CN104831362A

CN104831362A - Method for preparing tin selenide single-crystal nano-belt

Info

Publication number: CN104831362A
Application number: CN201510304669.4A
Authority: CN
Inventors: 简基康; 郭靓; 曹丙垒; 雷仁博
Original assignee: Guangdong University of Technology
Current assignee: Guangdong University of Technology
Priority date: 2015-06-08
Filing date: 2015-06-08
Publication date: 2015-08-12

Abstract

The invention relates to a method for preparing a tin selenide single-crystal nano-belt, in particular to method for directly using solvent thermal reaction to prepare the tin selenide single-crystal nano-belt, and belongs to the technical field of semiconductor nano materials. The method includes: adding a certain amount of Se powder and SnCl2.2H2O according to the mole ratio of 1:1 into a high-pressure reaction kettle, then adding organic solvent ethanol amine solution, keeping the high-pressure reaction kettle in the temperature of 200 DEG C for 12-48 hours to perform the solvent thermal reaction, washing reaction products with deionized water and anhydrous ethanol, and performing vacuum drying and collecting final products to obtain the tin selenide single-crystal nano-belt. The method has the advantages that the tin selenide single-crystal nano-belt prepared by the method is good in product crystallinity and dispersity and low in environment pollution, and the method is simple, and easy to operate and popularize.

Description

A kind of method preparing Tin diselenide single crystal nano-belt

Technical field

The present invention relates to a kind of method preparing Tin diselenide single crystal nano-belt, be a kind of method directly being prepared Tin diselenide single crystal nano-belt by solvent thermal, belong to semiconductor nano material technical field.

Background technology

Tin diselenide is a kind of promising lead-free binary IV-VI race's compound semiconductor material, and be a kind of P-type semiconductor, its direct band gap and indirect band gap are respectively 1.3eV and 0.9eV, meet optimal absorption bandgap range 1.0eV to the 1.5eV of solar cell.Tin diselenide is the crystalline structure of rhombic system, in Tin diselenide tin atom and selenium atom be strapped in tightly together with become stratiform and C uranium pile along crystallization is long-pending together, between layers by faint Van der Waals force bonding, Tin diselenide is made to present laminate structure, this structure causes Tin diselenide compound physical property demonstrates obvious anisotropy, makes all to have great importance to its application and fundamental research.Tin diselenide semiconductor compound is at switch device, and infrared electro device, all has application in various degree in the fields such as the anode material of chargeable lithium battery and solar cell device.

Scientific research in recent years shows, nano material can demonstrate the physicochemical property of some excellences, has important using value in industrial technical field.At present, have some achievements report to the research of Tin diselenide nanostructure growth, common preparation method has: electrochemical deposition method, hydro-thermal solvent-thermal method etc.

Electrochemical deposition method: N.R.Mathews adopted the method for electrochemical deposition plated film to prepare SnSe film as 2012, and had photoelectric response, and the thin-film solar cells of preparation has the efficiency of 0.03%.Its electrolytic solution uses SnCl ₂and H ₂seO ₃the pH value be made into is the acidic solution between 2-3, uses HCl solution to regulate its pH value; Transparent conductive oxide is as working electrode and negative electrode, and saturated calomel electrode makes reference electrode, and platinized platinum, as to electrode, finally obtains the SnSe film that average crystal grain size is 18 nm, consults SOLAR ENERGY. the 86th volume the 1010th page.

Hydrothermal method (solvent-thermal method): if the people such as S.Z.Kang in 2012 are with SnCl ₂2H ₂0, dimethyl diselenide ether is that precursor has prepared the SnSe nanometer sheet of high crystalline quality, wherein SnCl ₂2H ₂0 is made into aqueous phase solution, dimethyl diselenide ether is then made into oil-phase solution, the solution of two kinds of phases joins in autoclave and reacts, obtaining nanometer sheet mean size is 120 nm × 120nm, and the nanocrystalline of synthesis has obvious electrochemical activity and can be used as in lithium ion battery, consults COLLOIDS AND SURFACES A-PHYSICOCHEMICAL AND ENGINEERING ASPECTS the 406th volume page 1.

Existing technology, operation process is numerous and diverse, and use solvent thermal single stage method to prepare Tin diselenide single crystal nano-belt to have not been reported, the method technical process is simple, pollute little, products therefrom crystallinity, dispersiveness better, are easy to promote, therefore can be applicable to the preparation of other IV-VI race semiconductor material nanostructures.

Summary of the invention

The object of this invention is to provide a kind of method preparing Tin diselenide single crystal nano-belt.

For achieving the above object, the technical solution used in the present invention is as follows:

In autoclave, in molar ratio for 1:1 adds a certain amount of Se powder and SnCl ₂2H ₂o, then add organic solvent ethanolamine solutions, autoclave is put and keeps 12 ~ 48 hours at 200 DEG C of temperature, carry out solvent thermal reaction; By reaction product deionized water, washes of absolute alcohol, vacuum-drying also collects final product, is Tin diselenide single crystal nano-belt.

The add-on of described organic solvent is every mmole selenium powder or SnCl ₂2H ₂o adds 30-40mL; Described selenium powder and SnCl ₂2H ₂o is that business is bought.

The invention has the beneficial effects as follows: compared with prior art, the present invention uses solvent thermal single stage method to prepare Tin diselenide single crystal nano-belt, product crystallinity, dispersiveness are better, environmental pollution is little, experimental technique is simple, easy handling, popularization, thus have important researching value and wide application prospect.

Accompanying drawing explanation

Fig. 1 is the X-ray diffractogram of gained sample in embodiment 1;

Fig. 2 is the scanning electron microscope diagram sheet of gained sample in embodiment 1;

Fig. 3 is the transmission electron micrograph of gained sample in embodiment 1;

Fig. 4 is the selected area electron diffraction picture of gained sample in embodiment 1.

Embodiment

Be described in further details the present invention below by example, these examples are only used for the present invention is described, do not limit the scope of the invention.

Embodiment 1

In autoclave, add the Se powder of 1mmol and the SnCl of 1mmol ₂2H ₂o, then add 30mL organic solvent ethanolamine solutions, autoclave is put and keeps 24 hours at 200 DEG C of temperature, carry out solvent thermal reaction; By reaction product deionized water, washes of absolute alcohol, vacuum-drying also collects final product.The X-ray diffractogram analytical results of products therefrom shows that it is the rhombic system Tin diselenide along (400) direction preferential growth, as shown in Figure 1; Scanning electron microscope diagram microcosmic shows this technique prepares Tin diselenide nano belt, and be with well-regulated geometric shape, as shown in Figure 2; The thinner thickness of the visible gained sample of its transmission electron microscope figure, as shown in Figure 3; Selected area electron diffraction pattern can find out that this product is monocrystalline, as shown in Figure 4.

Embodiment 2

In autoclave, add the Se powder of 2mmol and the SnCl of 2mmol ₂2H ₂o, then add 80mL organic solvent ethanolamine solutions, autoclave is put and keeps 48 hours at 200 DEG C of temperature, carry out solvent thermal reaction; By reaction product deionized water, washes of absolute alcohol, vacuum-drying also collects final product.

Embodiment 3

In autoclave, add the Se powder of 1mmol and the SnCl of 1mmol ₂2H ₂o, then add 40mL organic solvent ethanolamine solutions, autoclave is put and keeps 12 hours at 200 DEG C of temperature, carry out solvent thermal reaction; By reaction product deionized water, washes of absolute alcohol, vacuum-drying also collects final product.

Embodiment 4

In autoclave, add the Se powder of 3mmol and the SnCl of 3mmol ₂2H ₂o, then add 90mL organic solvent ethanolamine solutions, autoclave is put and keeps 36 hours at 200 DEG C of temperature, carry out solvent thermal reaction; By reaction product deionized water, washes of absolute alcohol, vacuum-drying also collects final product.

Claims

1. prepare a method for Tin diselenide single crystal nano-belt, it is characterized in that: comprise the steps:

In autoclave, in molar ratio for 1:1 adds selenium Se powder, SnCl ₂2H ₂o and organic solvent, put autoclave and keep 12-48 hour at 200 DEG C of temperature, carry out solvent thermal reaction; Then by reaction product deionized water and washes of absolute alcohol, vacuum-drying also collects final product.

2. a kind of method preparing Tin diselenide single crystal nano-belt according to claim 1, is characterized in that: described organic solvent is ethanolamine solutions.

3. a kind of method preparing Tin diselenide single crystal nano-belt according to claim 1 or 2, is characterized in that: the add-on of described organic solvent is every mmole selenium powder or SnCl ₂2H ₂o adds 30-40mL.