WO2013151763A1 - Systèmes et procédés pour le dépôt physique en phase vapeur sous vide poussé et ultravide avec un champ magnétique in situ - Google Patents

Systèmes et procédés pour le dépôt physique en phase vapeur sous vide poussé et ultravide avec un champ magnétique in situ Download PDF

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Publication number
WO2013151763A1
WO2013151763A1 PCT/US2013/032359 US2013032359W WO2013151763A1 WO 2013151763 A1 WO2013151763 A1 WO 2013151763A1 US 2013032359 W US2013032359 W US 2013032359W WO 2013151763 A1 WO2013151763 A1 WO 2013151763A1
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WIPO (PCT)
Prior art keywords
sample
magnetic field
film
vacuum chamber
sputtering
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PCT/US2013/032359
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English (en)
Inventor
Cheng Cheng
William E. Bailey
Noah Andrew STURCKEN
Kenneth L. Shepard
Sioan ZOHAR
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The Trustees Of Columbia University In The City Of New York
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Application filed by The Trustees Of Columbia University In The City Of New York filed Critical The Trustees Of Columbia University In The City Of New York
Publication of WO2013151763A1 publication Critical patent/WO2013151763A1/fr
Priority to US14/504,083 priority Critical patent/US20150125622A1/en

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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
    • C23C14/22—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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/50—Substrate holders
    • C23C14/505—Substrate holders for rotation of the substrates
    • 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
    • C23C14/54—Controlling or regulating the coating process
    • C23C14/548—Controlling the composition
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3411—Constructional aspects of the reactor
    • H01J37/345—Magnet arrangements in particular for cathodic sputtering apparatus
    • H01J37/3458—Electromagnets in particular for cathodic sputtering apparatus

Definitions

  • the disclosed subject matter relates to techniques for high and ultra-high vacuum physical vapor deposition with in-situ magnetic field.
  • Well-defined magnetic anisotropy can be used for soft magnetic materials used in a wide range of applications, for example thin-film magnetic recording heads, magnetic random access memory, on-chip magnetic field sensors, and power management devices.
  • it can be useful for magnetic thin films to have enhanced soft magnetic properties. Reduced coercive field (He) and enhanced magnetic permeability ( ⁇ ) along particular axes of the devices can be desirable.
  • Techniques for inducing uniaxial or unidirectional anisotropy in an alloy thin film, either amorphous or polycrystalline can include deposition or postannealing in the presence of a magnetic field.
  • Deposition in the presence of a magnetic field can save a processing procedure and can be useful for multilayer devices or device structures that are temperature-sensitive.
  • the magnetic field applied during deposition can be applied by a permanent magnet fixed to a sample holder, and the entire sample holder-magnet assembly can rotate during deposition, which can be by sputtering, evaporative deposition, or other physical vapor deposition process. It can be difficult to change the direction of anisotropy in different layers of a multilayer device.
  • An exemplary method can include introducing a sample into the vacuum chamber.
  • the sample can be rotated, and a magnetic field can be applied that rotates synchronously with the rotating sample.
  • Atoms can be deposited onto the sample while the sample is rotating with the magnetic field.
  • the magnetic field can rotate synchronously with the sample at a first phase difference.
  • the magnetic field can be generated by applying sinusoidal currents through first and second pairs of coils wrapped around a quadrupole electromagnet core, where the sinusoidal current in the first pair of coils is ⁇ /4 out of phase from the sinusoidal current in the second pair of coils.
  • a second magnetic field can be applied that rotates synchronously with the sample at a second phase difference that is different than the first phase difference.
  • Atoms can be deposited onto the sample while the sample is rotating with the second magnetic field to cause a portion of the atoms to be deposited on the sample as a second layer of firm while the second magnetic field induces magnetic anisotropy in the second film.
  • the applied magnetic field that rotates synchronously with the sample at a first phase difference can be adjusted in-situ to have a second phase difference.
  • a second magnetic field that rotates synchronously with the sample at a second phase difference can be applied after applying the first magnetic field.
  • the first phase difference and the second phase difference can be ⁇ /2 out of phase.
  • the film layers deposited in the magnetic fields with the first and second phase differences can thus have orthogonal anisotropy.
  • the application of a magnetic field and atom depositing procedure can be repeated in order to deposit successive layers of film.
  • the system can use one of direct current (DC) magnetron sputtering, radio frequency (RF) sputtering, or ion beam sputtering (IBS), ion beam deposition (IBD), or electron beam evaporation.
  • DC direct current
  • RF radio frequency
  • IBS ion beam sputtering
  • IBD ion beam deposition
  • electron beam evaporation In some embodiments, the frequency of the rotation can be 1 revolution per second or less.
  • the sample can be centered in the vacuum chamber.
  • the atoms can be sputtered from at least one target disposed in the vacuum chamber.
  • the targets can be symmetrically arranged.
  • the targets can also be inclined towards the sample.
  • An exemplary system can include a vacuum chamber.
  • a physical vapor deposition device can be disposed in the vacuum chamber.
  • a sample holder can be disposed in the vacuum chamber.
  • a motor can be configured to rotate the sample holder.
  • a magnetic field source can be adapted to rotate a magnetic field synchronously with the sample holder.
  • the magnetic field source can be a quadrupole electromagnet.
  • the quadrupole electromagnet can include a metallic core, a first pair of coils, and a second pair of coils.
  • the metallic core can include a circular core ring and first, second, third, and fourth poles equidistantly spaced around the interior of the circular core ring. Each of the poles can protrude towards the center of the circular core ring.
  • the first pair of coils can include a first coil wrapped around the metallic core between the first and fourth poles and a second coil wrapped around the metallic core between the second and third poles.
  • the second pair of coils can include a third coil wrapped around the metallic core between the first and second poles and a fourth coil wrapped around the metallic core between the third and fourth poles.
  • a motor controller can be configured to control the motor.
  • At least one power supply can be configured to generate alternating current (AC) currents through the first and second pairs of coils.
  • a data acquisition device can be connected to the motor controller and the at least one power supply to synchronize the rotating of the magnetic field and the rotating of the sample holder.
  • the quadrupole electromagnet can be positioned to be centered with the sample holder. Thus a uniform in-plane magnetic field can exist across the sample holder.
  • the sample holder can be configured such that a sample placed thereon will face the bottom of the vacuum chamber.
  • the quadrupole electromagnet can be configured to generate a magnetic field that rotates synchronously with the sample holder at a phase difference.
  • the physical vapor deposition device can be one of a DC magnetron sputtering system, a RF sputtering system, an IBS system, and IBD system, or an electron beam evaporation system.
  • the physical vapor deposition device can be a sputtering device adapted to sputter atoms from at least one sputter target disposed in the vacuum chamber.
  • FIG. 1 shows an exemplary system for vacuum film depositing in accordance with some embodiments of the disclosed subject matter.
  • FIG. 2 shows an exemplary core of an electromagnet in accordance with some embodiments of the disclosed subject matter.
  • FIG. 3 shows an exemplary electromagnet in accordance with some embodiments of the disclosed subject matter.
  • FIG. 4 shows (a) an exemplary schematic of the vector sum of two orthogonal magnetic fluxes at the center point of an electromagnet and (b) an exemplary graph of the correspondence between the sputtering field and the applied AC currents in accordance with some embodiments of the disclosed subject matter.
  • FIG. 5 shows an exemplary graph of the linear relationship between the applied voltage control and measured magnitude of the rotating magnetic field in accordance with some embodiments of the disclosed subject matter.
  • FIG. 6 shows an exemplary alignment of a sample on a sample holder in accordance with some embodiments of the disclosed subject matter.
  • FIG. 7 shows (a) an exemplary BH loop of a first sample in a first set, (b) an exemplary BH loop of a second sample in a first set, (c) an exemplary BH loop of a first sample in a second set, and (d) an exemplary FMR Kittel relation of the first sample in the second set in accordance with some embodiments of the disclosed subject matter.
  • FIG. 8 shows an exemplary graph of the change of ferromagnetic resonance field H 0 at 4 GHz, as the angle a between the FMR bias field H B and the sample reference axis R varies from 0° to 180° in accordance with some embodiments of the disclosed subject matter.
  • FIG. 9 shows an exemplary graph of the change of ferromagnetic resonance field H 0 at
  • FIG. 10 shows an exemplary method for depositing a film in an evacuated vacuum chamber in accordance with some embodiments of the disclosed subject matter.
  • the disclosed subject matter provides techniques for high and ultra-high vacuum physical vapor deposition with in-situ magnetic field.
  • a magnetic field can be applied across a rotating sample during physical vapor deposition in order to deposit a magnetically anisotropic film on the sample.
  • the magnetic field can rotate synchronously with the rotating sample. There can he a phase difference between the rotating sample and the rotating magnetic field.
  • the anisotropy of a layer of film can be adjusted by adjusting the phase difference.
  • a rotating field can be generated by applying alternating current (AC) currents to the coils of an electromagnet without moving the electromagnet.
  • the phase difference between the rotating magnetic field and the rotating sample can be adjusted by adjusting the AC currents in the coils without moving the electromagnet.
  • AC alternating current
  • the system 100 can include a vacuum chamber 101.
  • the vacuum chamber 101 can have a base pressure up to 10 "6 torr, although higher and lower base pressures are contemplated within the scope of the disclosed subject matter depending on the particular application.
  • a physical vapor deposition device (not pictured) can be adapted to deposit atoms onto the surface of a sample.
  • the physical vapor deposition device can be a sputtering device, an ion beam deposition system, an electron-beam evaporation system, or any other suitable physical vapor deposition system.
  • a sputtering device can include a direct current (DC) magnetron sputtering system, a radio frequency (RF) sputtering system, an ion beam sputtering (IBS) system, or any other suitable sputtering system.
  • DC direct current
  • RF radio frequency
  • IBS ion beam sputtering
  • at least one sputter target 102 can be disposed in the vacuum chamber 101.
  • a sputtering device (not pictured) can be adapted to sputter atoms from at least one sputter target 102.
  • a sample holder 104 can be disposed in the vacuum chamber 101.
  • a motor 105 can be configured to rotate the sample holder 104.
  • a magnetic field source 103 can be adapted to rotate a magnetic field synchronously with the sample holder 104.
  • the magnetic field source 103 can be a quadrupole electromagnet.
  • the quadrupole electromagnet can be custom designed to meet the specifications of the vacuum film depositing system 100.
  • the magnetic field source 103 can include a metallic core.
  • the metallic core can include a circular core ring 103 a and first, second, third, and fourth poles 103b.
  • the quadrupole electromagnet can be well fitted in the vacuum chamber 101, leaving enough space at the interior of the metallic core ring 103 a for accommodating the sample holder 104.
  • the power of the electromagnet can be suited for the desired magnetic field strength, depending on the magnitude of the magnetic anisotropy desired in the film.
  • the poles 103b can be equidistantly spaced around the interior of the circular core ring 103a. Each of the poles 103b can protrude towards the center of the circular core ring 103 a.
  • the magnetic field source 103 can include coils.
  • the magnetic field source 103 can include a first pair of coils 103 c and a second pair of coils 103 d.
  • the first pair of coils 103c can include a first coil wrapped around the metallic core 103a between p4 and i and a second coil wrapped around the metallic core 103a between p2 and p3.
  • the second pair of coils 103d can include a third coil wrapped around the metallic core 103a between pi and p2 and a fourth coil wrapped around the metallic core 103 a between p3 and p4.
  • the motor 105 can be controlled by a motor controller 111.
  • At least one power supply can generate AC currents through the pairs of coils 103c and 103d.
  • a first power supply 113 and a second power supply 114 can generate AC currents through the first pair of coils 103 c and the second pair of coils 103 d, respectively.
  • a data acquisition device 112 can be connected to the motor controller 111 and the power supplies 113 and 114 to synchronize the rotating of the magnetic field and the sample holder 104.
  • one or more of the motor controller 111, the data acquisition device 112, the first power supply 113, or the second power supply 114 can be connected to a personal computer 120.
  • the magnetic field source 103 can be a quadrupole electromagnet, as described above, positioned to be centered with the sample holder 104.
  • a substantially uniform magnetic field can thus be applied across the sample holder 104.
  • the magnitude of the magnetic field can vary depending on the magnitude of the magnetic anisotropy desired in the film.
  • the magnetic field can be in the range of 0 - 300 Oe, as illustrated in FIG. 5, discussed below.
  • the sample holder 104 can be configured such that a sample placed thereon will be centered in the vacuum chamber. Atoms can be sputtered from targets 102 disposed at the bottom of the vacuum chamber 101.
  • the sputtering device can be a DC magnetron sputtering system, a RF magnetron sputtering system, or an IBS system.
  • the targets 102 can be mounted on sputtering guns (not pictured) and at least one power supply (not pictured) can be attached to the sputtering guns.
  • an Advanced Energy MDX 500 Magnetron Drive can be used as the power supply and a Kurt J. Lesker Torus 2 Magnetron Sputtering Source can be used as the sputtering gun for a DC magnetron sputtering system.
  • the sputter targets 102 can be arranged in any suitable arrangement.
  • four targets 102 can be symmetrically arranged at the bottom of the vacuum chamber 101.
  • the four targets 102 can be arranged to have four-fold rotational symmetry, with the symmetry axis coinciding with the shaft connecting the sample holder 104 and the motor 105.
  • the targets 102 can be inclined towards the sample holder 104.
  • the sample holder 104 can be configured such that a sample placed thereon will face the bottom of the vacuum chamber 101.
  • a sample 106 can be placed on a sample holder 104.
  • the sample holder 104 can have at least one alignment pin 107.
  • four alignment pins 107 can be symmetrically arranged on sample holder 104, and the first, second, third, and fourth alignment pins 107 can be referred to as al, a2, a3, and a4, respectively.
  • a clip 108 can hold the sample 106 onto the sample holder 104.
  • the sample 106 can be placed on the sample holder 104 such that the axis of rotation intersects the sample 106.
  • the sample 106 can be placed on the sample holder 104 such that the axis of rotation does not intersect the sample 106.
  • the axis of rotation can coincide with the center of the sample holder 104, and the sample 106 can be placed away from the center of the sample holder 104 such that the axis of rotation does not intersect the sample 106.
  • the incidence angle of the adatoms from an individual target 102 can have an asymmetric distribution across the surface of the sample 106. This asymmetric distribution can be due to the target 102 having an inclination angle with respect to the surface of the sample 106.
  • Physical rotation of the sample holder 104 can enhance the homogeneity of the sputtered film. The rotation can be controlled by the combination of a motor 105 and a motor controller 111.
  • the magnetic field source 103 can be fixed to the chamber walls and remain stationary. The magnetic field generated by magnetic field source 103 can rotate by programming AC currents ramiing through the coils 103 c and 103d.
  • the data acquisition device 112 can be a National Instruments multiple 10 data acquisition device (NI6212) configured to communicate between the power supplies 113 and 114 and the motor controller 111 and to synchronize the rotating magnetic field with the physical rotation of the sample holder 104.
  • NI6212 National Instruments multiple 10 data acquisition device
  • the motor 105 can be any suitable motor.
  • the motor 105 can be a stepper motor.
  • the motor 105 can be a Lin Engineering 5718M high torque stepper motor.
  • the motor 105 can be installed on top of the vacuum chamber 101.
  • the motor 105 can be installed on top of the vacuum chamber 101 by a 2 3/4" conflat flange (CF) magnetically-coupled rotary feedthrough (Thermionics FRMRE-275-38 MS- EDR) which can be mounted on a linear translator with 2" of z travel (Thermionics Z-B275C- T275T- 1.53-2).
  • the sample holder 104 can be attached to the motor 105 by a shaft.
  • the motor controller 111 can be a programmable Thermionics TMC 1-C motor controller configured to control the motor 105 at 800 steps per cycle with a designated angular speed.
  • the motor controller 111 can have a plurality of user input outputs (I/Os) that can be digital or analog.
  • I/Os user input outputs
  • the motor controller 111 can have 11 I Os.
  • One of the I Os can be programmed to change the digital output level between high and low after a desired number of steps, sending out a square wave with a corresponding number of rising edges for each full rotation of the motor 105.
  • one of the I/Os can be programmed to change the digital output level between high and low every 5 steps, sending out a square wave with 80 rising edges for each full rotation of the motor 105.
  • the square wave which can also be referred to as a pulse train, can be sent to the data acquisition device 112.
  • the clock rate of the data acquisition device 112 can be controlled by the motor controller 111, and the clock rate can be proportional to the rotation speed of the sample holder 104.
  • 80 clock pulses can occur for each rotation of the motor 105.
  • the magnetic field source 103 can apply a magnetic field.
  • the magnetic field source 103 can be a quadrupoie electromagnet, as described above.
  • the electromagnet can have a metallic core.
  • the metallic core can be made of any soft ferromagnetic metal with high permeability and low hysteresis.
  • the metal can be an alloy, such as an alloy based on iron (Fe), cobalt (Co), or nickel (Ni).
  • the core can be a silicon (Si) steel (Fe) core, such as 4% Si Fe from Scientific Alloys.
  • the pairs of coils 103 c and 103 d can each have a plurality of turns of wire.
  • the wire can be coated in an insulator.
  • each coil in the pairs of coils 103 c and 103 d can have 250 turns of 14 gauge copper (Cu) wire coated with polyamideimde (NEMA MW 35-C, class 200).
  • the magnetic field source can be suspended from the top of vacuum chamber 101 and fixed as an integrated part of the system 100.
  • the magnetic field source 103 can be centered on the sample holder 104 to form a uniform in-plane magnetic field across the sample holder 104.
  • the power supplies 113 and 114 can each be a Kepco bipolar operational power supply (BOP 20-20M).
  • the power supplied 113 and 114 can be connected to the pairs of coils 103c and 103d by a 2 3/4" CF electrical feedthrough on the vacuum chamber 101.
  • the power supplies 113 and 114 can be controlled by signals from output channels of the data acquisition device 112.
  • Magnetic flux "a” can be generated by the first pair of coils 103c, while flux “b” can be generated by the second pair of coils 103d.
  • the flux flowing through poles p2 5 p4 can be a + b, and the flux through pi, p3 can be a - b.
  • the magnetic field can be determined by the vector sum of a + b and a - b, as illustrated in FIG. 4(a).
  • 80 evenly spaced sampling points can be defined on each of the two AC curves il and i2. These two sets of values can be sent to the data acquisition device 112 at the clock rate, which is determined by the motor controller 111. Since there are 80 sampling points for one period of the magnetic field rotation and 80 digital pulses for one rotation of the motor 105, the magnetic field can rotate synchronously with the sample 106. Note that a different number of sampling points can be chosen based on the number of digital pulses representing one full rotation of the motor 105, as described above. To change the angle between the sample reference axis and the magnetic field, the initial phase ⁇ of the AC current curve sin(aX + ⁇ f>)xcos(G>t + ) can b e adjusted.
  • the data acquisition device 112 can be programmed directly or can be programmed by an attached computer 120.
  • a different choice for the initial phase ⁇ can make the magnetic field start rotating at a different angle ⁇ .
  • the linear relationship between the applied voltage control from the data acquisition device 112 and the measured magnitude of the rotating magnetic field is shown.
  • the sample rotation speed can be set to 0.25 RPM and the magnetic field strength can be measured at the sample holder 104 in the x-direction using a Gauss probe.
  • the Gauss probe can be a LakeShore 421 Gauss probe.
  • the input voltage from the data acquisition device 112 can be varied, e.g., from 0 V to 4 V.
  • the measured field strength can show sinusoidal variation with a period of 4 seconds.
  • the amplitudes of the measured sinusoidal curves are shown in FIG. 5.
  • a linear dependence can be observed between the magnetic field amplitude and the amplitude of the AC voltage output of the power supplies.
  • a Ta 3 nm/Co9 1 . 5 Zr 4 .oTa 4 .5 200 nm/Si0 2 10 nm film can be deposited on 1 cm by 1 cm Si/thermal Si0 2 sample 106 using the system 100 described above with a magnetic field strength of 50 Oe.
  • the 3 nm tantalum (Ta) layer is the seed layer to improve adhesion and homogeneity of the film, and the top silicon dioxide (Si0 2 ) layer protects the metallic film from oxidation.
  • the ferromagnetic cobalt (Co)-zirconium (Zr)- Ta layer (Co9 1 . 5 Zr 4 ,oTa 4 , 5 200 nm) can be DC magnetron sputtered onto the sample 106, with
  • the alignment of the sample 106 with the sputtering field is demonstrated in FIG. 6.
  • one edge of the sample 106 can be chosen to be the reference axis for the sample 106.
  • the reference axis can be aligned with the alignment pins 107 labeled a2 and a4 in the ⁇ -direction, which can be the default direction of the magnetic field when the initial phase is set to zero.
  • the initial phase ⁇ can be set to any suitable value to change the relative angle between the sputtering field direction and the sample reference axis.
  • FIGS. 7(a) and (b) hysteresis (BH) loops of exemplary films are shown.
  • the film was deposited with the sample holder 104 and the magnetic field remaining stationary during sputtering (no rotation).
  • FIG. 7(b) the film was deposited with the sample holder 104 and the magnetic field rotating synchronously during sputtering.
  • FIGS. 7(c) and (d) the BH loop and ittel relation of a ferromagnetic resonance (FMR) field of an exemplary film are shown.
  • FMR ferromagnetic resonance
  • Ta 3 nm/Co9 1 , 5Zr4.oTa4.5 200 nm/Si0 2 10 nm films can be deposited on 1 cm by 1 cm Si/thermal Si0 2 sample 106 using the system 100 described above with a magnetic field strength of 50 Oe and with phase differences.
  • the magnetic properties of the exemplary films can be studied with a BH loop tracer and parallel-condition FMR spectra.
  • the BH loop and Kittel relation of the FMR field and frequency for the exemplary film with — 0° are shown in FIGS. 7 (c) and (d), respectively.
  • the easy axis of the film was measured by the BH loop tracer to be parallel with the sample 106 reference axis, along which the sputtering field was applied.
  • the anisotropy field H K can be 21.5 Oe.
  • the second set of samples can be deposited at a different period of the life time of the Co ⁇ .sZr ⁇ oTa ⁇ s target 107, and a slight change in the sputtered film composition can occur compared with the first set of samples.
  • There can be a phase offset of 8.8° which can be the result of the error in alignment when loading the samples 106 into the sample holder 104.
  • an exemplary method for depositing a film in an evacuated vacuum chamber 101 is disclosed.
  • the exemplary method can include introducing the sample 106 into the vacuum chamber 101, as described above (1001).
  • the sample 106 can be rotated, as described above (1002).
  • a magnetic field can be applied that rotates synchronously with the rotating sample 106, as described above (1003).
  • Atoms can be deposited onto the sample 106 while the sample 106 is rotating with the magnetic field to thereby cause a portion of the atoms to be deposited on the sample 106 as the film while the magnetic field induces magnetic anisotropy in the film, as described above (1004).
  • the application of the magnetic field (1003) and atom depositing procedure (1004) can be repeated to deposit successive layers of film, as described above (1005).
  • the magnetic field can rotate synchronously with the sample 106 with a phase difference, as described above (1003).
  • the rotating of the magnetic field can be achieved by applying sinusoidal AC currents through first and second pairs of coils 103c and 103d wrapped around a quadrupole electromagnet acting as the magnetic field source 103, as described above (1003).
  • the sinusoidal current in the first pair of coils 103c can be ⁇ /4 out of phase from the sinusoidal current in the second pair of coils 103d (1003).
  • the sinusoidal currents in the coils could have any suitable phase difference to apply a rotating magnetic field (1003).
  • a second magnetic field that rotates synchronously with the sample 106 at a second phase difference can be applied, as described above (1005).
  • the first phase difference and the second phase difference can be ⁇ /2 out of phase, thereby depositing successive layers with orthogonal anisotropy, as described above (1005).
  • the first and second phase differences can be any desired value out of phase, including an arbitrary value, thereby depositing successive layers with anisotropies that can form any angle, including an arbitrary angle, according to the phase difference (1005).
  • the application of the magnetic field (1003) and atom depositing procedure (1004) can be repeated multiple times to deposit multiple successive layers of film, as described above (1005).
  • a magnetic field can be applied that rotates synchronously with the sample 106 at a desired phase difference that is different than the phase difference of the preceding layer (1005).
  • Atoms can be deposited while the sample 106 is rotating with the magnetic field to thereby cause a portion of the atoms to be deposited on the sample 106 as a film layer with different anisotropy than the preceding layer, as described above (1005).
  • the atoms can be deposited by DC magnetron sputtering, RF sputtering, IBS, IBD, electron beam evaporation, or any other suitable film deposition process, as described above (1004).
  • atoms can be sputtered from at least one target 102 disposed in the vacuum chamber 101 while the sample 106 is rotating with the magnetic field to thereby cause a portion of the atoms to be deposited on the sample 106 as the film while the magnetic field induces magnetic anisotropy in the film, as described above (1004).
  • the rotating of the sample 106 and the magnetic field can have a frequency up to 1 revolution per second (1002).

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  • Electromagnetism (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

La présente invention porte sur des systèmes et sur des procédés qui permettent le dépôt physique en phase vapeur sous vide poussé et ultravide avec un champ magnétique in situ. Un procédé illustratif de dépôt d'un film dans une chambre à vide mise sous vide peut comprendre l'introduction d'un échantillon dans la chambre à vide. L'échantillon peut être amené à tourner. Un champ magnétique peut être appliqué, celui-ci tournant de façon synchronisée avec l'échantillon qui tourne. Des atomes peuvent être déposés sur l'échantillon pendant que celui-ci tourne avec le champ magnétique afin de déposer un film alors que le champ magnétique induit une anisotropie magnétique dans le film.
PCT/US2013/032359 2010-04-01 2013-03-15 Systèmes et procédés pour le dépôt physique en phase vapeur sous vide poussé et ultravide avec un champ magnétique in situ WO2013151763A1 (fr)

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US12024568B2 (en) 2013-09-13 2024-07-02 Cornell University Treatment of brain cancers using central nervous system mediated gene transfer of monoclonal antibodies

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EP0801421B1 (fr) * 1996-03-25 2003-09-17 United Microelectronics Corporation Procédé pour la croissance de silicium à grains hémisphériques
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US12024568B2 (en) 2013-09-13 2024-07-02 Cornell University Treatment of brain cancers using central nervous system mediated gene transfer of monoclonal antibodies

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