CN106744728B - A kind of method that room temperature liquid phase method prepares SnSe micron ball - Google Patents
A kind of method that room temperature liquid phase method prepares SnSe micron ball Download PDFInfo
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- CN106744728B CN106744728B CN201611180033.4A CN201611180033A CN106744728B CN 106744728 B CN106744728 B CN 106744728B CN 201611180033 A CN201611180033 A CN 201611180033A CN 106744728 B CN106744728 B CN 106744728B
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Abstract
The present invention provides a kind of method that room temperature liquid phase method prepares SnSe micron ball, and the size of SnSe micron ball is about 0.5~1 μm.It weighs a certain amount of selenium powder first to be added in hydrazine hydrate, stirring is completely dissolved to form claret solution A to selenium powder；Then a certain amount of SnCl is weighed2·2H2O is added in above-mentioned solution A, and stirring is to becoming lurid solution B；Finally solution B is placed on magnetic stirrer, a period of time is stirred with certain speed, black powder is collected by centrifugation, drying obtains SnSe micron ball.Present invention process process is simple, short preparation period, and repeatability is high, and room temperature reaction greatly reduces energy consumption, saved production cost, be suitble to large-scale production preparation without heating without adding template and catalyst.
Description
[technical field]
The present invention relates to SnSe micron ball preparation technical fields, and in particular to a kind of room temperature liquid phase method preparation SnSe micron ball
Method.
[background technique]
Group IV-VI semiconducting compound stannic selenide is capable of forming the compound of a variety of stoichiometric ratios, such as SnSe,
SnSe2And Sn2Se3, wherein SnSe and SnSe2Have and compares broad application prospect.Stannous selenide (SnSe) is a kind of important
Semiconductor material, forbidden bandwidth is about 0.9eV, have preferable electrical and optical property, be widely used in infrared electro
Instrument and memory switching switch, the solid-phase media of hologram, the research of lithium ion/sodium ion battery electrode material, the film sun
The directions such as the absorbing material of energy battery.It therefore, is a hot spot direction for the research of stannous selenide.
According to the literature, the size and shape of material has the performance (optical property, electric property etc.) of material huge
Big influence, thus become the hot spot of researcher's research for the regulation of material structure.For example, Cui Qiliang etc. uses electric arc legal system
The standby stannous selenide of square laminated structure (Cui Qiliang, Zhang Jian, Wang Qiu are real etc., a kind of stannous selenide square nanometer sheet and
Preparation method, Chinese Patent Application No.: 201510086479.X)；Cui Qiliang etc. is prepared using but also using same method not only
Stannous selenide stannous selenide nanosphere (Cui Qiliang, Zhang Jian, Wang Qiu are real etc., a kind of preparation method of stannous selenide nanosphere, in
State's number of patent application: 201510086485.5)；Sheng Liu et al. uses hot injection method, has synthesized stannous selenide list at 290 DEG C
Brilliant nano wire (Solution-Phase Synthesis and Characterization of Single-Crystalline
SnSe Nanowires,Angew.Chem.Int.Ed.2011,50,12050–12053)。
The synthetic method for the stannic selenide reported at present is broadly divided into two classes: wet chemistry method (solvent-thermal method, sink by hydro-thermal method
Shallow lake method, sol-gel method etc.) and solid-phase synthesis (chemical/physical vapor deposition, high-energy ball milling etc.).But above-mentioned preparation method
Generally existing reaction time consumption is long, and high temp/high pressure environment, yield is small, needs to add catalysts, surfactant, relies on base
The features such as bottom growth, this keeps synthesis cost excessively high, and preparation process generates secondary pollution etc. to environment.
[summary of the invention]
The purpose of the present invention is to provide a kind of method that room temperature liquid phase method prepares SnSe micron ball, prepared SnSe is micro-
Rice ball is a kind of micron ball assembled by rodlike little particle.
In order to achieve the above objectives, the invention adopts the following technical scheme:
A kind of method that room temperature liquid phase method prepares SnSe micron ball, comprising the following steps:
Under room temperature, selenium powder is added in hydrazine hydrate, stirring is completely dissolved to form claret solution A to selenium powder；Take nothing
Machine pink salt is added in above-mentioned solution A, and to lurid solution B is become, the molar ratio of selenium atom and tin ion is 1:(1.5 for stirring
~2)；Solution B is stirred to solution B and gradually becomes black；Then, solution B is centrifuged to obtain black powder, and uses dehydrated alcohol
Washing, drying obtain SnSe micron ball.
The inorganic tin salts are SnCl2·2H2O。
Specifically includes the following steps:
0.1579~6.316 part of selenium powder is added in 5~30mL hydrazine hydrate, stirring is completely dissolved to form claret to selenium powder
Solution A；Weigh 0.2256~9 part of SnCl2·2H2O is added in above-mentioned solution A, and stirring is to becoming lurid solution B；By solution
B is placed on magnetic stirrer and stirs 1~6h with the speed of 400~1000r/min, and rear solution B gradually becomes black；Then, will
Solution B is centrifuged to obtain black powder, and is washed repeatedly with dehydrated alcohol, dries and obtain SnSe micron ball.
Selenium powder dosage is 0.6316 part；Hydrazine hydrate dosage is 25mL；SnCl2·2H2O dosage is 1.0 parts.
Prepared SnSe micron ball is assembled by nanometer rods, and the size of micron ball is 0.5~1 μm.
Stirring is magnetic agitation, and mixing speed is 400~1000r/min, 1~6h of mixing time.
Compared with the existing technology, the beneficial effects of the present invention are embodied in:
Preparation method of the invention is not necessarily to high temperature and high pressure environment, and using inorganic tin salts as tin source, selenium powder is selenium source, and hydrazine hydrate is made
For reducing agent；Reaction a few hours can be obtained product at room temperature, and product is uniform micron ball, assembled by countless nanometer rods and
At.Preparation method of the invention is simple, and repeatability is high, and without adding any template and catalyst, room temperature liquid phase synthesis is existing
Conducive to control product morphology, and energy consumption and manufacturing cost are saved, extensive generate is suitble to manufacture.SnSe prepared by the present invention
For a kind of ball assembled by many nanometer rods.The size of SnSe micron ball is about 0.5~1 μm.Product size is small, purity
It is high, it is contemplated that have preferable application in electrochemical field, semiconductor field and photocatalysis field.
[Detailed description of the invention]
Fig. 1 is X-ray diffraction (XRD) map of SnSe prepared by embodiment 3；
Fig. 2 is scanning electron microscope (SEM) photo of SnSe micron ball prepared by embodiment 3.
[specific embodiment]
It elaborates with reference to the accompanying drawings and examples to the present invention.
A kind of method that room temperature liquid phase method prepares SnSe micron ball, according to parts by weight, comprising: by 0.1579~6.316
Part selenium powder is added in 5~30mL hydrazine hydrate, and stirring is completely dissolved to form claret solution A to selenium powder；Weigh 0.2256~9 part
SnCl2·2H2O is added in above-mentioned solution A, and stirring is to becoming lurid solution B；By solution B be placed on magnetic stirrer with
The speed of 400~1000r/min stirs 1~6h, and rear solution B gradually becomes black.Then, solution B is centrifuged to obtain black powder
Body, and wash 3 drying repeatedly with dehydrated alcohol and obtain SnSe micron ball.The selenium powder and SnCl2·2H2The molar ratio of O is 1:
(1.5~2).
Prepared SnSe micron ball is assembled by rodlike little particle, and the size of micron ball is about 0.5~1 μm.
Embodiment 1
0.1579g selenium powder is added in 10mL hydrazine hydrate, stirring is completely dissolved to form claret solution A to selenium powder；It weighs
0.2256g SnCl2·2H2O is added in above-mentioned solution A, and stirring is to becoming lurid solution B；Solution B is placed in magnetic agitation
2h is stirred with the speed of 500r/min on machine, rear solution B gradually becomes black.Then, solution B is centrifuged to obtain black powder,
And it washs 3 drying repeatedly with dehydrated alcohol and obtains SnSe micron ball.
Embodiment 2
0.3158g selenium powder is added in 20mL hydrazine hydrate, stirring is completely dissolved to form claret solution A to selenium powder；It weighs
0.6g SnCl2·2H2O is added in above-mentioned solution A, and stirring is to becoming lurid solution B；Solution B is placed in magnetic stirrer
On 3h stirred with the speed of 800r/min, rear solution B gradually becomes black.Then, solution B is centrifuged to obtain black powder, and
It washs 3 drying repeatedly with dehydrated alcohol and obtains SnSe micron ball.
Embodiment 3
0.6316g selenium powder is added in 25mL hydrazine hydrate, stirring is completely dissolved to form claret solution A to selenium powder；It weighs
1.0g SnCl2·2H2O is added in above-mentioned solution A, and stirring is to becoming lurid solution B；Solution B is placed in magnetic stirrer
On 3h stirred with the speed of 900r/min, rear solution B gradually becomes black.Then, solution B is centrifuged to obtain black powder, and
It washs 3 drying repeatedly with dehydrated alcohol and obtains SnSe micron ball.
Sample (SnSe micron ball) is analyzed with Rigaku D/max2000PCX- x ray diffractometer x, finds sample and JCPDS
The SnSe structure for the rhombic system that number is 65-3811 is consistent, illustrates that the SnSe of pure phase can be made in this method.By the sample use
Transmitting scanning electron microscope (FESEM) is observed, it can be seen that prepared SnSe product is uniform 0.5~1 μm
Micron ball, and micron ball is assembled by countless nanometer rods.
Embodiment 4
1.68g selenium powder is added in 30mL hydrazine hydrate, stirring is completely dissolved to form claret solution A to selenium powder；It weighs
3.2g SnCl2·2H2O is added in above-mentioned solution A, and stirring is to becoming lurid solution B；Solution B is placed in magnetic stirrer
On 5h stirred with the speed of 800r/min, rear solution B gradually becomes black.Then, solution B is centrifuged to obtain black powder, and
It washs 3 drying repeatedly with dehydrated alcohol and obtains SnSe micron ball.
Embodiment 5
0.21g selenium powder is added in 20mL hydrazine hydrate, stirring is completely dissolved to form claret solution A to selenium powder；It weighs
0.33g SnCl2·2H2O is added in above-mentioned solution A, and stirring is to becoming lurid solution B；Solution B is placed in magnetic stirrer
On 4h stirred with the speed of 600r/min, rear solution B gradually becomes black.Then, solution B is centrifuged to obtain black powder, and
It washs 3 drying repeatedly with dehydrated alcohol and obtains SnSe micron ball.
Embodiment 6
0.1579g selenium powder is added in 5mL hydrazine hydrate, stirring is completely dissolved to form claret solution A to selenium powder；It weighs
0.2256g SnCl2·2H2O is added in above-mentioned solution A, and stirring is to becoming lurid solution B；Solution B is placed in magnetic agitation
1h is stirred with the speed of 1000r/min on machine, rear solution B gradually becomes black.Then, solution B is centrifuged to obtain black powder,
And it washs 3 drying repeatedly with dehydrated alcohol and obtains SnSe micron ball.
Embodiment 7
6.316g selenium powder is added in 30mL hydrazine hydrate, stirring is completely dissolved to form claret solution A to selenium powder；Weigh 9g
SnCl2·2H2O is added in above-mentioned solution A, and stirring is to becoming lurid solution B；By solution B be placed on magnetic stirrer with
The speed of 800r/min stirs 6h, and rear solution B gradually becomes black.Then, solution B is centrifuged to obtain black powder, and uses nothing
Water-ethanol washs 3 drying repeatedly and obtains SnSe micron ball.
In short, the present invention is prepared for SnSe micron ball using room temperature liquid phase method, micron ball is assembled by many nanometer rods.
The method that the present invention uses is very simple, and repeatability is high, and reaction is not necessarily to the environment and Large expensive equipment of high-temperature high-pressure, greatly saves
About energy consumption and manufacturing cost, and Product size prepared by the present invention is small, purity is high, it is contemplated that in electrochemical field, semiconductor
Field and photocatalysis field have preferable application.
Claims (2)
1. a kind of method that room temperature liquid phase method prepares SnSe micron ball, it is characterised in that: the following steps are included:
Under room temperature, selenium powder is added in hydrazine hydrate, stirring is completely dissolved to form claret solution A to selenium powder；Take inorganic tin
Salt is added in above-mentioned solution A, and to lurid solution B is become, the molar ratio of selenium atom and tin ion is 1:(1.5~2 for stirring)；
Solution B is stirred to solution B and gradually becomes black, is stirred as magnetic agitation, mixing speed is 400~1000r/min；Then,
Solution B is centrifuged to obtain black powder, and washed with dehydrated alcohol, dried and obtain SnSe micron ball；
Prepared SnSe micron ball is assembled by nanometer rods, and the size of micron ball is 0.5~1 μm；
The inorganic tin salts are SnCl2·2H2O；
Specifically includes the following steps:
0.1579~6.316g selenium powder is added in 5~30mL hydrazine hydrate, stirring is completely dissolved to form claret solution to selenium powder
A；Weigh 0.2256~9g SnCl2·2H2O is added in above-mentioned solution A, and stirring is to becoming lurid solution B；Solution B is set
In stirring 1~6h on magnetic stirrer with the speed of 400~1000r/min, rear solution B gradually becomes black；Then, by solution
B is centrifuged to obtain black powder, and is washed repeatedly with dehydrated alcohol, dries and obtain SnSe micron ball.
2. the method that a kind of room temperature liquid phase method according to claim 1 prepares SnSe micron ball, it is characterised in that: selenium powder is used
Amount is 0.6316g；Hydrazine hydrate dosage is 25mL；SnCl2·2H2O dosage is 1.0g.
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Families Citing this family (6)
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| CN107177887B (en) * | 2017-06-26 | 2019-03-26 | 陕西科技大学 | A kind of room temperature water solution growth stannous selenide nanometer rods cone monocrystalline and its method |
| CN107601441B (en) * | 2017-10-10 | 2020-01-14 | 陕西科技大学 | Method for synthesizing tin selenide microcrystalline powder by hydrothermal method |
| CN108147376B (en) * | 2018-01-17 | 2021-02-12 | 陕西科技大学 | Method for synthesizing tin selenide powder at room temperature |
| CN113005328B (en) * | 2021-02-23 | 2021-12-07 | 西安航空学院 | Tin-selenium-sulfur ternary alloy cathode material for sodium ion battery and preparation method and application thereof |
| CN112978685A (en) * | 2021-04-01 | 2021-06-18 | 陕西科技大学 | Pure-phase SnSe nano-particles and preparation method thereof |
| CN114300568B (en) * | 2021-10-22 | 2024-03-26 | 中国石油大学(华东) | SnSe nano rod array heterojunction device with room temperature ultrafast infrared response and preparation method thereof |
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