CN106498359A - Magnetic control co-sputtering prepares the method that Haas strangles alloy firm that magnetize in face - Google Patents
Magnetic control co-sputtering prepares the method that Haas strangles alloy firm that magnetize in face Download PDFInfo
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- CN106498359A CN106498359A CN201611147545.0A CN201611147545A CN106498359A CN 106498359 A CN106498359 A CN 106498359A CN 201611147545 A CN201611147545 A CN 201611147545A CN 106498359 A CN106498359 A CN 106498359A
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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
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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Abstract
Magnetic control co-sputtering is prepared in face and magnetizes the method that Haas strangles alloy firm, is carried out according to the following steps：（1）Using SiO2The sample stage in magnetron sputtering vacuum chamber is sent into as backing material after ultrasonic wave cleaning treatment；（2）Required target is put on the target position of magnetron sputtering vacuum chamber；（3）Vacuumize；（4）Haas is prepared in substrate material surface by magnetron sputtering and strangles alloy firm, or first Cr films are made in substrate material surface, then prepare Haas in substrate material surface strangle alloy firm.The present invention adopts magnetic control co-sputtering method, and parallel to magnetic anisotropy, its roughness and coercivity are changed significantly the high purity films of preparation, and preparation time is short, and purity is high, and equipment is simple, easily operates, low cost.
Description
Technical field
The invention belongs to field of magnetic material, is more particularly to used for a kind of magnetic control of magnetic memory device and various kinds of sensors
Cosputtering prepares the method that Haas strangles alloy firm that magnetize in face.
Background technology
In traditional microelectronics, traditional electronics device, typically using the charge characteristic of electronics, is not consider
The spin states of electronics.But with developing rapidly for computer science, the requirement of the volume of computer chip is constantly
Reduce, and the requirement of memory capacity also expands constantly, based on electronics charge characteristic conventional electronics oneself can not meet
Scientific development and the requirement of the mankind.Under promotion of the science with demand, the spin properties of electronics are closed by scientist and researchers
Note and be used come the speed and storage density for further improving information processing.In this context, new
One spintronics of section is born.Spin electric device is utilized due to the spin properties to electronics, is greatly increased
The performance of electronic device, this kind of device have the high-quality that non-volatile, data processing speed is fast, energy consumption is low and integrated level is high
Characteristic.Although spin electric device has so many high-performance, on actual materials demand, there is higher requirement,
It requires that material has high spinning polarizability, i.e., be respectively provided with the downward electron number that spins up and spin near fermi level
Mesh is uneven, and more uneven more have.
Heusler（Haas is strangled）Alloy is a kind of intermetallic compound with body-centered cubic structure of high-sequential, one
As be divided into two kinds of alloys of Full-Heusler and Half-Heusler, chemical general formula is respectively X2YZ and XYZ, wherein X
Different transiting group metal elements are represented with Y, Z represents sp（III, the IV, V main group）Element.
At present the result of study of Heusler alloys shows, the band structure of the complexity that Heusler alloys have be by
The transition element for having the d electron orbits of local has the major element of the sp electron orbits of non-local to combine again.With
When, and the Occupation due to Heusler alloys is closely related with its physical characteristic, makes the alloy of same sample ingredient through different
Preparation method and heat treatment process influence whether the degree of order of crystal structure and atom, and then regulate and control its electronic structure, magnetic
Property, phase transformation etc..These factors cause Heusler alloys to produce many New function materials, such as ferromagnetic shape memory alloy with
Elastic material, giant magnetic resistor material, superconductor, magnetic field driven martensitic transformation material, semi-metallic, thermoelectric material with
And many New function materials such as topological insulator.Just because of containing so many performance in Heusler alloys so as to
Have huge using value and prospect in the exploitation of new material, and become one of key areas for exploring new function material；
Simultaneously because the high ordered structure of Heusler alloys, can study its electronic structure with the calculating of first principle system for us
Provide and greatly facilitate.
Content of the invention
The present invention is the above-mentioned weak point for strangling alloy preparation method in order to solve above-mentioned Haas, there is provided a kind of magnetic control splashes altogether
The method that magnetization Haas strangles alloy firm in the preparation face of penetrating, using Co targets, three target co-sputtering of Mn targets and Al targets, by adjusting three targets
Sputtering power adjust the thickness and composition of growing film well, so as to control the superconductivity of film, in being in
The ferrimagnet of temperature and absolutely spin polarizability so as to should as ferromagnetic layer in Spin Valve and magnetic tunnel-junction
Used time, the magneto-resistance effect of device is improved, the magnetic storage density of superelevation is realized,
One of method of the present invention is comprised the following steps：
1st, SiO is adopted2As backing material, by backing material after ultrasonic wave cleaning treatment, by pass specimen holder transmit into
On sample stage in magnetron sputtering vacuum chamber；
2nd, required target is put on the target position of magnetron sputtering vacuum chamber；Described target material respectively purity >=
99.999% metal material X、Y and Z；Described metal material X is Cu, Ni or Co；Described metal material Y be Fe, Cr or
Mn, described metal material Z are Al, Si, Ge or B；
3rd, vacuum≤2 × 10 of magnetron sputtering chamber are evacuated to-5Pa；
4th, Haas is prepared in substrate material surface by magnetic control co-sputtering and strangles alloy firm, working gas is purity >=99.999%
High-purity argon gas, 0.01 ~ 0.4Pa of sputtering pressure, sedimentation rate is 5 ~ 10nm/min, the distance of target to backing material for 20 ~
30cm, sputtering time set 5 ~ 10 min, make Haas in substrate material surface and strangle alloy firm.
The two of the method for the present invention comprise the following steps：
1st, SiO is adopted2As backing material, by backing material after ultrasonic wave cleaning treatment, by pass specimen holder transmit into
On sample stage in magnetron sputtering vacuum chamber；
2nd, required target is put on the target position of magnetron sputtering vacuum chamber；Described target material respectively purity >=
99.999% metal material Cr, X, Y and Z；Described metal material X is Cu, Ni or Co；Described metal material Y is Fe, Cr
Or Mn, described metal material Z are Al, Si, Ge or B；
3rd, vacuum≤2 × 10 of magnetron sputtering chamber are evacuated to-5Pa；
4th, Haas is prepared in substrate material surface by magnetron sputtering and strangles alloy firm, working gas is purity >=99.999%
High-purity argon gas, 0.01 ~ 0.4Pa of sputtering pressure, sedimentation rate is 5 ~ 10nm/min, the distance of target to backing material for 20 ~
30cm, 1 ~ 2 min of sputtering time, makes Cr films in substrate material surface；
5th, Haas is prepared in substrate material surface by magnetic control co-sputtering and strangles alloy firm, working gas is purity >=99.999%
High-purity argon gas, 0.01 ~ 0.4Pa of sputtering pressure, sedimentation rate is 5 ~ 10nm/min, the distance of target to backing material for 20 ~
30cm, 5 ~ 10 min of sputtering time, make Haas in substrate material surface and strangle alloy firm.
The step of above-mentioned ultrasonic wave cleaning treatment is：Backing material is respectively placed in order successively acetone, ethanol and
In deionized water, and cleaned with ultrasonic wave, be cleaned by ultrasonic the time in every kind of liquid for 15 ~ 20min, then dried up with nitrogen,
8 ~ 10min is heat-treated under the conditions of 200 ± 10 DEG C, substrate material surface removing residues are made.
In above two method, it is X that Haas strangles the composition of alloy firm2YZ, thickness are 48 ~ 56nm.
In the two of above-mentioned method, the thickness of Cr films is 9 ~ 12nm.
Above-mentioned SiO2Purity >=99.9%.
Beneficial effects of the present invention are：Using magnetic control co-sputtering method, high-purity argon gas in preparation process, are passed through, effect is Ar
Bombardment target, parallel to magnetic anisotropy, its roughness and coercivity are changed significantly the high purity films of preparation, during preparation
Between short, purity is high, and equipment is simple, easily operates, low cost.
Description of the drawings
Fig. 1 is the structural representation that Haas prepared by the embodiment of the present invention 1 strangles alloy firm；
Fig. 2 is the X-ray polycrystalline diffraction pattern that Haas prepared by the embodiment of the present invention 1 strangles alloy firm；
Fig. 3 is the structural representation that Haas prepared by the embodiment of the present invention 2 strangles alloy firm；
Fig. 4 is the X-ray polycrystalline diffraction pattern that Haas prepared by the embodiment of the present invention 2 strangles alloy firm；
Fig. 5 is different substrate temperature and to whether there is the magnetization curve figure of Cr films in the embodiment of the present invention；
Fig. 6 is different substrate temperature and to whether there is the surface roughness curve figure of Cr films in the embodiment of the present invention.
Specific embodiment
The metal material of purity >=99.999% adopted in the embodiment of the present invention（Cr, X, Y and Z）For commercial products.
The X-ray polycrystalline diffraction device model ULTIMA IV adopted in the embodiment of the present invention（Japan）.
In the embodiment of the present invention, the test equipment that adopts of magnetization curve is for vibrating specimen magnetometer, model Lake Shore
7410 VSM.
In the embodiment of the present invention, test surfaces roughness adopts AFM, model FM-Nanoview 6600.
The SiO of backing material purity >=99.9% adopted in the embodiment of the present invention2For commercial products.
When carrying out magnetron sputtering in the embodiment of the present invention, the flow 30SCCM of high-purity argon gas, sample stage rotational velocity is
40rpm, 20 ~ 40W of sputtering power.
The backing material specification adopted in the embodiment of the present invention is for 1cm × 1cm.
In the embodiment of the present invention the step of ultrasonic wave cleaning treatment it is：Backing material is respectively placed in third in order successively
In ketone, ethanol and deionized water, and cleaned with ultrasonic wave, be cleaned by ultrasonic the time in every kind of liquid for 15 ~ 20min, Ran Houyong
Nitrogen is dried up, and is heat-treated 8 ~ 10min, makes substrate material surface removing residues under the conditions of 200 ± 10 DEG C.
Embodiment 1
Using SiO2As backing material, by backing material after ultrasonic wave cleaning treatment, transmitted into magnetic by passing specimen holder
On sample stage in control sputtering vacuum chamber；
Required target is put on the target position of magnetron sputtering vacuum chamber；Described target material respectively purity >=
99.999% metal material X、Y and Z；Described metal material X is Co；Described metal material Y be Mn, described metal material
Material Z is Al；
It is evacuated to vacuum≤2 × 10 of magnetron sputtering chamber-5Pa；
Haas is prepared in substrate material surface by magnetic control co-sputtering and strangles alloy firm, working gas is purity >=99.999%
High-purity argon gas, sputtering pressure 0.01Pa, sedimentation rate is 5nm/min, and the distance of target to backing material is 20cm, sputtering time
10 min being set, Haas being made in substrate material surface and is strangled alloy firm, composition is Co2MnAl, thickness are 50nm, and structure is as schemed
Shown in 1, X-ray polycrystalline diffraction patterns are as shown in Fig. 2 magnetization curve is as shown in figure 5, surface roughness curve is as shown in Figure 6.
Embodiment 2
Using SiO2As backing material, by backing material after ultrasonic wave cleaning treatment, transmitted into magnetic by passing specimen holder
On sample stage in control sputtering vacuum chamber；
Required target is put on the target position of magnetron sputtering vacuum chamber；Described target material respectively purity >=
99.999% metal material Cr, X, Y and Z；Described metal material X is Co；Described metal material Y be Mn, described metal
Material Z is Al；
It is evacuated to vacuum≤2 × 10 of magnetron sputtering chamber-5Pa；
Haas is prepared in substrate material surface by magnetron sputtering and strangles alloy firm, height of the working gas for purity >=99.999%
Pure argon, sputtering pressure 0.01Pa, sedimentation rate is 5nm/min, and the distance of target to backing material is 20cm, sputtering time 2
Min, makes Cr films in substrate material surface, and thickness is 10nm；
Haas is prepared in substrate material surface by magnetic control co-sputtering and strangles alloy firm, working gas is purity >=99.999%
High-purity argon gas, sputtering pressure 0.01Pa, sedimentation rate is 5nm/min, and the distance of target to backing material is 20cm, sputtering time
10 min, make Haas in substrate material surface and strangle alloy firm, and composition is Co2MnAl, thickness is 50nm, structure such as Fig. 3 institutes
Show, X-ray polycrystalline diffraction patterns are as shown in figure 4, magnetization curve is as shown in figure 5, surface roughness curve is as shown in Figure 6.
Embodiment 3
With embodiment 1, difference is method：
（1）Metal material X is Ni；Described metal material Y is Cr, and described metal material Z is Si；
（2）Sputtering pressure 0.1Pa, sedimentation rate is 6nm/min, and the distance of target to backing material is 24cm, and sputtering time sets
Fixed 8 min, make Haas in substrate material surface and strangle alloy firm, and composition is Ni2CrSi, thickness are 48nm.
Embodiment 4
With embodiment 1, difference is method：
（1）Metal material X is Cu；Described metal material Y is Fe, and described metal material Z is Ge；
（2）Sputtering pressure 0.2Pa, sedimentation rate is 8nm/min, and the distance of target to backing material is 28cm, and sputtering time sets
Determining 7min, Haas being made in substrate material surface and strangle alloy firm, composition is Cu2FeGe, thickness are 56nm.
Embodiment 5
With embodiment 2, difference is method：
（1）Metal material X is Ni；Described metal material Y is Cr, and described metal material Z is Si；
（2）Sputtering pressure 0.1Pa, sedimentation rate is 6nm/min, and the distance of target to backing material is 24cm, sputtering time 1.5
Min, makes Cr films in substrate material surface, and thickness is 9nm；
（3）Sputtering pressure 0.1Pa, sedimentation rate is 6nm/min, and the distance of target to backing material is 24cm, sputtering time
8min, makes Haas in substrate material surface and strangles alloy firm, and composition is Ni2CrSi, thickness are 48nm.
Embodiment 6
With embodiment 2, difference is method：
（1）Metal material X is Cu；Described metal material Y is Fe, and described metal material Z is Ge；
（2）Sputtering pressure 0.2Pa, sedimentation rate is 8nm/min, and the distance of target to backing material is 28cm, sputtering time 1.5
Min, makes Cr films in substrate material surface, and thickness is 12nm；
（3）Sputtering pressure 0.2Pa, sedimentation rate is 8nm/min, and the distance of target to backing material is 28cm, sputtering time 7
Min, makes Haas in substrate material surface and strangles alloy firm, and composition is Cu2FeGe, thickness are 56nm.
Embodiment 7
With embodiment 1, difference is method：
（1）Metal material X is Cu；Described metal material Y is Mn, and described metal material Z is B；
（2）Sputtering pressure 0.4Pa, sedimentation rate is 10nm/min, and the distance of target to backing material is 30cm, and sputtering time sets
Fixed 5 min, make Haas in substrate material surface and strangle alloy firm, and composition is Cu2MnB, thickness are 50nm.
Embodiment 8
With embodiment 2, difference is method：
（1）Metal material X is Cu；Described metal material Y is Fe, and described metal material Z is B；
（2）Sputtering pressure 0.4Pa, sedimentation rate is 10nm/min, and the distance of target to backing material is 30cm, sputtering time 1
Min, makes Cr films in substrate material surface, and thickness is 10nm；
（3）Sputtering pressure 0.4Pa, sedimentation rate is 10nm/min, and the distance of target to backing material is 30cm, sputtering time
5min, makes Haas in substrate material surface and strangles alloy firm, and composition is Cu2FeB, thickness are 50nm.
Claims (5)
1. a kind of magnetic control co-sputtering prepares the method that Haas strangles alloy firm that magnetize in face, it is characterised in that enter according to the following steps
OK：
（1）Using SiO2As backing material, by backing material after ultrasonic wave cleaning treatment, by pass specimen holder transmit into
On sample stage in magnetron sputtering vacuum chamber；
（2）Required target is put on the target position of magnetron sputtering vacuum chamber；Described target material respectively purity >=
99.999% metal material X、Y and Z；Described metal material X is Cu, Ni or Co；Described metal material Y be Fe, Cr or
Mn, described metal material Z are Al, Si, Ge or B；
（3）It is evacuated to vacuum≤2 × 10 of magnetron sputtering chamber-5Pa；
（4）Haas is prepared in substrate material surface by magnetic control co-sputtering and strangles alloy firm, working gas is purity >=99.999%
High-purity argon gas, 0.01 ~ 0.4Pa of sputtering pressure, sedimentation rate is 5 ~ 10nm/min, the distance of target to backing material for 20 ~
30cm, sputtering time set 5 ~ 10 min, make Haas in substrate material surface and strangle alloy firm.
2. a kind of magnetic control co-sputtering prepares the method that Haas strangles alloy firm that magnetize in face, it is characterised in that enter according to the following steps
OK：
（1）Using SiO2As backing material, by backing material after ultrasonic wave cleaning treatment, by pass specimen holder transmit into
On sample stage in magnetron sputtering vacuum chamber；
（2）Required target is put on the target position of magnetron sputtering vacuum chamber；Described target material respectively purity >=
99.999% metal material Cr, X, Y and Z；Described metal material X is Cu, Ni or Co；Described metal material Y is Fe, Cr
Or Mn, described metal material Z are Al, Si, Ge or B；
（3）It is evacuated to vacuum≤2 × 10 of magnetron sputtering chamber-5Pa；
（4）Haas is prepared in substrate material surface by magnetron sputtering and strangles alloy firm, working gas is purity >=99.999%
High-purity argon gas, 0.01 ~ 0.4Pa of sputtering pressure, sedimentation rate is 5 ~ 10nm/min, the distance of target to backing material for 20 ~
30cm, 1 ~ 2 min of sputtering time, makes Cr films in substrate material surface；
（5）Haas is prepared in substrate material surface by magnetic control co-sputtering and strangles alloy firm, working gas is purity >=99.999%
High-purity argon gas, 0.01 ~ 0.4Pa of sputtering pressure, sedimentation rate is 5 ~ 10nm/min, the distance of target to backing material for 20 ~
30cm, 5 ~ 10 min of sputtering time, make Haas in substrate material surface and strangle alloy firm.
3. magnetic control co-sputtering according to claim 1 and 2 is prepared
It is that the step of described ultrasonic cleaning is processed is：Backing material is respectively placed in acetone, ethanol and deionization in order successively
In water, and cleaned with ultrasonic wave, it is 15 ~ 20min to be cleaned by ultrasonic the time in every kind of liquid, is then dried up with nitrogen, 200 ±
8 ~ 10min is heat-treated under the conditions of 10 DEG C, substrate material surface removing residues are made.
4. magnetic control co-sputtering according to claim 1 and 2 is prepared
It is X to be that described Haas strangles the composition of alloy firm2YZ, thickness are 48 ~ 56nm.
5. magnetic control co-sputtering according to claim 2 prepares the method that Haas strangles alloy firm that magnetize in face, and its feature exists
In described Cr films thickness be 9 ~ 12nm.
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Cited By (5)
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| CN108411272A (en) * | 2018-05-30 | 2018-08-17 | 上海电机学院 | A kind of preparation method of bearing AlCrCuFeNi systems high-entropy alloy coating |
| CN109913816A (en) * | 2019-04-29 | 2019-06-21 | 天津城建大学 | Temperature gradient magneto-caloric material and preparation method thereof |
| CN110484802A (en) * | 2019-08-30 | 2019-11-22 | 广州大学 | A kind of ferromagnetic shape memory alloy with nanometer Eutectic structure |
| CN111549317A (en) * | 2020-05-13 | 2020-08-18 | 中国科学院空天信息创新研究院 | Cobalt-based Heusler alloy structure and preparation method for improving ordering of cobalt-based Heusler alloy structure |
| CN112962075A (en) * | 2021-02-04 | 2021-06-15 | 西南交通大学 | Method for preparing second-generation high-temperature superconducting tape by three-target co-sputtering |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108411272A (en) * | 2018-05-30 | 2018-08-17 | 上海电机学院 | A kind of preparation method of bearing AlCrCuFeNi systems high-entropy alloy coating |
| CN109913816A (en) * | 2019-04-29 | 2019-06-21 | 天津城建大学 | Temperature gradient magneto-caloric material and preparation method thereof |
| CN109913816B (en) * | 2019-04-29 | 2021-03-02 | 天津城建大学 | Temperature gradient magnetocaloric material and preparation method thereof |
| CN110484802A (en) * | 2019-08-30 | 2019-11-22 | 广州大学 | A kind of ferromagnetic shape memory alloy with nanometer Eutectic structure |
| CN111549317A (en) * | 2020-05-13 | 2020-08-18 | 中国科学院空天信息创新研究院 | Cobalt-based Heusler alloy structure and preparation method for improving ordering of cobalt-based Heusler alloy structure |
| CN112962075A (en) * | 2021-02-04 | 2021-06-15 | 西南交通大学 | Method for preparing second-generation high-temperature superconducting tape by three-target co-sputtering |
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| Publication number | Publication date |
|---|---|
| CN106498359B (en) | 2019-06-25 |
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