CN104291279A

CN104291279A - Preparation method of SnS3 nano powder

Info

Publication number: CN104291279A
Application number: CN201410502599.9A
Authority: CN
Inventors: 赵立东; 宫声凯; 常诚; 裴延玲
Original assignee: Beihang University
Current assignee: Beihang University
Priority date: 2014-09-26
Filing date: 2014-09-26
Publication date: 2015-01-21

Abstract

The invention discloses a preparation method of SnSe nano powder and belongs to the technical field of nano materials. The preparation method of the SnSe nano powder comprises the following steps: preparing high-purity substances of Sn element and Se element according to a stoichiometric ratio of a final product, putting the substances into a planet type high energy ball-milling machine for mechanical alloying under the protection of inert gas, carrying out dry grinding at a certain rotating speed, directly synthesizing a compound, then adding a certain amount of absolute ethyl alcohol, carrying out wet grinding, and finally drying, so that SnSe superfine powder is obtained. The preparation method of the SnSe nano powder has the advantages of available raw materials, short time and controllable particle size, and is easy to operate, so that the preparation method of the SnSe nano powder is applicable to mass production.

Description

A kind of preparation method of SnSe nano-powder

Technical field

The invention belongs to technical field of nano material, relate generally to a kind of preparation method of brand-new SnSe nano-powder.

Background technology

SnSe is a kind of important semiconductor material.It has potential using value in the field such as thermoelectricity, photodetection.In addition, its band gap is 1.0-1.5eV, is well suited for for thermoelectricity and photovoltaic cell field.For nanoparticle, size and the distribution situation of nanoparticle are most important, they directly affect its surface effects, quantum effect, small-size effect and macro quanta tunnel effect etc., thus cause its characteristic on optics, magnetics, electricity, calorifics and mechanics.Visible, the particle diameter yardstick of powder and pattern most important for the performance of material.Before, people explore various method and prepare SnSe nano structural material.Such as, the hybrid target of pulsed laser deposition Sn and Se powder is adopted to prepare SnSe film [Ming-Zhe Xue, Sun-Chao Cheng, Jia Yao, Zheng-Wen Fu.Electrochemical Properties of SnSe Thin Film Electrode Fabricated by Pulsed Laser Deposition.Acta Phys.Chim.Sin., 2006,22 (3): 383 ~ 387]; The SnSe powder of conventional solid reaction preparation and Se powder is utilized to utilize chemical vapour deposition (CVD) to prepare SnSe nano wire [Faheem K.Butt, Misbah Mirza, Chuanbao Cao, Faryal Idrees, Muhammad Tahir, Muhammad Safdar, Zulfiqar Ali, M.Tanveer and Imran Aslam.Synthesis of mid-infrared SnSe nanowires and their optoelectronic properties.CrystEngComm, 2014,16,3470]; Physical vaporous deposition prepares SnSe thin slice [Xing-Hua Ma, Ki-Hyun Cho and Yun-Mo Sung.Growth mechanism of vertically aligned SnSe nanosheets via physical vapour deposition.CrystEngComm, 2014,16,5080]; Evaporative condenser technique is utilized to prepare nanometer SnSe monocrystalline [Faheem K.Butt, Chuanbao Caoa, Waheed S.Khana, Zulfiqar Ali, R.Ahmed, Faryal Idrees, Imran Aslama, M.Tanveer, Jili Li, Sher Zaman, Tariq Mahmood.Synthesis of highly pure single crystalline SnSe nanostructures by thermal evaporation and condensation route.Mater.Chem.Phys.137 (2012) 565-570] etc.

Aforesaid method all adopts the method for vapour deposition to prepare nanometer SnSe, nanometer rete dense uniform prepared by CVD (Chemical Vapor Deposition) method, and some retes have excellent optics, calorifics and electric property.But vapour deposition product is the shortcomings such as fixing film layer structure, output is little, the time is long limits its application in real technique.Therefore seek a kind ofly easyly save time and the technique of mass-produced preparation nanometer SnSe powder can seem very necessary, and Mechanical Alloying just in time has these advantages.And Mechanical Alloying can make up the deficiency of CVD (Chemical Vapor Deposition) method.Simultaneously Mechanical Alloying can prepare the larger alloy cpd of alloying element fusing point difference, avoids being similar to the phenomenon such as uneven components and element evaporation in the material of smelting process synthesis.As for using the problems such as the incident reactant reaction of Mechanical Alloying is insufficient, reactant is oxidized, the invention provides solution.

Summary of the invention

The object of the present invention is to provide a kind of preparation method of SnSe nano-powder, achieve the simple preparation of nanometer SnSe powder, cost is low, the time is short, particle size is stable, can produce in enormous quantities.

The present invention adopts Mechanical Alloying to synthesize SnSe nano-powder, and concrete steps are as follows:

(1), adopt quality purity be greater than 99.5% granularity be 100 object Sn, Se simple substance powder as initial feed, by Sn:Se=1:1 atomic ratio batching, be mixed into powder;

(2), by (1) step mixed powder put into ball grinder, in order to prevent at ma process Raw Powder Oxidation, first carried out vacuumizing process by the ball grinder installing mixed powder, vacuum tightness is less than 6 Pa.In tank body, rare gas element (argon gas) is filled with after exhausting vacuum.In order to get rid of the air in tank body, by vacuumizing above-gas replenishment process circulation carries out more than 3 times.

(3), adopt the ball grinder that (2) step is equipped with the argon shield of mixed powder to start to carry out ball milling, rotating speed is 200 ~ 550rpm, and the time is 1h ~ 8h;

(4), in order to prevent powder agglomates, make its ball milling more even, in powder, add dehydrated alcohol after ball milling as medium wet-milling, while inlet mouth passes into argon gas, in air outlet, the graduated needle tubing of band injects dehydrated alcohol, to make in ball grinder steel ball by the complete submergence of dehydrated alcohol.First close air outlet after having injected dehydrated alcohol and close inlet mouth again; Wet-milling rotating speed is 100 ~ 250rpm, and the time is 15min ~ 180min;

(5), by the powder that (4) step obtains dry, bake out temperature is 30 DEG C, and the time is 3-12h, finally obtains SnSe powder;

The invention has the advantages that: compared with prior art, the generated time of SnSe powder body material be short, technique is simple, practical, can large-scale industrial production be carried out.

Accompanying drawing explanation

Fig. 1: the X ray diffracting characteristic collection of illustrative plates of SnSe powder prepared by the present invention;

Fig. 2: SnSe powder prepared by the present invention SnSe morphology microstructure under scanning electron microscope.

Embodiment

Below in conjunction with drawings and Examples, the present invention is described in detail.

The invention provides a kind of preparation method of SnSe nano-powder; in described preparation method; adopt Mechanical Alloying; first by high-purity Sn and Se elemental powders according to 1:1 atomic ratio proportioning; put into planetary ball mill together and carry out mechanical alloying under rare gas element (argon gas) protection; carry out wet-milling again after dry grinding synthetic compound, finally dry and obtain SnSe powder.

Table 1 gives and adopts preparation method provided by the invention, prepares several preferred embodiments of SnSe powder:

Table 1

Preferred reality

Mechanical alloying is dry grinded

Mechanical alloying wet-milling

Whether

Particle size

Execute example	Rotating speed (rpm)	Time (h)	Rotating speed (rpm)	Time (min)	Synthesis	(nm)
							Example 1	250	1	100	15	Be	90～100
Example 2	250	2	100	45	Be	90～100
							Example 3	250	4	100	90	Be	90～100
Example 4	250	8	100	120	Be	90～100
							Example 5	300	1	100	180	Be	90～100
Example 6	300	2	150	15	Be	90～100
							Example 7	300	4	150	45	Be	90～100
Example 8	300	8	150	90	Be	90～100
							Example 9	400	1	150	120	Be	90～100
Example 10	400	2	150	180	Be	90～100
							Example 11	400	4	200	15	Be	90～100
Example 12	400	8	200	45	Be	90～100
							Example 13	450	1	200	90	Be	90～100
Example 14	450	2	200	120	Be	90～100
							Example 15	450	4	200	180	Be	90～100
Example 16	450	8	250	15	Be	90～100
							Example 17	550	1	250	45	Be	90～100
Example 18	550	2	250	90	Be	90～100
							Example 19	550	4	250	120	Be	90～100
Example 20	550	8	250	180	Be	90～100

Above-described embodiment 1 ~ 20 is the SnSe nano-powder adopting preparation method provided by the invention to prepare.For mechanical alloying dry grinding rotating speed, be preferably 250 ~ 550 rpm.

Fig. 1 is the X-ray diffractogram of the SnSe nano-powder of preparation in embodiment 12, and all characteristic peaks of powder are SnSe characteristic spectral line (PDF#48-1224) as can be seen from Figure 1, show that mechanical alloying can synthesize SnSe compound.

Fig. 2 is the stereoscan photograph of the SnSe nano-powder of preparation in embodiment 12.From Fig. 2, we observe the particle size of SnSe powder at about 90 ~ 100 nm.On the basis can synthesizing single-phase SnSe powder, the particle size range of powder is substantially constant.

In sum, the present invention has been combined to SnSe nanometer powder by mechanical alloy.

Claims

1. a preparation method for SnSe nano-powder, is characterized in that:

The first step, adopts high-purity Sn, Se simple substance as initial feed, by Sn:Se=1:1 atomic ratio batching, is mixed into powder;

Second step, the first step mixed powder is put into ball grinder, carries out vacuumizing process, vacuum tightness is less than 6Pa, after exhausting vacuum, tank body is filled with rare gas element;

3rd step, adopts the ball grinder that second step is equipped with the protection of inert gas of mixed powder to carry out ball milling;

4th step, add dehydrated alcohol after ball milling as medium wet-milling, while ball grinder inlet mouth passes into rare gas element, in air outlet, needle tubing injects dehydrated alcohol, first closes air outlet and close inlet mouth again after having injected dehydrated alcohol;

5th step, dries the powder that the 4th step obtains, finally obtains SnSe nano-powder.

2. the preparation method of a kind of SnSe nano-powder as claimed in claim 1, it is characterized in that: in the first step, the quality purity of Sn powder, Se powder is all more than or equal to 99.5%, granularity is 100 orders.

3. the preparation method of a kind of SnSe nano-powder as claimed in claim 1, is characterized in that: rare gas element described in second step is argon gas.

4. the preparation method of a kind of SnSe nano-powder as claimed in claim 1, is characterized in that: vacuumize in second step-gas replenishment process circulation carries out 3 times.

5. the preparation method of a kind of SnSe nano-powder as claimed in claim 1, it is characterized in that: in the 3rd step, rotational speed of ball-mill is 200 ~ 550rpm, the time is 1 ~ 8h.

6. the preparation method of a kind of SnSe nano-powder as claimed in claim 1, it is characterized in that: in the 4th step, wet-milling rotating speed is 100 ~ 250rpm, the time is 15min ~ 180min.

7. the preparation method of a kind of SnSe nano-powder as claimed in claim 1, it is characterized in that: the 5th step, bake out temperature is 30 DEG C, and the time is 3 ~ 12h.

8. the preparation method of a kind of SnSe nano-powder as claimed in claim 1, is characterized in that: the particle diameter of the SnSe nano-powder prepared is 90 ~ 100nm.