CN106119801A - A kind of Cr Al binary alloy material and preparation method thereof - Google Patents
A kind of Cr Al binary alloy material and preparation method thereof Download PDFInfo
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- CN106119801A CN106119801A CN201610832873.8A CN201610832873A CN106119801A CN 106119801 A CN106119801 A CN 106119801A CN 201610832873 A CN201610832873 A CN 201610832873A CN 106119801 A CN106119801 A CN 106119801A
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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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/06—Alloys based on chromium
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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
Abstract
The invention discloses a kind of Cr Al binary alloy material, described alloy material is the single-phase thin film of long-range order, and its chemical formula is: CryAl, wherein, 2.8≤y≤4.2；By improving deposited particles energy, carry out the technical thought of " forcing high orderly " metastable structure film preparation, utilize the method for magnetron sputtering enhanced deposition particle energy to prepare CryAl thin film, the most successfully synthesis has DO3The Cr of structure3Al alloy, and prepared a series of CryThe single-phase thin film of Al.
Description
Technical field
The present invention relates to a kind of binary alloy material, particularly to a kind of Cr-Al binary alloy material and preparation method thereof.
Background technology
Spintronics is an emerging cross discipline in physics, because it reads at magnetic resistance sensor, magnetic head
And the field such as information storage demonstrates that wide application prospect receives much concern.Be different from traditional electronics, it not merely with
The electric charge attribute of electronics also utilizes the spin attribute carrier as information of electronics simultaneously.Research at modern spintronics
In, the spin of electronics, as transmission and the carrier of the information of process, greatly improves the performance of electronic device, effectively reduces
The power consumption of device.Utilizing electron spin attribute is the central characteristics of future new era electronic device, and develops filming high-spin
Polarization material and technique thereof are then the key foundation problems of spintronics devices research.
Substantial amounts of semimetal (half-metal, spin polarizability reaches the material of 100%) and high spinning polarizability material
All find in Heusler alloy.And the generation of Half-metallic or high spinning polarizability characteristic all with Heusler alloy
In three kinds of metallic elements high-sequential arrangement closely related.High spin-polarization Heusler alloy research result is shown by people,
The anti-occupy-place defect of about 5% just can result in the forfeiture of material high spinning polarizability.And the Occupation situation in material
Substantial connection is had with the concrete preparation method of material.So, even the material that composition is identical, if we use different systems
Preparation Method or different Technologies for Heating Processing, also can obtain the diverse material of the degree of order, to its electronic structure, magnetic and defeated
Fortune character etc. has an immense impact on.Up to the present, most of high spinning polarizability materials are all the gold being made up of three kinds of elements
Compound between genus, and owing to constitution element kind is more, and the most often there is the metallic element composition that characteristic is similar, this just makes
Become alloy easily occurs anti-occupy-place defect and then reduced the congenital defect of polarizability.And in bianry alloy, due to element
Kind only has two kinds, and is made up of a kind of transition element and another main group metal, and element property difference is the biggest.
This most formerly determines the sky, and the probability that anti-occupy-place occurs in bianry alloy will be well below ternary Heusler alloy.But,
The element forming bianry alloy the most just only has two kinds, and up to the present, the high spinning polarizability material developed is the most little.
Wherein there is the Cr3Al alloy of DO3 structure, it is simply that the binary high spinning polarizability material few in number that people predict in theory
One of material.
Cr-Al alloy just had begun in 1963 be studied by Koster et al., and delineated Cr1-XAlX alloy phase
Figure, and propose orderly Cr1-xAlx (x=0.19-0.26) be exist because having shown nonlinear magnetization at x
Rate relation, but on XRD, do not provide enough evidences.In 1981, Den Broeder et al. was less than 400 DEG C
At a temperature of utilize transmission electron microscope observation to arrive extra point diffraction, be interpreted superlattices point, this ordered phase is claimed
For X phase.But according to the principle of dark-field imaging, this X phase is shortrange order rather than long-range order.By 2012,
Z.Boekelheide et al. utilizes electron beam evaporation to obtain the Cr3Al thin film with cubic structure, synthesizes during less than 400 DEG C
Thin film be X phase structure, be C11b structure during higher than 400 DEG C.
It is to say, up to the present, whether at Cr3Al bulk or low-dimensional materials, people the most successfully close
Become there is the Cr3Al alloy of DO3 structure.Although what Z.Boekelheide et al. utilized that electron beam deposition synthesizes is and DO3 structure
Close cubic structure, but its atomic ordered degree and and orderly fashion completely different with DO3 structure, material spin polarizability is also
Estimate that with theory the spin polarizability of DO3 structure C r3Al alloy greatly differs from each other, say, that material can not embody theory at all
Anticipated most important high spin-polarization feature.
Summary of the invention
In view of this, it is an object of the invention to provide a kind of Cr-Al binary alloy material and preparation method thereof, by carrying
High deposited particles energy, carries out the technical thought of " forcing high orderly " metastable structure film preparation, utilizes magnetron sputtering to strengthen
The method of deposited particles energy prepares CryAl thin film, the most successfully synthesis has DO3The Cr of structure3Al alloy, and prepare
A series of CryThe single-phase thin film of Al.
The Cr-Al binary alloy material of the present invention, described alloy material is the single-phase thin film of long-range order, its chemical formula
For: CryAl, wherein, 2.8≤y≤4.2；
Further, during y=2.90-3.05, CryAl alloy is the magnetic alloy material with high spinning polarizability.
Further, during y=3, CryAl is the DO with high spinning polarizability3Structure；
Further, described CryThe spin polarizability of Al is up to 85-100%；
Further, described CryAl synthesizes through magnetron sputtering.
Invention additionally discloses the preparation method of a kind of Cr-Al binary alloy material, utilize three target superhigh vacuum magnetron sputterings
Method, obtain Cr by regulation sputtering power, underlayer temperature and argon flow amountyThe single-phase thin film of Al alloy；
Further, described Cr target sputtering power scope be 10-90W, Al target sputtering power scope be 10-50W；
Further, described underlayer temperature is 100-400 DEG C, and argon flow amount is 30-70sccm；
Further, by adjusting the sputtering power of Cr target and Al target than acquisition CryThe different values of y in Al；
Further, by improving the energy of deposited particles, enable what Al atom was more uniformly distributed to be dispersed in cubic structure,
Force Cr3Al forms high orderly DO3Metastable state, final synthesis has DO3The Cr of structure3Al alloy.
Beneficial effects of the present invention: the present invention compared with other Cr-Al alloys:
(1) the most of high spinning polarizability materials having now been found that all concentrate on ternary Heusler alloy system, and,
Heusler alloy often has two kinds of close transition elements, easily causes anti-occupy-place defect and then reduce spin polarization
Rate.For this problem, the present invention have selected the bianry alloy Cr with high spin-polarization3Al is as synthetic material.Because it is high
The formerly generation advantageously reducing anti-occupy-place defect in the sky of spin polarization bianry alloy, maintains high spinning polarizability, therefore has DO3
The Cr of structure3Al is one of binary high spin-polarization material few in number of theoretical prediction.
(2) whether at Cr3Al bulk or low-dimensional materials, people the most successfully synthesize and have DO3Structure
Cr3Al alloy.Main cause is that Al atom skewness in cubic structure homogenizes, and DO3Structure is then that Al atom is the most uniform
A kind of embodiment changed.For this problem, the present invention proposes the energy by improving deposited particles, enables Al atom the most equal
Even is dispersed in cubic structure, forces " Cr3Al forms high orderly DO3Metastable state ", the most successfully synthesis has DO3Structure
Cr3Al alloy.
(3) Cr-Al alloy just had begun in 1963 be studied by Koster et al., but Cr1-xAlx(x=0.19-
0.26) it is shortrange order, longrange disorder.And the Cr of our synthesis1-xAlx(x=0.19-0.26) alloy shows synthesis from XRD
Thin film be single-phase.
(4) Cr of material of the present invention3Al alloy is the DO with high spinning polarizability3Structure, its spin polarizability can reach
98%.
(5) material C r of the present invention1-xAlx(x=0.19-0.26) it is the single-phase thin film with long-range order.
(6) as long as controlling power ratio well, Cr in suitable power bracket1-xAlx(x=0.19-0.26) it is all that there is length
The single-phase thin film of Cheng Youxu.
Accompanying drawing explanation
The present invention is further described with embodiment below in conjunction with the accompanying drawings.
Fig. 1 is the Cr that embodiment 1 obtains3The XRD curve of Al alloy firm.
Fig. 2 is the Cr that embodiment 3 obtains2.95The XRD curve of Al alloy firm.
Fig. 3 is the Cr that embodiment 6 obtains2.0The XRD curve of Al alloy firm.
Fig. 4 is the Cr that embodiment 8 obtains3.79The XRD curve of Al alloy firm.
Fig. 5 is the Cr that embodiment 11 obtains4.2The XRD curve of Al alloy firm.
Detailed description of the invention
Embodiment one
Be there is than preparation the DO of high spin-polarization by regulation power3The Cr of structure3Al material.
Three target superhigh vacuum magnetron sputtering devices are used to prepare Cr3Al alloy, in order to obtain Cr3The ratio of Al, by regulation
Power ratio realizes, and concrete technology is as follows:
The first step, processes substrate
Choose 2.24 × 1.5mm2Glass substrate, ultrasonic in acetone, ethanol, deionized water successively, then use argon
Dry up.Substrate is placed on electronic scale and weighs its quality, and write down registration number m0.Again substrate is fixed on substrate bracket, places
In cavity.Cr target and Al target it is respectively mounted on two direct current targets.
Second step, evacuation
(1) opening cooling water switch, the outlet temperature of cooling water is stable in the range of 25 ± 10 DEG C.
(2) A cabinet master control power supply is opened.
(3) opening mechanical pump, open side and take out angle valve, open vacuometer power supply, the pressure being evacuated in cavity with mechanical pump is 5.0Pa
Close side during left and right and take out angle valve, and open electromagnetic valve, open a sluice gate plate valve.When the pressure in cavity reaches 3.0 × 10-3Pa to chamber
Body toasts, in order to reach more preferably to reach preferable vacuum faster.Turn off baking after 30 minutes, continue to take out to cavity
Vacuum, until chamber pressure reaches 5.0 × 10-3About Pa.
3rd step, silicon
Rotary heating current knob, pointer points to 0.7A, makes silicon to 100 DEG C.
4th step, logical argon
When underlayer temperature reaches 100 DEG C, close fine vacuum display meter, then open V3And V8.Drive argon bottle main valve, lock
Plate valve, toward drop by half, prevents more argon to be pumped.Opening gas flowmeter power supply, regulation argon flow amount is 30-70sccm.
Low-voltage vacuum display meter registration is made to be 5.0Pa by regulator plate valve.
5th step, d.c. sputtering
(1) B cabinet master control power supply is opened.
(2) opening corresponding target position DC sputtering power in B cabinet, regulation power makes argon ionization starter above target.Again
Make low-voltage vacuum display meter registration be 0.5Pa by regulator plate valve, be operating pressure.
(3) rotary power adjusting knob, makes Cr target sputtering power reach 60.45W, Al target sputtering power and reaches 38.24W,
After plate pressure and plate current are stable, opening rotation of substrate button, flap shutter, start sputtering timing, sputtering time is 30 minutes.
(4) after sputtering, flap shutter is kept in the center, and stops substrate and rotates, is transferred to counterclockwise by power regulating knob
Minimum, presses stop button.
(5) B cabinet master control power supply is closed.
6th step, closes argon
(1) V is closed3And V8, close argon bottle main valve, then MFC1 got to closedown, after effusion meter is shown as 0, closes stream
Gauge power supply.Drive big damper valve, allow molecular pump that vacuum chamber is evacuated to fine vacuum.
7th step, shutdown
(1) treat that vacuum chamber is extracted into fine vacuum (10-5Pa), close slide valve.
(2) vacuum display meter is closed.
(3) pressing molecular pump stop button, molecular pump slows down, and when frequency is shown as 0, closes electromagnetic valve.By mechanical pump
Button, stops mechanical pump.
(4) A cabinet master control power supply is closed
(5) recirculated water is closed.
8th step, thin film weighs
(1) open vent valve, make vacuum chamber and outside pressure equal after, close vent valve.
(2) open recirculated water and A cabinet master control power supply, press a liter button, rise button, rise vacuum room cover to the highest
Degree.
(3) take off sample carrier, turn on screw with screwdriver, take out sample.
(4) sample of taking-up being placed on electronic scale weighing, obtaining quality is m1, therefore the quality that can obtain thin film is m=
m1-m0。
The material using said method to obtain is Cr3Al thin film, its structure is DO3Structure, and there is the high-spin of 97%
Polarizability, the range finding recorded is 3 μB。
Embodiment two
Be there is than preparation the Cr of high spin-polarization by regulation power2.90Al material.
Difference from Example 1 is: Cr target sputtering power is that 58.51W, Al target sputtering power reaches 38.24W, other
Technique is with embodiment 1.
The method is used to obtain Cr2.90Al alloy firm, measures its spin polarizability and saturation magnetization is respectively
85% and 5.0 μB。
Embodiment three
Be there is than preparation the Cr of high spin-polarization by regulation power2.95Al material.
Difference from Example 1 is: Cr target sputtering power is that 59.65W, Al target sputtering power reaches 38.24W, other
Technique is with embodiment 1.
The method is used to obtain Cr2.95Al alloy firm, measures its spin polarizability and saturation magnetization is respectively
91% and 4.2 μB。
Embodiment four
Be there is than preparation the Cr of high spin-polarization by regulation power3.05Al material.
Difference from Example 1 is: Cr target sputtering power is that 61.15W, Al target sputtering power reaches 38.24W, other
Technique is with embodiment 1.
The method is used to obtain Cr2.95Al alloy firm, measures its spin polarizability and saturation magnetization is respectively
91% and 4.2 μB。
Embodiment five
Be there is than preparation the Cr of high spin-polarization by regulation power3.10Al material.
Difference from Example 1 is: Cr target sputtering power is that 62.33W, Al target sputtering power reaches 38.24W, other
Technique is with embodiment 1.
The method is used to obtain Cr3.10Al alloy firm, measures its spin polarizability and saturation magnetization is respectively
80% and 2.34 μB。
Embodiment six
By regulation power than preparation Cr2.80Al material.
Difference from Example 1 is: Cr target sputtering power is that 52.13W, Al target sputtering power reaches 38.24W, other
Technique is with embodiment 1.
The method is used to obtain Cr2.80Al alloy firm, may indicate that from XRD the thin film of synthesis is single-phase.
Embodiment seven
By regulation power than preparation Cr3.5Al material.
Difference from Example 1 is: Cr target sputtering power is that W, Al target sputtering power reaches 38.24W, and other techniques are same
Embodiment 1.
The method is used to obtain Cr3.5Al alloy firm, may indicate that from XRD the thin film of synthesis is single-phase.
Embodiment eight
By regulation power than preparation Cr4.0Al material.
Difference from Example 1 is: Cr target sputtering power is that 50.08W, Al target sputtering power reaches 38.24W, other
Technique is with embodiment 1.
The method is used to obtain Cr4.0Al alloy firm, may indicate that from XRD the thin film of synthesis is single-phase.
Embodiment nine
By regulation power than preparation Cr4.2Al material.
Difference from Example 1 is: Cr target sputtering power is that 50.08W, Al target sputtering power reaches 38.24W, other
Technique is with embodiment 1.
The method is used to obtain Cr4.2Al alloy firm, may indicate that from XRD the thin film of synthesis is single-phase.
Embodiment ten
Be there is than preparation the Cr of high spin-polarization by regulation power3.0Al material.
Difference from Example 1 is: Cr target sputtering power is that 15.81W, Al target sputtering power reaches 10W, other techniques
With embodiment 1.
The method is used to obtain Cr3.0Al alloy firm, may indicate that from XRD the thin film of synthesis is single-phase.
Embodiment 11
Be there is than preparation the Cr of high spin-polarization by regulation power3.0Al material.
Difference from Example 1 is: Cr target sputtering power is that 31.62W, Al target sputtering power reaches 20W, other techniques
With embodiment 1.
The method is used to obtain Cr3.0Al alloy firm, may indicate that from XRD the thin film of synthesis is single-phase.
Embodiment 12
Be there is than preparation the Cr of high spin-polarization by regulation power3.0Al material.
Difference from Example 1 is: Cr target sputtering power is that 49.84W, Al target sputtering power reaches 31.53W, other
Technique is with embodiment 1.
The method is used to obtain Cr3.0Al alloy firm, may indicate that from XRD the thin film of synthesis is single-phase.
Embodiment 13
Be there is than preparation the Cr of high spin-polarization by regulation power3.0Al material.
Difference from Example 1 is: Cr target sputtering power is that 79.45W, Al target sputtering power reaches 50.26W, other
Technique is with embodiment 1.
The method is used to obtain Cr3.0Al alloy firm, may indicate that from XRD the thin film of synthesis is single-phase.
Embodiment 14
By regulation power than preparation CryAl (except y=3.0) material.
Being a difference in that with embodiment 1-9: regulation Cr target and Al target simultaneously, but its power ratio is constant, Al target power output becomes
Change scope is 10-55W, and as embodiment 10-13, other techniques are with embodiment 1.
The method is used to obtain CryAl alloy firm, may indicate that from XRD the thin film of synthesis is single-phase.
Embodiment 15
Be there is than preparation the Cr of high spin-polarization by regulation power3.0Al material.
Difference from Example 1 is: underlayer temperature is 200 DEG C.
The method is used to obtain Cr3.0Al alloy firm, may indicate that from XRD the thin film of synthesis is single-phase, simply pattern
On have a little change.
Embodiment 16
Be there is than preparation the Cr of high spin-polarization by regulation power3.0Al material.
Difference from Example 1 is: underlayer temperature is 300 DEG C.
The method is used to obtain Cr3.0Al alloy firm, may indicate that from XRD the thin film of synthesis is single-phase, simply pattern
On have a little change.
Embodiment 17
Be there is than preparation the Cr of high spin-polarization by regulation power3.0Al material.
Difference from Example 1 is: underlayer temperature is 400 DEG C
The method is used to obtain Cr3.0Al alloy firm, may indicate that from XRD the thin film of synthesis is single-phase, simply pattern
On have a little change.
Embodiment 18
By regulation power than preparation CryAl (except y=3.0) material.
It is a difference in that with embodiment 1-9: keeping power constant, underlayer temperature excursion is 200-400 DEG C, the most strictly according to the facts
Executing example 15-17, other techniques are with embodiment 1.
The method is used to obtain Cr3.0Al alloy firm, may indicate that from XRD the thin film of synthesis is single-phase.
Material used in above-mentioned all embodiments all by commercially available, involved equipment and magnetron sputtering operation side
Method is known to those skilled in the art.
Finally illustrating, above example is only in order to illustrate technical scheme and unrestricted, although with reference to relatively
The present invention has been described in detail by good embodiment, it will be understood by those within the art that, can be to the skill of the present invention
Art scheme is modified or equivalent, and without deviating from objective and the scope of technical solution of the present invention, it all should be contained at this
In the middle of the right of invention.
Claims (10)
1. a Cr-Al binary alloy material, it is characterised in that: described alloy material is the single-phase thin film of long-range order, and it is changed
Formula is: CryAl, wherein, 2.8≤y≤4.2.
Cr-Al binary alloy material the most according to claim 1, it is characterised in that: during y=2.90-3.05, CryAl alloy
For having the magnetic alloy material of high spinning polarizability.
Cr-Al binary alloy material the most according to claim 2, it is characterised in that: during y=3, CryAl is to have high-spin
The DO of polarizability3Structure.
Cr-Al binary alloy material the most according to claim 3, it is characterised in that: described CryThe spin polarizability of Al can
Reach 85-100%.
5. according to the Cr-Al binary alloy material described in any one of claim 1-4, it is characterised in that: described CryAl is through magnetic control
Sputtering synthesis.
The preparation method of Cr-Al binary alloy material the most according to claim 1, it is characterised in that: utilize three target superelevation
The method of vacuum magnetic-control sputtering, obtains Cr by regulation sputtering power, underlayer temperature and argon flow amountyAl alloy is single-phase thin
Film.
The preparation method of Cr-Al binary alloy material the most according to claim 6, it is characterised in that: described Cr target sputters
Power bracket be 10-90W, Al target sputtering power scope be 10-50W.
The preparation method of Cr-Al binary alloy material the most according to claim 7, it is characterised in that: described underlayer temperature
For 100-400 DEG C, argon flow amount is 30-70sccm.
The preparation method of Cr-Al binary alloy material the most according to claim 7, it is characterised in that: by adjusting Cr target
Cr is obtained with the sputtering power ratio of Al targetyThe different values of y in Al.
10. according to the preparation method of the Cr-Al binary alloy material described in right 9, it is characterised in that: by improving deposited particles
Energy, enable what Al atom was more uniformly distributed to be dispersed in cubic structure, force Cr3Al forms high orderly DO3Metastable state,
Final synthesis has DO3The Cr of structure3Al alloy.
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| CN110629176A (en) * | 2019-09-05 | 2019-12-31 | 西安交通大学 | Cr-Al alloy film with Zr as substrate and preparation method thereof |
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| CN110629176A (en) * | 2019-09-05 | 2019-12-31 | 西安交通大学 | Cr-Al alloy film with Zr as substrate and preparation method thereof |
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