CN103046110A - Method for preparing monocrystal Bi2Se3 nano structure - Google Patents

Method for preparing monocrystal Bi2Se3 nano structure Download PDF

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CN103046110A
CN103046110A CN2011103102821A CN201110310282A CN103046110A CN 103046110 A CN103046110 A CN 103046110A CN 2011103102821 A CN2011103102821 A CN 2011103102821A CN 201110310282 A CN201110310282 A CN 201110310282A CN 103046110 A CN103046110 A CN 103046110A
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high temperature
powder
substrate
nanostructure
bi2se3
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CN103046110B (en
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唐皓颖
江鹏
王中林
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National Center for Nanosccience and Technology China
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National Center for Nanosccience and Technology China
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Abstract

The invention provides a method for preparing a monocrystal Bi2Se3 nano structure. The Bi2Se3 nano structure comprises a nano belt and a nano sheet, wherein the width of the Bi2Se3 nano belt is 50nm to 4Mum, the length of the Bi2Se3 nano belt is 1-200Mum, and diameter of the Bi2Se3 nano sheet is 50nm to 20Mum. According to the method provided by the invention, high temperature thermal evaporation and gas phase transmission methods are adopted, Bi powder and Se powder or Bi2Se3 powder are taken as raw materials, thermal evaporation is carried out in a high temperature diffusion furnace, and the Bi2Se3 nano structure is obtained on a substrate. The Bi2Se3 nano structure obtained by the invention is a high-quality monocrystal material, no catalyst is used in a synthetic process, influence of introduced foreign impurity to material property is avoided, the method provided by the invention is simple and practicable, repeatability is good, raw materials and the substrate are available, and preparation cost is low.

Description

A kind of monocrystalline Bi for preparing 2Se 3The method of nanostructure
Technical field
The present invention relates to a kind of monocrystalline Bi for preparing 2Se 3The method of nanostructure belongs to the field of semiconductor electronic material and device.
Background technology
Bi 2Se 3Being the narrow-band semiconductor that energy gap is about 0.3eV, is a kind of traditional thermoelectric material, also is used for the fields such as infrared eye.Recently research work theoretical and experiment has all confirmed Bi 2Se 3Be a kind of topological isolator, in fields such as spintronics and quantum computers very wide application prospect arranged, therefore caused the extensive concern of whole world Condensed Matter Physics educational circles.In order to realize Bi 2Se 3The above-mentioned application of topology isolator requires to obtain high-quality Bi 2Se 3Material.At present, Bi 2Se 3Common material shape has bulk single crystal, film and nano structural material.The concrete grammar of Film synthesis comprises by electrochemical deposition (Mater.Chem.Phys., 55,51 (1998), Mater.Res.Bull., 36,1915 (2001)), chemical bath method (Mater.Sci.Eng., B 55,102 (1998)), thermal evaporation (Cryst.Res.Technol.35,1087 (2000)), reactive evaporation (Solid State Commun.85,879 (1993)), compound evaporation (Mater.Res.Bull.40,1314 (2005), J.Phys.D 36,994 (2003)) and metal-organic chemical vapor deposition equipment (J.Mater.Sci.:Mater.Electron.14,599 (2003)) etc.At Bi 2Se 3In the synthetic method of nanostructure, existing method by sonochemistry (J.Cryst.Growth, 271,456 (2004)) is synthesized Bi at present 2Se 3Zonal structure is (hereinafter referred to as Bi 2Se 3Nano belt), by solvent thermal (Mater.Res.Bull.34,131 (1999), J.Cryst.Growth, 253,455 (2003)) and metal-organic chemical vapor deposition equipment (J.Phys.Chem.C, 111,18538 (2007)) method is synthesized Bi 2Se 3Sheet structure is (hereinafter referred to as Bi 2Se 3Nanometer sheet).But that traditional synthetic method obtains is the Bi of polycrystalline 2Se 3, the needs of normally using in order to satisfy thermoelectric field, and be not suitable for topological isolator for the requirement of high-quality material.Based on this, the people (Appl.Phys.Lett., 95,053114 (2009)) such as the people such as Xue Qikun (Appl.Phys.Lett., 97,143118 (2010)) and Wu Kehui have been developed respectively use molecular beam epitaxial growth Bi 2Se 3The method of epitaxial film, and obtained some important achievements (Nature Physics 6,584 (2010), Phys.Rev.Lett., 105,076801 (2010), Phys.Rev.Lett., 105,176602 (2010)) based on this.Simultaneously, the people such as Peng Hailin (Nano Lett., 10,329-333 (2010)) use gold nano grain as catalyzer, by thermal evaporation Bi in silicon chip substrate 2Se 3Powder has developed a kind of by gas-liquid-solid machine-processed catalytic growth Bi 2Se 3The method of nanostructure, can obtain the patterns such as nano belt and nanometer sheet, utilize the character of the large specific surface of nano belt, observe therein a class and be called as quantum oscillatory occurences (the Nature Materials that Aharonov-Bohm vibrates, 9,225-229 (2010)).But, because Bi 2Se 3Be laminate structure, allow between layers other impurity to enter, the tramp materiaies such as use gold nano grain have affected the purity of material, might change Bi 2Se 3The character of material intrinsic.For example, by doping Ca, can regulate Bi 2Se 3The position of the Fermi surface of bulk single crystal can make it change p-type semiconductor material (Phys.Rev.Lett., 103,246601 (2009)) into from the N-shaped semi-conductor continuously, but in the situation that temperature changes repeatedly, the Bi of doping Ca 2Se 3Unpredictable variation occurs in the one-tenth branch of bulk single crystal, is unfavorable for following the realization based on Bi 2Se 3Spintronics and the research of the device of quantum computer; In addition, by doped with Cu, can obtain the superconductor that superconducting transition temperature is 3.8K (Phys.Rev.Lett., 104,057001 (2010)).These two examples have proved that all tramp material can change Bi 2Se 3The character of material intrinsic.In order to overcome above-mentioned shortcoming, be necessary by preparing high-quality Bi without the method for catalysis 2Se 3Nanostructure.
Summary of the invention
One object of the present invention is to provide a kind of catalyzer that do not use, and prepares a kind of monocrystalline Bi by high temperature thermal evaporation and gas phase transmission 2Se 3The method of nanostructure.Another object of the present invention is to provide a kind of high-quality monocrystalline Bi according to described method preparation 2Se 3Nanostructure.Another purpose of the present invention is to provide a kind of described monocrystalline Bi 2Se 3The purposes of nanostructure.
The objective of the invention is to be achieved through the following technical solutions:
On the one hand, the invention provides a kind of monocrystalline Bi for preparing 2Se 3The method of nanostructure, wherein, described method is take Bi powder and Se powder mixture as raw material or with Bi 2Se 3Powder is raw material, and preferably, the purity of described raw material is 99.99% (weight ratio), does not use catalyzer, take rare gas element or nitrogen as source of the gas carries out gas phase transmission, prepares Bi by the high temperature thermal evaporation at substrate 2Se 3Nanostructure.
Further, according to aforesaid method, it may further comprise the steps:
1) take the Bi powder that mixes and Se powder as raw material or with Bi 2Se 3Powder is raw material, and it is upper as growth source to be put into high-temperature resistant container (equipment that does not at high temperature react such as quartz boat or ceramic boat etc.);
2) high-temperature resistant container is put into the middle part of high temperature dispersing furnace (equipment that is used for gas phase transmission such as horizontal tube growth furnace etc.), in high temperature dispersing furnace, places substrate to collect resultant away from an end of inlet mouth;
3) with the high temperature dispersing furnace sealing, vacuumize;
4) pass in the high temperature dispersing furnace after vacuumize rare gas element or nitrogen as source of the gas to carry out gas phase transmission;
5) in gas phase transmission, high temperature dispersing furnace is heated to certain temperature and under this temperature, is incubated, to carry out the high temperature thermal evaporation, at this moment, if raw material is Bi powder and Se powder, then Bi powder and Se powder react with the form of gaseous state under the high temperature thermal evaporation and generate the Bi of gaseous state 2Se 3If raw material is Bi 2Se 3Powder, then Bi 2Se 3Powder directly becomes gaseous form under the high temperature thermal evaporation, no matter be the Bi of the gaseous state that obtains of which kind of situation 2Se 3The capital is with gas transmission end away from inlet mouth to the high temperature diffusion furnace, i.e. substrate place, the Bi of gaseous state 2Se 3Meeting forms crystallization at the substrate that temperature is lower than the thermal evaporation temperature, can obtain Bi in suitable temperature range 2Se 3Nanostructure;
6) after the high temperature thermal evaporation finished, substrate was cooled to room temperature naturally with high temperature dispersing furnace, passes into an amount of rare gas element or nitrogen, and stop gas phase transmission, and make the pressure in the high temperature dispersing furnace get back to a normal atmosphere, open high temperature dispersing furnace, take out substrate, prepare the Bi that is grown on the substrate 2Se 3Nanostructure.
Further, according to aforesaid method, wherein,
The mol ratio that described Bi powder and Se powder mix is 2: 3～2: 20, according to the Bi-Se phasor, when the mole number of Se during more than the mole number of 1.5 times of Bi, all can obtain Bi 2Se 3Nanostructure is if from the angle of conservation, can be preferably 2: 3;
Described substrate comprises: monocrystalline silicon piece, by thermal oxidation method at the monocrystalline silicon piece SiO that grows 2After the silicon chip or the alumina ceramic plate that obtain, be preferably alumina ceramic plate owing to adopt alumina ceramic plate as substrate, avoided the reaction of Se powder and silicon chip, can use the powder preparation Bi of simple substance Bi and Se 2Se 3Nanostructure is because the powder of simple substance Bi and Se compares Bi 2Se 3The easier acquisition of powder, thus cost saved;
Described substrate in the horizontal tube growth furnace with quartz boat distance 5～15cm, in fact in a comparatively broad warm area, all can obtain Bi 2Se 3Nanostructure;
The argon gas that described rare gas element preferably is easy to get;
Described step 3) in, the pressure that vacuumizes rear horizontal tube growth furnace is not higher than 20Pa, is preferably 1Pa;
During described gas phase transmission, the flow that passes into gas is 10～500sccm, is preferably 100sccm, makes the pressure in the high temperature dispersing furnace reach 300～3000Pa, is preferably 500Pa.
During described high temperature thermal evaporation, Heating temperature is 480～550 ℃, is preferably 500 ℃, and soaking time is 0.5～24h, is preferably 10h.
On the other hand, the invention provides a kind of Bi according to aforesaid method preparation 2Se 3Nanostructure comprises Bi 2Se 3Nano belt and Bi 2Se 3Nanometer sheet, preferred, the width of described nano belt is 50nm～4 μ m, length is 1～200 μ m, described Bi 2Se 3The transverse width of nanometer sheet is 50nm～20 μ m.
Another aspect, the present invention also provides a kind of described monocrystalline Bi 2Se 3Nanostructure is as the application of topological isolator in fields such as spintronics and quantum computers.
The invention has the advantages that:
The first, method of the present invention is not used catalyzer, has avoided the introducing tramp material to Bi 2Se 3The impact of material character, less demanding to carrier gas, less demanding to airshed, simple, good reproducibility, raw material and substrate are easy to get, and preparation cost is cheap;
The second, the Bi of method preparation of the present invention 2Se 3Nano belt and nanometer sheet are a kind of high-quality monocrystal materials, are expected in topological isolator field acquisition important application.
Description of drawings
Describe the present invention below in conjunction with accompanying drawing.
Fig. 1 is the Bi of preparation among the embodiment 2 2Se 3The X-ray diffractogram of nanostructure and alumina ceramic plate substrate.
Fig. 2 is the Bi for preparing at the alumina ceramic plate substrate among the embodiment 2 2Se 3The electron scanning micrograph of nanostructure, wherein, (a) be a nano belt that stand on the substrate, (b) and (c) be the partial enlarged drawing of (a), (d) be a jagged nano belt, (e) being the side-view of a nano belt, (f) is a nanometer sheet.
Fig. 3 is the Bi of preparation among the isolated embodiment 2 2Se 3The transmission electron microscope photo of nano belt, wherein, (a) be the transmission electron microscope photo of low power, (b) be the energy dispersion X ray spectrum of nano belt in (a), (c) be the middle portion of nano belt in (a), (c) illustration in the upper left corner is its selected area electron diffraction pattern in, (d) is the high resolution transmission electron microscopy photo in corresponding zone in (c).
Embodiment
Below in conjunction with embodiment the present invention is further described in detail, the embodiment that provides is only in order to illustrate the present invention, rather than in order to limit the scope of the invention.
Embodiment 1
The first step, be 2: 3 Bi powder (purity 99.99% (weight ratio) with mol ratio, Alfa Aesa) and Se powder (purity 99.99% (weight ratio), Alfa Aesa) mix, it is upper as growth source to be put into quartz boat (reach peace open up science and technology);
Second step, quartz boat is put into horizontal tube growth furnace (ring experimental electric furnace company limited in the Tianjin, model SK2-4-13) middle part, and in the horizontal tube growth furnace apart from quartz boat 5～15cm place and away from an end of inlet mouth place monocrystalline silicon piece as substrate to collect resultant;
In the 3rd step, with the sealing of horizontal tube growth furnace, vacuumize, so that the pressure of horizontal tube growth furnace reaches 1Pa;
In the 4th step, the flow with 50sccm in the horizontal tube growth furnace passes into argon gas (purity 99.99% (weight ratio)), makes the pressure of horizontal tube growth furnace reach 500Pa;
In the 5th step, the horizontal tube growth furnace is heated to 500 ℃, and keeps this temperature 5h;
The 6th step, substrate is cooled to room temperature naturally with the horizontal tube growth furnace, pass into an amount of argon gas, make the pressure of horizontal tube growth furnace get back to a normal atmosphere, open the horizontal tube growth furnace, take out substrate, atrament occurs at substrate surface, this material is carried out X-ray diffractogram spectrum analysis, scanning electron microscope analysis and tem study, confirm that the material that is grown on the substrate is single crystal Bi 2Se 3Nano belt and nanometer sheet.
Embodiment 2
The first step is that 2: 20 Bi powder (purity 99.99% (weight ratio), Alfa Aesa) and Se powder (purity 99.99% (weight ratio), Alfa Aesa) mixes with mol ratio, is put on the quartz boat as growth source;
Second step is put into the middle part of horizontal tube growth furnace with quartz boat, and in the horizontal tube growth furnace apart from quartz boat 5～15cm place and away from an end of inlet mouth place alumina ceramic plate as substrate to collect resultant;
In the 3rd step, with the sealing of horizontal tube growth furnace, vacuumize, so that the pressure of horizontal tube growth furnace reaches 1Pa;
In the 4th step, the flow with 100sccm in the horizontal tube growth furnace passes into argon gas, makes the pressure of horizontal tube growth furnace reach 800Pa;
In the 5th step, the horizontal tube growth furnace is heated to 500 ℃, and keeps this temperature 10h;
The 6th step, substrate is cooled to room temperature naturally with the horizontal tube growth furnace, pass into an amount of argon gas, make the pressure of horizontal tube growth furnace get back to a normal atmosphere, open the horizontal tube growth furnace, take out substrate, atrament occurs at substrate surface, this material is carried out X-ray diffractogram spectrum analysis (as shown in Figure 1), scanning electron microscope analysis (as shown in Figure 2) and tem study (as shown in Figure 3), confirm that the material that is grown on the substrate is Bi 2Se 3Nano belt and nanometer sheet, Fig. 3 (c) and Fig. 3 (d) have proved that from the crystallography angle material that present embodiment makes is single crystal, illustrate that it is high-quality monocrystalline Bi 2Se 3Structure.
Embodiment 3
The first step is with Bi 2Se 3Powder (purity 99.999% (weight ratio), the prosperous imperial tellurium industry science and technology limited Company in Sichuan) be put on the quartz boat as growth source;
Second step is put into the middle part of horizontal tube growth furnace with quartz boat, and in the horizontal tube growth furnace apart from quartz boat 5～15cm place and away from an end of inlet mouth place alumina ceramic plate and with thermal oxidation method at the monocrystalline silicon piece SiO that grows 2After the silicon chip that obtains as substrate to collect resultant;
In the 3rd step, with the sealing of horizontal tube growth furnace, vacuumize, so that the pressure of horizontal tube growth furnace reaches the Schwellenwert that vacuum apparatus can provide;
In the 4th step, the flow with 50sccm in the horizontal tube growth furnace passes into nitrogen (purity 99.99% (weight ratio)), makes the pressure of horizontal tube growth furnace reach 2000Pa;
In the 5th step, the horizontal tube growth furnace is heated to 550 ℃, and keeps this temperature 24h;
The 6th step, substrate is cooled to room temperature naturally with the horizontal tube growth furnace, pass into an amount of nitrogen, make the pressure of horizontal tube growth furnace get back to a normal atmosphere, open the horizontal tube growth furnace, take out substrate, this material is carried out X-ray diffractogram spectrum analysis, scanning electron microscope analysis and tem study, confirm that the material that is grown on the substrate is Bi 2Se 3Nano belt and nanometer sheet.
Certainly; the present invention also can have other various embodiments; in the situation that does not deviate from spirit of the present invention and essence thereof; those of ordinary skill in the art can make according to the present invention various corresponding changes and modification, but these corresponding changes and distortion all should belong in the protection domain of claim of the present invention.

Claims (10)

1. one kind prepares monocrystalline Bi 2Se 3The method of nanostructure is characterized in that, described method is take Bi powder and Se powder mixture as raw material or with Bi 2Se 3Powder is raw material, and preferably, the purity of described raw material is 99.99% (weight ratio), does not use catalyzer, take rare gas element or nitrogen as source of the gas carries out gas phase transmission, prepares Bi by the high temperature thermal evaporation at substrate 2Se 3Nanostructure.
2. method according to claim 1 is characterized in that, said method comprising the steps of:
1) take the Bi powder that mixes and Se powder as raw material or with Bi 2Se 3Powder is raw material, is put on the high-temperature resistant container as growth source;
2) high-temperature resistant container is put into the middle part of high temperature dispersing furnace, in high temperature dispersing furnace, places substrate to collect resultant away from an end of inlet mouth;
3) with the high temperature dispersing furnace sealing, vacuumize;
4) pass in the high temperature dispersing furnace after vacuumize rare gas element or nitrogen as source of the gas to carry out gas phase transmission;
5) in gas phase transmission, high temperature dispersing furnace is heated to certain temperature and under this temperature, is incubated, to carry out the high temperature thermal evaporation, the Bi of gaseous state 2Se 3Meeting forms crystallization at the substrate that temperature is lower than the thermal evaporation temperature, can obtain Bi in suitable temperature range 2Se 3Nanostructure;
6) after the high temperature thermal evaporation finished, substrate was cooled to room temperature naturally with high temperature dispersing furnace, passes into an amount of rare gas element or nitrogen, and stop gas phase transmission, and make the pressure in the high temperature dispersing furnace get back to a normal atmosphere, open high temperature dispersing furnace, take out substrate, prepare the Bi that is grown on the substrate 2Se 3Nanostructure.
3. method according to claim 1 and 2 is characterized in that, the mol ratio that described Bi powder and Se powder mix is 2: 3～2: 20, is preferably 2: 3.
4. method according to claim 1 and 2 is characterized in that, described substrate comprises: monocrystalline silicon piece, by thermal oxidation method at the monocrystalline silicon piece SiO that grows 2After the silicon chip or the alumina ceramic plate that obtain, be preferably alumina ceramic plate; Described substrate in the horizontal tube growth furnace with quartz boat distance 5～15cm.
5. method according to claim 1 and 2 is characterized in that, the preferred argon gas of described rare gas element.
6. method according to claim 2 is characterized in that, described step 3) in, the pressure that vacuumizes rear horizontal tube growth furnace is not higher than 20Pa, preferred 1Pa.
7. method according to claim 1 and 2 is characterized in that, during described gas phase transmission, the flow that passes into source of the gas is 10～500sccm, and preferred 100sccm makes the pressure in the high temperature dispersing furnace reach 300～3000Pa, is preferably 500Pa.
8. method according to claim 1 and 2 is characterized in that, during described high temperature thermal evaporation, Heating temperature is 480～550 ℃, is preferably 500 ℃, and soaking time is 0.5～24h, preferred 10h.
9. Bi of each described method preparation according to claim 1-10 2Se 3Nanostructure is characterized in that, described nanostructure comprises Bi 2Se 3Nano belt and Bi 2Se 3Nanometer sheet, preferred, the width of described nano belt is 50nm～4 μ m, length is 1～200 μ m, described Bi 2Se 3The transverse width of nanometer sheet is 50nm～20 μ m.
10. a nanostructure according to claim 9 using at spintronics and quantum computer field as topological isolator.
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