CN107934924A - A kind of Hydrothermal preparation method for controlling laminated structure stannic selenide thickness - Google Patents
A kind of Hydrothermal preparation method for controlling laminated structure stannic selenide thickness Download PDFInfo
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- CN107934924A CN107934924A CN201711148116.XA CN201711148116A CN107934924A CN 107934924 A CN107934924 A CN 107934924A CN 201711148116 A CN201711148116 A CN 201711148116A CN 107934924 A CN107934924 A CN 107934924A
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- 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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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- 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
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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Abstract
A kind of Hydrothermal preparation method for controlling sheet stannic selenide thickness, tartaric acid is dissolved in distilled water, add stannous chloride, stir to solution clear, solution A is made, selenium dioxide, sodium hydroxide and sodium borohydride are sequentially added in distilled water again, solution B is made, A is slowly added to stir in B, Morphological control agent 1 is separately added into again, 10 phenanthrolines, 2,2 bipyridyls or 4,4 bipyridyls, stirring, when reaction 6 24 is small at 180 DEG C in hydrothermal reaction kettle, is then centrifuged for, washs, dry sheet stannic selenide black powder.The present invention controls the thickness of sheet SnSe using by adding Morphological control agent in water-heat process, the solution of raw material and generation in whole technical process is disposable and pollution-free, and manufacturing cost is low, and operating process is simple, it is repeatable high, the sheet stannic selenide powder of high-purity can be prepared.
Description
Technical field
The invention belongs to the Hydrothermal Synthesiss technical field of two-dimensional material, and in particular to a kind of control sheet stannic selenide thickness
Hydrothermal preparation method.
Background technology
Stannic selenide (SnSe) is a kind of very important group IV-VI two-dimensional semiconductor material, its component earth reserves
Abundant and nontoxic, chemical property is stablized.SnSe interlayers are attached by weaker Van der Waals for, while electronics is limited
In the environment of two dimension, therefore the characteristic of the physical chemistry of many uniquenesses etc. is shown, in photovoltaic (Li L, Chen Z, Hu
Y,et al.Single-layer single-crystalline SnSe nanosheets[J].Journal of the
American Chemical Society,2013,135(4):1213-6.), thermoelectricity (Zhao L D, Lo S H, Zhang Y,
et al.Ultralow thermal conductivity and high thermoelectric figure of merit
in SnSe crystals[J].Nature,2014,508(7496):And energy storage (Yuan S, Zhu Y H, Li W, et 373)
al.Surfactant-Free Aqueous Synthesis of Pure Single-Crystalline SnSe
Nanosheet Clusters as Anode for High Energy-and Power-Density Sodium-Ion
Batteries [J] .Advanced Materials, 2016,29 (4)) etc. various fields possess huge commercial application prospect.
Therefore the research for seeking the new preparation method on sheet SnSe materials has important meaning.
The preparation method of sheet SnSe is many at present, mainly there is solvent-thermal method, the precipitation method, hydro-thermal method etc., but on piece
The report of the control of shape pure phase SnSe thickness is seldom, and especially during hydro-thermal method prepares sheet SnSe, thickness exists
150nm or so, applicant have discovered that the thickness of sheet SnSe is small, its degradation rate in ultraviolet region to rhdamine B
Just fast, it is therefore necessary to provide a kind of method for the thickness that can control sheet SnSe.
The content of the invention
The object of the present invention is to provide a kind of Hydrothermal preparation method of simple and practicable control sheet stannic selenide thickness, this method
The sheet stannic selenide of 50-100 nano thickness can be prepared.
To achieve the above objectives, technical scheme comprises the following steps：
A kind of Hydrothermal preparation method for controlling sheet stannic selenide thickness, comprises the following steps：
1) SnCl is added into tartaric acid solution2, after stirring and dissolving, clear transparent solutions A is obtained, by SeO2, NaOH and
NaBH4Add in distilled water, clear solution B is made in stirring；
2) clear transparent solutions A is added in clear solution B, is stirring evenly and then adding into Morphological control agent, stirs evenly
After pour into autoclave, kept the temperature at 180 DEG C 6-24 it is small when, be subsequently cooled to room temperature, black flaky stannic selenide obtained after dry.
Of the invention further improve be, tartaric acid solution is, and wine obtained by the way that tartaric acid is added to the water
Stone acid and the ratio of water are 1.2g：20mL.
The present invention, which further improves, to be, SnCl2、SeO2, NaOH and NaBH4The ratio between the amount of material be 1：1：20：2.
Further improve of the invention is that Morphological control agent is 1,10- phenanthrolines, 2,2- bipyridyls or 4,4- join pyrrole
Pyridine.
The present invention, which further improves, to be, Morphological control agent and SnCl2The amount ratio of material is 1：1、1：2 or 2：1.
Further improve of the invention is, 180 DEG C are warming up to the programming rate of 5-10 DEG C/min from room temperature.
The present invention, which further improves, to be, cooled to room temperature.
Further improve of the invention is that drying carries out under vacuo, and dry temperature is 60-90 DEG C, the time
For 1-5 it is small when.
Compared with prior art, the beneficial effects of the invention are as follows：The present invention uses stannous chloride (SnCl2) and selenium dioxide
(SeO2) it is respectively tin source and selenium source, SeO2It is changed into SeO in the environment of highly basic NaOH32-, NaBH4Being added as reducing agent makes
It is further reduced into Se2-Ion, so that and Sn2+Ionic reaction, further generates stannic selenide.Added in water-heat process
The Morphological control agent of the amount of variety classes and material carries out SnSe the control of laminated structure thickness.Raw material in whole technical process
And the solution produced is disposable and pollution-free, manufacturing cost is low, and operating process is simple, and repeatability is high, can prepare high-purity
The sheet stannic selenide micron crystalline flour body of degree.In addition, the thickness of sheet SnSe can influence its photocatalysis performance in ultraviolet region, it is thick
Spend it is small, it is fast to the degradation rate of rhdamine B, so the present invention provides a kind of side for the thickness that can control sheet SnSe
Method.
Brief description of the drawings
Fig. 1 is the SEM photograph for the sheet SnSe for not adding phenanthroline in comparative example 1.
The XRD spectrum of Fig. 2 embodiments 1.
Fig. 3 is the SEM photograph of embodiment 1.
Fig. 4 is the correlation curve of the light degradation rhodamine B solution of SnSes of the SnSe with not adding phenanthroline in embodiment 1
Figure.
Fig. 5 is the XRD spectrum of embodiment 2.
Fig. 6 is the SEM photograph of embodiment 2.
Fig. 7 is the XRD spectrum of embodiment 3.
Fig. 8 is the SEM photograph of embodiment 3.
Embodiment
By specific embodiment, the present invention is described in detail below in conjunction with the accompanying drawings.
Embodiment 1
1) weigh 1.2g tartaric acid to be dissolved in 20mL distilled water, stirring is to dissolving, then weighs the stannous chloride addition of 1mmol
Wherein, it is in clear to stir to solution, and clear transparent solutions A is made.Selenium dioxide, the 0.8g hydrogen-oxygens of 1mmol is weighed respectively
The sodium borohydride for changing sodium and 2mmol is sequentially added in 15mL distilled water, stirs to obtain clear solution B.
2) clear transparent solutions A is slowly added into clear solution B, stirs 10min at room temperature, add 1mmol 1,
After 10- phenanthrolines stir evenly, it is transferred in the autoclave with polytetrafluoroethyllining lining, is subsequently placed into baking oven and carries out instead
Should, since room temperature, 180 DEG C are risen to the heating rate of 5 DEG C/min, when insulation 12 is small, following reaction system naturally cools to
Room temperature, opens water heating kettle, centrifuges and collects sample, at 60 DEG C of vacuum it is dry 5 it is small when after black flaky stannic selenide powder.
Comparative example 1
Prepare stannic selenide powder：Preparation process is in the same manner as in Example 1, and difference is to be added without 1,10- phenanthrolines.
Fig. 1 is the SEM photograph for not adding 1,10- phenanthrolines in comparative example 1, and the thickness of display sheet SnSe is about
150nm.Fig. 2 is the XRD spectrum of 1 product of embodiment, and imply that product is pure stannic selenide.1mmol is added as can be seen from Figure 3
1,10- phenanthrolines after, the thickness of sheet SnSe is reduced to about 70nm.Fig. 4 is shown in same time, and it is adjacent to add 1,10-
SnSe made from phenanthroline is about 88% in light degradation speed of the ultraviolet region to rhdamine B, adjacent more luxuriant and rich with fragrance than not adding 1,10-
SnSe made from Luo Lin improves about 20%.
Embodiment 2
1) weigh 1.2g tartaric acid to be dissolved in 20mL distilled water, stirring is to dissolving, then weighs the stannous chloride addition of 1mmol
Wherein, it is in clear to stir to solution, and clear transparent solutions A is made.Selenium dioxide, the 0.8g hydrogen-oxygens of 1mmol is weighed respectively
The sodium borohydride for changing sodium and 2mmol is sequentially added in 15mL distilled water, stirs to obtain clear solution B.
2) clear transparent solutions A is slowly added into clear solution B, stirs 10min at room temperature, add 1mmol 2,
After 2- bipyridyls stir evenly, it is transferred in the autoclave with polytetrafluoroethyllining lining, is subsequently placed into baking oven and is reacted, from
Room temperature starts, and 180 DEG C are risen to the heating rate of 5 DEG C/min, when insulation 12 is small, following reaction system cooled to room temperature,
Open water heating kettle, centrifuge and collect sample, at 90 DEG C of vacuum it is dry 1 it is small when after black flaky stannic selenide powder.
Fig. 5 is the XRD spectrum of product, and imply that product is pure stannic selenide.Fig. 6 shows the thickness of sheet SnSe in 50-
Between 100nm scopes.
Embodiment 3
1) weigh 1.2g tartaric acid to be dissolved in 20mL distilled water, stirring is to dissolving, then weighs the stannous chloride addition of 1mmol
Wherein, it is in clear to stir to solution, and clear transparent solutions A is made.Selenium dioxide, the 0.8g hydrogen-oxygens of 1mmol is weighed respectively
The sodium borohydride for changing sodium and 2mmol is sequentially added in 15mL distilled water, stirs to obtain clear solution B.
2) clear transparent solutions A is slowly added into clear solution B, stirs 10min at room temperature, add 1mmol 4,
After 4- bipyridyls stir evenly, it is transferred in the autoclave with polytetrafluoroethyllining lining, is subsequently placed into baking oven and is reacted, from
Room temperature starts, and 180 DEG C are risen to the heating rate of 5 DEG C/min, when insulation 12 is small, following reaction system cooled to room temperature,
Open water heating kettle, centrifuge and collect sample, at 70 DEG C of vacuum it is dry 2 it is small when after black flaky stannic selenide powder.
Fig. 7 is the XRD spectrum of product, and imply that product is pure stannic selenide.Fig. 8 illustrates that the thickness of sheet SnSe is about
60-70nm。
Embodiment 4
1) weigh 1.2g tartaric acid to be dissolved in 20mL distilled water, stirring is to dissolving, then weighs the stannous chloride addition of 1mmol
Wherein, it is in clear to stir to solution, and clear transparent solutions A is made.Selenium dioxide, the 0.8g hydrogen-oxygens of 1mmol is weighed respectively
The sodium borohydride for changing sodium and 2mmol is sequentially added in 15mL distilled water, stirs to obtain clear solution B.
2) clear transparent solutions A is slowly added into clear solution B, stirs 10min at room temperature, add 0.5mmol
1,10- phenanthrolines stir evenly after, be transferred in the autoclave with polytetrafluoroethyllining lining, be subsequently placed into baking oven progress
Reaction, since room temperature, rises to 180 DEG C, when insulation 12 is small, following reaction system natural cooling with the heating rate of 5 DEG C/min
To room temperature, open water heating kettle, centrifuge and collect sample, at 80 DEG C of vacuum it is dry 4 it is small when after sheet black stannic selenide powder.
Embodiment 5
1) weigh 1.2g tartaric acid to be dissolved in 20mL distilled water, stirring is to dissolving, then weighs the stannous chloride addition of 1mmol
Wherein, it is in clear to stir to solution, and clear transparent solutions A is made.Selenium dioxide, the 0.8g hydrogen-oxygens of 1mmol is weighed respectively
The sodium borohydride for changing sodium and 2mmol is sequentially added in 15mL distilled water, stirs to obtain clear solution B.
2) clear transparent solutions A is slowly added into clear solution B, stirs 10min at room temperature, then be separately added into
After 2, the 2- bipyridyls of 2.0mmol stir evenly, it is transferred in the autoclave with polytetrafluoroethyllining lining, is subsequently placed into baking oven
Reacted, since room temperature, rise to 180 DEG C, when insulation 12 is small with the heating rate of 5 DEG C/min, following reaction system is natural
Be cooled to room temperature, open water heating kettle, centrifuge and collect sample, at 80 DEG C of vacuum it is dry 2 it is small when after black flaky stannic selenide
Powder.
Embodiment 6
1) weigh 1.2g tartaric acid to be dissolved in 20mL distilled water, stirring is to dissolving, then weighs the stannous chloride addition of 1mmol
Wherein, it is in clear to stir to solution, and clear transparent solutions A is made.Selenium dioxide, the 0.8g hydrogen-oxygens of 1mmol is weighed respectively
The sodium borohydride for changing sodium and 2mmol is sequentially added in 15mL distilled water, stirs to obtain clear solution B.
2) clear transparent solutions A is slowly added into clear solution B, stirs 10min at room temperature, add 1.0mmol
4,4- bipyridyls stir evenly after, be transferred to one have polytetrafluoroethyllining lining autoclave in, be subsequently placed into baking oven into
Row reaction, since room temperature, rises to 180 DEG C, when insulation 6 is small, following reaction system natural cooling with the heating rate of 5 DEG C/min
To room temperature, open water heating kettle, centrifuge and collect sample, at 60 DEG C of vacuum it is dry 4 it is small when after black flaky stannic selenide powder.
Embodiment 7
1) it is 1.2g by the ratio of tartaric acid and water：Tartaric acid is added to the water obtained tartaric acid solution by 20mL, presses
SnCl2、SeO2, NaOH and NaBH4The ratio between the amount of material be 1：1：20：2, SnCl is added into tartaric acid solution2, stir molten
Xie Hou, obtains clear transparent solutions A, by SeO2, NaOH and NaBH4It is added sequentially in distilled water, clear solution B is made in stirring；
2) clear transparent solutions A is added in clear solution B, is stirring evenly and then adding into Morphological control agent, stirs evenly
After pour into autoclave, from room temperature with the programming rate of 5 DEG C/min be warming up to 180 DEG C and keep the temperature 6 it is small when, then naturally cool to
Room temperature, when vacuum drying 1-5 is small at 60-90 DEG C, obtains black flaky stannic selenide.
Wherein, Morphological control agent is 1,10- phenanthrolines, Morphological control agent and SnCl2The amount ratio of material is 1：1.
Embodiment 8
1) it is 1.2g by the ratio of tartaric acid and water：Tartaric acid is added to the water obtained tartaric acid solution by 20mL, presses
SnCl2、SeO2, NaOH and NaBH4The ratio between the amount of material be 1：1：20：2, SnCl is added into tartaric acid solution2, stir molten
Xie Hou, obtains clear transparent solutions A, by SeO2, NaOH and NaBH4It is added sequentially in distilled water, clear solution B is made in stirring；
2) clear transparent solutions A is added in clear solution B, is stirring evenly and then adding into Morphological control agent, stirs evenly
After pour into autoclave, from room temperature with the programming rate of 7 DEG C/min be warming up to 180 DEG C and keep the temperature 24 it is small when, then natural cooling
To room temperature, when vacuum drying 1-5 is small at 60-90 DEG C, black flaky stannic selenide is obtained.
Wherein, Morphological control agent is 2,2- bipyridyls, Morphological control agent and SnCl2The amount ratio of material is 1：2.
Embodiment 9
1) it is 1.2g by the ratio of tartaric acid and water：Tartaric acid is added to the water obtained tartaric acid solution by 20mL, presses
SnCl2、SeO2, NaOH and NaBH4The ratio between the amount of material be 1：1：20：2, SnCl is added into tartaric acid solution2, stir molten
Xie Hou, obtains clear transparent solutions A, by SeO2, NaOH and NaBH4It is added sequentially in distilled water, clear solution B is made in stirring；
2) clear transparent solutions A is added in clear solution B, is stirring evenly and then adding into Morphological control agent, stirs evenly
After pour into autoclave, from room temperature with the programming rate of 10 DEG C/min be warming up to 180 DEG C and keep the temperature 15 it is small when, then natural cooling
To room temperature, when vacuum drying 1-5 is small at 60-90 DEG C, black flaky stannic selenide is obtained.
Wherein, Morphological control agent is 4,4- bipyridyls, Morphological control agent and SnCl2The amount ratio of material is 2：1.
Claims (8)
1. a kind of Hydrothermal preparation method for controlling sheet stannic selenide thickness, it is characterised in that comprise the following steps：
1) SnCl is added into tartaric acid solution2, after stirring and dissolving, clear transparent solutions A is obtained, by SeO2, NaOH and NaBH4
Add in distilled water, clear solution B is made in stirring；
2) clear transparent solutions A is added in clear solution B, is stirring evenly and then adding into Morphological control agent, fallen after stirring evenly
Enter in autoclave, when insulation 6-24 is small at 180 DEG C, is subsequently cooled to room temperature, black flaky stannic selenide is obtained after dry.
A kind of 2. Hydrothermal preparation method for controlling sheet stannic selenide thickness according to claim 1, it is characterised in that tartaric acid
Solution is obtained by the way that tartaric acid is added to the water, and the ratio of tartaric acid and water is 1.2g：20mL.
A kind of 3. Hydrothermal preparation method for controlling sheet stannic selenide thickness according to claim 1, it is characterised in that SnCl2、
SeO2, NaOH and NaBH4The ratio between the amount of material be 1：1：20：2.
A kind of 4. Hydrothermal preparation method for controlling sheet stannic selenide thickness according to claim 1, it is characterised in that pattern tune
Control agent is 1,10- phenanthrolines, 2,2- bipyridyls or 4,4- bipyridyl.
A kind of 5. Hydrothermal preparation method of control sheet stannic selenide thickness according to claim 1 or 4, it is characterised in that shape
Looks adjusting control agent and SnCl2The amount ratio of material is 1：1、1：2 or 2：1.
6. a kind of Hydrothermal preparation method for controlling sheet stannic selenide thickness according to claim 1, it is characterised in that from room temperature
180 DEG C are warming up to the programming rate of 5-10 DEG C/min.
7. a kind of Hydrothermal preparation method for controlling sheet stannic selenide thickness according to claim 1, it is characterised in that naturally cold
But to room temperature.
8. a kind of Hydrothermal preparation method for controlling sheet stannic selenide thickness according to claim 1, it is characterised in that drying exists
Carried out under vacuum, and dry temperature is 60-90 DEG C, when the time is 1-5 small.
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| CN109742353A (en) * | 2018-12-29 | 2019-05-10 | 陕西科技大学 | A kind of SnSe quantum dot/r-GO compound and its preparation method and application |
| CN110240126A (en) * | 2019-06-14 | 2019-09-17 | 西安交通大学 | A kind of two stannic selenides of nanometer flower structure and preparation method thereof |
| CN110299510A (en) * | 2019-07-11 | 2019-10-01 | 青岛科技大学 | A kind of preparation using conductive carbon cloth as the bimetallic sulfide of substrate and its application in terms of negative electrode of lithium ion battery |
| CN111139519A (en) * | 2020-01-02 | 2020-05-12 | 深圳大学 | Preparation method of flaky SnSe monocrystal |
| WO2023082212A1 (en) * | 2021-11-13 | 2023-05-19 | 广东暨创硒源纳米研究院有限公司 | Tin selenide nanoparticle complex and use thereof with tumor-associated macrophages |
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| CN109742353A (en) * | 2018-12-29 | 2019-05-10 | 陕西科技大学 | A kind of SnSe quantum dot/r-GO compound and its preparation method and application |
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| CN110240126A (en) * | 2019-06-14 | 2019-09-17 | 西安交通大学 | A kind of two stannic selenides of nanometer flower structure and preparation method thereof |
| CN110240126B (en) * | 2019-06-14 | 2021-01-19 | 西安交通大学 | Tin diselenide with nanoflower structure and preparation method thereof |
| CN110299510A (en) * | 2019-07-11 | 2019-10-01 | 青岛科技大学 | A kind of preparation using conductive carbon cloth as the bimetallic sulfide of substrate and its application in terms of negative electrode of lithium ion battery |
| CN110299510B (en) * | 2019-07-11 | 2022-03-29 | 青岛科技大学 | Preparation of bimetallic sulfide with conductive carbon cloth as substrate and application of bimetallic sulfide in aspect of lithium ion battery cathode |
| CN111139519A (en) * | 2020-01-02 | 2020-05-12 | 深圳大学 | Preparation method of flaky SnSe monocrystal |
| WO2023082212A1 (en) * | 2021-11-13 | 2023-05-19 | 广东暨创硒源纳米研究院有限公司 | Tin selenide nanoparticle complex and use thereof with tumor-associated macrophages |
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| Publication number | Publication date |
|---|---|
| CN107934924B (en) | 2020-06-05 |
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