CN107523796A - A kind of preparation method of the rare-earth transition alloy composite materials with wall - Google Patents

A kind of preparation method of the rare-earth transition alloy composite materials with wall Download PDF

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CN107523796A
CN107523796A CN201710601531.XA CN201710601531A CN107523796A CN 107523796 A CN107523796 A CN 107523796A CN 201710601531 A CN201710601531 A CN 201710601531A CN 107523796 A CN107523796 A CN 107523796A
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rare earth
target
wall
sputtering
layer
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CN107523796B (en
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王可
董硕
凌福进
徐展
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Huaqiao University
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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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering

Abstract

The present invention discloses a kind of preparation method of the rare-earth transition alloy composite materials with wall, rare earth paster and ferrocobalt target are fitted to form combined tessera target, first use magnetron sputtering combined tessera target or ternary alloy three-partalloy target, the thick first layer rare-earth transition alloy firms (laminated magnetic film I) of 20~50nm are grown on substrate, then the thick metal spacing layers of 0.5~2.5nm or oxide spacers (wall) are sputtered, finally continue to sputter combined tessera target or ternary alloy three-partalloy target, the thick second layer rare-earth transition alloy firms (laminated magnetic film II) of 7~15nm are grown on wall, what is obtained is the composite that a kind of same Ferrimagnetic rare-earth transition alloy (TbFeCo or DyFeCo) with wall is formed.The composite property that the preparation method is prepared is stable, and the structure of the composite and vertical magnetoelectronic devices are completely compatible, can be used for as a kind of new magnetoelectronic devices material in vertical spin valve or magnetic tunnel device.

Description

A kind of preparation method of the rare earth-transition alloy composite materials with wall
Technical field
The invention belongs to magnetic spin electronics and Magnetographic Technology Material Field, refers to a kind of perpendicular magnetic spinning electron The preparation method of device composite film material, and in particular to be a kind of rare earth-transition alloy composite materials with wall Preparation method.
Background technology
In recent years, the magnetoelectronic devices such as vertical spin valve and magnetic tunnel-junction are due to device in highdensity advantage and specific surface Part has the characteristics of more preferable heat endurance and turns into the research and development direction of this area.Wherein, based on vertical magnetic tunnel-junction Magnetic memory is considered as one of representative technology of high-density nonvolatile memory of future generation.Free layer in vertical magnetic tunnel-junction Require it is the material with the vertical film surface of easy axle with basic training ergospheres such as reference layers.So find particular easy axis film and its Simple growth method turns into the key for preparing high density magnetoelectronic devices.
Conventional magneto-optic records rare earth-transition race's alloy firm such as TbFeCo and DyFeCo alloy materials due to big vertical Magnetic anisotropy and high heat endurance are good, are currently also widely used in high density magnetoelectronic devices field.This ferrimag is thin Arranged anti-parallel is presented in the magnetic moment of membrane material rare earth elements (Tb or Dy) and transition elements (FeCo) sublattice, causes this kind of A specific compensation point composition is there may be in material, the coercivity corresponding to this compensation point composition alloy film is unlimited Greatly.The rare earth-transition alloy firm composition of the vertical film surface of easy axle is normally at a compensation point composition little Composition Region nearby In domain.The magnetic moment of alloy film material rare earth elements sublattice is more than the magnetic moment then alloy of transition element sublattice during room temperature Film is Nd-rich phase, on the contrary then be rich transitional face.It is larger that vertical magnetoelectronic devices part requires that rare earth-transition race alloy firm has The perpendicular coercive force of difference, to meet that free layer in device (coercivity is small, and the direction of magnetization is easily with outer field direction) and pinning layer (are rectified Stupid power is big, the direction of magnetization be not easy with outer field direction change) etc. difference in functionality layer requirement.Searching has the vertical adverse field of big difference Rare earth-transition alloy film material preparation method, it is direct in current high density magnetic spin electronics device particularly electric current The Novel low power consumption information-storing device fields such as induced magnetization reversion are significant, and are possible to produce huge economic effect Benefit.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the rare earth-transition alloy composite materials with wall, Preparation technology is simple, and the composite property being prepared is stable, and the structure of the composite is completely simultaneous with vertical magnetoelectronic devices Hold, can be used for as a kind of new magnetoelectronic devices material in vertical spin valve or magnetic tunnel device.
In order to reach above-mentioned purpose, solution of the invention is：
A kind of preparation method of the rare earth-transition alloy composite materials with wall, comprises the following steps：
(1) using the combined tessera target or ternary alloy three-partalloy target of rare earth paster and ferrocobalt target composition as magnetron sputtering Target, it is fixed on the sputtering target stand of magnetron sputtering chamber, the rare earth paster is Tb pasters or Dy pasters, the ternary Alloys target is TbFeCo alloy target or DyFeCo alloys targets, the quantity of the combined tessera target middle rare earth paster and is fixed on The rare earth-transition alloy that content of rare earth in the position of the sputtering target stand or the ternary alloy three-partalloy target to be prepared is answered Rare earth elements in condensation material are 25~27.5% (rich rare earths)；
(2) by after cleaning, drying substrate placement be fixed on the chip bench of magnetron sputtering chamber, adjustment target-substrate distance be 4~ 8cm；
(3) sputtering vacuum chamber is reached into vacuum 1 × 10-5Below Pa, the argon gas for being passed through purity >=99.99% are made For working gas, the charge flow rate of argon gas is controlled in the range of 30~100sccm；
(4) under conditions of 0.2~1.0Pa of operating air pressure is sputtered, to 10~30min of the target pre-sputtering；
(5) the chip bench circle of rotation 5~15 per minute is adjusted, chip bench is opened and sputters the baffle plate between target stand, with 1.5~ 6.5W/cm2Sputtering power density sputter the target, sputter rate be 0.1~0.3nm/s, controls sputtering time to cause The thick rare earth-transition alloy firms of 20~50nm are obtained on the substrate, are formed with first layer rare earth-transition alloy firm Substrate；
(6) wall and then on the substrate with first layer rare earth-transition alloy firm is sputtered, when control sputters Between cause growth the wall thickness in 0.5~2.5nm, formation carries wall and first layer rare earth-transition alloy The substrate of film, the wall are metal spacing layer or oxide spacers；
(7) finally continue on the substrate with wall and first layer rare earth-transition alloy firm described in sputtering Target, control sputtering time so that the second layer rare earth-transition alloy firm grown on the wall thickness for 7~ 15nm, obtain the rare earth-transition alloy composite materials with wall.
In step (1), the rare earth paster is in the rare earth paster of purity >=99.9% of isosceles triangle, the iron cobalt Purity >=99.9% of alloys target, each rare earth paster point centered on the center of circle of the ferrocobalt target are attached to the iron On cobalt alloy target, the combined tessera target of sputtering is formed.
In step (2), the substrate is single crystalline Si substrate or typical commercial band thermal oxide layer single crystalline Si substrate.
In step (4), before target described in pre-sputtering, first splash-proofing sputtering metal cushion or oxide delay on the substrate Rush layer, control sputtering time causes the thickness of the metal buffer layer or oxide buffer layer to be 0.5~2.5nm, the metal Cushion is Ta cushions, Ru cushions, Cu cushions, Pd cushions or Pt cushions, and the oxide buffer layer is SiO2Cushion, MgO cushions or Al2O3Cushion.
In step (6), the metal spacing layer is between Ta walls, Ru walls, Cu walls, Pd walls or Pt Interlayer, the oxide spacers are SiO2Wall, MgO walls or Al2O3Wall.
In step (6), splashed on the substrate with first layer rare earth-transition alloy firm by direct current or radio frequency The metal spacing layer is penetrated, passes through oxygen described in radio-frequency sputtering on the substrate with first layer rare earth-transition alloy firm Compound wall.
In step (7), protected on the obtained rare earth-transition alloy composite materials by direct current or radio-frequency sputtering Layer, to prevent oxidation, control sputtering time to cause the thickness of the protective layer to be 2~20nm, the protective layer be Ta protective layers, Ru protective layers, Cu protective layers, Pd protective layers or Pt protective layers.
In Magnetographic Technology Material Field, the magnetic being widely used in the magnetoelectronic devices such as Spin Valve and MTJ is more Film structure, by nonmagnetic spacer layer produce spin-exchange-coupled effect can make adjacent magnetic layers the intensity of magnetization presentation it is parallel or The antiparallel arrangement of person, and magnetic state can be maintained stable in the range of a certain size outfield.
A kind of after adopting the above technical scheme, preparation of the rare earth-transition alloy composite materials with wall of the present invention Method, what is be prepared is the sandwich that a kind of same Ferrimagnetic rare earth-transition alloy with wall is formed, Mainly it is made up of laminated magnetic film I/ walls/laminated magnetic film II.Adjacent with wall is the magnetic of two different-thickness Film layer can pass through fixation, it is necessary to by the preparation of same Ferrimagnetic rare earth-transition alloy material (TbFeCo or DyFeCo) The quantity of target rare earth elements paster and position, or realized using the ternary alloy three-partalloy target of fixed proportion composition.With The magnetic moment direction of the laminated magnetic film of two adjacent different-thickness of wall can be with parallel or arranged anti-parallel, and can be with This stable state is maintained in the range of a certain size outfield.By the thickness for adjusting two laminated magnetic films in the composite Realize different rich phases, using Interlayer Exchange Coupling act on caused by interface wall energy expand two laminated magnetic film magnetization inversion fields Variation, have big difference magnetization inversion field the rare earth-transition alloy composite materials can be directly used for vertical spin valve Or in magnetic tunnel device.
A kind of preparation method of the rare earth-transition alloy composite materials with wall of the present invention, there is preparation method letter The characteristics of single, reproducible and cost is cheap, the composite property that is prepared is stable, the structure of the composite with it is vertical Magnetoelectronic devices are completely compatible, can be used for vertical spin valve or magnetic tunnel-junction device as a kind of new magnetoelectronic devices material In part.
Brief description of the drawings
Fig. 1 is the main unusual Hall Curve of TbFeCo (20nm)/Pd (2nm)/TbFeCo (10nm) composite and small Unusual Hall Curve；
Fig. 2 is the unusual Hall Curve of TbFeCo (20nm)/Pd (1nm)/TbFeCo (7.5nm) composite.
Embodiment
In order to which technical scheme is explained further, the present invention is explained in detail below by specific embodiment State.
Embodiment one
First, the preparation of composite
A kind of preparation method of the rare earth-transition alloy composite materials with wall, comprises the following steps：
(1) it is 1 inch four Tb pasters in the high-purity (purity 99.95%) of isosceles triangle to be attached into radius On the ferrocobalt target of high-purity (purity 99.9%), the combined tessera target of sputtering is formed, each Tb paster is closed with iron cobalt Point is distributed on ferrocobalt target centered on the center of circle of gold target, and the drift angle of Tb pasters is 28 °, a length of 2cm of waist of Tb pasters, thickness For 2mm；
(2) target using combined tessera target as magnetron sputtering, is fixed on the sputtering target stand of magnetron sputtering chamber；
(3) dried after being cleaned by ultrasonic successively with acetone, alcohol, isopropanol to single crystalline Si substrate, by the list after drying and processing Brilliant Si substrates placement is fixed on the chip bench of magnetron sputtering chamber, and adjustment target-substrate distance is 6.5cm；
(4) sputtering vacuum chamber is reached into vacuum for 1 × 10-5Pa, being passed through the argon gas of high-purity, (purity is 99.999%) working gas is used as, controls the charge flow rate of argon gas in 60sccm；
(5) degree that slide valve is closed is adjusted, stablizes sputtering operating air pressure and maintains 0.6Pa, first with 1.48W/cm2 Sputtering power density to the MgO cushions of single crystalline Si substrate radio-frequency sputtering 1nm thickness, sputter rate 0.022nm/s, sputtering Time is 45s, obtains the single crystalline Si substrate with MgO cushions, then to combined tessera target pre-sputtering 20min；
(6) the chip bench circle of rotation 10 per minute is adjusted, chip bench is opened and sputters the baffle plate between target stand, with 5.9W/cm2 Sputtering power density sputtering combined tessera target, sputter rate 0.167nm/s, sputtering time 120s, in single crystalline Si substrate On obtain the thick rare earth-transition alloy firms of 20nm, form the single crystalline Si substrate with first layer rare earth-transition alloy firm；
(7) the d.c. sputtering Pd walls and then on the single crystalline Si substrate with first layer rare earth-transition alloy firm, splash Firing rate rate is 0.125nm/s, sputtering time 16s so that the thickness of the Pd walls of growth is 2nm, and formation carries wall With the single crystalline Si substrate of first layer rare earth-transition alloy firm；
(8) finally sputtering is continued again on the single crystalline Si substrate with wall and first layer rare earth-transition alloy firm Close mosaic target, sputter rate 0.167nm/s, sputtering time 60s so that the second layer rare earth-mistake grown on wall The thickness for crossing alloy firm is 10nm, obtains the rare earth-transition alloy composite materials with wall, is designated as TbFeCo (20nm)/Pd (2nm)/TbFeCo (10nm) composite, its rare earth elements are~26%.
2nd, performance test
The magnetic characteristic of the TbFeCo (20nm)/Pd (2nm)/TbFeCo (10nm) composite is characterized as shown in figure 1, result Show：The magnetic characteristic for sputtering the TbFeCo laminated magnetic films with 10nm thickness and 20nm thickness being prepared is shown as respectively Rich transition and Nd-rich phase, its perpendicular magnetization adverse field are respectively 8.5kOe and 2.8kOe, difference 5.7kOe, wherein, pass through The small unusual Hall go-and-return measurement for only inverting 20nm TbFeCo layers confirms that high level platform is also in main unusual Hall Curve One stable magnetic state.
Therefore, different rich phases is realized by adjusting the thickness of two laminated magnetic films in the composite, it is two different thick The magnetic moment direction of the laminated magnetic film of degree can (4 corresponded in main unusual Hall loop line be flat with parallel or arranged anti-parallel Platform magnetic state), using Interlayer Exchange Coupling act on caused by interface wall energy expand the changes of two laminated magnetic film magnetization inversion fields Change difference, and this stable magnetic state can be maintained in the range of a certain size outfield.
Embodiment two
First, the preparation of composite
A kind of preparation method of the rare earth-transition alloy composite materials with wall, comprises the following steps：
(1) it is 1 inch four Tb pasters in the high-purity (purity 99.95%) of isosceles triangle to be attached into radius On the ferrocobalt target of high-purity (purity 99.9%), the combined tessera target of sputtering is formed, each Tb paster is closed with iron cobalt Point is distributed on ferrocobalt target centered on the center of circle of gold target, and the drift angle of Tb pasters is 28 °, a length of 2cm of waist of Tb pasters, thickness For 2mm；
(2) target using combined tessera target as magnetron sputtering, is fixed on the sputtering target stand of magnetron sputtering chamber；
(3) to typical commercial band 300nm thermal oxides SiO2The single crystalline Si substrate of layer is surpassed with acetone, alcohol, isopropanol successively Dried after sound cleaning, the single crystalline Si substrate placement after drying and processing is fixed on the chip bench of magnetron sputtering chamber, adjusts target base Away from for 6.5cm；
(4) sputtering vacuum chamber is reached into vacuum for 1 × 10-5Pa, being passed through the argon gas of high-purity, (purity is 99.999%) working gas is used as, controls the charge flow rate of argon gas in 60sccm；
(5) degree that slide valve is closed is adjusted, stablizes sputtering operating air pressure and maintains 0.6Pa, to combined tessera target Pre-sputtering 20min；
(6) the chip bench circle of rotation 10 per minute is adjusted, chip bench is opened and sputters the baffle plate between target stand, with 5.9W/cm2 Sputtering power density sputtering combined tessera target, sputter rate 0.167nm/s, sputtering time 120s, in single crystalline Si substrate On obtain the thick rare earth-transition alloy firms of 20nm, form the single crystalline Si substrate with first layer rare earth-transition alloy firm；
(7) the radio-frequency sputtering Pd walls and then on the single crystalline Si substrate with first layer rare earth-transition alloy firm, splash Firing rate rate is 0.125nm/s, sputtering time 8s so that the thickness of the Pd walls of growth is 1nm, formed with wall and The single crystalline Si substrate of first layer rare earth-transition alloy firm；
(8) finally sputtering is continued again on the single crystalline Si substrate with wall and first layer rare earth-transition alloy firm Close mosaic target, sputter rate 0.167nm/s, sputtering time 45s so that the second layer rare earth-mistake grown on wall The thickness for crossing alloy firm is 7.5nm, obtains the rare earth-transition alloy composite materials with wall, is designated as TbFeCo (20nm)/Pd (1nm)/TbFeCo (7.5nm) composite, its rare earth elements are~26%.
2nd, performance test
The magnetic characteristic of the TbFeCo (20nm)/Pd (1nm)/TbFeCo (7.5nm) composite characterizes as shown in Fig. 2 knot Fruit shows：Sputter the magnetic characteristic difference table for the TbFeCo laminated magnetic films with 7.5nm thickness and 20nm thickness being prepared It is now rich transition and Nd-rich phase, its perpendicular magnetization adverse field is respectively 7.6kOe and 1.5kOe, difference 6.1kOe.
Therefore, different rich phases is realized by adjusting the thickness of two laminated magnetic films in the composite, it is two different thick The magnetic moment direction of the laminated magnetic film of degree can be with parallel or arranged anti-parallel (4 platforms corresponded in unusual Hall loop line Magnetic state), using Interlayer Exchange Coupling act on caused by interface wall energy expand the changes of two laminated magnetic film magnetization inversion fields Difference.
Embodiment three
A kind of preparation method of the rare earth-transition alloy composite materials with wall, comprises the following steps：
(1) it is 1 inch four Tb pasters in the high-purity (purity 99.95%) of isosceles triangle to be attached into radius On the ferrocobalt target of high-purity (purity 99.9%), the combined tessera target of sputtering is formed, each Tb paster is closed with iron cobalt Point is distributed on ferrocobalt target centered on the center of circle of gold target, and the drift angle of Tb pasters is 28 °, a length of 2cm of waist of Tb pasters, thickness For 2mm；
(2) target using combined tessera target as magnetron sputtering, is fixed on the sputtering target stand of magnetron sputtering chamber；
(3) dried after being cleaned by ultrasonic successively with acetone, alcohol, isopropanol to single crystalline Si substrate, by the list after drying and processing Brilliant Si substrates placement is fixed on the chip bench of magnetron sputtering chamber, and adjustment target-substrate distance is 6.5cm；
(4) sputtering vacuum chamber is reached into vacuum for 1 × 10-5Pa, being passed through the argon gas of high-purity, (purity is 99.999%) working gas is used as, controls the charge flow rate of argon gas in 60sccm；
(5) degree that slide valve is closed is adjusted, stablizes sputtering operating air pressure and maintains 0.6Pa, first with 0.86W/cm2 Sputtering power density to the Ta cushions of single crystalline Si substrate d.c. sputtering 2nm thickness, sputter rate 0.1nm/s, during sputtering Between be 20s, the single crystalline Si substrate with Ta cushions is obtained, then to combined tessera target pre-sputtering 20min；
(6) the chip bench circle of rotation 10 per minute is adjusted, chip bench is opened and sputters the baffle plate between target stand, with 5.9W/cm2 Sputtering power density sputtering combined tessera target, sputter rate 0.167nm/s, sputtering time 120s, in single crystalline Si substrate On obtain the thick rare earth-transition alloy firms of 20nm, form the single crystalline Si substrate with first layer rare earth-transition alloy firm；
(7) the d.c. sputtering Pd walls and then on the single crystalline Si substrate with first layer rare earth-transition alloy firm, splash Firing rate rate is 0.125nm/s, sputtering time 8s so that the thickness of the Pd walls of growth is 1nm, formed with wall and The single crystalline Si substrate of first layer rare earth-transition alloy firm；
(8) finally sputtering is continued again on the single crystalline Si substrate with wall and first layer rare earth-transition alloy firm Close mosaic target, sputter rate 0.167nm/s, sputtering time 60s so that the second layer rare earth-mistake grown on wall The thickness for crossing alloy firm is 10nm, obtains the rare earth-transition alloy composite materials with wall；
(9) with 0.86W/cm on obtained rare earth-transition alloy composite materials2Sputtering power density d.c. sputtering The Ta protective layers of 2nm thickness, sputter rate 0.1nm/s, sputtering time 20s, to prevent oxidation, obtained rare earth-transition Alloy composite materials are designated as TbFeCo (20nm)/Pd (1nm)/TbFeCo (10nm) composite, its rare earth elements for~ 26%.
Rare earth paster, ferrocobalt target and single crystalline Si substrate in the various embodiments described above are commercially commercially available, It need to only be bought according to purity requirement.
Above-described embodiment and non-limiting product form of the invention and style, the ordinary skill people of any art The appropriate change or modification that member is done to it, it all should be regarded as not departing from the patent category of the present invention.

Claims (7)

  1. A kind of 1. preparation method of the rare earth-transition alloy composite materials with wall, it is characterised in that：Including following step Suddenly：
    (1) target using the combined tessera target or ternary alloy three-partalloy target of rare earth paster and ferrocobalt target composition as magnetron sputtering Material, it is fixed on the sputtering target stand of magnetron sputtering chamber, the rare earth paster is Tb pasters or Dy pasters, and the ternary is closed Gold target is TbFeCo alloy target or DyFeCo alloys targets, the quantity of the combined tessera target middle rare earth paster and is fixed on institute The content of rare earth in the position for sputtering target stand or the ternary alloy three-partalloy target is stated so that the rare earth-transition alloy being prepared is compound Rare earth elements in material are 25~27.5%；
    (2) the substrate placement after cleaning, drying is fixed on the chip bench of magnetron sputtering chamber, adjustment target-substrate distance is 4~8cm；
    (3) sputtering vacuum chamber is reached into vacuum 1 × 10-5Below Pa, the argon gas of purity >=99.99% is passed through as work Make gas, control the charge flow rate of argon gas in the range of 30~100sccm；
    (4) under conditions of 0.2~1.0Pa of operating air pressure is sputtered, to 10~30min of the target pre-sputtering；
    (5) the chip bench circle of rotation 5~15 per minute is adjusted, chip bench is opened and sputters the baffle plate between target stand, with 1.5~ 6.5W/cm2Sputtering power density sputter the target, sputter rate be 0.1~0.3nm/s, controls sputtering time to cause The thick rare earth-transition alloy firms of 20~50nm are obtained on the substrate, are formed with first layer rare earth-transition alloy firm Substrate；
    (6) wall and then on the substrate with first layer rare earth-transition alloy firm is sputtered, control sputtering time makes The thickness for the wall that must be grown carries wall and first layer rare earth-transition alloy firm in 0.5~2.5nm, formation Substrate, the wall is metal spacing layer or oxide spacers；
    (7) finally continue to sputter the target on the substrate with wall and first layer rare earth-transition alloy firm, Sputtering time is controlled so that the thickness of the second layer rare earth-transition alloy firm grown on the wall is 7~15nm, is obtained To the rare earth-transition alloy composite materials with wall.
  2. 2. a kind of preparation method of rare earth-transition alloy composite materials with wall according to claim 1, it is special Sign is：In step (1), the rare earth paster is in the rare earth paster of purity >=99.9% of isosceles triangle, the iron cobalt Purity >=99.9% of alloys target, each rare earth paster point centered on the center of circle of the ferrocobalt target are attached to the iron On cobalt alloy target, the combined tessera target of sputtering is formed.
  3. 3. a kind of preparation method of rare earth-transition alloy composite materials with wall according to claim 1, it is special Sign is：In step (2), the substrate is single crystalline Si substrate or typical commercial band thermal oxide layer single crystalline Si substrate.
  4. 4. a kind of preparation method of rare earth-transition alloy composite materials with wall according to claim 1, it is special Sign is：In step (4), before target described in pre-sputtering, first splash-proofing sputtering metal cushion or oxide delay on the substrate Rush layer, the metal buffer layer is Ta cushions, Ru cushions, Cu cushions, Pd cushions or Pt cushions, the oxidation Thing cushion is SiO2Cushion, MgO cushions or Al2O3Cushion.
  5. 5. a kind of preparation method of rare earth-transition alloy composite materials with wall according to claim 1, it is special Sign is：In step (6), the metal spacing layer is between Ta walls, Ru walls, Cu walls, Pd walls or Pt Interlayer, the oxide spacers are SiO2Wall, MgO walls or Al2O3Wall.
  6. 6. a kind of preparation method of rare earth-transition alloy composite materials with wall according to claim 1, it is special Sign is：In step (6), splashed on the substrate with first layer rare earth-transition alloy firm by direct current or radio frequency The metal spacing layer is penetrated, passes through oxygen described in radio-frequency sputtering on the substrate with first layer rare earth-transition alloy firm Compound wall.
  7. 7. a kind of preparation method of rare earth-transition alloy composite materials with wall according to claim 1, it is special Sign is：In step (7), protected on the obtained rare earth-transition alloy composite materials by direct current or radio-frequency sputtering Layer, to prevent oxidation, control sputtering time to cause the thickness of the protective layer to be 2~20nm, the protective layer be Ta protective layers, Ru protective layers, Cu protective layers, Pd protective layers or Pt protective layers.
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