CN107827087A

CN107827087A - A kind of preparation method of the tellurium nano-wire of rule bending

Info

Publication number: CN107827087A
Application number: CN201711413606.8A
Authority: CN
Inventors: 韩金玲; 吕振瑞
Original assignee: Individual
Current assignee: Individual
Priority date: 2017-12-24
Filing date: 2017-12-24
Publication date: 2018-03-23
Anticipated expiration: 2037-12-24
Also published as: CN107827087B

Abstract

A kind of preparation method of the tellurium nano-wire of rule bending, deionized water is handled using high-intensity magnetic field, its polarity of deionized water after treatment has a very large change, in nano materials, this different and common deionized water, afterwards, under the collective effect of reducing agent and surfactant, the tellurium nano-wire for the rule bending being not directly available before having synthesized, the pattern of tellurium nano-wire is widened, when synthesizing other materials as hard mould agent using tellurium nano-wire, change the pattern and performance of respective material.

Description

A kind of preparation method of the tellurium nano-wire of rule bending

Technical field

The present invention relates to a kind of morphology controllable preparing technical field of semiconductor nano material, and in particular to a kind of tellurium nanometer The bending controlledly synthesis of line.

Background technology

Monodimension nanometer material includes nano wire, nanotube, nanofiber and nanobelt etc., compared to the nanometer of zero dimension Grain, quantum dot, two-dimentional nanometer sheet, the structure such as three-dimensional macroscopic view, the unique structure of monodimension nanometer material, especially it is very high Draw ratio, this causes monodimension nanometer material to have the properties such as good light, electricity, sound and calorifics, and the shape of monodimension nanometer material Looks have very big influence to its property, because when the size of material is less than to a certain degree, such as less than 10nm, this is to receive Rice material shows very strong quantum tunneling effect in a direction so that the property of material is different from conventional bulk body.Thus, it is right There is extensive research in its synthesis.

At present, the synthesis mechanism on one-dimensional nano line mainly has what University of California Berkeley professor Yang Peidong proposed VLS（Vapor-Liquid-Solid）Growth mechanism, its main points of view are the formation at the top of nano wire by catalyst droplets, Follow-up atom to be synthesized is promoted constantly to assemble growth, the wherein diameter of nano wire is mainly the size control by catalyst droplets System；Also traditional solvent process for thermosynthesizing, especially hydrothermal method have consequence wherein；Except above-mentioned chemistry Synthetic method, also Many researchers synthesize length, the nano wire of morphology controllable using the method for physics, such as use anodic oxidation Aluminium（AOO）Do hard template, it is synthetic after by removing template, you can obtain the controllable suitable nano wire of length and diameter.

Tellurium nano-wire, it is a kind of p-type semiconductor monodimension nanometer material, its band-gap energy is 0.35eV, can widely be answered For opto-electronic device, there is good response characteristics to light.Also there are very extensive research and application for it, as TaiWan, China is big An entitled " Preparation of Fluorescent of the Huan-Tsung Chang professors in 2010 In Tellurium Nanowires at Room Temperature " article, it passes through with tellurium dioxide（TeO2）For tellurium Source, add reducing agent hydrazine hydrate after direct-reduction prepare tellurium nano-wire, by the regulation and control to the reaction time, can be very good to control The draw ratio of tellurium nano-wire, such as controlling the reaction time, the length for the tellurium nano-wire prepared rises to from 251 from 40-120min 879nm, and its diameter only increases to 19nm from 8nm.Chinese patent（CN102910595A）Disclose a kind of ultra-fine tellurium nano-wire Magnanimity preparation method, comprise the following steps：The effect of sodium tellurite and reducing agent in polyvinylpyrrolidone pH value regulator Under react, obtain reactant mixture；The reactant mixture is rapidly cooled down with cold water and obtains tellurium nano-wire mother liquor, solubilizer Tellurium nano-wire is obtained after extraction.After present invention reaction obtains reactant mixture, rapidly cooling is carried out to it using cold water and prepares tellurium Nano wire, gained tellurium nano-wire quality is more homogeneous, and diameter is thinner；Further, the present invention is easy to big by optimizing preparation condition Amount synthesis, easy popularization and application；Although the tellurium nano-wire prepared by this method can realize prepared by magnanimity, it is prepared Nano wire be all linear pattern, during as template, the product necessarily obtained is also linear pattern.And it is known that nanometer Material, especially small-sized nano material, its pattern have a great impact to property, and different patterns can be brought in nature Huge difference.

The content of the invention

It is single in order to solve the above-mentioned tellurium nano-wire pattern synthesized, it is linear shortcoming, widens tellurium nano-wire Pattern, when synthesizing other materials as hard mould agent using tellurium nano-wire, change the pattern and performance of respective material, applicant passes through Substantial amounts of literature survey and continuous experiment Innovatation, spy propose following technical scheme, are received with synthesizing a kind of tellurium of rule bending Rice noodles.

A kind of preparation method of the tellurium nano-wire of rule bending, comprises the following steps：

1）, weigh appropriate tellurium source, be dissolved in treated deionized water, after stirring, obtain solution A；

2）, under conditions of stirring, appropriate cationic surfactant is added into solution A, continues stirring and obtains solution B；

3）, obtained solution B is transferred in three-necked flask, three-necked flask is placed in oil bath pan and carries out heating stirring, is added Enter appropriate reducing agent and be passed through the inert atmosphere of nitrogen maintenance reaction system into reaction bulb simultaneously；

4）, under continuous stirring, after certain time, stop reaction, reaction bulb be placed in cold water and is down to room temperature, i.e., It can obtain the tellurium nano-wire of final rule bending.

Preferably, step 1）In, described tellurium source includes the one or more in tellurium dioxide, sodium tellurite, llurate.

Preferably, step 1）In, described treated deionized water refers to deionized water in 2-5T magnetic field Magnetization treatment is carried out, the magnetization is completed in Chinese Academy of Sciences's high-intensity magnetic field center.

Preferably, step 2）In, described cationic surfactant refers to dodecylamino acetic acid, octadecyl three One or more in ammonio methacrylate, alkyl dimethyl octyl group ammonium chloride, mainly some quaternaries cation surfaces are lived Property agent.

Preferably, step 3）In, the temperature setting of oil bath pan is 100-120 DEG C, and the reaction time is 0.5-2 hours.

Preferably, step 3）In, the nitrogen flow refers to 10-50ml/min.

Preferably, step 3）In, the reducing agent refers to the one or more in hydrazine hydrate, ammoniacal liquor, HI, vulcanized sodium.

Preferably, step 4）In, stirring refers to that rotating speed is 100-200rpm.

The principle of the present invention is, is first handled deionized water using high-intensity magnetic field, deionization after treatment Its polarity of water has a very large change, and in nano materials, this different and common deionized water, afterwards, is reducing Under the collective effect of agent and surfactant, the tellurium nano-wire for the rule bending being not directly available before having synthesized.

Compared with prior art, the present invention has technique effect beneficial below：

1）, the invention used magnetization after deionized water do reaction dissolvent, successfully prepare rule bending tellurium Nano wire；

2）, the present invention provide the reaction energy using oil bath pan, the defects of avoiding traditional hydrothermal synthesis method, Hydrothermal Synthesiss need To carry out at high temperature under high pressure, this constitutes very big obstacle for extension production；

3）, present invention uses cationic surfactant, especially quaternary ammonium salt surface active agent, this kind of surfactant tool There is very strong alkalescence, can avoid with the acid-base value of maintenance reaction system and reuse alkaline matter regulation reaction system, optimization Experiment condition so that reaction is simpler, and obtained tellurium nano-wire has very homogeneity, and its draw ratio is more than 1000.

Brief description of the drawings

The high power SEM photograph of the tellurium nano-wire of rule bending prepared by Fig. 1 present invention；

The low power SEM photograph of the tellurium nano-wire of rule bending prepared by Fig. 2 present invention；

The XRD piece of the tellurium nano-wire of rule bending prepared by Fig. 3 present invention；

The SEM photograph of tellurium nano-wire prepared by Fig. 4 comparative examples 1 of the present invention.

Embodiment

Technical scheme is further described below, but is not so limited, it is every to the technology of the present invention Scheme is modified or equivalent substitution, without departing from the spirit and scope of technical solution of the present invention, all should cover in the present invention Protection domain in.

Embodiment 1

0.1g sodium tellurite is weighed, is dissolved in deionized waters of the 100ml after the magnetic field magnetization that field strength is 2T, stirs After mixing uniformly, solution A is obtained；Under conditions of stirring, 5g OTACs are added into solution A, continue to stir Mix to obtain solution B；Obtained solution B is transferred in three-necked flask, three-necked flask is placed in 100 DEG C of oil bath pan and carried out Heating stirring, add 15ml hydrazine hydrate and be passed through the inert atmosphere of nitrogen maintenance reaction system, nitrogen into reaction bulb simultaneously Throughput is controlled in 100ml/min；Under continuous stirring, after 30min, stop reaction, reaction bulb is placed on cold water In be down to room temperature, you can obtain the tellurium nano-wire of final rule bending.

Embodiment 2

0.1g tellurium dioxide is weighed, is dissolved in deionized waters of the 100ml after the magnetic field magnetization that field strength is 3T, stirs After mixing uniformly, solution A is obtained；Under conditions of stirring, 5g OTACs are added into solution A, continue to stir Mix to obtain solution B；Obtained solution B is transferred in three-necked flask, three-necked flask is placed in 110 DEG C of oil bath pan and carried out Heating stirring, add 15ml hydrazine hydrate and be passed through the inert atmosphere of nitrogen maintenance reaction system, nitrogen into reaction bulb simultaneously Throughput is controlled in 100ml/min；Under continuous stirring, after 30min, stop reaction, reaction bulb is placed on cold water In be down to room temperature, you can obtain the tellurium nano-wire of final rule bending.

Embodiment 3

0.5g tellurium dioxide is weighed, is dissolved in deionized waters of the 200ml after the magnetic field magnetization that field strength is 3T, stirs After mixing uniformly, solution A is obtained；Under conditions of stirring, 10g OTACs are added into solution A, continue to stir Mix to obtain solution B；Obtained solution B is transferred in three-necked flask, three-necked flask is placed in 120 DEG C of oil bath pan and carried out Heating stirring, add 10ml HI and be passed through the inert atmosphere of nitrogen maintenance reaction system, nitrogen stream into reaction bulb simultaneously Amount control is in 150ml/min；Under continuous stirring, after 60min, stop reaction, reaction bulb is placed in cold water and dropped To room temperature, you can obtain the tellurium nano-wire of final rule bending.

Comparative example 1

Other steps are same as Example 1, and difference is to do reaction dissolvent, gained experiment knot without using the deionized water after magnetization Fruit is linear pattern tellurium nano-wire.

Claims

A kind of 1. preparation method of the tellurium nano-wire of rule bending, it is characterised in that：By in the three-necked flask in oil bath pan The deionized water added after tellurium source, cationic surfactant, reducing agent and magnetization is stirred and is passed through under conditions of nitrogen and prepares Go out the tellurium nano-wire of rule bending.
2. preparation method according to claim 1, it is characterised in that：Deionized water after described magnetization refer to go from Sub- water carries out magnetization treatment in 2-5T magnetic field.
3. preparation method according to claim 1, it is characterised in that：Described anion surfactant is some quaternary ammoniums Salt cationic surfactant, such as dodecylamino acetic acid, OTAC, alkyl dimethyl octyl group chlorine Change the one or more in ammonium.
4. preparation method according to claim 1, it is characterised in that：The reducing agent refers to hydrazine hydrate, ammoniacal liquor, HI, sulphur Change the one or more in sodium.
5. preparation method according to claim 1, it is characterised in that：The temperature setting of the oil bath pan is 100-120 DEG C, Reaction time is 0.5-2 hours.