CN108251805A - It is a kind of to realize hexagonal Mn with Ru buffer layers3The method of Ga film preparations - Google Patents
It is a kind of to realize hexagonal Mn with Ru buffer layers3The method of Ga film preparations Download PDFInfo
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- CN108251805A CN108251805A CN201711407729.0A CN201711407729A CN108251805A CN 108251805 A CN108251805 A CN 108251805A CN 201711407729 A CN201711407729 A CN 201711407729A CN 108251805 A CN108251805 A CN 108251805A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 25
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 9
- 238000000137 annealing Methods 0.000 claims abstract description 4
- 238000004544 sputter deposition Methods 0.000 claims description 49
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 238000010586 diagram Methods 0.000 description 8
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 230000005355 Hall effect Effects 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010606 normalization Methods 0.000 description 2
- 229910016797 Mn3Sn Inorganic materials 0.000 description 1
- 229910002370 SrTiO3 Inorganic materials 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004630 atomic force microscopy Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000032258 transport Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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Abstract
The present invention provides a kind of hexagonal Mn is realized with Ru buffer layers3The method of Ga film preparations, i.e., by rf magnetron sputtering, room temperature growth 5nm Ta, 30nm Ru and 200nm Mn successively on a si substrate3After Ga, then carry out 550 DEG C of annealings.The preparation process of the present invention is simple, using the Si substrates of relative low price and Ta/Ru buffer layers, [002] the type hexagonal Mn prepared3Ga keeps the topological Hall conductivity of 8n Ω cm in the large temperature range of 10~100K.
Description
Technical field
The invention belongs to hexagonal Mn3Ga field of film preparation, it is more particularly to a kind of to realize hexagonal Mn with Ru buffer layers3Ga is thin
The method of film preparation.
Background technology
Hexagonal Mn3Ga is due to its special magnetic property and transports performance, can be applied to spin-transfer torque and spin pump
It send.In the Mn of the non-colinear antiferromagnet of hexagonal3Sn and Mn3In Ge monocrystalline, due to the presence of Mn-kagome lattices, in reality
The extraordinary Hall effect (AHE) of super large is confirmed the existence of in testing, this causes Mn3Sn and Mn3Ge monocrystalline is set in antiferromagnet spinning electron
Standby above gather around has wide practical use.In recent years, people's prediction was in the Mn of the hexagonal of homologous series3Ga polycrystal, which has to be less than, to be faced
The topological Hall effect of boundary's temperature.Everybody is to alloy and film-form tetragonal phase Mn3Ga has carried out a large amount of research, but still lacks
To film-form hexagonal Mn3The correlative study of Ga.In addition, film-form can also enhance specific domain (such as Skyrmion) formation
Stability, and application of the film in spin electric device is indispensable, therefore studies hexagonal Mn3Ga films have very much
Necessity.People are by selecting SrTiO3It (001) and the special buffer layer such as Pt of MgO (001) Grown etc., can be with extension
Grow the Mn of hexagonal phase3Ga, but corresponding buffer layer is expensive, and manufacturing process is complicated, receives one in practical applications
Definite limitation.Therefore, study what is grown on ordinary buffer layer, the simple hexagonal Mn of preparation process3Ga films are still challenging.
Invention content
Technical problem：The defects of in order to solve the prior art, realizes hexagonal the present invention provides a kind of with Ru buffer layers
Mn3The method of Ga film preparations.
Technical solution：It is provided by the invention to realize hexagonal Mn with Ru buffer layers3The method of Ga film preparations, mainly by penetrating
Frequency magnetron sputtering, on a si substrate room temperature growth 5nm Ta, 30nm Ru and 200nm Mn successively3After Ga, then carry out 550 DEG C and move back
Fire processing.
Preferably：The concrete operation step of growth Ta is on a si substrate：By rf magnetron sputtering in Si
(001) room temperature growth 5nm Ta on substrate；Wherein background air pressure is 2.0 × 10-5Pa, sputtering pressure 1Pa, sputtering power are
80W, sputtering time 20s.
As further preferred scheme：The concrete operation step of growth Ru is on a si substrate：It will be raw on Si substrates
Continue room temperature growth 30nm Ru on the sample of long 5nm Ta；Wherein background air pressure is 2.0 × 10-5Pa, sputtering pressure 1Pa, splashes
Power is penetrated as 80W, sputtering time 7.5min.
As further preferred scheme：Mn is grown on a si substrate3The concrete operation step of Ga is：By on Si substrates
It grows and continues room temperature growth 200nm Mn3Ga on the sample of 30nm Ru；Wherein background air pressure is 2.0 × 10-5Pa, sputtering pressure
For 1Pa, sputtering power 80W, sputtering time 20min.
As further preferred scheme：It is described 550 DEG C annealing concrete operation step be：The sample for terminating to obtain will be grown
Product, which are placed under high vacuum environment, is warming up to 550 DEG C, and heating source is closed after keeping 20min, treat the sample be cooled to 50 DEG C hereinafter,
Take out sample.
As further preferred scheme：Above-mentioned Si substrates are [001] type Si substrates.
As further preferred scheme：Above-mentioned Mn3Ga is [002] type Mn3Ga。
Advantageous effect：The preparation process of the present invention is simple, using the Si substrates of relative low price and Ta/Ru buffer layers,
[002] the type hexagonal Mn prepared3Ga keeps the topological Hall conductivity of 8n Ω cm in the large temperature range of 10~100K.
Description of the drawings
Fig. 1 is sample difference film stack schematic diagram；
Fig. 2 is Mn3The atomic force microscopy surface shape appearance figure of Ga；
Fig. 3 is the XRD spectra after sample 1-4 normalization；
Fig. 4 is hysteresis loop figure outside the faces of sample 1-3 at various temperatures；
Fig. 5 is the saturation magnetization variation with temperature rule contrast schematic diagram of sample 1-3；
Fig. 6 is the magneto-resistor contrast schematic diagram of sample 1 and 2 at various temperatures；
Fig. 7 is sample 1-3 Hall resistance rate ρ at different temperaturesxyWith the changing rule schematic diagram in magnetic field；
Fig. 8 is the null field abnormality Hall resistance rate obtained after sample 1-3 is fitted(e) common Hall coefficient R0 is with temperature
Changing rule schematic diagram；
Fig. 9 is that unusual Hall resistance rate is subtracted gray line RoB+RsM obtains topological Hall resistance rateSchematic diagram；
Figure 10 is the topological Hall resistance rate of sample 1 at different temperaturesChange schematic diagram.
Specific embodiment
In the following with reference to the drawings and specific embodiments, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate
It the present invention rather than limits the scope of the invention, after the present invention has been read, those skilled in the art are to of the invention each
The modification of kind equivalent form falls within the application range as defined in the appended claims.
Embodiment 1
Step 1：By rf magnetron sputtering on Si [001] substrate room temperature growth 5nm Ta：Background air pressure 2.0 × 10- 5Pa, sputtering pressure 1Pa, sputtering power 80W, sputtering time 20s.
Step 2：Room temperature growth 30nm Ru on the sample obtained in above-mentioned steps 1：Background air pressure 2.0 × 10-5Pa, sputtering
Air pressure 1Pa, sputtering power 80W, sputtering time 7.5min.
Step 3：In the sample room temperature growth 200nm Mn that above-mentioned steps 2 obtain3Ga：Background air pressure 2.0 × 10-5Pa splashes
Pressure of emanating 1Pa, sputtering power 80W, sputtering time 20min.
Step 4：The sample that above-mentioned steps 3 are obtained is warming up to 550 DEG C under a high vacuum, is directly closed after keeping 20min
Heating source is cooled to less than 50 DEG C taking-up samples, obtains sample 1.
Comparative example 1
Step 1：By rf magnetron sputtering on Si [001] substrate room temperature growth 5nm Ta：Background air pressure 2.0 × 10- 5Pa, sputtering pressure 1Pa, sputtering power 80W, sputtering time 20s.
Step 2：Room temperature growth 200nm Mn on the sample obtained in above-mentioned steps 13Ga：Background air pressure 2.0 × 10-5Pa,
Sputtering pressure 1Pa, sputtering power 80W, sputtering time 20min.
Step 3：The sample that above-mentioned steps 2 are obtained is warming up to 550 DEG C under a high vacuum, is directly closed after keeping 20min
Heating source is cooled to less than 50 DEG C taking-up samples, obtains sample 2.
Comparative example 2
Step 1：By rf magnetron sputtering on Si [001] substrate room temperature growth 5nm Ta：Background air pressure 2.0 × 10- 5Pa, sputtering pressure 1Pa, sputtering power 80W, sputtering time 20s.
Step 2：Room temperature growth 10nm Ru on the sample obtained in above-mentioned steps 1：Background air pressure 2.0 × 10-5Pa, sputtering
Air pressure 1Pa, sputtering power 80W, sputtering time 7.5min.
Step 3：Room temperature growth 200nm Mn on the sample obtained in above-mentioned steps 23Ga：Background air pressure 2.0 × 10-5Pa,
Sputtering pressure 1Pa, sputtering power 80W, sputtering time 20min.
Step 4：The sample that above-mentioned steps 3 are obtained is warming up to 550 DEG C under a high vacuum, is directly closed after keeping 20min
Heating source is cooled to less than 50 DEG C taking-up samples and obtains sample 3.
Comparative example 3
Step 1：By rf magnetron sputtering on Si [001] substrate room temperature growth 5nm Ta：Background air pressure 2.0 × 10- 5Pa, sputtering pressure 1Pa, sputtering power 80W, sputtering time 20s.
Step 2：Room temperature growth 20nm Ru on the sample obtained in above-mentioned steps 1：Background air pressure 2.0 × 10-5Pa, sputtering
Air pressure 1Pa, sputtering power 80W, sputtering time 7.5min.
Step 3：Room temperature growth 200nm Mn on the sample obtained in above-mentioned steps 23Ga：Background air pressure 2.0 × 10-5Pa,
Sputtering pressure 1Pa, sputtering power 80W, sputtering time 20min.
Step 4：The sample that step 3 is obtained is warming up to 550 DEG C under a high vacuum, and heating is directly closed after keeping 20min
Source is cooled to less than 50 DEG C taking-up samples, obtains sample 4.
As shown in figure 3, the XRD spectra after the normalization of the sample with different buffer layer thicknesses, i.e. sample 1-4, culminant star
Number represent the Mn of tetragonal phase3Ga, dot represent the Mn of hexagonal phase3Ga, left side illustration are cubic D022Type Mn3Ga crystal structures are illustrated
Figure, the right illustration is hexagonal D019Type Mn3Ga crystal structure schematic diagrames.
As shown in figure 4, hysteresis loop figure outside the face of different buffer layer thickness samples at various temperatures；Wherein figure (a) is
Sample 2, i.e. Ta (5nm)/Ru (0nm) show tetragonal phase and hexagonal phase and deposit；(b) is wherein schemed for sample 3, i.e. Ta (5nm)/Ru
Content of tetragonal phase is reduced in (10nm), but is still two-phase coexistent state；(c) is wherein schemed for sample 1, i.e. Ta (5nm)/Ru
(30nm) is close to pure hexagonal phase.
Claims (7)
1. a kind of realize hexagonal Mn with Ru buffer layers3The method of Ga film preparations, it is characterised in that：By rf magnetron sputtering,
Room temperature growth 5nm Ta, 30nm Ru and 200nm Mn successively on Si substrates3After Ga, then carry out 550 DEG C of annealings.
2. a kind of Ru buffer layers realization hexagonal Mn according to claim 13The method of Ga film preparations, it is characterised in that：
The concrete operation step of growth Ta is on a si substrate：Pass through rf magnetron sputtering room temperature growth 5nm Ta on a si substrate；Its
Middle background air pressure is 2.0 × 10-5Pa, sputtering pressure 1Pa, sputtering power 80W, sputtering time 20s.
3. a kind of Ru buffer layers realization hexagonal Mn according to claim 13The method of Ga film preparations, it is characterised in that：
The concrete operation step of growth Ru is on a si substrate：The room temperature growth 30nm in the Si substrate samples for grown 5nm Ta
Ru；Wherein background air pressure is 2.0 × 10-5Pa, sputtering pressure 1Pa, sputtering power 80W, sputtering time 7.5min.
4. a kind of Ru buffer layers realization hexagonal Mn according to claim 13The method of Ga film preparations, it is characterised in that：
Mn is grown on a si substrate3The concrete operation step of Ga is：The room temperature growth in the Si substrate samples for grown 30nm Ru
200nm Mn3Ga；Wherein background air pressure is 2.0 × 10-5Pa, sputtering pressure 1Pa, sputtering power 80W, sputtering time are
20min。
5. a kind of Ru buffer layers realization hexagonal Mn according to claim 13The method of Ga film preparations, it is characterised in that：
It is described 550 DEG C annealing concrete operation step be：The sample that growth terminates to obtain is placed under high vacuum environment and is warming up to 550
DEG C, heating source is closed after keeping 20min, treats that the sample is cooled to 50 DEG C hereinafter, taking out sample.
It is 6. a kind of with Ru buffer layers realization hexagonal Mn according to claim 1-53The method of Ga film preparations, feature exist
In：The Si substrates are [001] type Si substrates.
It is 7. a kind of with Ru buffer layers realization hexagonal Mn according to claim 1-53The method of Ga film preparations, feature exist
In：The Mn3Ga is [002] type Mn3Ga。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109097737A (en) * | 2018-08-07 | 2018-12-28 | 泉州凯华新材料科技有限公司 | The preparation method of perpendicular magnetic anisotropic magnetic recording thin film |
| CN110735119A (en) * | 2019-10-12 | 2020-01-31 | 南京理工大学 | method for preparing huge coercive force Mn3Ga film by magnetron sputtering |
| JP2020065006A (en) * | 2018-10-18 | 2020-04-23 | 株式会社アルバック | Manufacturing method of magnetic storage element |
| WO2022077679A1 (en) * | 2020-10-15 | 2022-04-21 | 北京工业大学 | Preparation method for sr-doped manganese-gallium alloy and high coercivity nanocrystalline magnet thereof |
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| GB201020308D0 (en) * | 2010-12-01 | 2011-01-12 | Trinity College Dublin | Tetragonal manganese gallium films |
| CN102345105A (en) * | 2011-09-28 | 2012-02-08 | 东北石油大学 | Preparation method of high-residual internal stress Ni-Mn-Ga magnetically-driven memory alloy film |
| CN104947053A (en) * | 2015-07-27 | 2015-09-30 | 大连大学 | Preparation method of high-manganese alloy film Mn53Ni23Ga24 |
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2017
- 2017-12-22 CN CN201711407729.0A patent/CN108251805A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB201020308D0 (en) * | 2010-12-01 | 2011-01-12 | Trinity College Dublin | Tetragonal manganese gallium films |
| CN102345105A (en) * | 2011-09-28 | 2012-02-08 | 东北石油大学 | Preparation method of high-residual internal stress Ni-Mn-Ga magnetically-driven memory alloy film |
| CN104947053A (en) * | 2015-07-27 | 2015-09-30 | 大连大学 | Preparation method of high-manganese alloy film Mn53Ni23Ga24 |
Non-Patent Citations (2)
| Title |
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| KURT H等: "Exchange-biased magnetic tunnel junctions with antiferromagnetic Ɛ-Mn3Ga" * |
| R. M. GUTIERREZ-PEREZ等: "Giant magnetization on Mn3Ga ultra-thin films grown by magnetron sputtering on SiO2/Si(001)" * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109097737A (en) * | 2018-08-07 | 2018-12-28 | 泉州凯华新材料科技有限公司 | The preparation method of perpendicular magnetic anisotropic magnetic recording thin film |
| JP2020065006A (en) * | 2018-10-18 | 2020-04-23 | 株式会社アルバック | Manufacturing method of magnetic storage element |
| CN110735119A (en) * | 2019-10-12 | 2020-01-31 | 南京理工大学 | method for preparing huge coercive force Mn3Ga film by magnetron sputtering |
| CN110735119B (en) * | 2019-10-12 | 2021-08-03 | 南京理工大学 | Method for preparing huge coercive force Mn3Ga film through magnetron sputtering |
| WO2022077679A1 (en) * | 2020-10-15 | 2022-04-21 | 北京工业大学 | Preparation method for sr-doped manganese-gallium alloy and high coercivity nanocrystalline magnet thereof |
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Application publication date: 20180706 |