CN106920623A - A kind of Ar particle irradiations strengthen the ZnO thin film doped ferromagnetic methods of Cr - Google Patents
A kind of Ar particle irradiations strengthen the ZnO thin film doped ferromagnetic methods of Cr Download PDFInfo
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- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/40—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials of magnetic semiconductor materials, e.g. CdCr2S4
- H01F1/401—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials of magnetic semiconductor materials, e.g. CdCr2S4 diluted
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Abstract
The present invention relates to a kind of Ar particle irradiations enhancing ZnO thin film doped ferromagnetic methods of Cr, irradiated so that the Ar particles of doses are ZnO thin film doped to Cr, the Cr ZnO thin film doped chemical formula is Zn1‑xCrxO, wherein 0 ＜ x≤0.05.The inventive method stabilization is effective, and ferromagnetism that can be to zno-based diluted semi-conductor thin-film on the premise of material is not destroyed carries out effectively significant enhancing, is conducive to the development of the spin electric device based on dilute magnetic semiconductor material.
Description
Technical field
The present invention relates to a kind of Ar particle irradiations enhancing ZnO thin film doped ferromagnetic methods of Cr, belong to new function half
Conductor Material Field.
Background technology
Dilute magnetic semiconductor is generally referred in nonmagnetic semiconductor material by introducing the metal unit with 3d or 4f electronics
Plain part substitutes the class new function semi-conducting material that non magnetic ion is formed.Traditional semiconductor devices only used electricity
Son electric charge attribute, magnetic memory device material merely with electronics spin attribute, the spin electric device for receiving much concern at present
Can simultaneously using the electric charge and this attribute that spins of electronics.Spin electric device has fast non-volatile, speed, small volume, power consumption
Low advantage, it is considered to be following most potential Novel electronic devices, such as spin fet, Spin Valve, spin hair
Optical diode etc..It is always limitation spin electric device that the injection efficiency of the spinning electron between magnetic metal and semiconductor is not high
The difficult point of development, and spin polarization mechanism be always limit its difficult point dilute magnetic semiconductor material for being converted into application be make spin
The preferable material of electronic device, it is possible to achieve efficient Spin Injection Efficiency.
ZnO is a kind of semiconductor material with wide forbidden band of direct band gap, and energy gap at room temperature is 3.37eV, and exciton is combined
Energy 60meV, with excellent photoelectric property., Dietl et al. in 2000[1]Calculated using mean field theory and predict transition metal
Doping ZnO has ferromagnetism more than room temperature, causes the great interest of researcher.By the research in more than ten years, people
The ferromagnetic of room temperature is obtained in transition metal (Fe, Co, Mn, Cr etc.) or rare earth metal (Er, Yb, Nd etc.) doping ZnO
Property[2-4], but the intensity of magnetization of zno-based dilute magnetic semiconductor material is weaker, and researcher is seeking to strengthen dilute magnetic semiconductor material always
The method for expecting magnetic.The ferromagnetic coupling of electronics and defect for the magnetic ion in regulation zno-based dilute magnetic semiconductor material material
Exchange plays the role of important, typically by extra implant, changes technological parameter, annealing etc. in preparation process and regulates and controls
The concentration of defect in material.
Background technology is related to document
[1]T.Dietl,H.Ohno,F.Matsukura,et al.Zener model description of
ferromagnetism in zinc-blende magnetic semiconductors,Science,2000,287(5455):
1019.
[2]P.Sharma,A.Gupta,K.V.Rao,et al.Ferromagnetism above room temperature
in bulk and transparent thin films of Mn-doped ZnO,Nature Materials,2003,2
(10):673.
[3]X.C.Liu,E.W.Shi,Z.Z.Chen,et al.Effect of donor localization on the
magnetic properties of Zn-Co-O system.Applied Physics Letters,2008,92(4):
042502.
[4]H.M.Chen,X.C.Liu,S.Y.Zhuo,et al.The dual effects of Al-doping on the
ferromagnetism of Zn0.98-yEr0.02AlyO thin films,AIP Advances,2013,3(8):
082121。
The content of the invention
Not high, the injection efficiency of spinning electron present invention is generally directed to the ZnO thin film doped saturation magnetizations of current Cr
Relatively low problem, object of the present invention is to provide a kind of method for improving problems.
Therefore, the invention provides a kind of Ar particle irradiations enhancing ZnO thin film doped ferromagnetic methods of Cr, with certain agent
The Ar particles of amount are ZnO thin film doped to Cr to be irradiated, and the Cr ZnO thin film doped chemical formula is Zn1-xCrxO, wherein 0 ＜
x≤0.05.The irradiation that the present invention passes through doses, it is possible to achieve the regulation and control to the defect in material.
It is preferred that 0.01≤x≤0.05.
It is preferred that the irradiation dose of the Ar particles is 7 × 1014~5 × 1016cm-2。
It is preferred that the irradiation energy of the Ar particles is 2.5~3.0MeV, irradiation process is carried out at room temperature.
It is preferred that the irradiation generates cation vacancy in Cr is ZnO thin film doped, by adjusting Ar particle irradiation agent
Amount and/or irradiation energy regulate and control the concentration of cation vacancy (cation vacancy defect).Additionally, the irradiation of Ar ions can keep away
Exempt from the introducing of compensation gap hydrogen defect.
It is preferred that being improve relative to predose through the ZnO thin film doped saturation magnetizations of the Cr after the irradiation
More than 65%.
It is preferred that described irradiate the composition and phase for not changing the film.
It is preferred that the Cr ZnO thin film doped preparation method is physical vaporous deposition, chemical vapour deposition technique, molten
At least one in glue-gel method and electrochemical method, preferably flux are tied up inductively coupled plasma enhancing physical vapor and are sunk
Area method.
Also, it is preferred that the Cr ZnO thin film doped preparation method includes：
(1) dry substrate, Zn will be cleaned1-xCrxO targets are put into chamber；
(2) chamber base vacuum is evacuated to≤5.0 × 10-4Pa, is passed through high-purity Ar, adjusts the pressure of cavity in 1.0-1.5Pa,
Then by silicon to 300-350 DEG C；
(3) radio-frequency power supply is finally opened, is sputtered 1.5-2 hours under the power of 100-150W.
Also, it is preferred that the material of the substrate is at least one in silicon chip, sapphire, carborundum and quartz glass.
The ZnO film that the present invention is adulterated with the non magnetic transition elements Cr of the Ar particle irradiations of doses, realizes to film
Ferromagnetic enhancing.By the saturation magnetization of the Cr of the method for the invention preparation ZnO thin film doped room-temperature ferromagnetic
Relative to the film enhancing more than 70% without Ar particle irradiations.The inventive method stabilization is effective, can not destroy material
Under the premise of effectively significant enhancing is carried out to the ferromagnetism of zno-based diluted semi-conductor thin-film, be conducive to based on dilute magnetic semiconductor material
The development of the spin electric device of material.
Brief description of the drawings
Fig. 1 is that irradiated dosage is 7 × 1014cm-2Zn before and after Ar particle irradiations0.99Cr0.01The XRD spectrum of O film samples；
Fig. 2 is Zn0.99Cr0.01The irradiated dosage of O film samples is 7 × 1014cm-2AFM photos before and after Ar particle irradiations；
Fig. 3 is Zn0.99Cr0.01The irradiated dosage of O film samples is 7 × 1014cm-2Room temperature magnetic hysteresis before and after Ar particle irradiations is returned
Line；
Fig. 4 is that irradiated dosage is 5 × 1016cm-2Zn before and after Ar particle irradiations0.95Cr0.05The XRD spectrum of O film samples；
Fig. 5 is Zn0.95Cr0.05The irradiated dosage of O film samples is 5 × 1016cm-2AFM photos before and after Ar particle irradiations；
Fig. 6 is Zn0.95Cr0.05The irradiated dosage of O film samples is 5 × 1016cm-2Room temperature magnetic hysteresis before and after Ar particle irradiations is returned
Line；
Fig. 7 is that irradiated dosage is 5 × 1015cm-2Zn before and after Ar particle irradiations0.95Cr0.05The XRD spectrum of O film samples；
Fig. 8 is Zn0.95Cr0.05The irradiated dosage of O film samples is 5 × 1015cm-2AFM photos before and after Ar particle irradiations；
Fig. 9 is Zn0.95Cr0.05The irradiated dosage of O film samples is 5 × 1015cm-2Room temperature magnetic hysteresis before and after Ar particle irradiations is returned
Line.
Specific embodiment
The present invention is further illustrated below in conjunction with accompanying drawing and following implementation methods, it should be appreciated that accompanying drawing and following implementation methods
The present invention is merely to illustrate, is not intended to limit the present invention.
The ZnO film that the present invention is adulterated using the non magnetic transition elements Cr of Ar particle irradiations, to realize to film ferromagnetism
Enhancing.The Cr ZnO thin film doped chemical formula can be Zn1-xCrxO, wherein 0 ＜ x≤0.05, preferably 0.01≤x≤
0.05。
In the present invention, the thickness of the ZnO film of Cr doping is preferably smaller than 0.5 μm, in this thickness range, doses
Ar particle irradiations can effectively be adjusted to the electronics in certain thickness film and defect, the larger film of thickness, regulation
Effect on driving birds is not good.
In the present invention, the ZnO film of Cr doping can be the film prepared by any suitable method.Its preparation method
Including but not limited in physical vaporous deposition, chemical vapour deposition technique, sol-gel process and electrochemical method at least one
Kind, preferably flux ties up inductively coupled plasma enhancing physical vaporous deposition.
In one example, inductively coupled plasma enhancing physical vaporous deposition is tied up using flux to be prepared on substrate
Zn1-xCrxO (0 ＜ x≤0.05) film.The substrate can be Sapphire Substrate, silicon chip, carborundum, glass etc..In deposition
Before, substrate is preferably and is cleaned up in advance, and cleaning method for example can be using using RCA techniques.As an example, use
RCA techniques clean up Si substrates, including：Si substrates are put into acetone and are cleaned by ultrasonic 15min, then rushed with deionized water
Wash 10min；2) Si substrates are put into and are cleaned by ultrasonic 15min in alcohol, then with rinsing 10min in deionized water；(3) Si is served as a contrast
Bottom high-purity N2Drying.
The Cr ZnO thin film doped preparation method includes：Dry substrate, Zn will be cleaned1-xCrxO targets are put into chamber
In.Chamber base vacuum is evacuated to≤5.0 × 10-4Pa, high-purity Ar is passed through with the flow of 20~30sccm, adjusts the pressure of cavity
In 1.0-1.5Pa, then by silicon to 300-350 DEG C.Radio-frequency power supply is finally opened, is splashed under the power of 100-150W
Penetrate 1.5-2 hours.In one example, deposition step may include：(1) by Si substrates and Zn1-xCrxO (0 ＜ x≤0.05, preferably
For the ceramic target of x=0.01~0.05) is put into equipment for producing thin film；(2) chamber base vacuum is evacuated to≤5.0 × 10-4Pa,
Then by Si silicons to 300 DEG C, then chamber base vacuum is evacuated to≤5.0 × 10-4Pa.(3) by being passed through 20sccm's
The high-purity Ar gas of flow, adjust cavity pressure in 1.0Pa, open radio-frequency power supply, accumulate 2h in the power dip of 150W.
(4) room temperature is naturally cooling to after the completion of preparing, the film sample for preparing is taken out.
Zn is irradiated using the Ar of doses1-xCrxO (x=0.01~0.05) films are improving film cationic room
The concentration of defect.During irradiation, Ar particle irradiations dosage can be 7 × 1014~5 × 1016cm-2.Should if Ar particle irradiations dosage is less than
Scope, then will not produce enough cation vacancies in the film, and enhancing regulating effect ferromagnetic to film is not obvious；If
Ar particle irradiations dosage is more than the scope, then the cation vacancy of high concentration can agglomerate into larger sized room cluster, and
Destroy the micro-structural of film.
Ar particle irradiations energy can be 2~3MeV, preferably 2.8MeV.If Ar particle irradiations energy is less than the scope,
Ar particles can be remained in the film；If Ar particle irradiations energy is more than the scope, the Ar particles of high-energy can destroy film
Micro-structural.Due to H+Ion irradiation ZnO can compensate hydrogen ion defect in gap therein, and the irradiation effect of Ar particles is compensated without other
Effect, it is better.
In addition, the present invention is not particularly limited to the environment temperature of radiative process, for example, can carry out at room temperature.
In one example, (1) is put into the chamber of film preparation after Si substrates are cleaned up；(2) by chamber background
Vacuum is evacuated to≤5.0 × 10-4Pa, then by Si silicons to 300 DEG C；(3) it is passed through high-purity Ar gas, and by the pressure of growth chamber
1.0Pa is maintained at by force, (4) prepare film in the power dip product 2h of 150W；(7) at room temperature, with energy as 2.8MeV, dosage
It is 7 × 1014~5 × 1016cm-2Ar particles radiation modification is carried out to film.
And, in the present invention, Ar particle irradiations do not produce destruction to zno-based diluted semi-conductor thin-film, i.e., will not change thin
The composition and thing phase of film, it is little on roughness of film and internal phase structure influence.The irradiated dosage of Fig. 1 be 7 ×
1014Zn before and after cm-2 proton irradiations0.99Cr0.01The XRD spectrum of O film samples, it can be seen that removing Si (100) substrate
Diffraction maximum outside, only observe ZnO (100) and (002) diffraction maximum, and (002) diffraction maximum intensity be much larger than (100) diffraction maximum
Intensity, shows there is no other things mutually to exist in film, and the characteristics of good c-axis preferred orientation is presented grows, and footpath spoke
Phase structure according to rear film and to change.Fig. 4 is that irradiated dosage is 5 × 1016cm-2After Ar particle irradiations
Zn0.95Cr0.05The XRD spectrum of O film samples.It can be seen that in addition to the diffraction maximum of Si (100) substrate, only observing
ZnO (100) and (002) diffraction maximum, and the intensity of (002) diffraction maximum is much larger than (100) diffraction peak intensity, shows do not have in film
Other things are mutually present, and the characteristics of good c-axis preferred orientation is presented grows, and footpath irradiation rear film phase structure simultaneously
To change.Fig. 7 is that irradiated dosage is 5 × 1015cm-2Zn before and after Ar particle irradiations0.95Cr0.05The XRD of O film samples
Spectrum, it can be seen that in addition to the diffraction maximum of Si (100) substrate, ZnO (100) and (002) diffraction maximum are only observed, and
(002) intensity of diffraction maximum is much larger than (100) diffraction peak intensity, shows there is no other things mutually to exist in film, and be presented good
The characteristics of good c-axis preferred orientation grows, and footpath irradiates the phase structure of rear film and to change.Fig. 2 is
Zn0.99Cr0.01The irradiated dosage of O film samples is 7 × 1014cm-2AFM photos before and after Ar particle irradiations, can be with from AFM results
Find out that the surface roughness change of irradiation rear film is little.Fig. 5 is Zn0.95Cr0.05The irradiated dosage of O film samples be 5 ×
1016cm-2AFM photos before and after Ar particle irradiations, can be seen that the surface roughness change of irradiation rear film is little from AFM results.Figure
8 is Zn0.95Cr0.05The irradiated dosage of O film samples is 5 × 1015cm-2AFM photos before and after Ar particle irradiations, can from figure
Know, can be seen that the surface roughness change of irradiation rear film is little from AFM results.
Fig. 3 is Zn0.99Cr0.01The irradiated dosage of O film samples is 7 × 1014cm-2Room temperature magnetic before and after Ar particle irradiations
Hysteresis curves, it can be seen that the ferromagnetism of Ar particle irradiation rear films is remarkably reinforced, compared to its saturation magnetization of predose by
0.146emu/cm3Improve 71% to 0.249emu/cm3。
Fig. 6 is Zn0.95Cr0.05The irradiated dosage of O film samples is 5 × 1016cm-2Room temperature magnetic before and after Ar particle irradiations
Hysteresis curves, it can be seen that the ferromagnetism of Ar particle irradiation rear films is remarkably reinforced, compared to its saturation magnetization of predose by
0.365emu/cm3Improve 75% to 0.64emu/cm3；
Fig. 9 is Zn0.95Cr0.05The irradiated dosage of O film samples is 5 × 1015cm-2Room temperature magnetic hysteresis before and after Ar particle irradiations is returned
Line, it can be seen that the ferromagnetism of Ar particle irradiation rear films is remarkably reinforced, compared to its saturation magnetization of predose by
0.322emu/cm3Improve 67% to 0.538emu/cm3。
Embodiment is enumerated further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this
Invention is further described, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright the above is made belong to protection scope of the present invention.Following examples are specific
Technological parameter etc. is also only that an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in the concrete numerical value of hereafter example.
If following examples are without specified otherwise, the Cr is ZnO thin film doped with Zn0.99Cr0.01O films and Zn0.95Cr0.05O
As a example by as a example by.
Embodiment 1
(1) Si substrates are put into and are cleaned by ultrasonic 15min in acetone, then use deionized water rinsing 10min；2) Si substrates are put into
It is cleaned by ultrasonic 15min in alcohol, then with rinsing 10min in deionized water；(3) by Si substrate high-purity Ns2Drying；(4) by Si
Substrate, Zn0.99Cr0.01O targets are put into chamber；(5) chamber base vacuum is evacuated to≤5.0 × 10-4Pa, with the stream of 20sccm
Amount is passed through high-purity Ar, and the air pressure of chamber is maintained 1.0Pa, and Sapphire Substrate then is heated into 300 DEG C；(6) finally open
Radio-frequency power supply is opened, 2.0h is sputtered under the power of 150W, obtain Zn0.99Cr0.01O films, thickness is 450nm；(7) at room temperature,
With energy as 2.8MeV, dosage is 7 × 1014cm-2Ar particle fluxes radiation modification is carried out to film；(8) Magnetic Test result table
Bright, the room temperature saturation magnetization after film irradiation is by 0.146emu/cm3Improve 71% to 0.249emu/cm3。
Embodiment 2
(1) Si substrates are put into and are cleaned by ultrasonic 15min in acetone, then use deionized water rinsing 10min；2) Si substrates are put into
It is cleaned by ultrasonic 15min in alcohol, then with rinsing 10min in deionized water；(3) by Si substrate high-purity Ns2Drying；(4) by Si
Substrate, Zn0.95Cr0.05O targets are put into chamber；(5) chamber base vacuum is evacuated to≤5.0 × 10-4Pa, with the stream of 20sccm
Amount is passed through high-purity Ar, and the air pressure of chamber is maintained 1.0Pa, and Sapphire Substrate then is heated into 300 DEG C；(6) finally open
Radio-frequency power supply is opened, 2.0h is sputtered under the power of 150W, obtain Zn0.95Cr0.05O films, thickness is 450nm；(7) at room temperature,
With energy as 2.8MeV, dosage is 5 × 1016cm-2Ar particle fluxes radiation modification is carried out to film；(8) Magnetic Test result table
Bright, the room temperature saturation magnetization after film irradiation is by 0.365emu/cm3Improve 75% to 0.64emu/cm3。
Embodiment 3
(1) Si substrates are put into and are cleaned by ultrasonic 15min in acetone, then use deionized water rinsing 10min；2) Si substrates are put into
It is cleaned by ultrasonic 15min in alcohol, then with rinsing 10min in deionized water；(3) by Si substrate high-purity Ns2Drying；(4) by Si
Substrate, Zn0.95Cr0.05O targets are put into chamber；(5) chamber base vacuum is evacuated to≤5.0 × 10-4Pa, with the stream of 20sccm
Amount is passed through high-purity Ar, and the air pressure of chamber is maintained 1.0Pa, and Sapphire Substrate then is heated into 300 DEG C；(6) finally open
Radio-frequency power supply is opened, 2.0h is sputtered under the power of 100W, obtain Zn0.95Cr0.05O films, thickness be 350nm (7) at room temperature,
With energy as 2.8MeV, dosage is 5 × 1015cm-2Ar particle fluxes radiation modification is carried out to film；(8) Magnetic Test result table
Bright, the room temperature saturation magnetization after film irradiation is by 0.322emu/cm3Improve 67% to 0.538emu/cm3。
The inventive method stabilization is effective, can be on the premise of material is not destroyed to the ZnO thin film doped room-temperature ferromagnetics of Cr
Notable, effective enhancing is carried out, this is conducive to being lifted for spin electric device performance practical with future.
Claims (10)
1. a kind of Ar particle irradiations strengthen the ZnO thin film doped ferromagnetic methods of Cr, it is characterised in that with Ar of doses
Son is ZnO thin film doped to Cr to be irradiated, and the Cr ZnO thin film doped chemical formula is Zn1-xCrxO, wherein 0 ＜ x≤
0.05。
2. method according to claim 1, it is characterised in that 0.01≤x≤0.05.
3. method according to claim 1 and 2, it is characterised in that the irradiation dose of the Ar particles is 7 × 1014~5 ×
1016 cm-2。
4. according to the method in any one of claims 1 to 3, it is characterised in that the irradiation energy of the Ar particles is 2.5
~3.0MeV, irradiation process is carried out at room temperature.
5. method according to any one of claim 1 to 4, it is characterised in that the irradiation is in Cr is ZnO thin film doped
Cation vacancy is generated, the concentration of cation vacancy is regulated and controled by adjusting Ar particle irradiations dosage and/or irradiation energy.
6. method according to any one of claim 1 to 5, it is characterised in that thin through the Cr doping ZnO after the irradiation
The saturation magnetization of film improves more than 65% relative to predose.
7. method according to any one of claim 1 to 6, it is characterised in that the irradiation does not change the film
Composition and phase.
8. method according to any one of claim 1 to 7, it is characterised in that the Cr ZnO thin film doped preparation side
Method is at least one in physical vaporous deposition, chemical vapour deposition technique, sol-gel process and electrochemical method, preferably
Flux ties up inductively coupled plasma enhancing physical vaporous deposition.
9. method according to claim 8, it is characterised in that the Cr ZnO thin film doped preparation method includes：
（1）Dry substrate, Zn will be cleaned1-xCrxO targets are put into chamber；
（2）Chamber base vacuum is evacuated to≤5.0 × 10-4Pa, is passed through high-purity Ar, adjusts the pressure of cavity in 1.0~1.5 Pa,
Then by silicon to 300~350 DEG C；
（3）Radio-frequency power supply is finally opened, is sputtered 1.5~2 hours under the power of 100~150 W.
10. method according to claim 9, it is characterised in that the material of the substrate is silicon chip, sapphire, carborundum
With at least one in quartz glass.
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Cited By (3)
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| CN108273511A (en) * | 2018-02-05 | 2018-07-13 | 西南石油大学 | A kind of novel photocatalyst and preparation method thereof for the azo dyes that adsorbs and degrade |
| CN110462769A (en) * | 2018-02-22 | 2019-11-15 | 株式会社爱发科 | The forming method of magnetic film and the manufacturing method of magnetic memory element |
| CN113421821A (en) * | 2021-06-21 | 2021-09-21 | 广东省科学院半导体研究所 | Perovskite oxide thin film with determined magnetism and preparation method thereof with adjustable magnetism |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110462769A (en) * | 2018-02-22 | 2019-11-15 | 株式会社爱发科 | The forming method of magnetic film and the manufacturing method of magnetic memory element |
| CN113421821A (en) * | 2021-06-21 | 2021-09-21 | 广东省科学院半导体研究所 | Perovskite oxide thin film with determined magnetism and preparation method thereof with adjustable magnetism |
| CN113421821B (en) * | 2021-06-21 | 2022-09-30 | 广东省科学院半导体研究所 | Perovskite oxide thin film with determined magnetism and preparation method thereof with adjustable magnetism |
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