CN106744728A - A kind of method that room temperature liquid phase method prepares SnSe micron balls - Google Patents
A kind of method that room temperature liquid phase method prepares SnSe micron balls Download PDFInfo
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- CN106744728A CN106744728A CN201611180033.4A CN201611180033A CN106744728A CN 106744728 A CN106744728 A CN 106744728A CN 201611180033 A CN201611180033 A CN 201611180033A CN 106744728 A CN106744728 A CN 106744728A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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Abstract
The present invention provides a kind of method that room temperature liquid phase method prepares SnSe micron balls, and the size of SnSe micron balls is about 0.5~1 μm.Weigh 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 balls.Present invention process process is simple, short preparation period, and repeatability is high, and room temperature reaction, without adding template and catalyst, greatly reduces energy consumption without heating, has saved production cost, is adapted to large-scale production and prepares.
Description
【Technical field】
The present invention relates to SnSe micron ball preparing technical fields, and in particular to a kind of room temperature liquid phase method prepares SnSe micron balls
Method.
【Background technology】
Group IV-VI semiconducting compound stannic selenide can form the compound of various stoichiometric proportions, such as SnSe,
SnSe2And Sn2Se3, wherein SnSe and SnSe2Have and compare the prospect of being widely applied.Stannous selenide (SnSe) is a kind of important
Semi-conducting material, energy gap is about 0.9eV, with preferable electrical and optical property, is 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.Therefore, it is a focus direction for the research of stannous selenide.
According to the literature, the size and pattern of material have huge for the performance (optical property, electric property etc.) of material
Big influence, thus for the focus of the regulation and control as researcher's research of material structure.For example, good grades of Cui Kai uses electric arc legal system
The standby stannous selenide of square laminated structure (Cui Kai is good, Zhang Jian, Wang Qiu are real etc., a kind of stannous selenide square nanometer sheet and
Its preparation method, Chinese Patent Application No.：201510086479.X)；The good grades of Cui Kai are prepared using but also using same method not only
Stannous selenide stannous selenide nanosphere (Cui Kai is good, 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 etc. use hot injection method, and stannous selenide list has been synthesized 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 of the stannic selenide reported at present is broadly divided into two classes：Wet chemistry method is (hydro-thermal method, solvent-thermal method, heavy
Shallow lake method, sol-gel process etc.) and solid-phase synthesis (chemical/physical vapour deposition, high-energy ball milling etc.).But above-mentioned preparation method
Generally existing reaction time consumption is long, high temp/high pressure environment, and yield is small, it is necessary to add catalysts, surfactant, relies on base
The features such as bottom growth, this makes synthesis high cost, and preparation process produces secondary pollution etc. to environment.
【The content of the invention】
It is an object of the invention to provide a kind of method that room temperature liquid phase method prepares SnSe micron balls, prepared SnSe is micro-
Rice ball is a kind of micron ball assembled by bar-shaped little particle.
To reach above-mentioned purpose, present invention employs following technical scheme：
A kind of method that room temperature liquid phase method prepares SnSe micron balls, comprises the following steps：
Under room temperature condition, 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 stirring is 1 with the mol ratio of tin ion to lurid solution B, selenium atom is become：(1.5
~2)；Solution B is stirred to solution B and gradually becomes black；Then, solution B centrifugation is obtained into black powder, and uses absolute ethyl alcohol
Washing, drying obtain SnSe micron balls.
Described inorganic tin salts are SnCl2·2H2O。
Specifically include following steps：
0.1579~6.316 part of selenium powder is added in 5~30mL hydrazine hydrates, 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 centrifugation obtains black powder, and obtains SnSe micron balls with absolute ethyl alcohol cyclic washing, drying.
Selenium powder consumption is 0.6316 part；Hydrazine hydrate consumption is 25mL；SnCl2·2H2O consumptions are 1.0 parts.
Prepared SnSe micron balls are assembled by nanometer rods, and the size of micron ball is 0.5~1 μm.
It is magnetic agitation to stir, and mixing speed is 400~1000r/min, 1~6h of mixing time.
Relative to prior art, beneficial effects of the present invention are embodied in：
Without high temperature and high pressure environment, with inorganic tin salts as Xi Yuan, selenium powder is selenium source to preparation method of the invention, and hydrazine hydrate is made
It is reducing agent；Reaction a few hours can obtain product at room temperature, and product is uniform micron ball, assembled by countless nanometer rods and
Into.Preparation method of the invention is simple, and repeatability is high, and without adding any template and catalyst, room temperature liquid phase synthesis are existing
Beneficial to control product morphology, energy consumption and manufacturing cost have been saved again, be adapted to extensive generation manufacture.SnSe prepared by the present invention
It is a kind of ball assembled by many nanometer rods.The size of SnSe micron balls is about 0.5~1 μm.Product size is small, purity
It is high, it is contemplated that to have preferably application in electrochemical field, semiconductor applications and photocatalysis field.
【Brief description of the drawings】
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the SnSe prepared by embodiment 3；
Fig. 2 is ESEM (SEM) photo of the SnSe micron balls prepared by embodiment 3.
【Specific embodiment】
The present invention is elaborated with reference to the accompanying drawings and examples.
A kind of method that room temperature liquid phase method prepares SnSe micron balls, according to parts by weight, including：By 0.1579~6.316
Part selenium powder is added in 5~30mL hydrazine hydrates, 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 centrifugation is obtained into black powder
Body, and obtain SnSe micron balls with 3 drying of absolute ethyl alcohol cyclic washing.The selenium powder and SnCl2·2H2The mol ratio of O is 1：
(1.5~2).
Prepared SnSe micron balls are assembled by bar-shaped little particle, and the size of micron ball is about 0.5~1 μm.
Embodiment 1
0.1579g selenium powders are added in 10mL hydrazine hydrates, stirring is completely dissolved to form claret solution A to selenium powder；Weigh
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 centrifugation is obtained into black powder,
And obtain SnSe micron balls with 3 drying of absolute ethyl alcohol cyclic washing.
Embodiment 2
0.3158g selenium powders are added in 20mL hydrazine hydrates, stirring is completely dissolved to form claret solution A to selenium powder；Weigh
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 is stirred with the speed of 800r/min, rear solution B gradually becomes black.Then, solution B centrifugation is obtained into black powder, and
SnSe micron balls are obtained with 3 drying of absolute ethyl alcohol cyclic washing.
Embodiment 3
0.6316g selenium powders are added in 25mL hydrazine hydrates, stirring is completely dissolved to form claret solution A to selenium powder；Weigh
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 is stirred with the speed of 900r/min, rear solution B gradually becomes black.Then, solution B centrifugation is obtained into black powder, and
SnSe micron balls are obtained with 3 drying of absolute ethyl alcohol cyclic washing.
Sample (SnSe micron balls) is analyzed with Rigaku D/max2000PCX- x ray diffractometer xs, sample and JCPDS is found
Numbering is that the SnSe structures of the rhombic system of 65-3811 are consistent, illustrates that the method can be obtained the SnSe of pure phase.By the sample use
Transmitting SEM (FESEM) is observed, it can be seen that prepared SnSe products are uniform 0.5~1 μm
Micron ball, and micron ball assembles by countless nanometer rods.
Embodiment 4
1.68g selenium powders are added in 30mL hydrazine hydrates, stirring is completely dissolved to form claret solution A to selenium powder；Weigh
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 is stirred with the speed of 800r/min, rear solution B gradually becomes black.Then, solution B centrifugation is obtained into black powder, and
SnSe micron balls are obtained with 3 drying of absolute ethyl alcohol cyclic washing.
Embodiment 5
0.21g selenium powders are added in 20mL hydrazine hydrates, stirring is completely dissolved to form claret solution A to selenium powder；Weigh
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 is stirred with the speed of 600r/min, rear solution B gradually becomes black.Then, solution B centrifugation is obtained into black powder, and
SnSe micron balls are obtained with 3 drying of absolute ethyl alcohol cyclic washing.
Embodiment 6
0.1579g selenium powders are added in 5mL hydrazine hydrates, stirring is completely dissolved to form claret solution A to selenium powder；Weigh
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 centrifugation is obtained into black powder,
And obtain SnSe micron balls with 3 drying of absolute ethyl alcohol cyclic washing.
Embodiment 7
6.316g selenium powders are added in 30mL hydrazine hydrates, 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 stirring 6h of 800r/min, rear solution B gradually becomes black.Then, solution B centrifugation is obtained into black powder, and uses nothing
3 drying of water-ethanol cyclic washing obtain SnSe micron balls.
In a word, the present invention is prepared for SnSe micron balls using room temperature liquid phase method, and micron ball is assembled by many nanometer rods.
The method that the present invention is used is very simple, and repeatability is high, and reaction is greatly saved without the environment and Large expensive equipment of high-temperature high-pressure
About energy consumption and manufacturing cost, and Product size prepared by the present invention is small, and purity is high, it is contemplated that in electrochemical field, semiconductor
Field and photocatalysis field have preferably application.
Claims (6)
1. a kind of method that room temperature liquid phase method prepares SnSe micron balls, it is characterised in that：Comprise the following steps：
Under room temperature condition, 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 stirring is 1 with the mol ratio of tin ion to lurid solution B, selenium atom is become：(1.5~2)；
Solution B is stirred to solution B and gradually becomes black；Then, solution B centrifugation is obtained into black powder, and with absolute ethanol washing,
Drying obtains SnSe micron balls.
2. a kind of method that room temperature liquid phase method prepares SnSe micron balls according to claim 1, it is characterised in that：Described nothing
Machine pink salt is SnCl2·2H2O。
3. the method that a kind of room temperature liquid phase method according to claim 1 prepares SnSe micron balls, it is characterised in that：According to weight
Amount number, specifically includes following steps：
0.1579~6.316 part of selenium powder is added in 5~30mL hydrazine hydrates, stirring is completely dissolved to form claret solution to selenium powder
A；Weigh 0.2256~9 part of SnCl2·2H2O is added in above-mentioned solution A, and stirring is to becoming lurid solution B；Solution B is put
In 1~6h is stirred with the speed of 400~1000r/min on magnetic stirrer, rear solution B gradually becomes black；Then, by solution
B centrifugations obtain black powder, and obtain SnSe micron balls with absolute ethyl alcohol cyclic washing, drying.
4. the method that a kind of room temperature liquid phase method according to claim 3 prepares SnSe micron balls, it is characterised in that：Selenium powder is used
Measure is 0.6316 part；Hydrazine hydrate consumption is 25mL；SnCl2·2H2O consumptions are 1.0 parts.
5. the method that a kind of room temperature liquid phase method according to any one in claim 1 prepares SnSe micron balls, its feature
It is：Prepared SnSe micron balls are assembled by nanometer rods, and the size of micron ball is 0.5~1 μm.
6. the method that a kind of room temperature liquid phase method according to claim 1 prepares SnSe micron balls, it is characterised in that：Stir and be
Magnetic agitation, mixing speed is 400~1000r/min, 1~6h of mixing time.
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Cited By (6)
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|---|---|---|---|---|
| CN107177887A (en) * | 2017-06-26 | 2017-09-19 | 陕西科技大学 | A kind of room temperature water solution growth stannous selenide nanometer rods cone monocrystalline and its method |
| CN107601441A (en) * | 2017-10-10 | 2018-01-19 | 陕西科技大学 | A kind of method of hydro-thermal method synthesis stannic selenide micron crystalline flour body |
| CN108147376A (en) * | 2018-01-17 | 2018-06-12 | 陕西科技大学 | A kind of method of room temperature synthesis stannic selenide powder |
| CN112978685A (en) * | 2021-04-01 | 2021-06-18 | 陕西科技大学 | Pure-phase SnSe nano-particles and preparation method thereof |
| CN113005328A (en) * | 2021-02-23 | 2021-06-22 | 西安航空学院 | Tin-selenium-sulfur ternary alloy cathode material for sodium ion battery and preparation method and application thereof |
| CN114300568A (en) * | 2021-10-22 | 2022-04-08 | 中国石油大学(华东) | SnSe nanorod array heterojunction device with room-temperature ultrafast infrared response and preparation method thereof |
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Cited By (9)
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|---|---|---|---|---|
| CN107177887A (en) * | 2017-06-26 | 2017-09-19 | 陕西科技大学 | A kind of room temperature water solution growth stannous selenide nanometer rods cone monocrystalline and its method |
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| CN107601441A (en) * | 2017-10-10 | 2018-01-19 | 陕西科技大学 | A kind of method of hydro-thermal method synthesis stannic selenide micron crystalline flour body |
| CN108147376A (en) * | 2018-01-17 | 2018-06-12 | 陕西科技大学 | A kind of method of room temperature synthesis stannic selenide powder |
| CN113005328A (en) * | 2021-02-23 | 2021-06-22 | 西安航空学院 | Tin-selenium-sulfur ternary alloy cathode material for sodium ion battery and preparation method and application thereof |
| 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 |
| CN114300568A (en) * | 2021-10-22 | 2022-04-08 | 中国石油大学(华东) | SnSe nanorod array heterojunction device with room-temperature ultrafast infrared response 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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