CN101898792A - Preparation method of Sb2S3 nanowire - Google Patents
Preparation method of Sb2S3 nanowire Download PDFInfo
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- CN101898792A CN101898792A CN 201010232197 CN201010232197A CN101898792A CN 101898792 A CN101898792 A CN 101898792A CN 201010232197 CN201010232197 CN 201010232197 CN 201010232197 A CN201010232197 A CN 201010232197A CN 101898792 A CN101898792 A CN 101898792A
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Abstract
The invention provides a preparation method of an Sb2S3 nanowire. 10 mmol of Sb2Cl3 is dissolved into 2 ml of glycol; after the Sb2Cl3 is totally dissolved, 10 ml of deionized water is added while stirring to form white emulsion A; 15 mmol of Na2S.9H2O is dissolved into 10 ml of deionized water to form solution B; the solution B is added into the solution A at the rate of 2 drips/ second to form a precursor; mineralizer is added into the precursor to prepare 30 ml of solution C, and the solution C is put in an agitated reactor; the agitated reactor is put into an incubator; when temperature rises to 240 DEG C, temperature is kept for 8-16 hours; and after reaction ends, the product is washed by deionized water to be neutral and is dried for 4h in vacuum in the incubator of 80 DEG C. The invention has simple preparation method, short reaction period and low cost.
Description
[technical field]
The present invention relates to a kind of nanometer Sb
2S
3Material preparation method, particularly a kind of Sb
2S
3The preparation method of nano wire.
[background technology]
Antimony trisulfide (Sb
2S
3) be the important direct band gap inorganic semiconductor material of V-VI, have the orthorhombic body structure, band-gap energy at room temperature is 1.72eV.Antimony trisulfide is considered to utilize the ideal material of solar energy owing to have high photosensitivity and thermoelectricity capability.In addition, antimony sulfide also is considered to be widely used in aspects such as infrared field, thermoelectric-cooled technology and photoelectron technology.
In recent years, many investigators utilize chemical Vapor deposition process (CVD), template, using vaporization condensation process and hydro-thermal (solvent thermal) method to prepare the antimony sulfide crystalline phase of various patterns.For example: Hu H M, Mo M S, (the Solvothermal synthesis of Sb such as YangB J
2S
3Nanowires on a large scale[J] .J CrystalGrowth, 2003,258:106-112) synthesized nano wire with solvent-thermal method; Yu Y, Wang R H, Chen Q, and Peng L M. (High-Quality Ultralong Sb
2S
3Nanoribbons on Large Scale[J] .JPhys Chem B, 2005,109:23312-23315) use SbCl
3With Na
2S
2O
3Directly overlength Sb has been synthesized in reaction
2S
3Nanobelt; Hu H M, Liu Z P, (the Solvothermal growth of Sb such as Yang B J
2S
3Microcrystallites with novel morphologies[J] .J Crystal Growth 2004,262:375-382) take antimony trisulfide and thiocarbamide as raw material, adopt solvent-thermal method directly at low temperatures reaction synthesized Sb
2S
3Nano flower; Cheng B, (One-step, the ambient-temperature synthesis of antimonysulfide (Sb such as Samulski E T
25
3) micron-size polycrystals with a spherical morphology[J] .Mater ResBull, 2003,38:297-301) synthesized at normal temperatures Sb
2S
3Microballoon.This shows that many researchers are devoted to prepare by the whole bag of tricks the Sb of different shape
2S
3Material.
Yet above-mentioned preparation method's complicated operation, reaction time are long, and with high costs.
[summary of the invention]
Technical problem to be solved by this invention provides a kind of Sb
2S
3The preparation method of nano wire, it is simple to operate, reaction time is short, and with low cost.
For achieving the above object, the invention provides a kind of Sb
2S
3The preparation method of nano wire gets the Sb of 10mmol
2Cl
3Be dissolved in the ethylene glycol of 2ml, treat Sb
2C1
3After the dissolving, pour the deionized water of 10ml while stirring into fully, form the emulsion A of white; Get the Na of 15mmol
2S9H
2O is dissolved in the deionized water of 10ml, forms solution B; With solution B being added in the solution A dropwise, form precursor; In precursor, add mineralizer, be made into the 30ml solution C after, be positioned in the reactor; Reactor is inserted in the thermostat container, when being warming up to 240 ℃, is incubated 8～16 hours, after question response finishes, with product with deionized water rinsing back vacuum-drying 4h in 80 ℃ of thermostat containers for several times.
As the preferred embodiments of the present invention, described mineralizer is CO (NH
2)
2
As the preferred embodiments of the present invention, 240 ℃ of insulations 8～12 hours;
As the preferred embodiments of the present invention, 240 ℃ of insulations 12 hours.
Sb of the present invention
2S
3The preparation method of nano wire compared with prior art has the following advantages at least: preparation method of the present invention is simple, reaction time short, and with low cost; In addition, by a process for preparing next Sb
2S
3Nano wire is the Sb of quadrature
2S
3Monocrystalline has higher draw ratio, and the nanowire diameter size evenly, and smooth surface, clean does not have the granule dephasign.
[description of drawings]
Fig. 1 is the Sb by the inventive method preparation
2S
3The X-ray diffraction of nano wire (XRD) collection of illustrative plates, wherein abscissa is the angle of diffraction 2 θ, unit is °; Ordinate is diffraction peak intensity, the cps of unit;
Fig. 2 is the Sb by the inventive method preparation
2S
3The SEM photo of nano wire high-amplification-factor;
Fig. 3 is the Sb that is prepared bunchy by the inventive method
2S
3The SEM photo of nano wire;
Fig. 4 is the Sb that is prepared bunchy by the inventive method
2S
3The TEM photo of nano wire;
Fig. 5 is the Sb by the inventive method preparation
2S
3Nano wire TEM photo, temperature retention time 8h;
Fig. 6 is the Sb by the inventive method preparation
2S
3Nano wire TEM photo, temperature retention time 16h.
[embodiment]
Below in conjunction with accompanying drawing to Sb of the present invention
2S
3The preparation method of nano wire is described in detail:
Embodiment 1
(1) takes by weighing the Sb of 10mmol
2Cl
3, be poured in the ethylene glycol of 2ml, stir until Sb with stirrer
2Cl
3Dissolving fully; Then, to the deionized water of wherein pouring 10ml while stirring into, form the emulsion A of white;
(2) take by weighing the Na of 15mmol
2S9H
2O is dissolved in the deionized water of 10ml, forms solution B;
(3) speed of solution B with 2 droplets/second is splashed in the solution A, form the precursor of orange;
(4) in predecessor, add CO (NH
2)
2, be made into the 30ml solution C;
(5) solution C is positioned in the reactor of 50ml, places insulating box to heat reactor, when treating that temperature rises to 240 ℃, be incubated 12 hours, after reaction finishes, with product with deionized water rinsing until pH is 7, vacuum drying 4h in 80 ℃ insulating box namely gets Sb then
2S
3Nano wire.
Products therefrom is analyzed with Rigaku D/max2550VB+/PC type x-ray diffractometer, as seen from Figure 1, all diffraction maximums and standard card (JCPDS-42-1393, a=1.122nm, b=1.131nm, c=0.3839nm) corresponding, there is not the diffraction maximum of other dephasigns, show: product is quadrature Sb
2S
3Crystalline phase, as calculated, its cell parameter is: a=1.123nm, b=1.131nm, c=0.3840nm.
As seen from Figure 2: the nano wire that is obtained by present method has high length-to-diameter ratio, and diameter is about 200nm, reaches 100 μ m, and the diameter of nano wire is even, and smooth surface, clean does not have the small-particle dephasign.And in the material of these linear structures, we have also found nanostructure a part of bunchy, ordered arrangement, as shown in Figure 3.
Embodiment 2
(1) takes by weighing the Sb of 10mmol
2Cl
3, be poured in the ethylene glycol of 2ml, stir until Sb with stirrer
2Cl
3Dissolving fully; Then, to the deionized water of wherein pouring 10ml while stirring into, form the emulsion A of white;
(2) take by weighing the Na of 15mmol
2S9H
2O is dissolved in the deionized water of 10ml, forms solution B;
(3) speed of solution B with 2 droplets/second is splashed in the solution A, the precursor of formation orange (;
(4) in predecessor, add CO (NH
2)
2, be made into the 30ml solution C;
(5) solution C is positioned in the reactor of 50ml, places insulating box to heat reactor, when treating that temperature rises to 240 ℃, be incubated 8 hours, after reaction finishes, with product with deionized water rinsing to pH be 7, vacuum drying 4h in 80 ℃ insulating box namely gets Sb then
2S
3Nano wire.
Embodiment 3
(1) takes by weighing the Sb of 10mmol
2Cl
3, be poured in the ethylene glycol of 2ml, stir until Sb with stirrer
2Cl
3Dissolving fully; Then, to the deionized water of wherein pouring 10ml while stirring into, form the emulsion A of white;
(2) take by weighing the Na of 15mmol
2S9H
2O is dissolved in the deionized water of 10ml, forms solution B; (3) speed of solution B with 2 droplets/second is splashed in the solution A, form the precursor of orange;
(4) in predecessor, add CO (NH
2)
2, be made into the 30ml solution C;
(5) solution C is positioned in the reactor of 50ml, places insulating box to heat reactor, when treating that temperature rises to 240 ℃, be incubated 12 hours, after reaction finishes, with product with deionized water rinsing to pH be 7, vacuum drying 4h in 80 ℃ insulating box namely gets Sb then
2S
3Nano wire.
See also Fig. 3 to shown in Figure 6, the Sb that is obtained by this method
2S
3The diameter of nano wire is about 200nm, and length is 20 μ m, and along the growth of [001] crystal face; In addition, it has higher draw ratio, and the diametric(al) of nano wire is substantially no longer grown up, and the diameter of nano wire is even, and length reaches 100 μ m.
Sb of the present invention
2S
3The formation mechanism of nano wire is: just begin, work as SbCl
3After being dissolved in the ethylene glycol, form Sb freely
3+Ion; After adding deionized water, form the indefinite form throw out of SbOCl white; Then, along with S
2-Ionic is introduced, Sb
3+Ion can be rapidly and S
2-Ionic bond, the and (Sb of formation orange
2S
3)
nThe indefinite form precipitation; Under the hydrothermal condition of mineralizer and High Temperature High Pressure, the indefinite form throw out of part orange is dissolved into Sb
3+Ion and S
2-Ion, along with the carrying out of reaction, the ionic concn in the solution raises gradually and forms supersaturated solution, at this moment, Sb
3+Ion and S
2-Ionic bond forms Sb
2S
3Small crystal nucleus; Ion around small crystal nucleus absorbs is constantly grown up.If the reaction time is too short, product mainly is made up of spherical nanocrystalline and indefinite form material; Prolong Sb when the reaction time
2S
3Little crystal grain continues ion in the absorbent solution and small crystal nucleus and grows up.Because Sb
2S
3Have unique chain structure and high anisotropy, therefore, some crystal face fast growth, Sb
2S
3The nanocrystalline structure that under suitable pressure and temperature, is easy to be self-assembled into along some crystal faces wire.When the reaction time extended to 12h, nano wire continued to form along this crystal face growth the nano wire of high length-diameter ratio; If the reaction time continues to prolong, because the ion in the solution runs out of, can't provide again the raw material of nanowire growth, therefore, Sb
2S
3Nano wire is substantially no longer long, and the nano thread structure of part bunchy is by Sb in the product
2S
3The aggregate of particle forms nanometer bundle along same direction growth jointly under hydrothermal condition.
The above only is one embodiment of the present invention, it or not whole or unique embodiment, the conversion of any equivalence that those of ordinary skills take technical solution of the present invention by reading specification sheets of the present invention is claim of the present invention and contains.
Claims (4)
1. Sb
2S
3The preparation method of nano wire is characterized in that: may further comprise the steps:
(1) gets the Sb of 10mmol
2Cl
3Be dissolved in the ethylene glycol of 2ml, treat Sb
2Cl
3After the dissolving, pour the deionized water of 10ml while stirring into fully, form the emulsion A of white;
(2) get the Na of 15mmol
2S9H
2O is dissolved in the deionized water of 10ml, forms solution B;
(3) speed of solution B with 2 droplets/second is added in the solution A, forms precursor;
(4) in precursor, add mineralizer, be made into the 30ml solution C after, be positioned in the reactor;
(5) reactor is inserted in the insulating box, when being warming up to 240 ℃, is incubated 8～16 hours, after question response finishes, with product with deionized water rinsing after neutral in 80 ℃ of insulating boxs vacuum drying 4h.
2. Sb as claimed in claim 1
2S
3The preparation method of nano wire is characterized in that: described mineralizer is CO (NH
2)
2
3. Sb as claimed in claim 1
2S
3The preparation method of nano wire is characterized in that: in the described step (5), 240 ℃ of insulations 8～12 hours.
4. Sb as claimed in claim 3
2S
3The preparation method of nano wire is characterized in that: in the described step (5), 240 ℃ of insulations 12 hours.
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|---|---|---|---|
| CN 201010232197 CN101898792A (en) | 2010-07-21 | 2010-07-21 | Preparation method of Sb2S3 nanowire |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102259912A (en) * | 2011-06-29 | 2011-11-30 | 天津市风船化学试剂科技有限公司 | Method for preparing high-purity antimony pentasulfide |
| CN103227054A (en) * | 2012-12-18 | 2013-07-31 | 南开大学 | Antimony sulfide counter electrode of dye-sensitized solar cell and a preparation method of antimony sulfide counter electrode |
| CN105056974A (en) * | 2015-08-03 | 2015-11-18 | 南京信息工程大学 | Flower-shaped cadmium sulfide-antimony sulfide compound, preparation method and application thereof |
| CN106025272A (en) * | 2016-06-27 | 2016-10-12 | 陕西科技大学 | Flower-like structure Sb2S3 material for sodium ion battery anode and preparation method of flower-like structure Sb2S3 material |
| CN106410152A (en) * | 2016-11-04 | 2017-02-15 | 华中科技大学 | One-dimensional antimony sulfide-carbon composite material and preparation method and application thereof |
| CN106542577A (en) * | 2016-11-29 | 2017-03-29 | 浙江大学 | A kind of nanometer antimony trisulfide particle preparation method under controlled condition |
| CN107715895A (en) * | 2017-09-27 | 2018-02-23 | 湖北工业大学 | A kind of ZnO/Ag/Sb2S3The preparation method of photocatalyst material |
| CN107892328A (en) * | 2017-11-17 | 2018-04-10 | 广西生富锑业科技股份有限公司 | A kind of preparation method of high-purity antimony trisulfide |
| CN110257311A (en) * | 2019-08-13 | 2019-09-20 | 中国科学院烟台海岸带研究所 | A kind of microorganism being used to prepare broccoli shape antimony trisulfide and its application |
-
2010
- 2010-07-21 CN CN 201010232197 patent/CN101898792A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 《仪器分析实验》 20090331 张剑荣等 纳米修饰电极及其分析应用 第177页第1段 , 1 * |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102259912B (en) * | 2011-06-29 | 2012-11-14 | 天津市风船化学试剂科技有限公司 | Method for preparing high-purity antimony pentasulfide |
| CN102259912A (en) * | 2011-06-29 | 2011-11-30 | 天津市风船化学试剂科技有限公司 | Method for preparing high-purity antimony pentasulfide |
| CN103227054A (en) * | 2012-12-18 | 2013-07-31 | 南开大学 | Antimony sulfide counter electrode of dye-sensitized solar cell and a preparation method of antimony sulfide counter electrode |
| CN103227054B (en) * | 2012-12-18 | 2015-10-14 | 南开大学 | The antimony trisulfide of DSSC is to electrode and preparation method thereof |
| CN105056974A (en) * | 2015-08-03 | 2015-11-18 | 南京信息工程大学 | Flower-shaped cadmium sulfide-antimony sulfide compound, preparation method and application thereof |
| CN106025272B (en) * | 2016-06-27 | 2018-11-30 | 陕西科技大学 | A kind of sodium-ion battery cathode flower-like structure Sb2S3Material and preparation method thereof |
| CN106025272A (en) * | 2016-06-27 | 2016-10-12 | 陕西科技大学 | Flower-like structure Sb2S3 material for sodium ion battery anode and preparation method of flower-like structure Sb2S3 material |
| CN106410152A (en) * | 2016-11-04 | 2017-02-15 | 华中科技大学 | One-dimensional antimony sulfide-carbon composite material and preparation method and application thereof |
| CN106410152B (en) * | 2016-11-04 | 2019-05-31 | 华中科技大学 | A kind of one-dimensional antimony trisulfide-carbon composite, preparation method and application |
| CN106542577B (en) * | 2016-11-29 | 2017-11-10 | 浙江大学 | A kind of nanometer antimony trisulfide particle preparation method under controlled condition |
| CN106542577A (en) * | 2016-11-29 | 2017-03-29 | 浙江大学 | A kind of nanometer antimony trisulfide particle preparation method under controlled condition |
| CN107715895A (en) * | 2017-09-27 | 2018-02-23 | 湖北工业大学 | A kind of ZnO/Ag/Sb2S3The preparation method of photocatalyst material |
| CN107715895B (en) * | 2017-09-27 | 2020-08-07 | 湖北工业大学 | ZnO/Ag/Sb2S3Preparation method of photocatalyst material |
| CN107892328A (en) * | 2017-11-17 | 2018-04-10 | 广西生富锑业科技股份有限公司 | A kind of preparation method of high-purity antimony trisulfide |
| CN110257311A (en) * | 2019-08-13 | 2019-09-20 | 中国科学院烟台海岸带研究所 | A kind of microorganism being used to prepare broccoli shape antimony trisulfide and its application |
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Application publication date: 20101201 |