CN110218975A - A kind of magnetic control co-sputtering growth antiferromagnetic Mn of non-colinear3The preparation method of Pt film - Google Patents
A kind of magnetic control co-sputtering growth antiferromagnetic Mn of non-colinear3The preparation method of Pt film Download PDFInfo
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- CN110218975A CN110218975A CN201910590656.6A CN201910590656A CN110218975A CN 110218975 A CN110218975 A CN 110218975A CN 201910590656 A CN201910590656 A CN 201910590656A CN 110218975 A CN110218975 A CN 110218975A
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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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- 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
Abstract
A kind of magnetic control co-sputtering growth antiferromagnetic Mn of non-colinear3The preparation method of Pt film, this method are grown using the MgO substrate of (001) crystal orientation as egative film and using two target co-sputterings, are additionally provided with Mn on the egative film3Pt and coating, the Mn3Pt is between MgO and coating；Magnetic control growth, easily prepared and film are with high purity；Growing film is monocrystal thin films, and thickness is conducive to magnetic and spin electric device preparation and transport property research in Nano grade.
Description
Technical field
The present invention relates to the antiferromagnetic Mn of Grown by Magnetron Sputtering high quality extension non-colinear3The technology and methods of Pt film are led
Domain, especially a kind of magnetic control co-sputtering grow the antiferromagnetic Mn of non-colinear3The preparation method of Pt film.
Background technique
Spintronics is the new branch of science risen in recent years, and spintronics application include hard disc magnetic head,
Magnetic Random Access Memory, spin traps ballistic transistor, spinning LED etc..Spintronics memory device is compared to tradition
Memory device, there is the multinomial advantages such as storage density is high, low energy consumption, response is fast, in a variety of materials, because ferromagnet have it is easy
In detection and response external magnetic field variation characteristic, so in terms of be widely used；Compared to ferromagnet, anti-iron
The age that magnetic is focused on will for a long time late, and antiferromagnet is to be found by Louis Nai Er in last century, because antiferromagnetic macroscopic view is magnetostatic
Square is zero so that being experimentally difficult to detect and there is huge anisotropy field (~10T) to lead to not manipulate its magnetic shape
State, therefore, it is considered that antiferromagnetic be interesting but technically have no using possible.However antiferromagnet in recent decades is physical
Matter is gradually excavated by the scientist of all parts of the world, becomes research spintronics information recording medium because having the following advantages that
And route of transmission " new lover:
1. the magnetostatic square of macroscopic view is zero: it is insensitive to magnetic field without stray magnetic field, reduce the interference between adjacent devices；
2. huge anisotropy field: resisting extraneous high-intensity magnetic field；
3. picosecond scale dynamic process: about two orders of magnitude faster than ferromagnetic material；
Having in antiferromagnetic a kind of is that non-colinear is antiferromagnetic, is considered as no unusual Hall in long time,
Cause it that can not be detected and be applied to storage aspect to which response will not be generated to external magnetic field, until De Kesa in 2014
This A.H.MacDonald seminar, Austin department of physics, university theoretical prediction for the first time antiferromagnetic Mn of non-colinear3Have in Ir
There are the unusual Hall of same order and solid-state physics research institute, Tokyo Univ Japan Satoru in 2015 in same ferromagnet
Nakatsuji seminar has found the antiferromagnetic Mn of non-colinear in an experiment for the first time3Sn has big unusual Hall, with ferromagnetic
Magnitude is consistent, demonstrates the calculated results of A.H.MacDonald seminar well, hereafter, antiferromagnetic each of non-colinear
Kind physical property is found in succession, such as Kerr magnetooptical effect, logic gates, and spin Nernst effect, spin polarization electricity
Stream and unusual Nernst effect etc..It is applied to magnetic storage and the experiment of transport agent also like a raging fire for non-colinear is antiferromagnetic
Development.Mn antiferromagnetic for non-colinear3Pt just had scientist to expand research early in 1967, experimentally north at the beginning of 2018
Capital Liu Zhiqi seminar, aerospace university is for the first time in piezoelectric strain material BaTiO3The Mn of high quality is grown on substrate3Pt is thin
Film.To sum up, forefathers antiferromagnetic mainly based on electric arc thawing method, the Mn of growth that grows non-colinear3X (X=Ir, Sn, Pt, Ge,
Ga, Rh) it is also bulk sample, it is unfavorable for the preparation and research of micro-nano device.Experimentally we are received using Grown by Magnetron Sputtering
The other Mn of meter level3Pt film grows Mn using double target co-sputtering3Pt non-colinear antiferromagnet film, from the thin film composition, degree of order, coarse
Degree etc. characterization sample needs to design a kind of new magnetic control co-sputtering growth antiferromagnetic Mn of non-colinear3The preparation of Pt film
Method.
The present invention be exactly in order to solve problem above and carry out improvement.
Summary of the invention
The technical problem to be solved by the invention is to provide a kind of growths of magnetic control, and easily prepared and film is with high purity, favorably
The antiferromagnetic Mn of non-colinear is grown in the magnetic control co-sputtering of magnetic and spin electric device preparation Yu transport property research3Pt is thin
The preparation method of film.
The present invention is that technical solution used by solving its technical problem is:
A kind of magnetic control co-sputtering growth antiferromagnetic Mn of non-colinear3The preparation method of Pt film, this method is with (001) crystal orientation
MgO substrate is egative film and is grown using two target co-sputterings, is additionally provided with Mn on the egative film3Pt and coating, the Mn3Pt
Between MgO and coating；
The implementation steps of described this method are as follows:
Substrate cleans before S1, long sample, with the ionized water again of alcohol after acetone, ultrasound 3min respectively, and mainly with acetone, alcohol,
Based on three step of deionized water, by step, first with alcohol after acetone, ionized water, difference ultrasound 3min use nitrogen after ultrasonic again
Spray gun makes substrate surface completely without spot；
S2, high growth temperature, substrate are passed to vacuum sputtering chamber after room temperature 30min indoors after pasting using elargol, and
To substrate pre-treatment, keep it uniform in substrate back with tweezers pressing elargol when pasting substrate.Room temperature indoors after elargol is pasted
It is passed to vacuum sputtering chamber after placing 30min, is evacuated down to 5.0 × 10-8Torr.Silicon rate remains 0.5 DEG C/min,
Substrate is maintained at 600 DEG C of 30min of growth temperature to substrate pre-treatment；
S3, production coating, sputtering power are maintained at Mn (56w), Pt (30w), and argon gas is maintained at 2.6mTorr, beats simultaneously
Opening baffle, sputter rate 0.4nm/min sputters 10min, simultaneously closes off baffle, and in-situ high temperature is annealed 3h, after annealing, from
So cool to room temperature, the SiN of sputtering 3nm thickness is used as coating, and sputtering growing film is double target co-sputtering, baffle opening and
Being consistent property of shut-in time；
Further, the MgO substrate is (001) orientation；
The Mn3Pt with a thickness of 6nm to 100nm；
The coating is the oxide of silicon or aluminium, and coating can be SiO2, and the oxides such as Al2O3 can also be metal；
Further, the target is Mn target and Pt target；
Specifically, the rate of heat addition of substrate is 0.5 DEG C/S in the step S2, heating rate is slower, can guarantee substrate
It is pasted on pallet securely and heating rate facilitates to protect substrate more slowly, piezoelectric strain material base protected especially pronounced；
Wherein, the Pt target can be replaced by Ir, Sn, Ge, Rh or Ga.
The present invention has the advantages that magnetic control is grown, easily prepared and film is with high purity；Growing film is monocrystal thin films, thick
Degree is conducive to magnetic and spin electric device preparation and transport property research in Nano grade.
Detailed description of the invention
Fig. 1 is a kind of magnetic control co-sputtering growth antiferromagnetic Mn of non-colinear proposed by the present invention3The preparation method of Pt film
Schematic diagram.
Fig. 2 is a kind of magnetic control co-sputtering growth antiferromagnetic Mn of non-colinear proposed by the present invention3In the preparation method of Pt film
Film growth temperature variation diagram.
Fig. 3 is a kind of magnetic control co-sputtering growth antiferromagnetic Mn of non-colinear proposed by the present invention3In the preparation method of Pt film
Film growth power variation diagram.
Fig. 4 is a kind of magnetic control co-sputtering growth antiferromagnetic Mn of non-colinear proposed by the present invention3In the preparation method of Pt film
The extraordinary Hall effect figure of film.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Diagram and specific embodiment are closed, the present invention is further explained.
The magnetic control co-sputtering grows the antiferromagnetic Mn of non-colinear3The specific growth pattern of the preparation method of Pt film is that double targets are total
Sputtering uses following calibration to reach n (Mn): n (Pt)=3:1 of the ratio between amount of Mn element and Pt elemental substance inside film
Mode:
One, Mn target Pt target uses d.c. sputtering (DC), because Pt target sputter rate is very fast, even if sputtering power is turned down
The growth rate of Mn is still greater than in starter power 8w, and growth rate is about twice of Mn target, is unable to reach the ratio between amount of substance
For the requirement of 3:1；
Two, Mn target d.c. sputtering, the exchange sputtering of Pt target change to 50w from 20w and calibrate exchange sputtering respectively using 10w as step-length
The growth rate and 10w of Pt target are step-length, the growth rate that 80w calibrates d.c. sputtering Mn target respectively are changed to from 30w, by X
Ray bounce technique characterize film thickness ratio, finally obtain Pt target 30w exchange sputtering, Mn target sputtering power 50w to 60w it
Between include 3:1 ratio, stringent sputtering power ratio in order to obtain keeps Pt target power output constant in 30w, by the sputtering function of Mn target
Rate is changed from 32w to 64w with the step-length of 8w, obtains Mn (56w) by X-ray energy dispersion spectrometer accurate measurement, Pt (30w) is
Final power ratio, it is this under the conditions of film substrate the closest 3:1 of the ratio between amount；
Wherein, it is higher than cosputtering growing film under high temperature with room temperature cosputtering growing film thickness under sputtering time；It is single
The thickness that solely sputtering Mn target or Pt target obtain is significantly larger than the film thickness of cosputtering growth.
The epitaxy single-crystal of high quality in order to obtain, substrate selective oxidation magnesium-based piece, with 100 DEG C for step-length, by growth temperature
Change from 26 DEG C to 800 DEG C, by X-ray diffraction to the sample characterization of growth, when growth temperature, annealing temperature are higher than 700 DEG C
When, the Mn atom in film can precipitate into the Mn layer that surface forms single layer inside film.
When growth temperature is 600 DEG C, being able to maintain good thin film epitaxy and being unlikely to excessive temperature again leads to Mn atom
It is precipitated, growth temperature is maintained at 600 degrees Celsius, in the case that Mn target Pt target power output remains unchanged, when growth air pressure is maintained at
When 2.6mTorr, the roughness of film is the best.
In conjunction with table 1, learn that keeping Pt target sputtering power is that 30w is constant, Mn using X-ray energy scattering spectrum analysis measurement
Target sputtering power, for a step-length, is changed with 8w and arrives 60w, and sputtering power has obtained the ratio between amount of optimisation substance when being 56w；
Table 1
In conjunction with table 2, under the same terms, only there is Mn on MgO substrate3The peak of Pt, therefore select substrate for MgO lining
Bottom；
Table 2
Referring to shown in Fig. 2, by changing film growth temperature, obtaining 500 degrees Celsius or more growing films can be grown
The preferable Mn of quality3Film surface can be precipitated in Pt film, Mn atom of 700 degrees Celsius or more the sputtering sedimentations on substrate, can not
At Mn3Pt phase, 600 degrees Celsius of optimum growth temps for film, at this temperature, deposition film can form the outer of better quality
Prolong non-colinear antiferromagnet film while Mn atom inside film will not be caused to be precipitated because temperature is excessively high, reaches one more
Ideal intermediate state.
Referring to shown in Fig. 3, Mn target sputtering power is illustrated, different growth powers, identical growth temperature and annealing
The film of temperature growth changes from 32w to 64w, XRD measurement display, Mn using 8w as step-length3Pt (001) peak value is with sputtering function
The raising of rate and deviate to the left, lattice constant is also gradually mutually close to block lattice constant.
Referring to shown in Fig. 4, identical growth temperature is grown, the unusual Hall of the film of different annealing conditions is illustrated,
600 DEG C of fixed growth temperature remain unchanged, and annealing temperature is changed from 600 DEG C to 750 DEG C with 50 DEG C for step-length, and obtained sample is anti-
Chang Huoer is widely different, the Cheng Xiangwei L inside 700 DEG C of films annealed above10MnPt, without unusual Hall loop, 700 DEG C or less
There is unusual Hall loop.
Double target co-sputtering target described in the present embodiment is not limited solely to Pt target, also can be used Ir, Sn, Ge, Ga, Rh,
The other materials such as Pd.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent defines.
Claims (5)
1. a kind of magnetic control co-sputtering grows the antiferromagnetic Mn of non-colinear3The preparation method of Pt film, this method is with the MgO of (001) crystal orientation
Substrate is egative film and is grown using two target co-sputterings, it is characterised in that:
Mn is additionally provided on the egative film3Pt and coating, the Mn3Pt is between MgO and coating；
The implementation steps of described this method are as follows:
S1: substrate cleans before long sample, with the ionized water again of alcohol after acetone, ultrasound respectively thereafter；
S2, high growth temperature, substrate is passed to vacuum sputtering chamber after room temperature after pasting using elargol indoors, and locates in advance to substrate
Reason；
S3, production coating.
2. a kind of magnetic control co-sputtering as described in claim 1 grows the antiferromagnetic Mn of non-colinear3The preparation method of Pt film, it is special
Sign is that the MgO substrate is (001) orientation；
The Mn3Pt with a thickness of 6nm to 100nm；
The coating is the oxide of silicon or aluminium.
3. a kind of magnetic control co-sputtering as described in claim 1 grows the antiferromagnetic Mn of non-colinear3The preparation method of Pt film, it is special
Sign is that the target is Mn target and Pt target.
4. a kind of magnetic control co-sputtering as described in claim 1 grows the antiferromagnetic Mn of non-colinear3The preparation method of Pt film, it is special
Sign is that the rate of heat addition of substrate is 0.5 DEG C/S in the step S2.
5. a kind of magnetic control co-sputtering as claimed in claim 3 grows the antiferromagnetic Mn of non-colinear3The preparation method of Pt film, it is special
Sign is that the Pt target can be replaced by Ir, Sn, Ge, Rh or Ga.
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Citations (3)
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|---|---|---|---|---|
| US7497007B2 (en) * | 2005-07-14 | 2009-03-03 | Headway Technologies, Inc. | Process of manufacturing a TMR device |
| US20130236720A1 (en) * | 2012-03-07 | 2013-09-12 | Northeastern University | Rare-earth-free or noble metal-free large magnetic coercivity nanostructured films |
| CN103904211A (en) * | 2014-04-15 | 2014-07-02 | 清华大学 | Magnetic field detector based on perpendicular exchange coupling and preparing and use methods thereof |
-
2019
- 2019-07-02 CN CN201910590656.6A patent/CN110218975A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7497007B2 (en) * | 2005-07-14 | 2009-03-03 | Headway Technologies, Inc. | Process of manufacturing a TMR device |
| US20130236720A1 (en) * | 2012-03-07 | 2013-09-12 | Northeastern University | Rare-earth-free or noble metal-free large magnetic coercivity nanostructured films |
| CN103904211A (en) * | 2014-04-15 | 2014-07-02 | 清华大学 | Magnetic field detector based on perpendicular exchange coupling and preparing and use methods thereof |
Non-Patent Citations (4)
| Title |
|---|
| DANICA SOLINA ET AL.: ""The magnetic structure of L10 ordered MnPt at room temperature determined using polarized neutron diffraction"", 《MATERIALS RESEARCH EXPRESS》 * |
| EDUARDO MENDIVE-TAPIA ET AL.: ""Ab initio theory of the Gibbs free energy and a hierarchy of local momnet correlation functions in itinerant electron systems:the magnetism of the Mn3A materials class"", 《PHYSICAL REVIEW》 * |
| SEUNGJUN OH ET AL.: ""Controlled growth and magnetic property of a-plane-oriented Mn3Sn thin films"", 《AIP ADVANCES》 * |
| TOMOKI IKEDA ET AL.: ""Anomalous Hall effect in polycrystalline Mn3Sn thin films"", 《APPLIED PHYSICS LETTERS》 * |
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