CN112048704A - Integrated processing equipment for ultrathin multilayer film and application method - Google Patents

Integrated processing equipment for ultrathin multilayer film and application method Download PDF

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CN112048704A
CN112048704A CN202010812789.6A CN202010812789A CN112048704A CN 112048704 A CN112048704 A CN 112048704A CN 202010812789 A CN202010812789 A CN 202010812789A CN 112048704 A CN112048704 A CN 112048704A
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cavity
magnetron sputtering
vacuum
characterization
regulation
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CN112048704B (en
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赵巍胜
程厚义
艾梅尔
张学莹
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Hefei Innovation Research Institute of Beihang University
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Hefei Innovation Research Institute of Beihang University
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Priority to PCT/CN2021/080604 priority patent/WO2022033026A1/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54Controlling or regulating the coating process

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
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  • Organic Chemistry (AREA)
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Abstract

The invention discloses integrated processing equipment and an application method of an ultrathin multilayer film, wherein the integrated processing equipment comprises: an ultrahigh vacuum multi-target magnetron sputtering device comprising a magnetron sputtering cavity; the rapid sample introduction chamber comprises a rapid sample introduction cavity, the rapid sample introduction chamber is in sealing connection with the magnetron sputtering cavity through a first gate valve, and various accessory accessories are connected outside the rapid sample introduction cavity; the regulation and characterization device comprises a regulation and characterization cavity which is internally provided with a high-temperature sample rack, the regulation and characterization cavity is communicated with the rapid sample injection cavity through a switching cavity, and the regulation and characterization cavity is also respectively connected with a magnetic characterization system and an ultrahigh vacuum sample transfer rod. The integrated processing equipment can deposit the ultrathin multilayer film and carry out high-temperature magnetic field annealing and magnetic measurement on the ultrathin multilayer film without a vacuum interconnection system or destroying a vacuum environment, can realize preparation, layered in-situ regulation and characterization of the ultrathin multilayer film, and has the characteristics of low cost and high operation efficiency.

Description

Integrated processing equipment for ultrathin multilayer film and application method
Technical Field
The invention belongs to the field of preparation and characterization of spin electron films, and particularly relates to integrated processing equipment and an application method of an ultrathin multilayer film.
Background
However, leakage current generated by tunneling effect in a semiconductor causes overlarge power consumption and poor data stability of a traditional microelectronic device, Moore's law meets a technical bottleneck which is difficult to exceed, and a spintronic information device is considered as one of key technologies for overcoming the power consumption bottleneck and has important significance for building an ultra-low power consumption integrated circuit in the post-Moore era.
The magnetic random access memory has the characteristics of non-volatility, low power consumption, unlimited reading and writing and the like, and the spin transfer torque-based magnetic random access memory (STT-MRAM) achieves better compromise in the aspects of speed, area, writing times and power consumption, so the STT-MRAM is considered to be an ideal device for constructing the next-generation non-volatile cache by the industry. The Magnetic Tunnel Junction (MTJ) is a core storage part of the STT-MRAM, mainly composed of two ferromagnetic layers and a tunneling barrier layer, the film thickness of each layer is usually nanometer magnitude, the classic structure of the magnetic tunnel junction is a CoFeB/MgO/CoFeB system, specifically, the two ferromagnetic layers include a reference layer 1 with a fixed and unchangeable magnetization direction and a free layer 2 with a magnetization direction which can be the same as or opposite to that of the reference layer 1. When the magnetization direction of the free layer 2 is parallel to the reference layer 1, the MTJ assumes a low resistance state, whereas the MTJ assumes a high resistance state. Such different resistance states may be used to represent "0" and "1" of binary data. It is therefore desirable to deposit ultra-thin multilayer films and then build the basic structural magnetic tunnel junctions of the magnetic memory by processing into devices.
The preparation of the ultrathin multilayer film is mainly prepared by a physical vapor deposition method, and the current mainstream physical vapor deposition equipment mainly comprises magnetron sputtering, molecular beam epitaxy, pulse laser deposition and the like, wherein the magnetron sputtering equipment is widely used in industrial fields due to the advantages of high deposition rate, small substrate damage, small temperature rise and the like. After the film is prepared, the magnetic layer is generally required to be measured, a magneto-optical Kerr test system or a vibration sample magnetometer and the like are generally used for measurement, and the magneto-optical Kerr test system is high in test speed and low in cost and is widely used in various scientific research institutions. The film regulation and control equipment mainly comprises two methods, namely ion irradiation and vacuum annealing, wherein the ion irradiation changes the element distribution of the multilayer film through ion bombardment, and the vacuum annealing regulates the element distribution of the film by utilizing the thermal motion of molecules. However, the number of cathodes contained in a single cavity of the conventional magnetron sputtering device is small, the preparation of various film layers is difficult to realize, and the general technological process needs to be switched among a plurality of devices, so that the efficiency is reduced, and the layered regulation and characterization are difficult to realize.
At present, the preparation, regulation and characterization method of the ultrathin multilayer film is mainly carried out by separation equipment, namely, firstly, thin film deposition equipment is used for depositing the thin film, then vacuum breaking is carried out, a sample is taken out, and then, the regulation and characterization equipment for the characteristics of the thin film is used for regulating and characterizing the characteristics of the thin film. This method requires a plurality of devices to be matched, and because some properties of the sample need to be measured in the atmosphere, a protective layer needs to be deposited to protect the magnetic layer of the core, etc., the design of the film layer is complicated, and the influence of the protective layer on the relevant characteristics cannot be avoided. And the method characterizes the characteristics of the whole multilayer film, the concerned film layer cannot be characterized independently, and the system needs a plurality of devices to be matched, so the cost is high.
In another method, the preparation, regulation and control of the ultrathin multilayer film and the characterization equipment are connected through a vacuum interconnection system, a sample can be transmitted in a plurality of cavities and equipment, and the in-situ regulation and control and measurement of the ultrathin multilayer film can be carried out under the condition of not damaging a vacuum environment. However, the method needs to be matched with a complex vacuum interconnection and a complex sample transmission system, so that the design cost of the system is increased, meanwhile, the reliability and the operation efficiency of the system are reduced due to the complex design, and meanwhile, the problems of system compatibility and the like are also involved.
Disclosure of Invention
In view of the above, the present invention provides an integrated processing apparatus for an ultra-thin multi-layer film and an application thereof, wherein the integrated processing apparatus integrates functions of preparation, regulation and characterization of the ultra-thin multi-layer film, and can realize layered in-situ regulation and characterization of the ultra-thin multi-layer film without a vacuum interconnection system or breaking a vacuum environment, so as to solve the above problems.
In order to achieve the purpose, the invention adopts the following technical scheme:
the present invention firstly provides an integrated processing apparatus of an ultrathin multilayer film, the integrated processing apparatus including:
the ultrahigh vacuum multi-target magnetron sputtering device comprises a magnetron sputtering cavity;
the rapid sample introduction chamber comprises a rapid sample introduction cavity, the rapid sample introduction cavity is in sealing connection with the magnetron sputtering cavity flange through a first gate valve and is used for sample introduction, and an air inlet valve is arranged outside the rapid sample introduction cavity;
the regulation and characterization device comprises a regulation and characterization cavity which is internally provided with a high-temperature sample rack, the regulation and characterization cavity is communicated with the rapid sample injection cavity through a switching cavity, and the regulation and characterization cavity is also respectively connected with a magnetic characterization system and an ultrahigh vacuum sample transfer rod.
Further, a vacuum sample holder, a second vacuum measurement system, a second vacuum obtaining system and a magnetron sputtering cathode are respectively connected to the outside of the magnetron sputtering cavity in a flange sealing manner, a first observation window is arranged on the magnetron sputtering cavity, the first observation window is formed by sealing a quartz observation window and the magnetron sputtering cavity through a flange, and a plurality of sealed reserved flange openings are also arranged on the magnetron sputtering cavity;
and the bottom of the side surface of the magnetron sputtering cavity is provided with a mounting hole for fixing the magnetron sputtering cavity.
Further, the second vacuum measuring system is composed of a three-stage vacuum gauge, wherein the three-stage vacuum gauge comprises a vacuum film gauge, a UHV ion gauge and a residual gas analyzer RGA;
the second vacuum obtaining system is in sealing connection with the magnetron sputtering cavity through a second gate valve, the second vacuum obtaining system is a three-stage vacuum pump set, and the three-stage vacuum pump set comprises a mechanical pump, a molecular pump and a cryogenic pump.
Furthermore, twelve magnetron sputtering cathodes with different angles are arranged on the same spherical surface and face the magnetron sputtering sample position in the magnetron sputtering cavity.
Further, the magnetron sputtering cavity is provided with a film thickness measuring device for realizing film thickness monitoring.
Further, the magnetron sputtering device further comprises a power supply system, and the power supply system comprises:
the switcher is connected with the magnetron sputtering cathode;
the direct current power supply is connected to the switcher through a direct current cable;
and the radio frequency power supply is connected into the switcher through a matcher.
Furthermore, but the rapid sampling cavity is inside to be equipped with lifting sample frame, the rapid sampling cavity still is equipped with the second observation window outward.
Further, the first vacuum obtaining system is a two-stage vacuum pump group, and the two-stage vacuum pump group comprises a mechanical pump and a molecular pump;
the first vacuum measurement system is a full-range vacuum gauge.
Furthermore, the high-temperature sample rack adopts a radiation heating mode, and a temperature sensor is arranged on the high-temperature sample rack;
the magnetic characterization and regulation system comprises:
the magnetic detection light path component is arranged at the upper end of the regulation and control and characterization cavity and comprises an input light path and an output light path;
the glass flange port is used for allowing the magnetic detection light path to enter the regulation and control and characterization cavity and is sealed at the upper end of the regulation and control and characterization cavity;
the first in-plane magnet and the second in-plane magnet are positioned in the regulation and characterization cavity and are oppositely arranged, the first in-plane magnet and the second in-plane magnet both comprise a left magnetic pole, a right magnetic pole and an auxiliary coil, the coils of the two magnetic poles are connected in series, and a Hall probe is arranged;
be located regulation and control and sign cavity and relative first perpendicular magnet and the perpendicular magnet of second that sets up, first perpendicular magnet is located regulation and control and sign cavity with between the magnetic detection light path, just be equipped with the hole that supplies the magnetic detection light path to pass through on the first perpendicular magnet, first perpendicular magnet with the perpendicular magnet of second is fixed air gap broken yoke magnet.
The invention also provides an application method of the integrated processing equipment, which comprises the following steps:
loading a substrate to be prepared into the rapid sample introduction chamber, and then sending the substrate into the magnetron sputtering cavity to deposit a magnetic multilayer film;
the sample after the magnetic multilayer film is deposited is transmitted into a regulation and control and characterization cavity to carry out magnetic characterization, if the magnetism does not meet the requirement, the sample can be subjected to ultrahigh vacuum magnetic field annealing and then to magnetic characterization, and the magnetism can be measured in the annealing process to characterize the influence of different annealing conditions on the magnetism;
and after the magnetic representation meets the requirement, the sample is transmitted back to the magnetron sputtering cavity to deposit other film layers, and then representation is carried out, or after a protective layer is deposited, the sample is transmitted to the rapid sample introduction chamber through the ultrahigh vacuum sample transmission rod and then taken out.
The integrated processing equipment for the ultrathin multilayer film integrates the functions of preparation, in-situ regulation and characterization of the ultrathin multilayer film, can realize in-situ regulation and characterization of a certain layer in the preparation process, can pertinently research the contribution or influence of different layers on the whole film layer, does not need to destroy the original vacuum environment in the process, does not need to arrange a vacuum interconnection system, and has the characteristics of excellent performance, reliable design, low cost and high operation efficiency.
Drawings
FIG. 1 is a schematic perspective view of an integrated processing tool according to a preferred embodiment of the present invention;
FIG. 2 is a top plan view of the integrated tool of FIG. 1;
FIG. 3 is a schematic perspective view of the integrated processing tool after being fixedly installed according to a preferred embodiment of the present invention;
FIG. 4 is a block diagram of the power system connections in accordance with a preferred embodiment of the present invention;
FIG. 5 is a schematic diagram of the conditioning and characterization device 30 of FIG. 1;
fig. 6 is a schematic flow chart of the integrated processing device in fig. 3 in the process of manufacturing the ultra-thin multilayer film.
In the figure: the device comprises an ultrahigh vacuum multi-target magnetron sputtering device 10, a magnetron sputtering cavity 101, a molecular pump 101-1, a low-temperature pump 101-2, a vacuum sample rack 102, a second vacuum measurement system 103, a residual gas analyzer RGA103-1, a second vacuum obtaining system 104, a magnetron sputtering cathode 105, a first observation window 106, a film thickness measuring instrument 107, a mounting hole 108, a second gate valve 109 and a third gate valve 110;
the rapid sampling device comprises a rapid sampling chamber 20, a rapid sampling cavity 201, a first gate valve 202, a first vacuum measurement system 203, a first vacuum obtaining system 204, an air inlet valve 205, a second observation window 206 and a mechanical arm sample transfer rod 207;
the device comprises a regulation and characterization device 30, a regulation and characterization cavity 301, a conversion cavity 302, a magnetic characterization system 303 and an ultrahigh vacuum sample transfer rod 304.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the specific embodiments illustrated. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The embodiment discloses integrated processing equipment for an ultrathin multilayer film, which comprises ultrahigh vacuum multi-target magnetron sputtering equipment 10, a rapid sampling chamber 20 and regulation and characterization equipment 30, wherein the integrated processing equipment for the ultrathin multilayer film, which is mentioned in the embodiment, can realize in-situ regulation and characterization on a certain layer of film without connecting related equipment through a complicated vacuum interconnection device and destroying a vacuum environment, and is favorable for distinguishing contributions of the certain layer of film.
The ultrahigh vacuum multi-target magnetron sputtering device 10 described in this embodiment may adopt a physical vapor deposition device for depositing a film layer, which is conventional in the art, and specifically, as shown in fig. 1, the ultrahigh vacuum multi-target magnetron sputtering device 10 includes a magnetron sputtering chamber 101, a magnetron sputtering chamber in the magnetron sputtering chamber is similar to a magnetron sputtering chamber conventional in the art, and the shape of the magnetron sputtering chamber 101 is not particularly limited, and may be designed as needed, and therefore, it is not specifically described here. A plurality of flange openings with different specifications are arranged outside the magnetron sputtering cavity 101, the specifications of the flange openings include but are not limited to CF60, CF100 and the like, and the flange openings are mainly used for connecting various accessory fittings. Specifically, please refer to fig. 1 and fig. 2, a vacuum sample holder 102, a second vacuum measuring system 103, a second vacuum obtaining system 104, and a magnetron sputtering cathode 105 are respectively connected to the outside of the magnetron sputtering chamber 101 in a flange-sealed manner, further, a first observation window 106 is provided on the magnetron sputtering chamber 101, the magnetron sputtering chamber 101 is further provided with a film thickness measuring instrument 107, in addition, the magnetron sputtering chamber 101 is further provided with a plurality of sealed reserved flange ports, the reserved flange ports are sealed by using a blind plate when not in use, different accessories can be connected to the flange according to different requirements, for example, a part of the flange is connected to a gas flow meter to realize gas introduction, a part of the flange can be connected to a Wedge-shaped film system to realize installation of the Wedge-shaped film Wedge system, or as shown in this embodiment, the film thickness measuring instrument 107 is installed to realize deposition thickness during preparation of the ultra-thin multi-layer film, the film thickness measuring instrument 107, The film thickness monitoring device comprises a baffle, a vacuum flange and a peripheral circuit, and the thickness of a film layer can be monitored in real time in the film preparation process through the relationship between the frequency change of a quartz crystal and the added mass. Since the film-thickness measuring instrument 107 is a conventional instrument in the art, it will not be described in detail here. It is understood that the layout, connection position, connection order, and the like of the above accessories and the like connected to the outside of the magnetron sputtering chamber 101 are not particularly limited, and may be adjusted as needed.
Further, in the present embodiment, the vacuum sample holder 102 (attached at the position of the flange opening in the drawing) is hermetically connected to the upper end of the magnetron sputtering chamber 101 through a flange, where the vacuum sample holder 102 may be a sample holder conventional in the art, and in the present embodiment, it is preferable that the vacuum sample holder 102 has X, Y, Z three movable degrees of freedom and the vacuum sample holder 102 can realize 360-degree rotation, and the degree of freedom is mainly realized by a stepping motor carried by the vacuum sample holder 102, and will not be specifically described herein.
Further, the second vacuum obtaining system 104 in the present embodiment refers to a vacuum pump device capable of providing vacuum in the magnetron sputtering chamber 101, and may be a vacuum pump device conventional in the art as long as it can provide a vacuum environment of the magnetron sputtering chamber 101. Specifically, in this embodiment, the second vacuum obtaining system 104 is flange-sealed connected to the magnetron sputtering chamber 101 through a second gate valve 109, preferably, in this embodiment, the second vacuum obtaining system 104 is a three-stage vacuum pump set, the three-stage vacuum pump set includes a mechanical pump (not shown), a molecular pump 101-1 and a cryogenic pump 101-2, the second vacuum obtaining system 104 is connected to the magnetron sputtering chamber 101 through the second gate valve 109, specifically, the cryogenic pump 101-2 is connected to the molecular pump 101-1 through a third gate valve 110, the mechanical pump is connected to the molecular pump 101-1 and the pre-stage of the cryogenic pump 101-2, the mechanical pump is connected to the molecular pump 101-1 and the cryogenic pump 101-2 through a bellows, firstly, the mechanical pump pumps the atmospheric pressure in the magnetron sputtering chamber 101 to a low vacuum, then the molecular pump 101-1 is started to pump the high vacuum from the low vacuum, then, the vacuum degree is further improved by adopting a baking cavity mode, and finally the low-temperature pump 101-2 is started, wherein the low-temperature pump 101-2 in the embodiment is an adsorption pump and is used for adsorbing the water vapor of molecules in the magnetron sputtering cavity 101, and the vacuum degree in the magnetron sputtering cavity 101 can be reduced to 1 × 10 by the second vacuum obtaining system 104-8Pa below for depositing the ultra-thin multilayer film in an ultra-high vacuum environment.
Further, the second vacuum measurement system 103 in the present embodiment refers to a vacuum detection device for measuring the vacuum environment in the magnetron sputtering chamber 101, and it can be understood thatIn the present embodiment, the second vacuum measurement system 103 is hermetically connected to the side of the magnetron sputtering chamber 101 through a flange, and is composed of three-stage vacuum gauges, specifically, a vacuum film gauge (not shown in the figure), a UHV ion gauge (not shown in the figure), and a residual gas analyzer RGA103-1, so that the vacuum degree that can be measured by the second vacuum measurement system 103 is as low as 1 × 10 from the atmosphere-10Pa pressure, and analyzing the residual gas through a residual gas analyzer RGA103-1, so as to improve the vacuum degree in the magnetron sputtering cavity 101 through a second vacuum obtaining system 104 according to the analysis result, the residual gas analyzer RGA103-1 can also measure the content of the gas in the cavity in the film deposition process so as to assist the debugging of the process parameters, and particularly, the residual gas analyzer RGA103-1 is connected between the second gate valve 109 and the third gate valve 110 in a flange manner. The specific working process is as follows: when the second vacuum measurement system 103 is used for measuring the vacuum degree, along with the increase of the pumping speed of the second vacuum acquisition system, firstly, the rough vacuum is measured by the vacuum film gauge, then, the UHV ion gauge is started to measure the high vacuum, and the residual gas analyzer RGA103-1 can analyze the components of residual gas in the cavity. It is understood that the three-stage vacuum gauges are all connected with the magnetron sputtering chamber 101 through flange port sealing, and the specific positions, sequence and the like of the three-stage vacuum gauges are not particularly limited and can be adjusted according to the layout of the whole integrated processing equipment.
Referring to fig. 1 and fig. 2, in the present embodiment, the first observation window 106 is formed by sealing a quartz window at one of the flange openings of the magnetron sputtering chamber 101, and mainly functions to transmit various light waves and electromagnetic waves such as ultraviolet light, visible light, or infrared light through the first observation window 106. In this embodiment, the first observation window 106 is disposed on a side surface of the magnetron sputtering chamber 101.
Further, the magnetron sputtering cathode 105 in this embodiment is disposed at the lower portion of the magnetron sputtering chamber 101, and specifically, twelve flange openings are disposed at the lower portion of the magnetron sputtering chamber 101, so that the connected twelve magnetron sputtering cathodes 105 are respectively on the same spherical surface, angles of the twelve magnetron sputtering cathodes 105 are different, and the angles of the twelve magnetron sputtering cathodes 105 are all facing to a central position in a magnetron sputtering chamber inside the magnetron sputtering chamber 101, that is, a sample deposition position. The magnetron sputtering cathode 105 can be selected from magnetron sputtering cathodes conventional in the art and can be assisted by an ion source, and preferably, the magnetron sputtering cathode 105 in the present embodiment is equipped with Z-axis freedom and angular freedom, so that the Z-axis freedom (adjustment of the target base distance) and the angle (angle of the target towards the sample holder) of the cathode 105 can be adjusted in situ without breaking vacuum. The magnetron sputtering cathode 105 in this embodiment is cooled by water cooling, and a circular sputtering target having a diameter of 2 inches and a thickness of less than 5mm can be mounted. Specifically, the magnetron sputtering cathode 105 is provided with a cathode cover, the cover is driven by compressed air, and the cathode cover can be opened at 90-180 degrees by controlling a compressed air path. And a process gas path is reserved in the magnetron sputtering cathode 105, so that the air intake of the target surface can be realized, and the starting air pressure is reduced. The cathode magnet is arranged below the target, a balanced magnet configuration and an unbalanced magnet configuration can be selected, balanced magnet distribution is preferred, the number of magnets can be increased aiming at the magnetic target so as to improve the ionization degree and realize high-speed deposition.
Further, as shown in fig. 2, in the present embodiment, a plurality of mounting holes 108 are further provided at a lower portion of the magnetron sputtering chamber 101 for mounting and fixing the magnetron sputtering chamber 101, where the fixing manner is not particularly limited, and the fixing manner may be a fixing manner conventional in the art, and preferably, the fixing manner is a screw-fastening manner to a support structure, such as a stainless steel bracket made of 304 stainless steel, as shown in fig. 3.
The ultrahigh vacuum multi-target magnetron sputtering apparatus 10 in this embodiment further includes a power supply system, specifically, the power supply system is composed of a dc power supply, a radio frequency power supply and a switch, specifically, as shown in fig. 4, the dc power supply is connected to the switch through a dc cable, and the radio frequency power supply is connected to the switch through a matcher. The switch in this embodiment can be set to two inputs and multiple outputs, and by the switching function of the switch, which power source is connected first and then which cathode is outputted can be selected. The cable between the radio frequency power supply and the matcher needs to meet the requirement of impedance matching, and the matcher and the switcher are directly connected, so that the loss is reduced to the maximum extent. The switch is placed directly below the cathode 105, typically about 1 meter in length. By this way, a DC voltage or a RF voltage can be applied to each cathode 105, which can greatly reduce the use of power supply and reduce the cost, and meanwhile, each device can realize the co-sputtering of several cathodes by being equipped with several sets of power supplies. It is understood that the modules such as the power supply system can be connected to the integrated processing device in the embodiment through the manufactured structure, and the specific installation position is not particularly limited and can be adjusted as required. In this embodiment, the switcher and the matcher are respectively fixed on the supporting frame and located at four corners of the supporting frame.
Further, please refer to fig. 1 and fig. 2, the rapid sample introduction chamber 20 includes a rapid sample introduction cavity 201, the rapid sample introduction cavity 201 is flange-sealed with the magnetron sputtering cavity 101 through a first gate valve 202, a plurality of flange ports for connecting various accessories are also provided outside the rapid sample introduction cavity 201, the connection sequence and position of the accessories are not specifically limited, and can be adjusted according to the actual layout. In this embodiment, a second observation window 206 is disposed at an upper end of the rapid sampling cavity 201, where the second observation window 206 is made of a glass flange seal, so as to realize observation of the state in the rapid sampling cavity 201. The side surface of the rapid sample introduction cavity 201 is respectively connected with a first vacuum measurement system 203 and a first vacuum obtaining system 204 in a flange sealing manner, specifically, the first vacuum obtaining system 204 is a two-stage vacuum pump set which comprises a mechanical pump and a molecular pump and is used for pumping the vacuum degree in the rapid sample introduction cavity 201 to 10-5Pa. The first vacuum measurement system 203 is a full-range vacuum gauge, and the measurement range can be from atmospheric pressure to 10-7Pa, the vacuum gauge has a digital pressure indication, which is convenient for observing the vacuum state in the rapid sampling cavity 201. In addition, in this embodiment, the side surface of the rapid sampling cavity 201 is provided with the air inlet valve 205, and the air inlet valve 205 can be connected to a gas pipeline and a gas flowmeter, for example, the air inlet valve 205 is connected to a nitrogen pipeline to recover the atmosphere of the rapid sampling cavity 201 or connected to a process gas pipeline to realize annealing in the gas atmosphereAnd (6) annealing. Furthermore, a liftable sample holder is arranged in the rapid sample injection cavity 201, and can be used for loading a plurality of substrates, and the liftable sample holder can be lifted up and down to facilitate the transmission of samples. Further, in this embodiment, the fast sampling cavity 201 is flange-connected with a mechanical arm sample transfer rod 207 for transferring samples.
Further, with continuing reference to fig. 1 and fig. 2, the control and characterization device 30 includes a control and characterization cavity 301, the control and characterization cavity 301 is communicated with the rapid sampling cavity 201 through a conversion cavity 302, and it should be noted that, with reference to fig. 5, the rapid sampling cavity 201, the conversion cavity 302 and the control and characterization cavity 301 are communicated with each other, and when the rapid sampling cavity 201 is vacuumized or vacuum-measured, the vacuum environment of the three communicating cavities of the rapid sampling cavity 201, the conversion cavity 302 and the control and characterization cavity 301 can be controlled in fact. Further, a magnetic characterization system 303 is connected to the upper end of the regulation and characterization cavity 301, specifically, the magnetic characterization system 303 includes a detection light path: the magnetic characterization system 303 comprises an input optical path and an output optical path, wherein the lower ends of the input optical path and the output optical path are provided with pole heads, a gap for the optical path to pass through is reserved in the middle of the pole heads, and an optical component is arranged inside the magnetic characterization system 303 and mainly comprises a laser, a polarizing and analyzing prism, a photoelectric detection device and a silicon photocell. In addition, the external control equipment further comprises a signal detection host machine and the like which are all conventional in the field and are not explained one by one, specifically, a first in-plane magnet and a second in-plane magnet which are oppositely arranged are fixedly arranged inside the regulation and characterization cavity 301, in the embodiment, the axes of the first in-plane magnet and the second in-plane magnet are perpendicular to a communication line of the regulation and characterization cavity 301 and the conversion cavity 302, and each of the first in-plane magnet and the second in-plane magnet comprises a left magnetic pole, a right magnetic pole and an auxiliary coil, the coils of the two magnetic poles are connected in series and are provided with Hall probes; still set firmly first perpendicular magnet and the perpendicular magnet of second of relative setting in regulation and control and sign cavity 301, first perpendicular magnet with the perpendicular magnet of second is fixed air gap yoke breaking magnet, in this embodiment, first perpendicular magnet is located regulation and control and sign cavity 301 and magnetism sign system 303 between, just be equipped with the hole that supplies magnetism detection light path to pass through on the first perpendicular magnet, be equipped with above-mentioned magnet in regulation and control and sign cavity 301, and be the electro-magnet, the maximum magnetic field of electro-magnet can reach 1T, can test the magnetic characteristic of film, also can realize annealing under the magnetic field. The electromagnet is provided with a direct current power supply, is connected with the electromagnet to realize output, and can be connected with a PC to realize remote control. The connection between the regulation and control and characterization cavity 301 and the magnetic characterization system 303 is sealed through a glass flange port, so that the light path of the magnetic characterization system 303 can penetrate through the glass flange port to enter the surface of a sample to realize magnetic measurement, and further, the conversion cavity 302 is set up as a magnet arrangement and a reserved space is set up for the light path, so that collision of all parts is prevented. Further, the side surface of the regulation and control and characterization cavity 301 is connected with an ultrahigh vacuum sample transmission rod 304 in a flange manner, and the ultrahigh vacuum sample transmission rod 304 adopts a magnetic coupling mode component, so that the ultrahigh vacuum sample transmission rod is used for sample transmission. Be equipped with high temperature sample frame (not shown in the figure) in regulation and control and sign cavity 301, the material of high temperature sample frame can select for use high temperature resistant materials such as molybdenum, and the sample holds in the palm the heatable to 600 ℃, and the high temperature sample frame adopts the radiant heating mode, can anneal under the gas atmosphere, is equipped with temperature sensor on the high temperature sample frame to realize the control to the temperature, can set up the temperature rise time and the hold time of annealing process. The process gas connected with the gas inlet valve 205 of the rapid sample introduction cavity 201 performs a radiation heating mode on the sample holder in the regulation and control and characterization cavity 301, and high-temperature magnetic field annealing is realized in a gas atmosphere.
The invention also discloses an application method of the integrated processing equipment, which comprises the following steps:
after the integrated processing equipment is safely fixed according to the method shown in fig. 3, a power supply system, a control system and the like (not shown in the figure) are arranged on a support frame, after the vacuum environment in the integrated processing equipment is controlled to a required value, a substrate to be prepared is loaded into a vacuum sample frame of a rapid sample loading chamber 20, and a first gate valve 202 is opened to transfer a sample into the magnetron sputtering cavity 101 to deposit a magnetic multilayer film;
transferring a sample on which the magnetic multilayer film is deposited into a regulation and control and characterization cavity 301 through a rapid sample introduction chamber 20 for magnetic characterization, if the magnetism does not meet the requirement, performing ultrahigh vacuum magnetic field annealing, then performing magnetic characterization, simultaneously opening an air inlet valve 205 according to the requirement to introduce process gas to realize annealing in a gas atmosphere, and simultaneously monitoring the change of the magnetism through a magnetic characterization system in the annealing process;
after the magnetic characterization meets the requirement, the sample is transmitted back to the magnetron sputtering cavity 101 to deposit other film layers, and the characterization process is repeated after deposition, or after a protective layer is deposited, the sample is transmitted out of the device through the ultrahigh vacuum sample transmission rod 304. The specific flow of the method is shown in fig. 6, and the method is controlled after being connected with each device in the integrated processing device through the control system and setting the corresponding program, which is not described in detail herein.
It can be seen that the integrated processing equipment for the ultrathin multilayer film integrates preparation, regulation and control and characterization, and does not need an ultrahigh vacuum interconnection system and a complex sample transmission system, thereby reducing the design cost of the system, reducing the complexity of operation and improving the preparation efficiency. And the integrated processing equipment can realize in-situ regulation and characterization of a certain layer of film, does not need to destroy the vacuum environment, and is favorable for distinguishing the contribution of the certain layer of film.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. An integrated processing apparatus of an ultra-thin multi-layered film, comprising:
the ultrahigh vacuum multi-target magnetron sputtering device comprises a magnetron sputtering cavity;
the rapid sample introduction chamber comprises a rapid sample introduction cavity, the rapid sample introduction cavity is in flange sealing connection with the magnetron sputtering cavity through a first gate valve, a first vacuum measurement system and a first vacuum obtaining system are connected outside the rapid sample introduction cavity, and an air inlet valve is arranged outside the rapid sample introduction cavity;
the regulation and characterization device comprises a regulation and characterization cavity which is internally provided with a high-temperature sample rack, the regulation and characterization cavity is communicated with the rapid sample injection cavity through a switching cavity, and the regulation and characterization cavity is also respectively connected with a magnetic characterization system and an ultrahigh vacuum sample transfer rod.
2. The integrated processing device according to claim 1, wherein a vacuum sample holder, a second vacuum measurement system, a second vacuum acquisition system and a magnetron sputtering cathode are respectively flange-connected outside the magnetron sputtering cavity, a first observation window is arranged on the magnetron sputtering cavity, the first observation window is formed by sealing a quartz observation window and the magnetron sputtering cavity through flanges, and a plurality of sealed reserved flange openings are also arranged on the magnetron sputtering cavity;
and the bottom of the side surface of the magnetron sputtering cavity is provided with a mounting hole for fixing the magnetron sputtering cavity.
3. The integrated processing tool according to claim 2, wherein the second vacuum measurement system is comprised of a three-stage vacuum gauge including a vacuum film gauge, a UHV ion gauge, and a residual gas analyzer RGA;
the second vacuum obtaining system is in sealing connection with the magnetron sputtering cavity through a second gate valve, the second vacuum obtaining system is a three-stage vacuum pump set, and the three-stage vacuum pump set comprises a mechanical pump, a molecular pump and a cryogenic pump.
4. The integrated processing apparatus according to claim 2, wherein the magnetron sputtering cathodes are arranged in twelve different angles, and are respectively located on the same spherical surface and face the magnetron sputtering sample position in the magnetron sputtering chamber.
5. The integrated processing tool of claim 2, wherein the magnetron sputtering chamber is equipped with a film thickness measuring device for film thickness monitoring, the film thickness measuring device being flanged to the magnetron sputtering chamber.
6. The integrated processing tool of claim 2, wherein the magnetron sputtering tool further comprises a power supply system comprising:
the switcher is connected with the magnetron sputtering cathode;
the direct current power supply is connected to the switcher through a direct current cable;
and the radio frequency power supply is connected into the switcher through a matcher.
7. The integrated processing apparatus according to claim 1, wherein the fast sampling cavity is provided therein with a liftable sample holder, and the fast sampling cavity is further provided with a second observation window.
8. The integrated processing tool of claim 1, wherein the first vacuum acquisition system is a two-stage vacuum pump set comprising a mechanical pump and a molecular pump;
the first vacuum measurement system is a full-range vacuum gauge.
9. The integrated processing apparatus according to claim 1, wherein the high temperature sample holder is heated by radiation, and a temperature sensor is provided on the high temperature sample holder;
the magnetic characterization and regulation system comprises:
the magnetic detection light path component is arranged at the upper end of the regulation and control and characterization cavity and comprises an input light path and an output light path;
the glass flange port is used for the magnetic detection light path to enter the regulation and control and characterization cavity and is sealed at the upper end of the regulation and control and characterization cavity;
the first in-plane magnet and the second in-plane magnet are positioned in the regulation and characterization cavity and are oppositely arranged, the first in-plane magnet and the second in-plane magnet both comprise a left magnetic pole, a right magnetic pole and an auxiliary coil, the coils of the two magnetic poles are connected in series, and a Hall probe is arranged;
be located regulation and control and sign cavity and relative first perpendicular magnet and the perpendicular magnet of second that sets up, first perpendicular magnet is located regulation and control and sign cavity with between the magnetic detection light path, just be equipped with the confession on the first perpendicular magnet the hole that the magnetic detection light path passed through, first perpendicular magnet with the perpendicular magnet of second is the disconnected yoke magnet of fixed air gap.
10. A method of using an integrated tool according to any of claims 1 to 9, comprising the steps of:
loading a substrate to be prepared into the rapid sample introduction chamber, and then sending the substrate into the magnetron sputtering cavity to deposit a magnetic multilayer film;
the sample after the magnetic multilayer film is deposited is transmitted into a regulation and control and characterization cavity to carry out magnetic characterization, if the magnetism does not meet the requirement, the sample can be subjected to ultrahigh vacuum magnetic field annealing and then to magnetic characterization, and the magnetism can be measured in the annealing process to characterize the influence of different annealing conditions on the magnetism;
and after the magnetic representation meets the requirement, the sample is transmitted back to the magnetron sputtering cavity to deposit other film layers, and then representation is carried out, or after a protective layer is deposited, the sample is transmitted to the rapid sample introduction chamber through the ultrahigh vacuum sample transmission rod and then taken out.
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WO2022033026A1 (en) * 2020-08-13 2022-02-17 北京航空航天大学合肥创新研究院 Integrated processing device of ultrathin multilayer film and application method
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