CN104451546A - Preparation method of doped ferrite material with giant plane Hall effect - Google Patents
Preparation method of doped ferrite material with giant plane Hall effect Download PDFInfo
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- 230000005355 Hall effect Effects 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 title claims description 12
- 229910000859 α-Fe Inorganic materials 0.000 title claims description 11
- 230000005291 magnetic effect Effects 0.000 claims abstract description 55
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000007747 plating Methods 0.000 claims abstract description 5
- 239000000758 substrate Substances 0.000 claims description 38
- 238000004544 sputter deposition Methods 0.000 claims description 31
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 239000007789 gas Substances 0.000 claims description 27
- 229910052786 argon Inorganic materials 0.000 claims description 17
- 229910052760 oxygen Inorganic materials 0.000 claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 13
- 238000005259 measurement Methods 0.000 claims description 13
- 239000001301 oxygen Substances 0.000 claims description 13
- 230000008859 change Effects 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 claims description 5
- 239000011575 calcium Substances 0.000 claims description 5
- 239000008186 active pharmaceutical agent Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 230000006641 stabilisation Effects 0.000 claims description 3
- 238000011105 stabilization Methods 0.000 claims description 3
- 238000003466 welding Methods 0.000 claims description 3
- 238000005546 reactive sputtering Methods 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 6
- 238000001755 magnetron sputter deposition Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000011161 development Methods 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 230000001276 controlling effect Effects 0.000 abstract 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 45
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 34
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 14
- 150000002500 ions Chemical class 0.000 description 12
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- 230000002463 transducing effect Effects 0.000 description 5
- 239000002019 doping agent Substances 0.000 description 4
- 238000001451 molecular beam epitaxy Methods 0.000 description 4
- 238000004549 pulsed laser deposition Methods 0.000 description 4
- -1 oxonium ions Chemical class 0.000 description 3
- 229920000314 poly p-methyl styrene Polymers 0.000 description 3
- 206010063401 primary progressive multiple sclerosis Diseases 0.000 description 3
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- Physical Vapour Deposition (AREA)
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Abstract
The invention relates to a preparation method of an epitaxial doped ferroferric oxide film through facing targets reactive sputtering, in which a DPS-III-type ultrahigh vacuum facing targets magnetron sputtering film-plating machine produced by Shenyang Scientific Instrument Development Center Co., Ltd. in Chinese Academy of Sciences is adopted. By a facing targets DC reactive magnetron sputtering technology, the Cr doping concentration can be regulated and controlled by placing different numbers of Cr sheets onto targets; the giant plane Hall effect is obtained by a vertical four-terminal mask method; the highest plane Hall resistivity can reach 105 microomega cm. The preparation method of the epitaxial CrxFe3-xO4 film has the advantages of compatibility with the existing industrial production, easiness for controlling the doping concentration, simple target selection, relatively high target utilization rate and the like; the giant plane Hall effect obtained from the CrxFe3-xO4 film optimizes a magnetic sensor and promotes the development of the magnetic sensor.
Description
Technical field
Patent of the present invention relates to the technology that a kind of preparation of ferrite doped calcium and huge planar Hall effect are applied in magnetic transducing device, more specifically, is a kind of a kind of method being obtained huge planar Hall effect by doping in ferrite.
Background technology
Huge planar Hall effect is early than within 2003, to find in dilute magnetic semiconductor (Ga, Mn) As epitaxial film device, but the scope of application is only at its below Curie temperature 50K (H.X.Tang, et al, Phys.Rev.B, 2003,90,107201).2004 Nian You research groups are at La
0.84sr
0.16mnO
3in found huge planar Hall effect, but it can observe that the scope of huge planar Hall effect is also only at below 140K (Y.Bason, et al, Appl.Phys.Lett., 2004,84,2593), the scope of application of the two is very little and all can not at room temperature use.Within 2008, Japanology group is at Fe
3o
4in the planar Hall effect that records can reach 10 at low temperatures
4the magnitude (A.Fern á ndez-Pacheco, et al, Phys.Rev.B, 2008,78,212402) of μ Ω cm, its planar Hall resistivity is similar to the shape of tunnel magneto resistance TMR with the change curve of externally-applied magnetic field.But the magnitude improving planar Hall resistivity can improve the sensitivity of magneticsensor effectively, thus magnetic transducing device is optimized, therefore obtains the focus that the material with huge planar Hall effect becomes people's concern.Huge planar Hall effect can not only be used for the upset of magneticanisotropy and the specific magnetising moment in test surface, can also be used in low magnetic transducing device after the match.Due to Fe
3o
4there is very high Curie temperature 858K, huge planar Hall effect can be obtained in larger temperature range by doping, have the possibility of alternative TMR in future, therefore ferrite doped calcium is a good candidate material, and more wide prospect has been opened up in the application for magneticsensor.
Fe
3o
4have a cube inverse spinel structure in room temperature and standard atmosphere pressure, lattice parameter is
56 ions are had in a unit cell.Wherein there are 32 oxonium ions, 8 Fe
3+(3d
5, S=5/2) and form tetrahedron with three oxonium ions of surrounding vicinity, be called A position.8 remaining Fe
2+(3d
6, S=2) and 8 Fe
3+(3d
5, S=5/2) and form octahedron with six contiguous oxonium ions, be called as B position.Ion on the secondary lattice of A and B position is all ferromegnetism arrangement, and the magnetic moment of A position and B interdigit then passes through O
2-superexchange form antiferromagnetic arrangement, formed ferrimagnetism.For ferrite doping, generally speaking, what ionic radius was larger tends to occupy B position, and less tends to occupy A position; And the larger high valence ion of positive charge tends to occupy B position, the low price ion that positive charge is less tends to occupy A position.If A position by magnetic moment lower than Fe
3+positively charged ion replace, or B position by magnetic moment higher than Fe
3+and Fe
2+positively charged ion replace, or space, B position is filled by magnetic ion, all can improve ferritic saturation magnetic moment, and to carry out ferritic modification, the effect of modification is relevant to the doping of substitutional ion.At present, consider the impact of doping on ferrite each side factor, find suitable doped element and go to improve ferritic performance, making it be applied to spintronics devices better becomes the focus that people pay close attention to.
The present invention can obtain larger huge planar Hall effect and the wider material of range of application based on finding, on the known basis with the Ferrite Material of maximum huge planar Hall effect, by mixing Cr element, to obtaining larger huge planar Hall effect.After mixing Cr element, Cr
3+ion tends to occupy B position and substitutes Fe
3+ion.Due to Cr
3+ionic radius
be slightly less than Fe
3+ionic radius
therefore along with the increase of Cr doping, the lattice parameter of spinel structure reduces gradually.Fe is prepared in this room
3o
4on the basis of epitaxial film technology maturation, regulated and controled the concentration of mixed Cr element by the Cr sheet putting into different quantities on Fe target, the advantage of preparation is: the Cr that can be obtained different levels of doping by increase and decrease Cr sheet quantity easily
xfe
3-xo
4, meet the Cr sheet quantity put in sputter procedure all the time more, the Cr prepared
xfe
3-xo
4the Cr concentration of sample is higher.And compare with preparation methods such as pulsed laser depositions with molecular beam epitaxy, magnetron sputtering method is more conducive to the demand meeting industrial thin film production in enormous quantities.
Summary of the invention
From the angle of suitability for industrialized production, need to use sputtering method and utilize simple as far as possible target to prepare epi dopant Fe
3o
4film.Namely the present invention from above two objects, develops facing targets reactive sputtering legal system for extension Cr
xfe
3-xo
4the method of film.
The equipment of facing targets reactive sputtering epi dopant ferriferrous oxide film of the present invention is the DPS-III type ultrahigh vacuum(HHV) subtend targets magnetic sputtering film plating machine adopting scientific instrument development center, Chinese Academy of Sciences Shenyang to produce.Facing targets reactive sputtering extension Cr
xfe
3-xo
4film process is studied and develops as follows:
One: extension Cr
xfe
3-xo
4the preparation of film
In order to prepare high-quality extension Cr
xfe
3-xo
4film, needs during experiment to consider following critical experiment condition:
(1) sputtering power, sputtering power is the speed of film forming in essence, and the size of sputtering power can affect the quality of film, and the sputtering power that therefore selection one is suitable is very important for the high-quality epitaxial film of preparation;
(2) sputtering pressure, sputtering pressure is actually the total amount determining the reactant gases passed in vacuum chamber, we only represent the gas volume that flows through of per minute under mark condition by the flow of gas meter setting reactant gases, therefore the setting of gas meter adds that both settings of sputtering pressure combine the total amount that just can determine to pass into vacuum chamber reaction gases, to guarantee that film has higher epitaxial quality;
(3) base reservoir temperature, experiment shows to prepare the good epitaxial ferroelectric ferrite thin film of crystalline quality, and the scope of experiment condition is very harsh and narrow, requires very high to required base reservoir temperature;
(4) ratio of reactant gases, during experiment, we need in vacuum chamber, pass into argon gas and oxygen two kinds of gases, and wherein the Main Function of argon gas is bombardment target, the atomic group on target is splashed in substrate and deposits film forming; And the effect of oxygen is mainly reacted with the Fe atomic group sputtered out from Fe target and from the Cr atomic group that Cr sheet sputters out, suitable oxygen partial pressure is selected to be form pure phase Cr
xfe
3-xo
4the key of compound.
Concrete technical scheme is as follows:
Have a preparation method for the ferrite doped calcium material of huge planar Hall effect, concrete operation step is as follows:
1) on the subtend target head of coating equipment, install the Fe target that a pair purity is 99.99%, the N pole as magnetic line of force, other end is S pole; The thickness of target is 3 ~ 5mm, and diameter is 60mm;
2) be covered with four-end method by above the MgO of base material polishing, substrate be arranged on the midperpendicular of subtend target line, the vertical range of two Fe target lines of substrate and subtend target is 4 ~ 6cm;
3) open subtend target magnetic control sputtering equipment, first take out one-level vacuum with mechanical pump, restart molecular pump and take out secondary vacuum, until the back end vacuum tightness of sputtering chamber is better than 8 × 10
– 6pa;
4) open gas meter and carry out preheating, regulate heating current to start, to substrate heating, until temperature rises to 450 ~ 500 DEG C, pass into argon gas and open shielding power supply, being cleaned up by the impurity on target surface, closing shielding power supply simultaneously;
5) pass into vacuum chamber sputter gas argon gas and the oxygen that purity is 99.999%, first pass into oxygen, after pass into argon gas, wherein argon stream amount is 100sccm, oxygen flow is 0.6 ~ 0.8sccm, and the vacuum tightness of sputtering chamber is remained on 0.5 ~ 0.8Pa, and stable;
6) open shielding power supply, a pair Fe target applies the electric current of 0.05 ~ 0.08A and the volts DS of 1150 ~ 1350V, pre-sputtering 15 ~ 20 minutes, electric current to be sputtered and voltage stabilization;
7) plate washer opened between Fe target side and substrate starts sputtering, and substrate position is fixed; In sputter procedure, base reservoir temperature continues to keep;
8) after sputtering terminates, close the plate washer between Fe target side and substrate, then close shielding power supply, stop passing into sputter gas Ar and O
2, continue to vacuumize, and regulate substrate temperature control power supply, make sample be reduced to room temperature with the speed of 1 ~ 3 DEG C/min, then close vacuum system, be filled with to vacuum chamber the nitrogen that purity is 99.999%, open vacuum chamber, take out sample.
Coating equipment adopts DPS-III type ultrahigh vacuum(HHV) subtend targets magnetic sputtering film plating machine.
The measuring method of the huge planar Hall effect that the present invention adopts, step is as follows:
1) will the conductive copper wire of 2 ~ 3cm be welded in the sample table of multifunctional sample bar by four of sample electrodes, be wherein connected with current channel by two of horizontal direction electrodes, two vertical electrodes be connected with voltage channel;
2) measure before, the sample table welding sample is arranged on the multifunctional sample bar of rotation, with Cr
xfe
3-xo
4the direction of film parallel applies magnetic field, the angle of magnetic field and electric current is realized by multifunctional rotary specimen holder, while rotary sample, the sense of current is also changing, and the angle being equivalent to magnetic field and electric current constantly changes, and the direction in magnetic field remains unchanged;
3), when measuring, two electrodes connecting electric current have electric current to pass through, and the resistance that the direction vertical with electric current records is planar Hall resistance.
As wanted measurement plane Hall resistance with the change in magnetic field, keep the position of sample to fix, the size changing magnetic field is measured.
As wanted measurement plane Hall resistance with the change of magnetic field and electric current angle, setting program makes multifunctional sample bar rotate, and changes the angle of sample.
Extension Cr involved in the present invention
xfe
3-xo
4method for manufacturing thin film has selects simple and target rate of utilization comparatively advantages of higher with existing suitability for industrialized production compatibility, target, and magnetic information storage with the preparation of reading isospin electronics related device are with a wide range of applications.
For confirming the embodiment of the best of the present invention, we have carried out X-ray diffraction to the film of Cr doping content series in the present invention, and adopt PPMS to carry out detailed analysis to the electrical property of film.
Extension Cr is prepared with other
xfe
3-xo
4the method of film and the method for acquisition planar Hall resistance are compared, facing targets reactive sputtering extension Cr involved in the present invention
xfe
3-xo
4the preparation method of film mainly has following advantage:
1, the epitaxial film preparation means that magnetron sputtering and laboratory are conventional is as pulsed laser deposition (Pulsed Laser Deposition, and molecular beam epitaxy (Molecular Beam epitaxy PLD), MBE) compare, magnetron sputtering method can not only prepare the single crystal epitaxial film of high crystalline quality, observes prepared extension Cr under a scanning electron microscope
xfe
3-xo
4film, there is no particle or non-uniform phenomenon, film surface is very smooth, also take advantage in speed and efficiency simultaneously, compared with the above-mentioned means being only applicable to make a search in laboratory, it is consuming time short that magnetically controlled sputter method prepares film, is more applicable for the demand of industrial mass production, and preparation doped samples is more convenient;
2, the acquisition of huge planar Hall effect, use four-end method mask to overlay in substrate, once form four end electrodes in sputter procedure, preparation method's simple and fast, is applicable to industrialized mass.Apply the magnetic field parallel with film surface during measurement, the direction vertical with electric current can obtain planar Hall resistance.The method of this use vertical four-end method mask acquisition electrode effectively ensures the direction exact vertical of the sense of current and measurement plane Hall resistance, eliminates the interference of other factors to planar Hall resistance.
The preparation method of facing targets reactive sputtering epi dopant ferriferrous oxide film involved in the present invention, have and to prepare with existing suitability for industrialized production compatibility, doping content easy-regulating, " four-end method " mask that electrode method is convenient, target selects simple and target rate of utilization comparatively advantages of higher, the acquisition of huge planar Hall effect makes magnetic transducing device obtain optimization, promote the development of magnetic transducing device, this this materials application with huge planar Hall effect has been with a wide range of applications in the preparation of spintronics related device.
Accompanying drawing explanation
Fig. 1 (a) for base reservoir temperature in the present invention be in MgO (100) substrate, prepare extension Cr under 500 DEG C of conditions
xfe
3-xo
4the X-ray diffractogram of film.
Fig. 1 (b) is Cr
xfe
3-xo
4lattice parameter with the change of x.
Fig. 1 (c) is the X-ray of x=0, x=0.54, x=0.87 tri-samples
scintigram.
Fig. 2 (a) for base reservoir temperature of the present invention be in MgO (100) substrate, prepare extension Cr under 500 DEG C of conditions
xfe
3-xo
4the x-ray photoelectron power spectrum of film.
Fig. 2 (b) for base reservoir temperature of the present invention be in MgO (100) substrate, prepare extension Cr under 500 DEG C of conditions
xfe
3-xo
4the x-ray photoelectron power spectrum of film.
Fig. 3 (a) for base reservoir temperature of the present invention be in MgO (100) substrate, prepare extension Cr under 500 DEG C of conditions
0.97fe
0.03o
4the planar Hall resistivity of film is with the variation relation of magnetic field and electric current angle.
Fig. 3 (b) is sample Cr
0.97fe
0.03o
4planar Hall resistivity with the variation relation in magnetic field.
Fig. 4 (a) for base reservoir temperature of the present invention be in MgO (100) substrate, prepare extension Cr under 500 DEG C of conditions
0.64fe
0.54o
4film planar Hall resistivity is at different temperatures with the variation relation of magnetic field and electric current angle.
Fig. 4 (b) is for differing temps lower plane Hall resistance rate is with the variation relation of Cr doping.
Fig. 5 (a) for base reservoir temperature of the present invention be in MgO (100) substrate, prepare extension Cr under 500 DEG C of conditions
xfe
3-xo
4the difference DELTA ρ of longitudinal resistivity under the differing temps of film
xx jump=ρ
//-ρ
⊥with the variation relation of Cr doping content.
Fig. 5 (b) for base reservoir temperature of the present invention be in MgO (100) substrate, prepare extension Cr under 500 DEG C of conditions
xfe
3-xo
4ρ under the differing temps of film
xywith Δ ρ
xx jumpratio is with the variation relation of Cr doping content.
Embodiment
According to the structures and characteristics analysis that we carry out sample prepared in the present invention, illustrating below is described in detail the preparation method of facing targets reactive sputtering epi dopant ferriferrous oxide film:
1, the DPS-III type ultrahigh vacuum(HHV) subtend targets magnetic sputtering film plating machine adopting scientific instrument development center, Chinese Academy of Sciences Shenyang to produce, the target head of subtend is installed the Fe target that a pair purity is 99.99%, each one of two target heads, a N pole as magnetic line of force, other end is S pole, then the Cr sheet putting different quantities on the surface of lower target mixes the concentration of Cr with regulation and control.The thickness of target is 3mm, and diameter is 60mm;
2, after surface impurity being removed by modes such as ultrasonic wave by the MgO of base material polishing, four-end method mask is covered with at substrate, to obtain four electrodes required for measurement plane Hall resistance rate in sputter procedure, substrate be arranged on the midperpendicular of subtend target line, the vertical range of two Fe target lines of substrate and subtend target is 4 ~ 6cm again;
3, open DPS-III subtend target magnetic control sputtering equipment, first start mechanical pump and take out one-level vacuum, being extracted into vacuum tightness is below 20Pa, meets the working conditions of molecular pump, restarts molecular pump and takes out secondary vacuum, until the back end vacuum tightness of sputtering chamber is better than 8 × 10
– 6pa;
4, open gas meter and carry out preheating (20 ~ 30 minutes), open substrate heating power supply simultaneously, regulate heating current, make base reservoir temperature rise to 450 ~ 500 DEG C, after 20 ~ 30 minutes, pass into the pure argon of 100sccm, adjustable pressure, at about 1 ~ 3Pa, opens shielding power supply, applies the electric current of 0.05 ~ 0.08A and the volts DS of 1150 ~ 1350V on Fe target, the impurity on cleaning target surface and zone of oxidation, closed shielding power supply after 5 ~ 7 minutes;
5, after the 4th EOS, sputter gas argon gas and the oxygen that purity is 99.999% is passed into again to vacuum chamber, wherein argon stream amount is 100sccm, oxygen flow is 0.6 ~ 0.8sccm, first pass into the oxygen that flow is less, hinder entering of oxygen with the argon gas avoiding flow large alluvial at mixing chamber.The vacuum tightness of sputtering chamber is remained on 0.5 ~ 0.8Pa, and stablizes 3 ~ 5 minutes;
6, open shielding power supply, a pair Fe target applies the electric current of 0.05 ~ 0.08A and the volts DS of 1150 ~ 1350V, and pre-sputtering 15 ~ 20 minutes, waits sputtering current and voltage stabilization;
7, the plate washer opened between Fe target side and substrate starts sputtering, and substrate position is fixed.In sputter procedure, base reservoir temperature continues to keep;
8, after sputtering terminates, close the plate washer between Fe target side and substrate, then close shielding power supply, stop passing into sputter gas Ar and O
2, continue to vacuumize, and regulate substrate temperature control power supply, make sample be reduced to room temperature with the speed of 1 ~ 3 DEG C/min, then close vacuum system, be filled with to vacuum chamber the nitrogen that purity is 99.999%, open vacuum chamber, take out sample.
Two: the acquisition of huge planar Hall effect
We use a kind of measuring system that can realize different measuring object of U.S. Quantum Design company designs: PPMS (Physical Property Measurement System, PPMS) measurement plane Hall resistance rate.
1, copper wire sand papering is ground off completely to zone of oxidation, guarantee that copper wire conducts electricity with volt ohm-milliammeter measurement, then copper wire is cut into every section of 2-3cm is long to be used as being welded in sample table by sample.
2, be welded in the sample table of multifunctional sample bar by the copper wire electric iron on four of sample electrodes, be wherein connected with current channel by two of horizontal direction electrodes, two vertical electrodes are connected with voltage channel.
3, measure before, the sample table welding sample is arranged on rotatable multifunctional sample bar, with Cr
xfe
3-xo
4the direction of film parallel applies magnetic field, the variable angle of magnetic field and electric current is realized by multifunctional rotary specimen holder, while rotary sample, the sense of current is also changing, and the angle being equivalent to magnetic field and electric current constantly changes, and the direction in magnetic field remains unchanged.
When 4, measuring, two electrodes connecting electric current have electric current to be passed through, and the resistance that the direction vertical with electric current records is planar Hall resistance.To the change of measurement plane Hall resistance with magnetic field, then keep the position of sample to fix, the size changing magnetic field is measured; To the change of measurement plane Hall resistance with magnetic field and electric current angle, setting program makes multifunctional sample bar rotate, and changes the angle of sample.
Fig. 1 (a) for base reservoir temperature in the present invention be in MgO (100) substrate, prepare extension Cr under 500 DEG C of conditions
xfe
3-xo
4the X-ray diffractogram of film; As can be seen from the figure, still only there is the peak of ferritic (00l) orientation, illustrated and do not change ferritic crystalline structure after mixing Cr element.
Fig. 1 (b) is Cr
xfe
3-xo
4lattice parameter with the change of x.As can be seen from the figure, after mixing Cr, lattice parameter reduces is due to Cr
3+ionic radius
be slightly less than Fe
3+ionic radius
Fig. 1 (c) is the X-ray of x=0, x=0.54, x=0.87 tri-samples
scintigram; From X-ray
can find out in scintigram that four diffraction peaks are uniform 90 ° of intervals, the quadruple reflecting isometric system is symmetrical, demonstrates Cr
xfe
3-xo
4epitaxial relationship in the face of film.
Fig. 2 (a) for base reservoir temperature of the present invention be in MgO (100) substrate, prepare extension Cr under 500 DEG C of conditions
xfe
3-xo
4the x-ray photoelectron power spectrum of film, the x-ray photoelectron power spectrum of Fe and Determination of Different Valence States.Reflect in figure that Fe ion main manifestations is Fe
2+and Fe
3+.
Fig. 2 (b) for base reservoir temperature of the present invention be in MgO (100) substrate, prepare extension Cr under 500 DEG C of conditions
xfe
3-xo
4the x-ray photoelectron power spectrum of film, the x-ray photoelectron power spectrum of Cr and Determination of Different Valence States.Reflect in figure that Cr ion main manifestations is Cr
2+and Cr
3+.
Fig. 3 (a) for base reservoir temperature of the present invention be in MgO (100) substrate, prepare extension Cr under 500 DEG C of conditions
0.97fe
0.03o
4the planar Hall resistivity of film is with the variation relation of magnetic field and electric current angle; As can be seen from the figure planar Hall resistivity increases along with the increase of externally-applied magnetic field.
Fig. 3 (b) is sample Cr
0.97fe
0.03o
4planar Hall resistivity with the variation relation in magnetic field.As can be seen from the figure, when magnetic field and electric current angle be 45 ° and 135 ° time planar Hall resistivity symbol just the opposite.
Fig. 4 (a) for base reservoir temperature of the present invention be in MgO (100) substrate, prepare extension Cr under 500 DEG C of conditions
0.64fe
0.54o
4film planar Hall resistivity at different temperatures, with the variation relation of magnetic field and electric current angle, can find out that planar Hall resistivity reduces along with the rising of temperature.
Fig. 4 (b) is for differing temps lower plane Hall resistance rate is with the variation relation of Cr doping.As can be seen from the figure maximum planar Hall resistivity is about 10
5μ Ω cm, appears at the Cr of 150K
0.29fe
0.71o
4in sample.
Fig. 5 (a) for base reservoir temperature of the present invention be in MgO (100) substrate, prepare extension Cr under 500 DEG C of conditions
xfe
3-xo
4the difference DELTA ρ of longitudinal resistivity under the differing temps of film
xx jump=ρ
//-ρ
⊥with the variation relation of Cr doping content.The transformation of symbol occurs in x=0.54, has reacted the symbol of AMR ratio along with the increase of Cr content is by just becoming negative.
Fig. 5 (b) for base reservoir temperature of the present invention be in MgO (100) substrate, prepare extension Cr under 500 DEG C of conditions
xfe
3-xo
4ρ under the differing temps of film
xywith Δ ρ
xx jumpratio is with the variation relation of Cr doping content.Its ratio increases along with the increase of Cr doping; Can find out that the ratio of planar Hall resistivity and longitudinal resistivity is very little, demonstrate planar Hall effect this fact identical with the source of anisotropic magnetoresistance, also demonstrate the accuracy of planar Hall resistivity measurement simultaneously.
Claims (5)
1. there is a preparation method for the ferrite doped calcium material of huge planar Hall effect, it is characterized in that operation steps is as follows:
1) on the subtend target head of coating equipment, install the Fe target that a pair purity is 99.99%, the N pole as magnetic line of force, other end is S pole; The thickness of target is 3 ~ 5mm, and diameter is 60mm;
2) be covered with four-end method by above the MgO of base material polishing, substrate be arranged on the midperpendicular of subtend target line, the vertical range of two Fe target lines of substrate and subtend target is 4 ~ 6cm;
3) open subtend target magnetic control sputtering equipment, first take out one-level vacuum with mechanical pump, restart molecular pump and take out secondary vacuum, until the back end vacuum tightness of sputtering chamber is better than 8 × 10
– 6pa;
4) open gas meter and carry out preheating, regulate heating current to start, to substrate heating, until temperature rises to 450 ~ 500 DEG C, pass into argon gas and open shielding power supply, being cleaned up by the impurity on target surface, closing shielding power supply simultaneously;
5) pass into vacuum chamber sputter gas argon gas and the oxygen that purity is 99.999%, first pass into oxygen, after pass into argon gas, wherein argon stream amount is 100sccm, oxygen flow is 0.6 ~ 0.8sccm, and the vacuum tightness of sputtering chamber is remained on 0.5 ~ 0.8Pa, and stable;
6) open shielding power supply, a pair Fe target applies the electric current of 0.05 ~ 0.08A and the volts DS of 1150 ~ 1350V, pre-sputtering 15 ~ 20 minutes, electric current to be sputtered and voltage stabilization;
7) plate washer opened between Fe target side and substrate starts sputtering, and substrate position is fixed; In sputter procedure, base reservoir temperature continues to keep;
8) after sputtering terminates, close the plate washer between Fe target side and substrate, then close shielding power supply, stop passing into sputter gas Ar and O
2, continue to vacuumize, and regulate substrate temperature control power supply, make sample be reduced to room temperature with the speed of 1 ~ 3 DEG C/min, then close vacuum system, be filled with to vacuum chamber the nitrogen that purity is 99.999%, open vacuum chamber, take out sample.
2. the method for claim 1, is characterized in that coating equipment adopts DPS-III type ultrahigh vacuum(HHV) subtend targets magnetic sputtering film plating machine.
3. a measuring method for huge planar Hall effect, is characterized in that step is as follows:
1) will the conductive copper wire of 2 ~ 3cm be welded in the sample table of multifunctional sample bar by four of sample electrodes, be wherein connected with current channel by two of horizontal direction electrodes, two vertical electrodes be connected with voltage channel;
2) measure before, the sample table welding sample is arranged on the multifunctional sample bar of rotation, with Cr
xfe
3-xo
4the direction of film parallel applies magnetic field, the angle of magnetic field and electric current is realized by multifunctional rotary specimen holder, while rotary sample, the sense of current is also changing, and the angle being equivalent to magnetic field and electric current constantly changes, and the direction in magnetic field remains unchanged;
3), when measuring, two electrodes connecting electric current have electric current to pass through, and the resistance that the direction vertical with electric current records is planar Hall resistance.
4. method as claimed in claim 3, is characterized in that the change of measurement plane Hall resistance with magnetic field, and keep the position of sample to fix, the size changing magnetic field is measured.
5. method as claimed in claim 3, it is characterized in that the change of measurement plane Hall resistance with magnetic field and electric current angle, setting program makes multifunctional sample bar rotate, the angle of change sample.
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| CN114775061A (en) * | 2022-04-19 | 2022-07-22 | 天津大学 | Preparation method of opposite-target magnetron sputtering epitaxial iron-tin alloy film |
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