CN105862122B - Indium antimonide nano wire based on multistep Glancing angledeposition is prepared and additive Mn method - Google Patents
Indium antimonide nano wire based on multistep Glancing angledeposition is prepared and additive Mn method Download PDFInfo
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Abstract
The present invention relates to a kind of, and the indium antimonide nano wire based on multistep Glancing angledeposition is prepared and additive Mn method.The pure In nano wires of monocrystalline are prepared using multistep glancing angle deposition technology first；Then Sb film layers are deposited in pure In nanowire surfaces, forms the nucleocapsid of In, Sb；Then the nucleocapsid of In, Sb are made annealing treatment, makes it that crystallization reaction occur in solid phase, form InSb nano wires.When carrying out additive Mn, the pure In nano wires of monocrystalline are prepared using multistep glancing angle deposition technology first；Then Mn film layers are deposited in pure In nanowire surfaces, forms the nucleocapsid of In, Mn；Then Sb film layers are deposited in Mn film surfaces, and is made annealing treatment, form the InSb nano wires of Mn doping.The present invention realizes the doping for preparing InSb nano wires at low temperature and carrying out Mn elements, can obtain the InSb nano wires of high Mn content.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of indium antimonide based on multistep Glancing angledeposition
(InSb) nano wire preparation and doping method.
Background technology
In decades recently, dilute magnetic semiconductor be always treated as it is a kind of in spinning electron using the material of upper great potential and
It is studied.The Group III-V semiconductor that Mn is adulterated in dilute magnetic semiconductor is always a kind of prototype being widely studied.It may go out
Existing Curie temperature is higher than the state of room temperature, very potential in the application of the following spin electric device.However, since Mn elements exist
Lower dissolution rate in Group III-V semiconductor obtains high Mn doping using common crystal growth pattern in equilibrium conditions
Dilute magnetic semiconductor be very difficult.Therefore, unbalanced growth is with doping way in Group III-V semiconductor nano wire
It is widely used to cross over this obstruction, to prepare the dilute magnetic semiconductor for possessing high-curie temperature.For example, will weight Mn doping and conjunction
Suitable nanostructure engineering is combined, and is combined with top-down photoetching technique using low temperature MBE (molecular beam epitaxy), success
The GaAs nano wires for preparing Mn doping, wherein successfully observing the Curie temperature of 200K or so.Using organic metal gas
While mutually deposition extension (MOVPE) method keeps mono-crystalline structures growth, ion implantation at a certain temperature is also used to
Prepare the GaAs nano wires of high Mn doped in concentrations profiled.
GaAs is removed, other Group III-V semiconductors also be used to adulterate Mn to prepare dilute magnetic semiconductor.InSb materials have
The electron effective mass of narrow band gap, high mobility, the big g factors and minimum is very suitable for making infrared electro device, quantum device
Part and UHF electronic device.The InSb materials of Mn doping be therefore sent to want to it is effective simultaneously keep electron transport and
Electron spin.Currently, people make some attempts in the InSb materials for preparing Mn doping.Dilute magnetic semiconductor material based on InSb
Material can be merged and be quickly cooled down by direct InSb, Mn and Sb powder.When being warming up to 600K, in the InSb prepared：In Mn products
It can observe ferromagnetic behavior.However, structural analysis show a large amount of MnSb merge be quickly cooled down after generate, and it is non-formation
The InSb dilute magnetic semiconductors of our desirable Mn doping.
The method of growth InSb nano wires has chemical vapor deposition (CVD), metallorganic meteorology extension at present
(MOCVD), chemical beam epitaxy (CBE) etc., but the research being doped to InSb nano wires is also seldom.So far, exist
There are no any reports to propose for the mode of progress Mn doping in InSb nano wires.Growth temperature in common growth pattern is (about
500 DEG C) it is too high for the doping of Mn elements, it is unfavorable for forming stable InSb lattice structures, so that serious shadow
Magnetic behavior is rung.In order to obtain Mn ion concentrations be higher than Mn solubility in InSb materials InSb nano wires, InSb nanometers
Line should grow or carry out subsequent processing at low temperature.
Invention content
The purpose of the present invention is to propose to a kind of novel methods preparing InSb nano wires, and are received to InSb based on this method
Rice noodles have carried out the doping of Mn elements.
To achieve the goals above, the present invention uses following technical scheme：
A kind of InSb nanowire preparation methods based on multistep Glancing angledeposition, include the following steps：
1) the pure In nano wires of monocrystalline are prepared using multistep glancing angle deposition technology；
2) Sb film layers are deposited in pure In nanowire surfaces, forms the nucleocapsid structure of In, Sb；
3) nucleocapsid structure of In, Sb are made annealing treatment, makes it that crystallization reaction occur in solid phase, formed InSb and receive
Rice noodles.
A kind of InSb nano wires Mn doping preparation methods based on multistep Glancing angledeposition, include the following steps：
1) the pure In nano wires of monocrystalline are prepared using multistep glancing angle deposition technology；
2) Mn film layers are deposited in pure In nanowire surfaces, forms the nucleocapsid structure of In, Mn；
3) Sb film layers are deposited in Mn film surfaces, forms the nucleocapsid structure of In, Mn, Sb；
4) nucleocapsid structure of In, Mn, Sb are made annealing treatment, makes it that crystallization reaction occur in solid phase, formed Mn and mix
Miscellaneous InSb nano wires.
The beneficial effects of the invention are as follows：The present invention realizes to be prepared InSb nano wires and carries out mixing for Mn elements at low temperature
It is miscellaneous.In this technique, the solubility limit that the content of Mn elements can not be by Mn in InSb materials contains to obtain high Mn
The InSb nano wires of amount.
Description of the drawings
Figure 1A~Fig. 1 D are the schematic diagram that multistep glancing angle method prepares InSb nano wires in the present invention.Wherein, Tu1AWei
Prepare the vacuum deposition system schematic diagram of In nano wires；Figure 1B is the schematic diagram that multistep glancing angle method prepares pure In nano wires；
Fig. 1 C are the schematic diagram that Sb films are deposited outside In lines；Fig. 1 D are the schematic diagram of formation InSb nano wires after annealing.
Fig. 2A~Fig. 2 D are the schematic diagram for the InSb nano wires that multistep glancing angle method prepares doping Mn in the present invention.Its
In, Fig. 2A is the vacuum deposition system schematic diagram for the In nano wires for preparing doping Mn；Fig. 2 B are the In nano wires for preparing doping Mn
Schematic diagram；Fig. 2 C are the schematic diagram that Sb films are deposited outside the In nano wires that Mn is adulterated；Fig. 2 D are formation Mn doping after annealing
InSb nano wires schematic diagram.
Fig. 3 is the scanning electron microscope micro-image (SEM) of In nano wires prepared by multistep glancing angle method.
Fig. 4 A and Fig. 4 B are the images of transmissive electron microscope (TEM) and X-ray energy spectrum analysis chart of InSb nano wires after annealing
(EDAX)。
Fig. 5 A and Fig. 5 B are the surface sweeping electron microscope images using the FET device of the InSb nano wires prepared in the present invention
(SEM) transfer characteristic curve and measured at room temperature.
Fig. 6 A and Fig. 6 B are that the images of transmissive electron microscope (TEM) for the InSb nano wires for adulterating Mn elements and X-ray energy spectrum are analyzed
Scheme (EDAX).
Specific implementation mode
Below by specific embodiments and the drawings, the present invention will be further described.
The present invention prepares the pure In of monocrystalline first on Si/SiO2 substrates, using multistep glancing angle deposition (GLAD) technology and receives
Rice noodles；Then the suitably uniform Sb film layers of thickness are superscribed outside pure In nano wires, form the core-shell (cores-of In, Sb
Shell) structure；The core-shell structures of In, Sb are made annealing treatment in suitable temperature finally, it is made to occur in solid phase
Crystallization reaction forms InSb nano wires.In this process, the present invention attempts the deposition between In and Sb and adulterates a small amount of magnetism
Element (Mn), to realize to the magnetic-doped of InSb nano wires.
The above-mentioned InSb nano wires based on multistep Glancing angledeposition prepare and doping method, as depicted in figs. 1 and 2, tool
Body includes the following steps：
(1) preparation of In nano wires
During multistep glancing angle method prepares pure In nano wires, the present embodiment uses the vacuum of resistance heating
Depositing system (ULVACVWR-400), Figure 1A are its structural schematic diagram.In deposition process, chamber is evacuated to about 3 × 10-3Pa
Below.The solid In particles that evaporation source is 99.99% using purity, are positioned in the tungsten boat below substrate.Substrate uses surface
There is the SiO of 300nm thickness2The silicon chip of layer.Substrate is fixed on a specimen holder, specimen holder make substrate center always with steaming
It rises and keeps the distance of about 150mm~200mm, preferred value 170mm.Between substrate normal direction and evaporation air source 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 wires.It is carried out 3 times or more in entire deposition process
Vacuum chamber is deflated during each interruption (10 minutes or so) and Rotary Specimen Rack (is typically by intentional interruption
90 °) to have the function that oxidation sample surface.In atoms are at original when the oxidation of sample surfaces can prevent plated film next time
The epitaxial growth on grain surface so that new In particles can all be formed each time by being deposited.In deposition process, the sources In evaporation rate exists
Between 0.5~1.5nm/s, preferred value 1nm/s, In deposition rates are 0.87nm/s, preceding deposition thickness three times on silicon chip at this time
Between 40~60nm, preferred value 50nm.In this way, three times be deposited after meeting, Si pieces surface can be formed one layer it is isotropic
In granular grows films, the growth for In nano wires in vapor deposition next time provide good growing environment.4th deposition thickness
Between 250nm~350nm, preferred value 300nm, to grow In nano wires.Fig. 3 is In prepared by multistep glancing angle method
The scanning electron microscope micro-image (SEM) of nano wire.
(2) formation of the core-shell structures of In, Sb
Fig. 1 C are the schematic diagram that Sb films are deposited outside In lines.During the vapor deposition of Sb films, the present embodiment uses
Magnetron sputtering plating instrument (Kurt J.Lesker PRO Line PVD 75).In deposition process, chamber is evacuated to less than 9
×10-5Pa.The metal Sb blocks that target is 99.99% using purity.In coating process, growth has the silicon wafer horizontal of In nano wires to put
It sets, is rotated with the rate uniform of 5~10rad/s, preferred rate 5rad/s.Operating power is set as 30W, then Sb elements with
The rate uniform of 0.1~0.3nm/s (preferred value 0.2nm/s) is deposited on silicon chip, total deposition thickness be 50nm~100nm it
Between, preferred value 70nm.
(3) the core-shell structures of In, Sb are made annealing treatment
After the Sb films of 50nm~100nm have been deposited, sample is positioned in tube furnace (Lindberg TF55035KC)
It anneals.Annealing process continues at least ten hour, in 5 initial hours, is uniformly heating to 150~250 DEG C, preferably
Value be 200 DEG C, then maintain the temperature at 200 DEG C it is 5 hours constant.Hydrogen is selected as carrier gas, gas in entire annealing process
Flow velocity rate is 80~120sccm, preferred value 100sccm.Fig. 1 D are the schematic diagram of formation InSb nano wires after annealing.
Fig. 4 A and Fig. 4 B are the images of transmissive electron microscope (TEM) and X-ray energy spectrum analysis chart of the InSb nano wires after annealing
(EDAX).Wherein, Fig. 4 A indicate the crystal structure figure that high resolution transmission electron microscopy (HR-TEM) is observed, illustration is high score
Distinguish the Fourier transform (FFT) of image, it can be seen that the nano wire is the zincblende lattce structure of InSb；Fig. 4 B are using in TEM
Energy dispersion X ray spectrum instrument (EDAX) elemental composition that nano wire is carried out analyze, indicate that the ingredient of nano wire is more pure,
Predominantly two kinds of elements of In, Sb, and In, Sb component ratio detected is about 1:1 or so.
(4) between In, Sb Mn elements doping
After step (1) prepares In nano wires using multistep glancing angle method, the vacuum deposition system in resistance heating is selected
The middle deposition in situ for carrying out Mn elements is to form the core-shell structures of In-Mn, as shown in Figure 2 A.Fig. 2 B are to prepare doping Mn
In nano wires schematic diagram.In deposition process, chamber is equally evacuated to 3 × 10-3Pa, evaporation source are that purity is
99.99% solid Mn thin slices, are positioned in the tungsten boat below silicon chip.In deposition process, the sources Mn evaporation rate be 0.05~
0.15nm/s, preferred value 0.1nm/s, at this time.On silicon chip Mn deposition rates be 0.087nm/s, deposition thickness be 5nm~
20nm, preferred value 20nm.In nano wires after Mn doping equally use the vapor deposition of magnetron sputtering plating instrument progress Sb films, with
The core-shell structures of In, Mn, Sb are formed, as shown in Figure 2 C.
(5) annealing of the InSb nano wires of Mn doping
After the Sb films of 70nm have been deposited, sample is transferred on silicon chip or micro-grid, then is positioned over tube furnace (Lindberg
TF55035KC it anneals in).Annealing process continues at least ten hour, in 5 initial hours, is uniformly heating to 150
~250 DEG C, preferred value be 200 DEG C, then maintain the temperature at 200 DEG C it is 5 hours constant.Hydrogen is selected in entire annealing process
As carrier gas, airflow rate is 80~120sccm, preferred value 100sccm.Fig. 2 D are to form the InSb that Mn is adulterated after annealing to receive
The schematic diagram of rice noodles.
Fig. 5 A and Fig. 5 B are the field-effect transistor with top gate structure of the InSb nano wires prepared using the present invention
(FETs) and at room temperature transfer characteristic curve figure, wherein Fig. 5 A are device figure, and corresponding source and drain has been marked on picture with grid
In.Fig. 5 B are to measure the transfer characteristic curve that obtains, and abscissa is grid voltage Vg, and ordinate is source-drain current Ids, and when measurement controls
Source-drain voltage Vds=1mV can be seen that the InSb nano wires are typical n-type semiconductor according to the curve.
Fig. 6 A and Fig. 6 B are the images of transmissive electron microscope and X-ray energy spectrum analysis chart for the InSb nano wires for adulterating Mn elements,
Middle Fig. 6 A indicate that the crystal structure figure that high resolution transmission electron microscopy (HR-TEM) is observed, illustration are Fu of full resolution pricture
In leaf conversion (FFT), it can be seen that the nano wire is similarly the zincblende lattce structure of InSb；Fig. 6 B are to use the energy color in TEM
It dissipates X-ray spectrometer (EDAX) to analyze the elemental composition that nano wire carries out, the ingredient of nano wire is more pure, predominantly In, Sb
Two kinds of elements contain a small amount of Mn elements, and In, Sb component ratio detected is about 1:1 or so.
Table 1 is component ratio of the InSb nano wires under X-ray energy spectrum analyzer (EDAX) after adulterating Mn elements.Wherein
Main component be In, Sb, ratio is 34% or so；In addition, there is a small amount of Mn elements, ratio is 4% or so, copper (Cu) member
Element is introduced by the copper mesh in micro-grid.The influence of copper is removed, ratios of the Mn in InSb nano wires is 5.19%, and general
The Mn contents of CVD growth doping are 2~3% or so, and after illustrating method using the present invention, the content of Mn elements can not be by Mn
Solubility limit in InSb materials has obtained the InSb nano wires of high Mn content.
Table 1. adulterates the component ratio of the InSb nano wires after Mn elements
| 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 structures of second step In, Sb, the present invention also can be used
Sb films are deposited in thermal evaporation deposition.
In another embodiment, in the step of core-shell structures of the processing of third step annealing In, Sb, which also may be used
It is transferred in Si pieces or micro-grid and anneals.
The above embodiments are merely illustrative of the technical solutions of the present invention rather than is limited, the ordinary skill of this field
Personnel can be modified or replaced equivalently technical scheme of the present invention, without departing from the spirit and scope of the present invention, this
The protection domain of invention should be subject to described in claims.
Claims (9)
1. a kind of InSb nanowire preparation methods based on multistep Glancing angledeposition, include the following steps：
1) the pure In nano wires of monocrystalline are prepared using multistep glancing angle deposition technology；
2) Sb film layers are deposited in pure In nanowire surfaces, forms the nucleocapsid structure of In, Sb；
3) nucleocapsid structure of In, Sb are made annealing treatment, makes it that crystallization reaction occur in solid phase, form InSb nano wires.
2. a kind of InSb nano wires Mn based on multistep Glancing angledeposition adulterates preparation method, include the following steps：
1) the pure In nano wires of monocrystalline are prepared using multistep glancing angle deposition technology；
2) Mn film layers are deposited in pure In nanowire surfaces, forms the nucleocapsid structure of In, Mn；
3) Sb film layers are deposited in Mn film surfaces, forms the nucleocapsid structure of In, Mn, Sb；
4) nucleocapsid structure of In, Mn, Sb are made annealing treatment, makes it that crystallization reaction occur in solid phase, form Mn doping
InSb nano wires.
3. method according to claim 1 or 2, which is characterized in that step 1) is in Si/SiO2The pure In of monocrystalline is prepared on substrate
Nano wire, substrate center are kept with evaporation source at a distance from 150mm~200mm, substrate normal direction and evaporation air source ascent direction
Between angle α be 80 °~90 °.
4. method according to claim 1 or 2, which is characterized in that step 1) is carried out in deposition process more than three times
It interrupts, by vacuum chamber deflation and Rotary Specimen Rack during each interrupt, with oxidation sample surface.
5. according to the method described in claim 4, it is characterized in that, step 1) is in deposition process, the sources In evaporation rate is 0.5
~1.5nm/s, preceding deposition thickness three times are 40~60nm；After being deposited three times, one layer of Si pieces surface formation is isotropic
In granular grows films；4th deposition thickness is 250nm~350nm, to grow In nano wires.
6. method according to claim 1 or 2, which is characterized in that use magnetron sputtering coating method or thermal evaporation deposition
The vapor deposition of Sb films is carried out, the deposition rate of Sb elements is 0.1~0.3nm/s, and total deposition thickness is 50nm~100nm.
7. method according to claim 1 or 2, which is characterized in that carry out the annealing using tube furnace, annealing process is held
Continuous at least ten hour is uniformly heating to 150~250 DEG C in 5 initial hours, then keeps temperature-resistant 5 hours；
Using hydrogen as carrier gas in entire annealing process, airflow rate is 80~120sccm.
8. according to the method described in claim 2, it is characterized in that, after step 1) prepares In nano wires, step 2) is in resistance
The deposition of Mn elements is carried out in the vacuum deposition system of heating in situ to form the nucleocapsid structure of In, Mn；The Mn in deposition process
Source evaporation rate is 0.05~0.15nm/s, and the deposition thickness of Mn is 5nm~20nm on silicon chip.
9. according to the InSb nano wires of doping Mn prepared by any claim the method in claim 2 to 8.
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