CN112978685A - Pure-phase SnSe nano-particles and preparation method thereof - Google Patents

Pure-phase SnSe nano-particles and preparation method thereof Download PDF

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Publication number
CN112978685A
CN112978685A CN202110353584.0A CN202110353584A CN112978685A CN 112978685 A CN112978685 A CN 112978685A CN 202110353584 A CN202110353584 A CN 202110353584A CN 112978685 A CN112978685 A CN 112978685A
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pure
snse
phase
solution
stirring
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黄剑锋
王芳敏
李嘉胤
曹丽云
刘倩
王璐杰
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Abstract

The invention discloses a pure phase SnSe nano particle and a preparation method thereof, wherein the preparation method takes inorganic tin salt as a tin source and selenium powder as a selenium source, and utilizes a reducing agent to obtain a product after reaction for several hours by a one-step hydrothermal method, and the product is uniform nano particles. The SnSe nano-particles prepared by the method have small size and high purity, and can be better applied to the fields of electrochemistry, semiconductors and photocatalysis.

Description

Pure-phase SnSe nano-particles and preparation method thereof
Technical Field
The invention relates to the technical field of nanoparticle preparation, in particular to a pure-phase SnSe nanoparticle and a preparation method thereof.
Background
SnSe is an important IV-VI semiconductor material, has a forbidden band width of about 0.9eV, has good electrical and optical properties, and can be widely usedThe method is widely applied to infrared photoelectric devices, storage switches, thin film electrodes, solar cells and the like. Meanwhile, in the cathode material of the sodium ion battery, tin selenide is used as one of alloy cathode materials, and the sodium insertion capacity of the tin selenide is 780mAh g-1Has great development potential. Therefore, research on stannous selenide is a hot direction. Therefore, it is extremely necessary to search for a method for synthesizing SnSe.
According to the literature, the micro-morphology and the size of the material have a great influence on the performance (optical performance, electrical performance, etc.) of the material, and thus the control of the micro-morphology and the size of the material becomes a hot spot for many researchers to study. For example, the Cuiyuzi 21855Liang and the like adopt an arc method to prepare stannous selenide with a square sheet structure; the Sheng Liu and the like adopt a heat injection method to synthesize the stannous selenide single-crystal nanowire at 290 ℃; shuang Yuan et al synthesized a single crystal SnSe nanosheet cluster by an ion exchange method.
The currently reported synthesis methods of tin selenide mainly fall into two categories: liquid phase methods (hydrothermal, solvothermal, precipitation, sol-gel, etc.) and solid phase methods (chemical/physical vapor deposition, high energy ball milling, etc.). However, the preparation method generally has the characteristics of long reaction time, small yield, complex chemical reaction process, need of adding a reaction catalyst, dependence on substrate growth and the like, so that the synthesis cost is overhigh, the preparation process is easy to generate secondary pollution to the environment and the like.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides the pure-phase SnSe nanoparticles and the preparation method thereof, the preparation method has simple process and high repeatability, no template agent or catalyst is required to be added, the liquid phase synthesis is favorable for controlling the morphology of the product, the energy consumption and the generation cost are saved, and the prepared pure-phase SnSe nanoparticles have the advantages of small size and high purity.
In order to achieve the above object, the present invention provides a method for preparing pure phase SnSe nanoparticles, comprising the steps of:
1) adding 0.02278 g-2.278 g of inorganic tin salt into 30-80 mL of ethylene glycol or glycerol, stirring, and adding 0.02 g-0.2 g of surfactant until the inorganic tin salt is completely dissolved to obtain a solution A;
2) adding 0.0079 g-0.79 g of selenium powder into 2-8 ml of reducing solvent, and stirring until the selenium powder is completely dissolved to obtain wine red solution B;
3) dropwise adding the solution B into the solution A and stirring to obtain a mixed solution C;
4) and carrying out hydrothermal reaction on the mixed solution C at the temperature of 120-240 ℃, cooling after the reaction is finished, separating to obtain black powder, and drying the obtained powder to obtain the pure-phase SnSe nanoparticles.
Further, the inorganic tin salt is SnCl2·2H2O。
Further, the surfactant is PVP, CTAB, or EDTA.
Further, the reducing solvent is ethylenediamine, triethanolamine, hydrazine hydrate or sodium borohydride aqueous solution.
Further, magnetic stirring is adopted for stirring, the stirring speed is 400-800 r/min, and the stirring time is 50-100 min.
Furthermore, the hydrothermal reaction adopts a hydrothermal kettle and is carried out in a hydrothermal reactor.
Further, the filling degree of the hydrothermal kettle is controlled to be 30-80%.
Further, after the reaction in the step 4) is finished, black powder is obtained through repeated washing and centrifugal separation.
The invention also provides a pure phase SnSe nanoparticle prepared by the preparation method of the pure phase SnSe nanoparticle.
Further, the size of the pure phase SnSe nano-particles is 7-15 nm.
Compared with the prior art, the preparation method takes the inorganic tin salt as a tin source, the selenium powder as a selenium source and the hydrazine hydrate as a reducing agent; the reaction lasts for several hours to obtain the product which is uniform nano-particles. The preparation method is simple, has high repeatability, does not need to add any template agent and catalyst, is beneficial to controlling the appearance of a product by liquid phase synthesis, saves energy consumption and production cost, and is suitable for large-scale production. The size of the SnSe nano-particles prepared by the method is about 7-15 nm, the size of the product is very small, the purity is high, and the SnSe nano-particles can be well applied to the fields of electrochemistry, semiconductors and photocatalysis.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of phase-pure SnSe nanoparticles prepared in example 3 of the present invention;
fig. 2 is a Scanning Electron Microscope (SEM) photograph of pure phase SnSe nanoparticles prepared in example 3 of the present invention.
Detailed Description
The present invention will be further explained with reference to the drawings and specific examples in the specification, and it should be understood that the examples described are only a part of the examples of the present application, and not all examples. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The invention provides a preparation method of pure-phase SnSe nanoparticles, which specifically comprises the following steps:
firstly, 0.02278 g-2.278 g of SnCl is added under the condition of room temperature2·2H2Adding O into 30-80 mL of ethylene glycol or glycerol, uniformly stirring, and then adding 0.02-0.2 g of surfactant until the surfactant is completely dissolved to form a solution A, wherein the surfactant is PVP, CTAB or EDTA; then weighing 0.0079 g-0.79 g of Se powder, adding the Se powder into 2-8 ml of reducing solvent, and stirring until the Se powder is completely dissolved to form a wine red solution B, wherein the reducing solvent is ethylenediamine, triethanolamine, hydrazine hydrate or sodium borohydride aqueous solution; secondly, dropwise adding the solution B into the solution A to form a mixed solution C, and uniformly stirring; and finally, transferring the mixed solution C into a hydrothermal kettle, placing the hydrothermal kettle into a hydrothermal reactor, fully reacting at 120-240 ℃, cooling to room temperature along with the furnace after the reaction is finished, repeatedly washing and centrifugally separating to obtain black powder, and drying the separated powder to obtain pure-phase SnSe nanoparticles. Preferably, the stirring is magnetic stirring, the stirring speed is 400-800 r/min, the stirring time is 50-100 min, the filling degree of the hydrothermal kettle is controlled to be 30-80%, and the hydrothermal reaction time is 8-1And 6 h. Washing is carried out by alternately washing with deionized water and absolute ethyl alcohol.
The invention also provides the pure-phase SnSe nanoparticles prepared by the preparation method, wherein the size of the pure-phase SnSe nanoparticles is about 7-15 nm, and the pure-phase SnSe nanoparticles can be applied to the fields of electrochemistry, semiconductors, photocatalysis and the like, and can be applied to infrared photoelectric devices, storage switches, thin film electrodes, solar cells and the like.
The present invention will be described with reference to specific examples.
Example 1:
0.02278g of SnCl are initially introduced2·2H2Adding O into 30mL of ethylene glycol, stirring uniformly, and then adding 0.02g of a surfactant PVP until the surfactant PVP is completely dissolved to form a solution A; then 0.0079g of selenium powder is weighed and added into 2ml of hydrazine hydrate, and the mixture is stirred until the selenium powder is completely dissolved to form a wine red solution B; secondly, dropwise adding the solution B into the solution A to form a mixed solution C, and stirring the solution C on a magnetic stirrer at the speed of 600r/min for 0.5 h; and finally, transferring the mixed solution C into a hydrothermal kettle, placing the hydrothermal kettle into a hydrothermal reactor, reacting for 12 hours at 120 ℃, cooling to room temperature along with the furnace after the reaction is finished, repeatedly washing and centrifuging to obtain black powder, and drying the powder obtained by separation to obtain pure-phase SnSe nanoparticles.
Example 2:
0.1623g SnCl2·2H2Adding O into 50mL of glycerol, stirring uniformly, and then adding 0.162g of surfactant CTAB until the surfactant CTAB is completely dissolved to form a solution A; then 0.0432g of selenium powder is weighed and added into 3ml of triethanolamine, and the mixture is stirred until the selenium powder is completely dissolved to form a wine red solution B; secondly, dropwise adding the solution B into the solution A to form a mixed solution C, and stirring the solution C on a magnetic stirrer at the speed of 500r/min for 1 h; and finally, transferring the mixed solution C into a hydrothermal kettle, placing the hydrothermal kettle into a hydrothermal reactor, reacting for 8 hours at 120 ℃, cooling to room temperature along with the furnace after the reaction is finished, repeatedly washing and centrifuging to obtain black powder, and drying the separated powder to obtain pure-phase SnSe nanoparticles.
Example 3:
0.3122g of SnCl are initially introduced2·2H2Adding O into 60mL of glycol, stirring uniformly, and then adding 0.1g of surfactant EDTA until the surfactant EDTA is completely dissolved to form a solution A; then 0.0811g of selenium powder is weighed and added into 5ml of hydrazine hydrate, and the mixture is stirred until the selenium powder is completely dissolved to form a wine red solution B; secondly, dropwise adding the solution B into the solution A to form a mixed solution C, and stirring the solution C on a magnetic stirrer at the speed of 400r/min for 1.5 h; and finally, transferring the mixed solution C into a hydrothermal kettle, then placing the hydrothermal kettle into a hydrothermal reactor, reacting for 12 hours at 140 ℃, cooling to room temperature along with the furnace after the reaction is finished, then repeatedly washing and centrifuging to obtain black powder, and drying the powder obtained by separation to obtain pure-phase SnSe nanoparticles.
The sample (SnSe nanoparticles) was analyzed by a Japanese science D/max2000 PCX-ray diffractometer, and as a result, referring to FIG. 1, it was found that the sample was consistent with the structure of SnSe of orthorhombic system with JCPDS numbers 89-0232, indicating that this method can produce pure phase SnSe nanoparticles. The sample is observed by a Field Emission Scanning Electron Microscope (FESEM), and the result is shown in figure 2, so that the prepared SnSe product is uniform nanoparticles of 7-15 nanometers, and the particle size of the nanoparticles is uniform.
Example 4:
0.4257g of SnCl are initially introduced2·2H2Adding O into 30mL of glycerin, stirring uniformly, and then adding 0.063g of surfactant CTAB until completely dissolving to form a solution A; then 0.138g of selenium powder is weighed and added into 2ml of sodium borohydride, and the mixture is stirred until the selenium powder is completely dissolved to form wine red solution B; secondly, dropwise adding the solution B into the solution A to form a mixed solution C, and stirring the solution C on a magnetic stirrer at the speed of 600r/min for 0.5 h; and finally, transferring the mixed solution C into a hydrothermal kettle, placing the hydrothermal kettle into a hydrothermal reactor, reacting for 10 hours at 160 ℃, cooling to room temperature along with the furnace after the reaction is finished, repeatedly washing and centrifuging to obtain black powder, and drying the powder obtained by separation to obtain pure-phase SnSe nanoparticles.
Example 5:
first, 1.139g of SnCl2·2H2Adding O into 70mL of ethylene glycol, stirring uniformly, and then adding 0.1g of PVP (polyvinyl pyrrolidone) as a surfactant until the PVP is completely dissolved to form a solution A; then 0.395g of Se powder is weighed and addedAdding into 6ml of ethylenediamine, and stirring until the ethylenediamine is completely dissolved to form a wine red solution B; secondly, dropwise adding the solution B into the solution A to form a mixed solution C, and stirring the solution C on a magnetic stirrer at the speed of 700r/min for 1.2 h; and finally, transferring the mixed solution C into a hydrothermal kettle, placing the hydrothermal kettle into a hydrothermal reactor, fully reacting at 240 ℃, cooling to room temperature along with the furnace after the reaction is finished, repeatedly washing and centrifugally separating to obtain black powder, and drying the separated powder to obtain pure-phase SnSe nanoparticles.
Example 6:
2.278g SnCl2·2H2Adding O into 80mL of glycerol, stirring uniformly, and then adding 0.2g of surfactant until the surfactant is completely dissolved to form a solution A; weighing 0.79g of selenium powder, adding the selenium powder into 8ml of hydrazine hydrate, and stirring until the selenium powder is completely dissolved to form a wine red solution B; then dropwise adding the solution B into the solution A to form a mixed solution C, and stirring the solution C on a magnetic stirrer at the speed of 500r/min for 1 h; and transferring the mixed solution C into a hydrothermal kettle, then placing the hydrothermal kettle into a hydrothermal reactor, reacting for 14h at 220 ℃, cooling to room temperature along with the furnace after the reaction is finished, then repeatedly washing and centrifuging to obtain black powder, and drying the powder obtained by separation to obtain pure-phase SnSe nanoparticles.
The pure-phase SnSe nano-particles are prepared by a one-step solvothermal method, and the size of the nano-particles is about 7-15 nm. The preparation method is simple, has high repeatability, does not need to add any template agent and catalyst, is beneficial to controlling the appearance of a product by liquid phase synthesis, saves energy consumption and production cost, and is suitable for large-scale production. The product has small size and high purity, and can be well applied to the fields of electrochemistry, semiconductors and photocatalysis.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. A preparation method of pure-phase SnSe nanoparticles is characterized by comprising the following steps:
1) adding 0.02278 g-2.278 g of inorganic tin salt into 30-80 mL of ethylene glycol or glycerol, stirring, and adding 0.02 g-0.2 g of surfactant until the inorganic tin salt is completely dissolved to obtain a solution A;
2) adding 0.0079 g-0.79 g of selenium powder into 2-8 ml of reducing solvent, and stirring until the selenium powder is completely dissolved to obtain wine red solution B;
3) dropwise adding the solution B into the solution A and stirring to obtain a mixed solution C;
4) and carrying out hydrothermal reaction on the mixed solution C at the temperature of 120-240 ℃, cooling after the reaction is finished, separating to obtain black powder, and drying the obtained powder to obtain the pure-phase SnSe nanoparticles.
2. The method of claim 1, wherein the inorganic tin salt is SnCl2·2H2O。
3. The method of claim 1, wherein the surfactant is PVP, CTAB, or EDTA.
4. The method of claim 1, wherein the reducing solvent is ethylenediamine, triethanolamine, hydrazine hydrate, or aqueous sodium borohydride solution.
5. The method for preparing the pure-phase SnSe nanoparticles as claimed in claim 1, wherein magnetic stirring is adopted, the stirring speed is 400-800 r/min, and the stirring time is 50-100 min.
6. The method for preparing the pure-phase SnSe nanoparticles as claimed in claim 1, wherein the hydrothermal reaction is carried out in a hydrothermal reactor.
7. The method for preparing pure-phase SnSe nanoparticles according to claim 6, wherein the filling degree of the hydrothermal kettle is controlled to be 30-80%.
8. The method for preparing pure-phase SnSe nanoparticles according to claim 1, wherein black powder is obtained by repeated washing and centrifugal separation after the reaction in the step 4).
9. A phase-pure SnSe nanoparticle prepared by the method of any one of claims 1 to 8.
10. The phase-pure SnSe nanoparticle of claim 9, wherein the size of the phase-pure SnSe nanoparticle is 7-15 nm.
CN202110353584.0A 2021-04-01 2021-04-01 Pure-phase SnSe nano-particles and preparation method thereof Pending CN112978685A (en)

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CN101214932A (en) * 2008-01-08 2008-07-09 上海大学 Method for preparing nanometer tin selenide
CN104617271A (en) * 2015-01-29 2015-05-13 中南大学 Stannic selenide/graphene oxide negative pole composite material for sodium ion battery and preparation method thereof
US20180170754A1 (en) * 2015-06-01 2018-06-21 Baoshan Iron & Steel Co., Ltd. Aqueous-based method of preparing metal chalcogenide nanomaterials
CN105923612A (en) * 2016-04-20 2016-09-07 南方科技大学 Metal-chalcogen semiconductor material as well as preparation method and application thereof
CN106744728A (en) * 2016-12-19 2017-05-31 陕西科技大学 A kind of method that room temperature liquid phase method prepares SnSe micron balls
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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Application publication date: 20210618