CN105862122A - Methods for InSb nanowire manufacturing and Mn doping both based on multi-step glancing-angle deposition process - Google Patents
Methods for InSb nanowire manufacturing and Mn doping both based on multi-step glancing-angle deposition process Download PDFInfo
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- CN105862122A CN105862122A CN201610300708.8A CN201610300708A CN105862122A CN 105862122 A CN105862122 A CN 105862122A CN 201610300708 A CN201610300708 A CN 201610300708A CN 105862122 A CN105862122 A CN 105862122A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/007—Growth of whiskers or needles
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- 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
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
Abstract
The invention relates to methods for InSb nanowire manufacturing and Mn doping both based on a multi-step glancing-angle deposition process. The method for InSb nanowire manufacturing includes the steps of (1), manufacturing monocrystal pure-In nanowires by the multi-step glancing-angle deposition technology; (2), depositing Sb coating on the surface of the pure In nanowires to form an In-Sb core-shell structure; (3), subjecting the In-Sb core-shell structure to annealing treatment to realize crystallization reaction when the In-Sb core-shell structure is in solid phase so as to form the InSb nanowires. The method for Mn doping includes the steps of (1), manufacturing the monocrystal pure-In nanowires by the multi-step glancing-angle deposition technology; (2), depositing Mn coating on the surface of the pure In nanowires to form an In-Mn core-shell structure; (3), depositing Sb coating on the surface of the Mn coating and then performing annealing treatment so as to form the Mn doped InSb nanowires. By the methods, manufacturing of InSb nanowires and Mn doping at a low temperature are achieved, and the InSb nanowires with high content of Mn are obtained.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of indium antimonide based on multistep Glancing angledeposition (InSb)
Nano wire preparation and doping method.
Background technology
The most in decades, dilute magnetic semiconductor is always treated as a kind of material of great potential in spinning electron application and studied.
In dilute magnetic semiconductor, the Group III-V semiconductor of Mn doping is always a kind of prototype being widely studied.It is likely to occur Curie's temperature
Degree is higher than the state of room temperature, the most potential in the application of following spin electric device.But, owing to Mn element is in iii-v
Dissolution rate relatively low in quasiconductor, uses common crystal growth pattern to obtain dilute magnetic half of high Mn doping in equilibrium conditions
Conductor is extremely difficult.Therefore, in Group III-V semiconductor nano wire, unbalanced growth and doping way are to be widely used
To cross over this obstruction, have the dilute magnetic semiconductor of high-curie temperature with preparation.Such as, will weight Mn doping and suitable nanometer
Structural Engineering combines, and uses low temperature MBE (molecular beam epitaxy) to combine with top-down photoetching technique, successfully prepares
The GaAs nano wire of Mn doping, the most successfully observes the Curie temperature of about 200K.Sink using Organometallic Vapor Phase
While long-pending extension (MOVPE) method keeps mono-crystalline structures growth, ion implantation at a certain temperature is also used for preparation
The GaAs nano wire of high Mn doped in concentrations profiled.
Removing GaAs, other Group III-V semiconductor are also used for adulterating Mn to prepare dilute magnetic semiconductor.InSb material has narrow
Band gap, high mobility, big g-factor and the electron effective mass of minimum, be especially suitable for making infrared electro device, quantum device
Part and UHF electronic device.The InSb material of Mn doping be therefore sent to want to the most effective keep electron transport with
Electron spin.At present, people make some attempts in the InSb material preparing Mn doping.Dilute magnetic based on InSb is partly led
Body material can be merged by direct InSb, Mn and Sb powder and quickly cool down.When being warming up to 600K, the InSb preparing:
Mn product can observe ferromagnetic behavior.But, structural analysis shows, a large amount of MnSb generate after merging and quickly cooling down,
And the InSb dilute magnetic semiconductor of non-formation our desired Mn doping.
At present the method for growth InSb nano wire have chemical gaseous phase deposition (CVD), metallorganic meteorology extension (MOCVD),
Chemical beam epitaxy (CBE) etc., but the research being doped InSb nano wire is the most little.Up to now, receive at InSb
The mode carrying out Mn doping in rice noodle does not also have any report to propose.Growth temperature (about 500 DEG C) in common growth pattern
For the doping of Mn element the highest, be unfavorable for being formed stable InSb lattice structure, to such an extent as to serious have impact on magnetic
Sexual behaviour.In order to obtain Mn ion concentration higher than Mn the InSb nano wire of dissolubility, InSb nano wire in InSb material
Should grow at low temperatures or carry out follow-up process.
Summary of the invention
The purpose of the present invention is to propose to a kind of novel method preparing InSb nano wire, and based on this method to InSb nano wire
Carry out the doping of Mn element.
To achieve these goals, the present invention is by the following technical solutions:
A kind of InSb nanowire preparation method based on multistep Glancing angledeposition, comprises the following steps:
1) multistep glancing angle deposition technology is used to prepare monocrystalline pure In nano wire；
2) deposit Sb film layer in pure In nanowire surface, form the nucleocapsid structure of In, Sb；
3) nucleocapsid structure of In, Sb is made annealing treatment so that it is crystallization reaction occurs when solid phase, forms InSb nano wire.
A kind of InSb nano wire Mn based on multistep Glancing angledeposition adulterates preparation method, comprises the following steps:
1) multistep glancing angle deposition technology is used to prepare monocrystalline pure In nano wire；
2) deposit Mn film layer in pure In nanowire surface, form the nucleocapsid structure of In, Mn；
3) deposit Sb film layer at Mn film surface, form the nucleocapsid structure of In, Mn, Sb；
4) nucleocapsid structure of In, Mn, Sb is made annealing treatment so that it is crystallization reaction occurs when solid phase, form Mn and mix
Miscellaneous InSb nano wire.
The invention has the beneficial effects as follows: present invention achieves and prepare InSb nano wire at low temperatures and carry out the doping of Mn element.
In this technique, the content of Mn element can not be limited by Mn dissolubility in InSb material, thus obtains high Mn
The InSb nano wire of content.
Accompanying drawing explanation
Figure 1A～Fig. 1 D is the schematic diagram that in the present invention, multistep glancing angle method prepares InSb nano wire.Wherein, Figure 1A is system
The vacuum deposition system schematic diagram of standby In nano wire；Figure 1B is the schematic diagram that multistep glancing angle method prepares pure In nano wire；Figure
1C is the schematic diagram being deposited with Sb film outside In line；Fig. 1 D be annealing after formed InSb nano wire schematic diagram.
Fig. 2 A～Fig. 2 D is the schematic diagram of the InSb nano wire of multistep glancing angle method preparation doping Mn in the present invention.Wherein,
Fig. 2 A is the vacuum deposition system schematic diagram of the In nano wire of preparation doping Mn；Fig. 2 B is the In nanometer of preparation doping Mn
The schematic diagram of line；Fig. 2 C is the schematic diagram being deposited with Sb thin film outside the In nano wire of Mn doping；Fig. 2 D is for being formed after annealing
The schematic diagram of the InSb nano wire of Mn doping.
Fig. 3 is the scanning electron microscope micro-image (SEM) of In nano wire prepared by multistep glancing angle method.
Fig. 4 A and Fig. 4 B is images of transmissive electron microscope (TEM) and the X-ray energy spectrum analysis chart of InSb nano wire after annealing
(EDAX)。
Fig. 5 A and Fig. 5 B is to use the surface sweeping electron microscope images (SEM) of the FET device of the InSb nano wire of preparation in the present invention
With the transfer characteristic curve measured under room temperature.
Fig. 6 A and Fig. 6 B is that the images of transmissive electron microscope (TEM) of the InSb nano wire of doping Mn element divides with X-ray energy spectrum
Analysis figure (EDAX).
Detailed description of the invention
Below by specific embodiments and the drawings, the present invention will be further described.
The present invention, first on Si/SiO2 substrate, uses multistep glancing angle deposition (GLAD) technology to prepare monocrystalline pure In nanometer
Line；Then thickness suitably uniformly Sb film layer in pure In nano wire outer wrap, formed In, Sb core-shell (core-
Shell) structure；Finally the core-shell structure of In, Sb is made annealing treatment in suitable temperature so that it is occur when solid phase
Crystallization reaction, forms InSb nano wire.In this process, the present invention attempts the magnetic that deposition doping is a small amount of between In and Sb
Property element (Mn), it is achieved thereby that magnetic-doped to InSb nano wire.
The preparation of above-mentioned InSb nano wire based on multistep Glancing angledeposition and doping method, as depicted in figs. 1 and 2, specifically wrap
Include following steps:
(1) preparation of In nano wire
During multistep glancing angle method prepares pure In nano wire, the present embodiment uses the vacuum moulding machine system that resistance heats
System (ULVACVWR-400), Figure 1A is its structural representation.In deposition process, chamber is evacuated to about 3 × 10-3Pa with
Under.The solid In granule that vapor deposition source uses purity to be 99.99%, is positioned in the tungsten boat below substrate.Substrate uses surface to have
The SiO of 300nm thickness2The silicon chip of layer.Substrate is fixed on a specimen holder, specimen holder make substrate center all the time with evaporation
Source keeps the distance of about 150mm～200mm, and preferred value is 170mm.Between substrate normal direction and evaporation source of the gas ascent direction
Angle α between 80 ° to 90 °；Preferably, α=85 °.
Figure 1B is the schematic diagram that multistep glancing angle method prepares pure In nano wire.In whole deposition process being carried out more than 3 times having a mind to
Disconnected, during each interruption (about 10 minutes), by vacuum chamber venting Rotary Specimen Rack (typically 90 °) with
Reach the effect on oxidation sample surface.The oxidation of sample surfaces can stop next time plated film time In atom at original particle surface
Epitaxial growth so that be deposited with each time and all can form new In granule.In deposition process, In source evaporation rate is 0.5～1.5nm/s
Between, preferred value is 1nm/s, and now on silicon chip, In sedimentation rate is 0.87nm/s, and first three time deposit thickness is between 40～60nm,
Preferred value is 50nm.So, meeting after three evaporations, Si sheet surface can form one layer of isotropic In granule growing film,
Good growing environment is provided for the growth of In nano wire in evaporation next time.4th time deposit thickness is between 250nm～350nm,
Preferred value is 300nm, to grow In nano wire.Fig. 3 is that the scanning electron microscope of In nano wire prepared by multistep glancing angle method is micro-
Image (SEM).
(2) formation of the core-shell structure of In, Sb
Fig. 1 C is the schematic diagram being deposited with Sb film outside In line.During the evaporation of Sb thin film, the present embodiment uses magnetic control to spatter
Penetrate plated film instrument (Kurt J.Lesker PRO Line PVD 75).In deposition process, chamber is evacuated to less than 9 × 10-5Pa.Target
The metal Sb block that material uses purity to be 99.99%.In coating process, growth has the silicon wafer horizontal of In nano wire to place, with 5～10rad/s
Rate uniform rotate, preferred rate is 5rad/s.Set operating power as 30W, then Sb element is with 0.1～0.3nm/s (preferred value
For 0.2nm/s) rate uniform be deposited on silicon chip, total deposit thickness is between 50nm～100nm, and preferred value is 70nm.
(3) the core-shell structure of In, Sb is made annealing treatment
After being deposited with the Sb thin film of 50nm～100nm, sample is positioned in tube furnace (Lindberg TF55035KC) and moves back
Fire.Annealing process persistently at least 10 hours, in initial 5 hours, is uniformly heating to 150～250 DEG C, and preferred value is 200
DEG C, then maintain the temperature at 200 DEG C constant 5 hours.In whole annealing process, hydrogen is selected as carrier gas, and airflow rate is
80～120sccm, preferred value is 100sccm.Fig. 1 D be annealing after formed InSb nano wire schematic diagram.
Fig. 4 A and Fig. 4 B is images of transmissive electron microscope (TEM) and the X-ray energy spectrum analysis chart of the InSb nano wire after annealing
(EDAX).Wherein, Fig. 4 A represents the crystal structure figure that high resolution transmission electron microscopy (HR-TEM) is observed, illustration
Fourier transformation (FFT) for full resolution pricture, it can be seen that this nano wire is the zincblende lattce structure of InSb；Fig. 4 B is for for using
The elemental composition analysis that nano wire is carried out by the energy dispersion X ray spectrum instrument (EDAX) in TEM, represents the composition of nano wire relatively
For pure, predominantly two kinds of elements of In, Sb, and In, Sb component ratio detected is about at about 1:1.
(4) doping of Mn element between In, Sb
After step (1) uses multistep glancing angle method to prepare In nano wire, select the vacuum deposition system situ in resistance heating
Carry out the deposition of Mn element to form the core-shell structure of In-Mn, as shown in Figure 2 A.Fig. 2 B is the In nanometer of preparation doping Mn
The schematic diagram of line.In deposition process, chamber is evacuated to 3 × 10 equally-3Pa, vapor deposition source be purity be the solid Mn of 99.99%
Thin slice, is positioned in the tungsten boat below silicon chip.In deposition process, Mn source evaporation rate is 0.05～0.15nm/s, and preferred value is
0.1nm/s, now.On silicon chip, Mn sedimentation rate is 0.087nm/s, and deposit thickness is 5nm～20nm, and preferred value is 20nm.
In nano wire after Mn doping uses magnetron sputtering plating instrument to carry out the evaporation of Sb thin film, to form In, Mn, Sb equally
Core-shell structure, as shown in Figure 2 C.
(5) annealing of the InSb nano wire of Mn doping
After being deposited with the Sb thin film of 70nm, sample is transferred on silicon chip or micro-grid, then is positioned over tube furnace (Lindberg
TF55035KC) anneal in.Annealing process persistently at least 10 hours, in initial 5 hours, is uniformly heating to
150～250 DEG C, preferred value is 200 DEG C, then maintain the temperature at 200 DEG C constant 5 hours.In whole annealing process, hydrogen is selected
Being taken as carrier gas, airflow rate is 80～120sccm, and preferred value is 100sccm.Fig. 2 D be annealing after formed Mn doping InSb
The schematic diagram of nano wire.
Fig. 5 A and Fig. 5 B be the field-effect transistor (FETs) with top gate structure of InSb nano wire using the present invention to prepare and
Transfer characteristic curve figure under room temperature, wherein Fig. 5 A is device figure, and corresponding source and drain and grid have been marked in picture.Fig. 5 B is
Measuring the transfer characteristic curve drawn, abscissa is grid voltage Vg, and vertical coordinate is source-drain current Ids, controls source-drain voltage during measurement
According to this curve, Vds=1mV, can be seen that this InSb nano wire is typical n-type semiconductor.
Fig. 6 A and Fig. 6 B is images of transmissive electron microscope and X-ray energy spectrum analysis chart, wherein Fig. 6 A of the InSb nano wire of doping Mn element
Representing the crystal structure figure that high resolution transmission electron microscopy (HR-TEM) is observed, illustration is the Fourier of full resolution pricture
Conversion (FFT), it can be seen that this nano wire is similarly the zincblende lattce structure of InSb；Fig. 6 B is to use the energy dispersion X in TEM
The elemental composition analysis that nano wire is carried out by X-ray spectrometer X (EDAX), the composition of nano wire is the purest, predominantly In, Sb
Two kinds of elements, containing a small amount of Mn element, and In, Sb component ratio detected is about at about 1:1.
Table 1 is the component ratio under X-ray energy spectrum analyser (EDAX) of the InSb nano wire after doping Mn element.Therein
Being mainly composed of In, Sb, ratio is all about 34%；Additionally, there is a small amount of Mn element, ratio is about 4%, copper (Cu)
Element is introduced by the copper mesh in micro-grid.Removing the impact of copper, Mn ratio in InSb nano wire is 5.19%, and general
The Mn content of CVD growth doping is 2～about 3%, and after the method for the employing present invention is described, the content of Mn element can not be by Mn
Dissolubility in InSb material limits, and has obtained the InSb nano wire of high Mn content.
Table 1. adulterates the component ratio of the InSb nano wire after Mn element
| Element | Weight% | Atomic% |
| Mn(K) | 2.059 | 3.788 |
| Cu(K) | 16.969 | 26.985 |
| In(K) | 40.317 | 35.483 |
| Sb(K) | 40.654 | 33.743 |
In another embodiment, in the forming step of the core-shell structure of second step In, Sb, the present invention also can use heat steaming
Plating method evaporation Sb thin film.
In another embodiment, in the step of the core-shell structure that three-step annealing processes In, Sb, this structure is the most transferable
Anneal to Si sheet or micro-grid.
Above example is only limited in order to technical scheme to be described, those of ordinary skill in the art can
Technical scheme is modified or equivalent, without departing from the spirit and scope of the present invention, the guarantor of the present invention
The scope of protecting should be as the criterion with described in claims.
Claims (10)
1. an InSb nanowire preparation method based on multistep Glancing angledeposition, comprises the following steps:
1) multistep glancing angle deposition technology is used to prepare monocrystalline pure In nano wire；
2) deposit Sb film layer in pure In nanowire surface, form the nucleocapsid structure of In, Sb；
3) nucleocapsid structure of In, Sb is made annealing treatment so that it is crystallization reaction occurs when solid phase, forms InSb nano wire.
2. InSb nano wire Mn based on a multistep Glancing angledeposition doping preparation method, comprises the following steps:
1) multistep glancing angle deposition technology is used to prepare monocrystalline pure In nano wire；
2) deposit Mn film layer in pure In nanowire surface, form the nucleocapsid structure of In, Mn；
3) deposit Sb film layer at Mn film surface, form the nucleocapsid structure of In, Mn, Sb；
4) nucleocapsid structure of In, Mn, Sb is made annealing treatment so that it is crystallization reaction occurs when solid phase, form Mn and mix
Miscellaneous InSb nano wire.
Method the most according to claim 1 and 2, it is characterised in that step 1) at Si/SiO2The pure In of monocrystalline is prepared on substrate
Nano wire, substrate center and evaporation source keep the distance of 150mm～200mm, substrate normal direction and evaporation source of the gas rising side
Angle α between to is 80 °～90 °.
Method the most according to claim 1 and 2, it is characterised in that step 1) carry out in more than three times in deposition process
Disconnected, by vacuum chamber venting Rotary Specimen Rack every time during interrupting, with oxidation sample surface.
Method the most according to claim 4, it is characterised in that step 1) in deposition process, In source evaporation rate is
0.5～1.5nm/s, the deposit thickness of first three time is 40～60nm；Meeting after three evaporations, Si sheet surface forms one layer respectively to same
The In granule growing film of property；The deposit thickness of the 4th time is 250nm～350nm, to grow In nano wire.
Method the most according to claim 1 and 2, it is characterised in that use magnetron sputtering coating method or hot vapour deposition method to carry out
The evaporation of Sb thin film, the sedimentation rate of Sb element is 0.1～0.3nm/s, and total deposit thickness is 50nm～100nm.
Method the most according to claim 1 and 2, it is characterised in that using tube furnace to carry out described annealing, annealing process is lasting
At least 10 hours, in initial 5 hours, it is uniformly heating to 150～250 DEG C, then keeps temperature-resistant 5 hours；
Using hydrogen as carrier gas in whole annealing process, airflow rate is 80～120sccm.
Method the most according to claim 2, it is characterised in that in step 1) prepare In nano wire after, step 2) at resistance
The vacuum deposition system situ of heating carries out the deposition of Mn element to form the nucleocapsid structure of In, Mn；In deposition process
Middle Mn source evaporation rate is 0.05～0.15nm/s, and on silicon chip, the deposit thickness of Mn is 5nm～20nm.
9. the InSb nano wire prepared according to method described in any claim in claim 1,3 to 7.
10. the InSb nano wire of the doping Mn prepared according to method described in any claim in claim 2 to 8.
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