying
2Se
3The four directions pipe.
2. submicron grade square pipe-shaped Sb according to claim 1
2Se
3The preparation method, the operating frequency that it is characterized in that microwave reactor is that 2.45GHz, power are 800W.
3. submicron grade square pipe-shaped Sb according to claim 1 and 2
2Se
3The preparation method, it is characterized in that microwave reactor adopts 40s work, the circulation heating mode that 60s stops.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100347711A CN101643938B (en) | 2009-09-08 | 2009-09-08 | Method for preparing submicron grade square pipe-shaped Sb2Se3 |
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| CN101643938A CN101643938A (en) | 2010-02-10 |
| CN101643938B true CN101643938B (en) | 2011-08-31 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583271A (en) * | 2012-01-21 | 2012-07-18 | 哈尔滨工业大学 | Spine-like SbSe3 semiconductor hydrogen storage material and preparation method thereof |
| CN102583272A (en) * | 2012-01-21 | 2012-07-18 | 哈尔滨工业大学 | Vermicular Sb2Se3 hydrogen storage material and preparation method thereof |
| CN105603532B (en) * | 2016-03-23 | 2018-05-22 | 岭南师范学院 | A kind of preparation method of antimony selenide micron single crystal grain |
| CN107140609B (en) * | 2017-05-27 | 2019-07-16 | 陕西科技大学 | A kind of method that microwave hydrothermal prepares sodium-ion battery cathode pencil antimony selenide electrode material |
| CN113235166B (en) * | 2021-05-13 | 2022-05-27 | 重庆文理学院 | Preparation method of large-size antimony selenide single crystal material |
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2009
- 2009-09-08 CN CN2009100347711A patent/CN101643938B/en not_active Expired - Fee Related
Non-Patent Citations (8)
| Title |
|---|
| Bo Zhou,Jun-Jie Zhu.《Nanotechnology》.《Microwave-assisted synthesis of Sb2Se3 submicron rods, compared with those of Bi2Te3 and Sb2Te3》.2009,(第20期),1-6. * |
| BoZhou Jun-Jie Zhu.《Nanotechnology》.《Microwave-assisted synthesis of Sb2Se3 submicron rods |
| Cui Zhao, Xuebo Cao , Xianmei Lan.《Microwave-enhanced rapid and green synthesis of well crystalline Sb2Se3 nanorods with a flat cross section》.《Materials Letters》.2007,(第61期),5083-5086. |
| Cui Zhao, Xuebo Cao, Xianmei Lan.《Microwave-enhanced rapid and green synthesis of well crystalline Sb2Se3 nanorods with a flat cross section》.《Materials Letters》.2007,(第61期),5083-5086. * |
| JIANG Wen-juan, LING Yun, LI Zhi-hua, CHEN Xiao-nong.《Preparation and Characterization of Tube-like Sb2Se3》.《Nanoscience ＆ Nanotechnology》.2008,第5卷(第6期),53-57. * |
| Minghai Chen, Lian Gao.《Polyol method synthesis and characterization of nanoscale Sb2Se3 wires》.《Materials Research Bulletin》.2005,第40卷1120-1125. * |
| Xiuwen Zheng et. al.《Growth of Sb2E3 (E ) S, Se) Polygonal Tubular Crystals via a Novel Solvent-Relief-Self-Seeding Process》.《Inorganic Chemistry》.2002,第41卷455-461. * |
| XiuwenZhenget.al.《GrowthofSb2E3(E)S Se) Polygonal Tubular Crystals via a Novel Solvent-Relief-Self-Seeding Process》.《Inorganic Chemistry》.2002 |
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