CN108517491A - A kind of more iron γ '-Fe of extension with big magnetoelectric effect4N/PMN-PT heterojunction structures and preparation method - Google Patents

A kind of more iron γ '-Fe of extension with big magnetoelectric effect4N/PMN-PT heterojunction structures and preparation method Download PDF

Info

Publication number
CN108517491A
CN108517491A CN201810217164.8A CN201810217164A CN108517491A CN 108517491 A CN108517491 A CN 108517491A CN 201810217164 A CN201810217164 A CN 201810217164A CN 108517491 A CN108517491 A CN 108517491A
Authority
CN
China
Prior art keywords
gas
pmn
sputtering
vacuum
iron
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810217164.8A
Other languages
Chinese (zh)
Inventor
米文博
赖征勋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tianjin University
Original Assignee
Tianjin University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tianjin University filed Critical Tianjin University
Priority to CN201810217164.8A priority Critical patent/CN108517491A/en
Publication of CN108517491A publication Critical patent/CN108517491A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C23C14/0641—Nitrides
    • 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
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
    • H01F41/18—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates by cathode sputtering

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Thin Magnetic Films (AREA)

Abstract

The present invention relates to a kind of more iron γ ' Fe of the extension with big magnetoelectric effect4N/PMN PT heterojunction structures and preparation method；In the 0.7Pb (Mg that (011) is orientated1/3Nb2/3)O3‑0.3PbTiO3Single crystal epitaxial γ ' the Fe of different-thickness are prepared in substrate4N thin film；It is 0.05A, sputtering voltage 750V, γ ' Fe in sputtering current4When N thin film thickness is 17nm, γ ' Fe4The opposite variation of the intensity of magnetization under the regulation and control of electric field of the more iron constructions of N/PMN PT is maximum.This develops opposite target magnetic control sputtering method and prepares γ ' Fe clearly4The more iron heterojunction structures of N/PMN PT, and it observes big magnetoelectric effect, 230% is up to the regulation and control of the intensity of magnetization using electric field, magnetron sputtering method of the present invention, compared with molecular beam epitaxy and chemical method, have a clear superiority in industrialized production.

Description

A kind of more iron γ '-Fe of extension with big magnetoelectric effect4N/PMN-PT hetero-junctions Structure and preparation method
Technical field
The invention patent relates to a kind of more iron heterojunction structure γ '-Fe of the extension with big magnetoelectric effect4N/PMN-PT (γ′-Fe4N/0.7Pb(Mg1/3Nb2/3)O3-0.3PbTiO3And preparation method (011)).More specifically, be it is a kind of have it is larger The preparation method of the heterojunction structure of magnetoelectric effect.
Background technology
Have wide practical use in magnetic storage isospin electronics material with strong magneto-electric coupled material. (1-x) Pb (Mg in recent years1/3Nb2/3)O3-xPbTiO3(PMN-PT) pass is received due to the electrostriction effect of its superelevation Note.People are mainly directed to magnetic material and PMN-PT is compound to realize strong magnetoelectric effect.
γ′-Fe4N is a kind of generally acknowledged very potential ferrimagnet.γ′-Fe4N has the spin polarization of superelevation Rate, high saturation magnetization, low-down coercivity and good metallic conductivity, therefore it is very suitable for being applied to In spintronics devices.In addition, also having good anticorrosive and anti abrasive property, the physicochemical properties of stabilization Deng this makes it be with a wide range of applications.
Currently, the ferromagnetic thin film prepared in ferromagnetic/ferroelectric heterostructures is mostly polycrystalline or noncrystal membrane, and The seldom of extension ferromagnetic thin film is studied, and realizes that the opposite variation of the intensity of magnetization of automatically controlled magnetic is maximum wherein and is no more than Δ M/M (0)=160% (direction [0-11]) [Scientific Report 4,3727 (2014)].Due to γ '-Fe4N and PMN-PT has There are good Lattice Matching, therefore γ '-Fe4N can form the heterojunction structure of extension with epitaxial growth in PMN-PT substrates.By In film and substrate epitaxial growth, the stress generated due to reciprocal piezoelectric effect can preferably be passed to film by base, to produce Raw larger magnetoelectric effect.Due to single-phase γ '-Fe4The growth conditions of N thin film on different substrates is very harsh, therefore It is there is no so far to γ '-Fe4The preparation of N/PMN-PT heterojunction structures and its research of automatically controlled magnetic.In addition, utilizing electric field controls In practical applications mostly based on thin-film material, preparation method mostly uses sputtering method for the variation of the intensity of magnetization.Patent of the present invention is logical A large amount of experimental study is crossed, single crystal epitaxial γ '-Fe are prepared for using opposite target magnetic control sputtering method4The more iron hetero-junctions of N/PMN-PT Structure, and obtain the regulation and control that the opposite variation of the intensity of magnetization has reached 230% in the direction [0-11].
Invention content
In terms of industrialized production angle, need to prepare film sample using magnetron sputtering method；In terms of practical application angle, Need sample to be prepared that there are the regulation and control of the structure and the larger intensity of magnetization of single crystal epitaxial.The present invention is i.e. from two above purpose It sets out, develops opposite target magnetic control sputtering method and prepare γ '-Fe4The more iron heterojunction structures of N/PMN-PT, and observe big magnetoelectricity Coupling effect is up to 230% using electric field to the regulation and control of the intensity of magnetization at room temperature, higher than reported values.
The present invention studies through a large number of experiments, including changes sputtering current, sputtering voltage, the sputtering gas in experimentation Pressure, sputter temperature, temperature fall time and film thickness, in the 0.7Pb (Mg that (011) is orientated1/3Nb2/3)O3-0.3PbTiO3In substrate Prepare the single crystal epitaxial γ '-Fe of different-thickness4N thin film.Finally find only to be 0.05A in sputtering current, sputtering voltage is 750V, γ '-Fe4When N thin film thickness is 17nm, γ '-Fe4The more iron constructions of N/PMN-PT intensity of magnetization under the regulation and control of electric field Opposite variation is maximum.
The present invention is preparing γ '-Fe4When N epitaxial films, used substrate is the PMN-PT monocrystalline that single side is scraped, wherein Pb(Mg1/3Nb2/3)O3And PbTiO3Accounting be divided into 7：3, thickness is 200 μm, and area is 3mm × 3mm；Used electrode is Air-dried elargol；The mode that used added electric field surveys magnetism is electric field perpendicular to film surface；Applied magnetic field is oriented parallel to film Face, along the direction [0-11].More iron hetero-junctions at room temperature with the electric field of 10kV/cm, 100Oe magnetic field under, the intensity of magnetization Opposite variation be 230%.
A kind of more iron γ '-Fe of extension with big magnetoelectric effect of the present invention4N/PMN-PT heterojunction structures；It is tied Structure is γ '-Fe4N/0.7Pb(Mg1/3Nb2/3)O3-0.3PbTiO3。
A kind of more iron γ '-Fe of extension with big magnetoelectric effect of the present invention4N/PMN-PT heterojunction structures are specifically made Preparation Method is realized by following steps：
1) it is the 0.7Pb that (011) of single-sided polishing is orientated to use vacuum opposite direction targets magnetic sputtering film plating machine, base material (Mg1/3Nb2/3)O3-0.3PbTiO3Single-chip；The Fe targets for the use of two pieces of purity being 99.99% are mounted on in target head, wherein one N pole of the head as the magnetic line of force, other end are the poles S；
2) vacuum opposite direction targets magnetic sputtering film plating machine vacuum system is opened, level-one mechanical pump and secondary molecules pump are successively started It vacuumizes, until the back end vacuum degree of sputtering chamber is better than 1 × 10–5Pa；
3) sputter gas Ar gas and the reaction gas N that purity is 99.999% are passed through to vacuum chamber2Gas, Ar gas and N2Gas Flow-rate ratio is 5：1, vacuum degree is maintained at 1Pa；
4) substrate is uniformly heating to 505 DEG C；
5) after temperature is stablized, shielding power supply is opened, applies the direct current of the electric current and 750V of 0.05A on a pair of of Fe targets Pressure, pre-sputtering 10 minutes reach sputtering current and voltage stabilization；
6) plate washer opened in substrate frame starts to sputter；Sputtering time is 7 minutes, obtains γ '-Fe4The thickness of N thin film is 17nm；
7) after sputtering, the plate washer in substrate frame is closed, is then shut off shielding power supply, stopping is passed through Ar gas and N2Gas, Slide valve is opened completely, is continued to vacuumize, so that substrate is at the uniform velocity down to room temperature using temperature-controlling system；The time of cooling is 3 hours；
8) temperature is cooled to room temperature, and closes vacuum system, is passed through the N that purity is 99.999%2Gas is beaten to 1 atmospheric pressure Vacuum chamber is opened, the γ '-Fe prepared are taken out4The more iron heterojunction structures of N/PMN-PT.
It is preferred that used substrate is the PMN-PT monocrystalline that single side is scraped, wherein Pb (Mg1/3Nb2/3)O3And PbTiO3Account for Score is 7：3, thickness is 200 μm, and area is 3mm × 3mm.
It is preferred that used electrode is air-dried elargol.
It is preferred that it is electric field perpendicular to film surface that used added electric field, which surveys magnetic mode,；Applied magnetic field is oriented parallel to film Face, along the direction [0-11].
It is preferred that vacuum opposite direction targets magnetic sputtering film plating machine uses the DPS- of Chinese Academy of Sciences Shenyang scientific instrument development center production Type III ultrahigh vacuum opposite direction targets magnetic sputtering film plating machine.
It is preferred that Fe target purity is 99.99%, thickness 4mm, a diameter of 60mm；The distance between two targets are 80mm, the axis of target are 80mm with the distance between substrate frame of PMN-PT base materials is placed with.
It is preferred that the flow of the mixed gas Ar gas led to is 100sccm, N2The flow of gas is 20sccm.
The time that preferred substrate uniformly heats up is 40 minutes；
It is preferred that the time to cool down is 3 hours.
To confirm the best embodiment of the present invention, we have carried out high-resolution to the heterojunction structure prepared by the present invention The measurement that transmission electron microscope characterizes and electric field regulation and control are magnetic.
γ '-the Fe prepared from the present invention4The high resolution transmission electron microscope figure of the more iron heterojunction structures of N/PMN-PT It can see as upper, PMN-PT substrates and γ '-Fe4N thin film lattice arrangement is orderly, γ '-Fe4N thin film is orientated extension in [011] Growth, as shown in Figure 1.
γ '-Fe are measured in the present invention4The application electric field schematic diagram of the electric field control magnetic of the more iron heterojunction structures of N/PMN-PT, such as Shown in Fig. 2.Direction of an electric field is parallel to film surface perpendicular to film surface, magnetic direction when measuring magnetic, along the direction [0-11].
The present invention measures γ '-Fe4The more iron heterojunction structures of N/PMN-PT in making alive and the hysteresis loop for being not added with voltage, As shown in Figure 3.Wherein measuring temperature is room temperature.From figure 3, it can be seen that after making alive, sample is significantly become by more difficult magnetization To be easier to magnetize.
The present invention measures γ '-Fe4The intensity of magnetization of the more iron heterojunction structures of N/PMN-PT is with applying alive variation, magnetic Field direction is parallel to direction [0-11] of film surface, and magnetic field size is 100Oe, and direction of an electric field is perpendicular to film surface towards the side of substrate To.From measurement result as can be seen that compared with being not added with voltage, the intensity of magnetization increased dramatically under positive voltage, the intensity of magnetization Opposite variation has reached 230%, as shown in Figure 4.
It is ferromagnetic thin prepared by the present invention compared with the method for the more iron heterojunction structures of ferromagnetic/ferroelectricity prepared by other methods Film γ '-Fe4N has the single crystal epitaxial structure of high quality, and γ '-Fe4N/PMN-PT heterojunction structures have greatly magneto-electric coupled Effect, used method simple practical, and be conducive to the popularization in industrial production.It is specific as follows：
Although 1) have preparation and the report of magneto-electric coupled property of the more iron heterojunction structures of ferromagnetic/ferroelectricity in the world, prepare Most of ferromagnetic material be polycrystalline either amorphous, therefore its magnetic anisotropy is almost without this makes it in reality It is restricted in the application of border.
2) the more iron heterojunction structures prepared in the world at present utilize the opposite variation of its intensity of magnetization of electric field controls to be up to To 160%.And the γ '-Fe that we prepare4N/PMN-PT is more, and iron heterojunction structure magnetization change has reached 230%；
3) since main method used by current industrialized production is sputtering method, magnetron sputtering of the present invention Method has a clear superiority compared with molecular beam epitaxy and chemical method in industrialized production.
Description of the drawings
Fig. 1 gives the γ '-Fe prepared in the present invention4The high-resolution transmitted electron of the more iron heterojunction structures of N/PMN-PT MIcrosope image.
Fig. 2 gives the γ '-Fe prepared in the present invention4The survey of the electric field regulation and control magnetism of the more iron heterojunction structures of N/PMN-PT Spirogram.
Fig. 3 gives the present invention γ '-Fe prepared4The more iron heterojunction structures of N/PMN-PT are under zero electric field with 10kV/cm's Hysteresis loop under electric field.
Fig. 4 gives the present invention γ '-Fe prepared4The more iron heterojunction structures of N/PMN-PT are under zero electric field with 10kV/cm's The size of the variation of the intensity of magnetization under electric field alternating variation, the magnetic field of application is 100Oe.
Specific implementation mode
According to us to the structure and property analysis of sample progress prepared in the present invention as a result, below by opposite target magnetic It controls sputtering method and prepares γ '-Fe4The preferred forms of the more iron heterojunction structures of N/PMN-PT are described in detail：
1) the DPS-III type ultrahigh vacuum opposite direction target magnetic control sputterings of Chinese Academy of Sciences Shenyang scientific instrument development center production are used Coating machine, base material are the 0.7Pb (Mg of single-sided polishing1/3Nb2/3)O3-0.3PbTiO3(011) single-chip.Use two pieces of purity For 99.99% Fe targets, it is mounted on in target head, wherein the poles N as the magnetic line of force, other end is the poles S；Thickness is 4mm, a diameter of 60mm；The distance between two targets be 80mm, the axis of target and be placed with PMN-PT base materials substrate frame it Between distance be 80mm；
2) first, by 0.7Pb (Mg1/3Nb2/3)O3-0.3PbTiO3(011) single-chip is put into substrate frame, after being put into baffle Face, and close vacuum chamber；
3) DPS-III ultrahigh vacuum opposite direction targets magnetic sputtering film plating machine vacuum systems are opened, level-one mechanical pump is successively started With secondary molecules pumping vacuum, until sputtering chamber back end vacuum degree be better than 1 × 10–5Pa；
4) sputter gas Ar gas and the reaction gas N that purity is 99.999% while to vacuum chamber are passed through2Gas, Ar gas and N2 The flow-rate ratio of gas is 5：1, vacuum degree is maintained at 1Pa；
5) substrate is uniformly heating to 505 DEG C, the time of heating is 40 minutes；
6) shielding power supply is opened, applies the DC voltage of the electric current and 750V of 0.05A on a pair of of Fe targets, pre-sputtering 10 is divided Clock waits for sputtering current and voltage stabilization；
7) plate washer opened in substrate frame starts to sputter, reactive sputtering γ '-Fe4During N thin film, 0.7Pb (Mg1/ 3Nb2/3)O3-0.3PbTiO3(011) single-chip position is fixed；
8)γ′-Fe4The sedimentation time of N thin film is 7 minutes, obtains γ '-Fe4The thickness of N thin film is 17nm；
9) after sputtering, the plate washer in substrate frame is closed, is then shut off shielding power supply, stopping is passed through Ar gas and N2Gas, Slide valve is opened completely, continues to vacuumize, and so that substrate is at the uniform velocity down to room temperature using temperature-controlling system, temperature fall time is 3 hours.
10) vacuum system is closed, the N that purity is 99.999% is passed through2Gas opens vacuum chamber to 1 atmospheric pressure, takes out system γ '-the Fe got ready4The more iron heterojunction structures of N/PMN-PT.
γ '-Fe according to the present invention4N/PMN-PT is more, and iron heterojunction structure has on multi-functional spintronics devices Application value, for example, can be as memory storage unit, logicality device etc., and the magnetron sputtering method that the present invention uses It is the common method of industrial production thin-film material, used Fe targets have target selection is simple and target utilization rate is higher etc. Advantage.
γ '-the Fe of preparation4High resolution transmission electron microscope image such as Fig. 1 institutes of the more iron heterojunction structures of N/PMN-PT Show, γ '-Fe4For N thin film in [011] direction epitaxial growth in PMN-PT substrates, lattice arrangement is orderly.γ′-Fe4N/PMN-PT The circuit diagram of the magnetic measurement of electric field regulation and control of more iron heterojunction structures, as shown in Figure 2.The voltage vertical applied is in film Face, magnetic field are applied in face the direction [0-11].Prepare γ '-Fe4The hysteresis loop of the more iron heterojunction structures of N/PMN-PT, such as Fig. 3 institutes Show；After the electric field for applying 10kV/cm, sample obviously becomes easy magnetization from hardly possible magnetization.Prepare γ '-Fe4N/PMN-PT is more, and iron is different The intensity of magnetization of matter structure is with applying alive modified-image as shown in figure 4, the remanent magnetization in the direction [0-11] is in 10kV/ Reach 230% compared to magnetization change under 0 electric field under the electric field of cm, and with repeatability.
γ '-the Fe with big magnetoelectric effect that the present invention is disclosed and proposed4The more iron heterojunction structures of N/PMN-PT and system Preparation Method, those skilled in the art can be by using for reference present disclosure, and the appropriate links such as condition route that change are realized, although of the invention Method and technology of preparing be described by preferred embodiment, related technical personnel can obviously not depart from the present invention Methods and techniques described herein route is modified or is reconfigured in content, spirit and scope, to realize final system Standby technology.In particular, it should be pointed out that all similar replacements and change are apparent for a person skilled in the art , they are considered as being included in spirit of that invention, range and content.

Claims (10)

1. a kind of more iron γ '-Fe of extension with big magnetoelectric effect4N/PMN-PT heterojunction structures；It is characterized in that structure is γ′-Fe4N/0.7Pb(Mg1/3Nb2/3)O3-0.3PbTiO3。
2. the preparation method of the heterojunction structure of claim 1, it is characterized in that steps are as follows：
1) it is the 0.7Pb (Mg that (011) of single-sided polishing is orientated to use vacuum opposite direction targets magnetic sputtering film plating machine, base material1/ 3Nb2/3)O3-0.3PbTiO3Single-chip；The Fe targets for the use of two pieces of purity being 99.99% are mounted on in target head, wherein a work For the poles N of the magnetic line of force, other end is the poles S；
2) vacuum opposite direction targets magnetic sputtering film plating machine vacuum system is opened, successively starts level-one mechanical pump and secondary molecules pumping is true Sky, until the back end vacuum degree of sputtering chamber is better than 1 × 10–5Pa；
3) sputter gas Ar gas and the reaction gas N that purity is 99.999% are passed through to vacuum chamber2Gas, Ar gas and N2The flow of gas Than being 5：1, vacuum degree is maintained at 1Pa；
4) substrate is uniformly heating to 505 DEG C；
5) after temperature is stablized, shielding power supply is opened, applies the DC voltage of the electric current and 750V of 0.05A on a pair of of Fe targets, in advance Sputtering 10 minutes, reaches sputtering current and voltage stabilization；
6) plate washer opened in substrate frame starts to sputter；Sputtering time is 7 minutes, obtains γ '-Fe4The thickness of N thin film is 17nm；
7) after sputtering, the plate washer in substrate frame is closed, is then shut off shielding power supply, stopping is passed through Ar gas and N2Gas is beaten completely Plate valve is opened a sluice gate, continues to vacuumize, so that substrate is at the uniform velocity down to room temperature using temperature-controlling system；The time of cooling is 3 hours；
8) temperature is cooled to room temperature, and closes vacuum system, is passed through the N that purity is 99.999%2Gas opens vacuum to 1 atmospheric pressure γ '-the Fe prepared are taken out in room4The more iron heterojunction structures of N/PMN-PT.
3. method as claimed in claim 2, it is characterized in that used substrate is the PMN-PT monocrystalline that single side is scraped, wherein Pb (Mg1/3Nb2/3)O3And PbTiO3Accounting be divided into 7：3, thickness is 200 μm, and area is 3mm × 3mm.
4. method as claimed in claim 2, it is characterized in that used electrode is air-dried elargol.
5. method as claimed in claim 2, it is characterized in that it is electric field perpendicular to film surface that used added electric field, which surveys magnetic mode,； Applied magnetic field is oriented parallel to film surface, along the direction [0-11].
6. method as claimed in claim 2, it is characterized in that vacuum opposite direction targets magnetic sputtering film plating machine uses Shenyang section of the Chinese Academy of Sciences Learn the DPS-III type ultrahigh vacuum opposite direction targets magnetic sputtering film plating machines of instrument development center production.
7. method as claimed in claim 2, it is characterized in that Fe target purity is 99.99%, thickness 4mm is a diameter of 60mm；The distance between two targets are 80mm, and the axis of target is with the distance between the substrate frame for being placed with PMN-PT base materials 80mm。
8. method as claimed in claim 2, it is characterized in that the flow of the mixed gas Ar gas led to is 100sccm, N2The stream of gas Amount is 20sccm.
9. method as claimed in claim 2, it is characterized in that the time that substrate uniformly heats up in step 4) is 40 minutes.
10. method as claimed in claim 2, it is characterized in that the time to cool down in step 7) is 3 hours.
CN201810217164.8A 2018-03-16 2018-03-16 A kind of more iron γ '-Fe of extension with big magnetoelectric effect4N/PMN-PT heterojunction structures and preparation method Pending CN108517491A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810217164.8A CN108517491A (en) 2018-03-16 2018-03-16 A kind of more iron γ '-Fe of extension with big magnetoelectric effect4N/PMN-PT heterojunction structures and preparation method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810217164.8A CN108517491A (en) 2018-03-16 2018-03-16 A kind of more iron γ '-Fe of extension with big magnetoelectric effect4N/PMN-PT heterojunction structures and preparation method

Publications (1)

Publication Number Publication Date
CN108517491A true CN108517491A (en) 2018-09-11

Family

ID=63433931

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810217164.8A Pending CN108517491A (en) 2018-03-16 2018-03-16 A kind of more iron γ '-Fe of extension with big magnetoelectric effect4N/PMN-PT heterojunction structures and preparation method

Country Status (1)

Country Link
CN (1) CN108517491A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110904417A (en) * 2019-11-18 2020-03-24 天津大学 Flexible epitaxial Fe with stress-regulated magnetization intensity4N film and preparation method
CN116018050A (en) * 2023-01-09 2023-04-25 中国矿业大学 Multiferroic heterostructure based on copper ferrite and preparation method thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
JU‐HYUN KIM 等: ""Effect of an electric field‐induced stress on the magnetic properties of amorphous Terfenol‐D films deposited on PMN‐PT single crystal substrates"", 《PHYSICA STATUS SOLIDI（A）》 *
封秀平: ""γ′–Fe4N 薄膜的结构、磁性和磁电阻效应"", 《中国优秀硕士学位论文全文数据库 基础科学辑》 *
米文博: "自旋电子学材料：Fe4N薄膜及其异质结构", 《物理学进展》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110904417A (en) * 2019-11-18 2020-03-24 天津大学 Flexible epitaxial Fe with stress-regulated magnetization intensity4N film and preparation method
CN110904417B (en) * 2019-11-18 2021-11-02 天津大学 Flexible epitaxial Fe with stress-regulated magnetization intensity4N film and preparation method
CN116018050A (en) * 2023-01-09 2023-04-25 中国矿业大学 Multiferroic heterostructure based on copper ferrite and preparation method thereof

Similar Documents

Publication Publication Date Title
CN103839928B (en) A kind of high pressure, Low dark curient, high polarization intensity bismuth ferrite thin film and preparation method thereof
CN101286545B (en) Compound film hetero-junction having magnetoelectric effect and preparing method thereof
CN108517491A (en) A kind of more iron γ '-Fe of extension with big magnetoelectric effect4N/PMN-PT heterojunction structures and preparation method
Ke et al. Highly c-axis oriented AlN film grown by unbalanced magnetron reactive sputtering and its electrical properties
CN101497986B (en) Apparatus for preparing extension ferriferrous oxide film by facing-target reactive sputtering and operation method
Hou et al. Self-polarization induced by lattice mismatch and defect dipole alignment in (001) BaTiO 3/LaNiO 3 polycrystalline film prepared by magnetron sputtering at low temperature
Hong et al. Enhanced piezoelectric and dielectric properties of Pb (Yb1/2Nb1/2) O3–Pb (Mg1/3Nb2/3) O3–PbTiO3 crystals by combining alternating and direct current poling
CN101235539B (en) Epitaxy growing method for La1-xCaxMnO3 single crystal thin film
CN102071399B (en) All-perovskite multiferroic magnetoelectric compound film and preparation method thereof
CN102330055B (en) Method for preparing titanium nitride epitaxial film serving as electrode material
CN112363096A (en) Magnetic sensor preparation method based on magnetic topological insulator film
CN101914751A (en) Preparation method of epitaxy Fe4N film by reactive sputtering with facing targets
Xie et al. Tuning of magnetic properties for epitaxial Y2NiMnO6 thin film: Substrate is crucial
CN104404464B (en) Preparation method of epitaxial lanthanum strontium cobalt oxide film based on radio-frequency reactive sputtering
Perrière et al. Epitaxial growth of non-polar ZnO films on MgO substrate
Wang et al. Microstructure and ferroelectric properties of epitaxial BaTiO3/SrRuO3/SrTiO3 (001) films grown by pulsed laser deposition under high oxygen pressure
CN103469156B (en) A kind of method thicker ferroelectric membranc enforcement stress engineering being used for material modification
CN105296946B (en) A kind of the bismuth niobate calcium thin film material system and preparation method height-oriented with a axles
CN108930017B (en) La0.7Sr0.3MnO3Preparation method of ferromagnetic thin film
CN103276360B (en) Magnetic nanowire array thin film and preparation method thereof
Gao et al. Off-easy-plane antiferromagnetic spin canting in coupled FePt/NiO bilayer structure with perpendicular exchange bias
Rafique et al. Annealing control of magnetic anisotropy and phase separation in CoFe2O4-BaTiO3 nanocomposite films
CN107119261B (en) A kind of huge logic gates alloy film material and its preparation method and application
CN102864414B (en) Method for preparing Fe film with pyramid structure
CN112680705B (en) Epitaxial Pt/gamma' -Fe with room temperature topological Hall effect 4 N/MgO heterostructure and preparation method

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20180911