CN108265268A - A kind of TiO of V doping2Film and preparation method thereof - Google Patents

A kind of TiO of V doping2Film and preparation method thereof Download PDF

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CN108265268A
CN108265268A CN201810167506.XA CN201810167506A CN108265268A CN 108265268 A CN108265268 A CN 108265268A CN 201810167506 A CN201810167506 A CN 201810167506A CN 108265268 A CN108265268 A CN 108265268A
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tio
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CN108265268B (en
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江凤仙
纪丽飞
曾泽亭
周国伟
许小红
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Shanxi University
Shaanxi Normal University
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/28Vacuum evaporation by wave energy or particle radiation
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08Oxides
    • C23C14/083Oxides of refractory metals or yttrium

Abstract

The invention belongs to technical field of semiconductor, and in particular to a kind of V doping TiO with metallic conductivity and room-temperature ferromagnetic2Film and preparation method thereof.The film selects nonmagnetic V to be doped as dopant, avoids the generation of ferromagnetism cluster, while V3+There is less than d electronics, local magnetic moment is provided for ferromagnetic generation.When the present invention prepares film using pulsed laser deposition, by controlling experiment condition, obtain that there is metallic conductivity and room-temperature ferromagnetic TiO2Film, carrier concentration is 5.4 × 1020‑8.0×1020cm‑3It is adjustable.This just provides possibility to regulate and control the carrier concentration in sample using electric field and then regulating and controlling its magnetism, so as to meet the requirement of the novel spin electric device with Good All-around Property, helps to substantially reduce the energy consumption of device.

Description

A kind of TiO of V doping2Film and preparation method thereof
Technical field
The invention belongs to technical field of semiconductor, and in particular to a kind of with metallic conductivity and room-temperature ferromagnetic The TiO of V doping2Film and preparation method thereof.
Background technology
In advanced information society, magnetic material and semi-conducting material respectively play very important effect.Information Storage is realized using the spin attribute of electronics in magnetic material, and the processing of information utilizes electronics in semi-conducting material Charge attribute is completed.Dilute magnetic semiconductor is to mix a kind of semi-conducting material formed after magnetic ion, energy in the semiconductors Simultaneously using electronics charge attribute and spin attribute, have both ferromagnetic property and semiconducting behavior, show many excellent magnetic, Magneto-optic and magnetic electricity performance, have broad application prospects in area of Spintronics.
The GaAs dilute magnetic semiconductors of Mn doping are acknowledged as a kind of intrinsic dilute magnetic semiconductor material, but it is most in In temperature also only have 200K, far from the requirement for meeting electronic component temperature in use.Since Matsumoto in 2001 et al. head The secondary Co doping TiO for being prepared for Curie temperature and being up to 400K2After diluted semi-conductor thin-film, people are to TiO2Based diluted magnetic semiconductor Extensive research is carried out.But in previous research, focus of concern is concentrated mainly on transient metal doped TiO2It is dilute The research of the preparation method of magnetic semiconductor, structure and magnetic aspect, and to transient metal doped TiO2Dilute magnetic semiconductor transport property Matter (i.e. electric conductivity and carrier concentration etc.) is paid close attention to seldom, and the electric conductivity of sample is poor, carrier concentration very little, this will cause People cannot regulate and control its carrier concentration to regulate and control its magnetism, so as to limit it in spintronics device by extra electric field Application in part.
Invention content
Therefore, the technical problem to be solved in the present invention is to overcome transient metal doped TiO in the prior art2Dilute magnetic is partly led The defects of body electric conductivity is poor, and carrier concentration is small, so as to provide a kind of V doping with metallic conductivity and room-temperature ferromagnetic TiO2Film and preparation method thereof.
In order to solve the above technical problems, the present invention adopts the following technical scheme that:
A kind of TiO of V doping2Film, the film is by Ti1-xVxO2Composition, wherein x=0.03-0.05;During room temperature, institute The carrier concentration for stating film is 5.4 × 1020-8.0×1020cm-3
Further, the film be Rutile structure, film thickness 30-250nm.
A kind of TiO of above-mentioned V doping2The preparation method of film, includes the following steps:
It is prepared by target:With TiO2And V2O5For raw material, required Ti is prepared using solid reaction process1-xVxO2Ceramic target;
Thin film deposition:By the Ti1-xVxO2Ceramic target is 2.0-5.0 × 10 in oxygen partial pressure-4Under Pa, pass through pulse Laser deposition is in SrTiO3Deposition on substrate V adulterates TiO2Film.Film can be controlled thick by controlling the thin film deposition time Degree.
Further, substrate temperature is 750-800 DEG C in the thin film deposition steps, and pulsed laser energy is about 1.0- 2.0J/cm2, laser frequency 5-10Hz.
Further, the average sedimentation rate in the thin film deposition steps is 0.1-0.3nm/s.
Further, the target preparation process detailed process is as follows:
Pretreatment of raw material:By TiO2And V2O5Powder is sufficiently mixed, and grinds 4-6h, tabletting, (purity is in high purity oxygen gas atmosphere 99.999%) pre-burning is carried out in, calcined temperature is 1000-1100 DEG C, time 8-10h;
Sintering:By the material grind into powder after pre-burning, tabletting carries out in high purity oxygen gas atmosphere (purity 99.999%) Sintering, sintering temperature are 1200-1300 DEG C, and time 12-14h obtains Ti1-xVxO2Ceramic target.
Further, the tabletting conditions in the feed pretreatment step is suppress 20- under the pressure of 20-25MPa 30min。
Further, the condition of tabletting is to suppress 30-60min under the pressure of 30-35MPa in the sintering step.
Technical solution of the present invention has the following advantages that:
V doping TiO provided by the invention with metallic conductivity and room-temperature ferromagnetic2Film selects non magnetic first V be doped as dopant because metal V and its oxide be all without ferromagnetism, so as to avoid ferromagnetism cluster It generates, due to having V in film3+In the presence of because it is with less than d electronics, local magnetic moment is provided for ferromagnetic generation.The Two, when the present invention prepares film using pulsed laser deposition, low oxygen partial pressure is selected in preparation process, this is because oxygen Oxygen vacancy concentration is bigger in the lower film of pressure, and the electric conductivity of film is better, can finally obtain with metallic conductivity and The V doping TiO of room-temperature ferromagnetic2Film, room temperature carrier concentration is 5.4 × 1020-8.0×1020cm-3.In addition, film is thick Spend smaller, the defects of film can be more, and carrier concentration also can be bigger, so as to the partial pressure of oxygen in preparation process and Thickness is to TiO2The carrier concentration of film is adjusted, this is just the carrier concentration and then tune regulated and controled using electric field in sample It controls its magnetism and provides possibility, so as to meet the requirement of the novel spin electric device with Good All-around Property, help In the energy consumption for substantially reducing device.
Description of the drawings
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution of the prior art Embodiment or attached drawing needed to be used in the description of the prior art are briefly described, it should be apparent that, in being described below Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor It puts, can also be obtained according to these attached drawings other attached drawings.
Fig. 1 is the X-ray diffractogram of the embodiment of the present invention 2 and embodiment 7;
Fig. 2 is the x-ray photoelectron spectroscopy figure of V2p energy levels in 7 film of the embodiment of the present invention;
Fig. 3 is the x-ray photoelectron spectroscopy figure of Ti2p energy levels in 7 film of the embodiment of the present invention;
Fig. 4 is the hysteresis loop figure of the embodiment of the present invention 1, embodiment 2, embodiment 3 and embodiment 4 in 300K;
Fig. 5 is the hysteresis loop figure of the embodiment of the present invention 5, embodiment 6, embodiment 7 and embodiment 8 in 300K;
Fig. 6 is that the resistivity of the embodiment of the present invention 1, embodiment 2, embodiment 3 and embodiment 4 varies with temperature curve graph;
Fig. 7 is that the resistivity of the embodiment of the present invention 5, embodiment 6, embodiment 7 and embodiment 8 varies with temperature curve graph.
Specific embodiment
It is conventional method unless otherwise specified in following embodiments.Raw material used in the embodiment, such as nothing Specified otherwise can obtain from commercial channels.
Embodiment 1
Thickness is the Ti of 30nm0.97V0.03O2Film
Prepare Ti0.97V0.03O2Target:(1) it is 0.97 according to the molar ratio of Ti in target and V:0.03 meter accurate in scale High-purity Ti O needed for calculating2And V2O5The quality of powder uses high Accuracy Electronic Balance precise;(2) load weighted various After powder is sufficiently mixed in agate mortar, 5h is firmly ground;(3) ground powder is poured into compression mold, in 20MPa Pressure under suppress 25min, the sheet target suppressed is put into corundum crucible, in high purity oxygen gas atmosphere, (purity is 99.999%) high temperature pre-burning is carried out in tube furnace, calcined temperature is 1000 DEG C, time 8h;(4) target after pre-burning is put Enter in agate mortar and be firmly ground into uniform fine powder, 30min is suppressed under the pressure of 30MPa with compression mold, by what is pressed Sheet target is put into corundum crucible, and high temperature sintering is carried out in the tube furnace of high purity oxygen gas atmosphere (purity 99.999%), is burnt Junction temperature is 1200 DEG C, time 12h, obtains fine and close Ti0.97V0.03O2Target.
Depositing Ti0.97V0.03O2Film:Using pulsed laser deposition technique, the Ti being prepared is utilized0.97V0.03O2Ceramics Target, in SrTiO3Deposition on substrate Ti0.97V0.03O2Film.When growth room's base vacuum is less than 6 × 10-5During Pa, begin to warm up Substrate starts deposition film when substrate temperature rises to 760 DEG C, and oxygen partial pressure is about 2.0 × 10 in film deposition process-4Pa, Pulsed laser energy is about 1.2J/cm2, laser frequency 10Hz, sedimentation time 5min, it is 30nm's to obtain thickness Ti0.97V0.03O2Film.
Embodiment 2
Thickness is the Ti of 50nm0.97V0.03O2Film
Ti0.97V0.03O2The preparation method of target is same as Example 1.
Depositing Ti0.97V0.03O2Film:Using pulsed laser deposition technique, the Ti being prepared is utilized0.97V0.03O2Ceramics Target, in SrTiO3Deposition on substrate Ti0.97V0.03O2Film.When growth room's base vacuum is less than 6 × 10-5During Pa, begin to warm up Substrate starts deposition film when substrate temperature rises to 760 DEG C, and oxygen partial pressure is about 2.3 × 10 in film deposition process-4Pa, Pulsed laser energy is about 1.5J/cm2, laser frequency 10Hz, sedimentation time 8min, it is 50nm's to obtain thickness Ti0.97V0.03O2Film.
Embodiment 3
Thickness is the Ti of 135nm0.97V0.03O2Film
Ti0.97V0.03O2The preparation method of target is same as Example 1.
Depositing Ti0.97V0.03O2Film:Using pulsed laser deposition technique, the Ti being prepared is utilized0.97V0.03O2Ceramics Target, in SrTiO3Deposition on substrate Ti0.97V0.03O2Film.When growth room's base vacuum is less than 6 × 10-5During Pa, begin to warm up Substrate starts deposition film when substrate temperature rises to 780 DEG C, and oxygen partial pressure is about 2.5 × 10 in film deposition process-4Pa, Pulsed laser energy is about 1.5J/cm2, laser frequency 10Hz, sedimentation time 13min, it is 135nm's to obtain thickness Ti0.97V0.03O2Film.
Embodiment 4
Thickness is the Ti of 240nm0.97V0.03O2Film
Ti0.97V0.03O2The preparation method of target is same as Example 1.
Depositing Ti0.97V0.03O2Film:Using pulsed laser deposition technique, the Ti being prepared is utilized0.97V0.03O2Ceramics Target, in SrTiO3Deposition on substrate Ti0.97V0.03O2Film.When growth room's base vacuum is less than 6 × 10-5During Pa, begin to warm up Substrate starts deposition film when substrate temperature rises to 800 DEG C, and oxygen partial pressure is about 2.8 × 10 in film deposition process-4Pa, Pulsed laser energy is about 1.8J/cm2, laser frequency 10Hz, sedimentation time 20min, it is 240nm's to obtain thickness Ti0.97V0.03O2Film.
Embodiment 5
Thickness is the Ti of 60nm0.95V0.05O2Film
Prepare Ti0.97V0.05O2Target:(1) it is 0.95 according to the molar ratio of Ti in target and V:0.05 meter accurate in scale High-purity Ti O needed for calculating2And V2O5The quality of powder uses high Accuracy Electronic Balance precise;(2) load weighted various After powder is sufficiently mixed in agate mortar, 6h is firmly ground;(3) ground powder is poured into compression mold, in 25MPa Pressure under suppress 30min, the sheet target suppressed is put into corundum crucible, in high purity oxygen gas atmosphere, (purity is 99.999%) high temperature pre-burning is carried out in tube furnace, calcined temperature is 1100 DEG C, time 10h;(4) by the target after pre-burning It is put into agate mortar and is firmly ground into uniform fine powder, suppress 60min under the pressure of 35MPa with compression mold, will press Sheet target be put into corundum crucible, high temperature sintering is carried out in the tube furnace of high purity oxygen gas atmosphere (purity 99.999%), Sintering temperature is 1250 DEG C, time 14h, obtains fine and close Ti0.95V0.05O2Target.
Depositing Ti0.97V0.05O2Film:Using pulsed laser deposition technique, the Ti being prepared is utilized0.97V0.05O2Ceramics Target, in SrTiO3(100) deposition on substrate Ti0.97V0.05O2Film.When growth room's base vacuum is less than 6 × 10-5During Pa, open Begin heating substrate, starts deposition film when substrate temperature rises to 780 DEG C, in film deposition process oxygen partial pressure be about 2.6 × 10-4Pa, pulsed laser energy are about 1.4J/cm2, laser frequency 10Hz, sedimentation time 5min, it is 60nm's to obtain thickness Ti0.97V0.05O2Film.
Embodiment 6
Prepare the Ti that thickness is 80nm0.95V0.05O2Film
Ti0.95V0.05O2The preparation method of target is same as Example 5.
Depositing Ti0.97V0.05O2Film:Using pulsed laser deposition technique, the Ti being prepared is utilized0.97V0.05O2Ceramics Target, in SrTiO3(100) deposition on substrate Ti0.97V0.05O2Film.When growth room's base vacuum is less than 6 × 10-5During Pa, open Begin heating substrate, starts deposition film when substrate temperature rises to 780 DEG C, in film deposition process oxygen partial pressure be about 3.0 × 10-4Pa, pulsed laser energy are about 1.6J/cm2, laser frequency 10Hz, sedimentation time 8min, it is 80nm's to obtain thickness Ti0.97V0.05O2Film.
Embodiment 7
Prepare the Ti that thickness is 100nm0.95V0.05O2Film
Ti0.95V0.05O2The preparation method of target is same as Example 5.
Depositing Ti0.97V0.05O2Film:Using pulsed laser deposition technique, the Ti being prepared is utilized0.97V0.05O2Ceramics Target, in SrTiO3(100) deposition on substrate Ti0.97V0.05O2Film.When growth room's base vacuum is less than 6 × 10-5During Pa, open Begin heating substrate, starts deposition film when substrate temperature rises to 800 DEG C, in film deposition process oxygen partial pressure be about 4.0 × 10-4Pa, pulsed laser energy are about 1.8J/cm2, laser frequency 10Hz, sedimentation time 10min obtain thickness as 100nm Ti0.97V0.05O2Film.
Embodiment 8
Prepare the Ti that thickness is 245nm0.95V0.05O2Film
Ti0.95V0.05O2The preparation method of target is same as Example 5.
Depositing Ti0.97V0.05O2Film:Using pulsed laser deposition technique, the Ti being prepared is utilized0.97V0.05O2Ceramics Target, in SrTiO3(100) deposition on substrate Ti0.97V0.05O2Film.When growth room's base vacuum is less than 6 × 10-5During Pa, open Begin heating substrate, starts deposition film when substrate temperature rises to 800 DEG C, in film deposition process oxygen partial pressure be about 5.0 × 10-4Pa, pulsed laser energy are about 2.0J/cm2, laser frequency 10Hz, sedimentation time 13min obtain thickness as 245nm Ti0.97V0.05O2Film.
Comparative example 1
Prepare the Ti that thickness is 120nm0.97V0.03O2Film
Ti0.97V0.03O2The preparation method of target is same as Example 1.
Depositing Ti0.97V0.03O2Film:Using pulsed laser deposition technique, the Ti being prepared is utilized0.97V0.03O2Ceramics Target, in SrTiO3Deposition on substrate Ti0.97V0.03O2Film.When growth room's base vacuum is less than 7 × 10-5During Pa, begin to warm up Substrate starts to be passed through high purity oxygen gas (purity 99.999%) to vacuum chamber when substrate temperature rises to 800 DEG C, adjusts oxygen point It presses as 1.3Pa, pulsed laser energy is about 2.5J/cm2, laser frequency 10Hz, sedimentation time 12min, obtaining thickness is The Ti of 120nm0.97V0.03O2Film.Obtained film is by testing, and with room-temperature ferromagnetic, but film conductivity is too poor, Resistivity has exceeded apparatus measures range, and carrier concentration is less than the detection limit of instrument, can not measure.
Comparative example 2
Prepare the Ti that thickness is 125nm0.95V0.05O2Film
Ti0.95V0.05O2The preparation method of target is same as Example 5.
Depositing Ti0.95V0.05O2Film:Using pulsed laser deposition technique, the Ti being prepared is utilized0.95V0.05O2Ceramics Target, in SrTiO3Deposition on substrate Ti0.95V0.05O2Film.When growth room's base vacuum is less than 8 × 10-5During Pa, begin to warm up Substrate starts to be passed through high purity oxygen gas (purity 99.999%) to vacuum chamber when substrate temperature rises to 800 DEG C, adjusts oxygen point It presses as 1.3Pa, pulsed laser energy is about 2.8J/cm2, laser frequency 10Hz, sedimentation time 13min, obtaining thickness is The Ti of 125nm0.95V0.05O2Film.Obtained film is by testing, and with room-temperature ferromagnetic, but film conductivity is too poor, Resistivity has exceeded apparatus measures range, and carrier concentration is less than the detection limit of instrument, can not measure.
Performance test
Film prepared by embodiment 2 and embodiment 7 is subjected to X-ray diffraction analysis, gained spectrogram is shown in Fig. 1.In order to more Whether in film have the diffraction maximum of impurity phase, we choose the logarithm of X-ray diffraction intensity as ordinate if being clearly viewed.From Fig. 1 can be seen that Ti1-xVxO2Film is Rutile structure, does not find the diffraction maximum of V metals and the oxide of V, illustrates V Ion enters TiO2In lattice, part is instead of Ti ions.
By the Ti prepared by embodiment 70.95V0.05O2Film carry out X-ray photoelectron spectroscopic analysis, gained spectrogram see Fig. 2- 3.Fig. 2 is the x-ray photoelectron spectroscopy figure of V2p energy levels in film, it can be seen from the figure that V2p3/2And V2p1/2Binding energy point Not Wei 515.4eV and 523.1eV, illustrate V with V3+The form of ion is present in film.Fig. 3 is that the X of Ti2p energy levels in film is penetrated Photoelectron spectra figure, it can be seen from the figure that Ti2p3/2And Ti2p1/2Binding energy be respectively 458.5eV and 464.3eV, say Bright Ti is with Ti4+The form of ion is present in film.
The room temperature hysteresis loop figure of film prepared by embodiment 1, embodiment 2, embodiment 3 and embodiment 4 is shown in Fig. 4, from Fig. 4 can be seen that V doping TiO2Film shows apparent room-temperature ferromagnetic, and thickness is the Ti of 30nm0.97V0.03O2Film Saturation magnetization is 1.9 μB/V。
The room temperature hysteresis loop figure of film prepared by embodiment 5, embodiment 6, embodiment 7 and embodiment 8 is shown in Fig. 5, from Fig. 5 can be seen that the Ti of different-thickness0.95V0.05O2Film also shows that apparent room-temperature ferromagnetic, and thickness is 60nm's Ti0.95V0.05O2The saturation magnetization of film is 0.2 μB/V。
The resistivity of film prepared by embodiment 1- embodiments 8 varies with temperature curve graph and sees Fig. 6-7.It can be with from figure Find out, the Ti of different-thickness1-xVxO2Film all shows metallic conductivity.
The room temperature resistivity and carrier concentration of film prepared by embodiment 1- embodiments 8 are shown in Table 1.The room temperature electricity of film Resistance rate is about 1.2 × 10-4-6.0×10-4Ω cm, carrier concentration are about 5.4 × 1020-8.0×1020cm-3.The institute of film To have preferable electric conductivity, mainly oxygen partial pressure (2.0-5.0 × 10 low with what is selected in our preparation process-4Pa) have It closes, oxygen partial pressure is lower in preparation process, and oxygen vacancy concentration is bigger in film, and the electric conductivity of film is better.This point from Comparative example 1 and 2 can prove.
The room temperature resistivity and carrier concentration of 1 film of table
Sample Carrier concentration/cm-3 Room temperature resistivity/10-4Ω·cm
Embodiment 1 8.0×1020 1.2
Embodiment 2 7.6×1020 2.4
Embodiment 3 7.2×1020 3.4
Embodiment 4 5.4×1020 6.0
Embodiment 5 7.9×1020 1.8
Embodiment 6 7.0×1020 3.7
Embodiment 7 6.0×1020 4.6
Embodiment 8 5.6×1020 5.2
Obviously, the above embodiments are merely examples for clarifying the description, and is not intended to limit the embodiments.It is right For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or It changes.There is no necessity and possibility to exhaust all the enbodiments.And the obvious variation thus amplified out or Among changing still in the protection domain of the invention.

Claims (8)

1. a kind of TiO of V doping2Film, which is characterized in that the film is by Ti1-xVxO2Composition, wherein x=0.03-0.05; During room temperature, the carrier concentration of the film is 5.4 × 1020-8.0×1020cm-3
2. the TiO of V doping according to claim 12Film, which is characterized in that the film is Rutile structure, thin Film thickness is 30-250nm.
3. a kind of TiO of claim 1-2 any one of them V doping2The preparation method of film, which is characterized in that including following Step:
It is prepared by target:With TiO2And V2O5For raw material, Ti is prepared using solid reaction process1-xVxO2Ceramic target;
Thin film deposition:By the Ti1-xVxO2Ceramic target is 2.0-5.0 × 10 in oxygen partial pressure-4Under Pa, pass through pulse laser Sedimentation is in SrTiO3The TiO of deposition on substrate V doping2Film.
4. the TiO of V doping according to claim 32The preparation method of film, which is characterized in that the thin film deposition steps Middle substrate temperature is 750-800 DEG C, and pulsed laser energy is about 1.0-2.0J/cm2, laser frequency 5-10Hz.
5. the TiO of V doping according to claim 32The preparation method of film, which is characterized in that the thin film deposition steps In average sedimentation rate 0.1-0.3nm/s.
6. the TiO adulterated according to claim 3-5 any one of them V2The preparation method of film, which is characterized in that the target Preparation process detailed process is as follows:
Pretreatment of raw material:By TiO2And V2O5Powder is sufficiently mixed, and grinds 4-6h, and tabletting carries out pre-burning in high purity oxygen gas atmosphere, Calcined temperature is 1000-1100 DEG C, time 8-10h;
Sintering:By the material grind into powder after pre-burning, tabletting is sintered in high purity oxygen gas atmosphere, sintering temperature 1200- 1300 DEG C, time 12-14h obtains Ti1-xVxO2Ceramic target.
7. the TiO of V doping according to claim 62The preparation method of film, which is characterized in that the pretreatment of raw material step Tabletting conditions in rapid is suppress 20-30min under the pressure of 20-25MPa.
8. the TiO adulterated according to V according to claim 62The preparation method of film, which is characterized in that the sintering step The condition of middle tabletting is suppresses 30-60min under the pressure of 30-35MPa.
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