EP3768871A1 - Dispositif de pulvérisation cathodique à magnétron - Google Patents

Dispositif de pulvérisation cathodique à magnétron

Info

Publication number
EP3768871A1
EP3768871A1 EP19720848.1A EP19720848A EP3768871A1 EP 3768871 A1 EP3768871 A1 EP 3768871A1 EP 19720848 A EP19720848 A EP 19720848A EP 3768871 A1 EP3768871 A1 EP 3768871A1
Authority
EP
European Patent Office
Prior art keywords
substrate
target
magnetron sputtering
reaction chamber
anode
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP19720848.1A
Other languages
German (de)
English (en)
Inventor
Bastian GAEDIKE
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hartmetall Werkzeugfabrik Paul Horn GmbH
Original Assignee
Hartmetall Werkzeugfabrik Paul Horn GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hartmetall Werkzeugfabrik Paul Horn GmbH filed Critical Hartmetall Werkzeugfabrik Paul Horn GmbH
Publication of EP3768871A1 publication Critical patent/EP3768871A1/fr
Pending legal-status Critical Current

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Classifications

    • 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
    • H01J37/3402—Gas-filled discharge tubes operating with cathodic sputtering using supplementary magnetic fields
    • H01J37/3405—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
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • 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
    • C23C14/3485—Sputtering using pulsed power to the target
    • 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
    • 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
    • H01J37/32431—Constructional details of the reactor
    • H01J37/32733—Means for moving the material to be treated
    • 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
    • H01J37/32431—Constructional details of the reactor
    • H01J37/32733—Means for moving the material to be treated
    • H01J37/32752—Means for moving the material to be treated for moving the material across the discharge
    • 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
    • H01J37/32431—Constructional details of the reactor
    • H01J37/32733—Means for moving the material to be treated
    • H01J37/32752—Means for moving the material to be treated for moving the material across the discharge
    • H01J37/32761—Continuous moving
    • H01J37/32779—Continuous moving of batches of workpieces
    • 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
    • H01J37/3414—Targets
    • H01J37/3417—Arrangements
    • 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
    • H01J37/3414—Targets
    • H01J37/3426—Material
    • H01J37/3429—Plural materials
    • 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
    • H01J37/3438—Electrodes other than cathode
    • 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
    • H01J37/3464—Operating strategies
    • H01J37/3467—Pulsed operation, e.g. HIPIMS
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/202—Movement
    • H01J2237/20214—Rotation

Definitions

  • the present invention relates to a magnetron sputtering apparatus and a method for magnetron sputtering.
  • Exemplary magnetron sputtering devices are already known from DE 10 2014 105 947
  • the term “sputtering”, which results from the English verb "to sputter” "atomize”, a physical process understood in which atoms from a solid, a so-called target, by a bombardment with high-energy ions be released and thereby go into a gas phase.
  • the leached atoms coat a body and settle on its surface as a thin layer.
  • the body to be coated is generally referred to as a "substrate”.
  • the technical application of the physical process for example, in the Coating used by cutting tools, tool holders and forming tools.
  • This type of coating process is also referred to as “sputter deposition” and belongs to the group of vacuum-based PVD processes.
  • the abbreviation PVD here refers to physical vapor deposition (English: “physical vapor deposition”).
  • the coating is usually used to increase the resistance, wear protection and mechanical hardness.
  • the atoms released from the target are accelerated by an energy input to the substrate to be coated and are deposited on the surface of the substrate as a boundary layer.
  • the material to be deposited i.
  • the target material is usually present as a solid in a PVD process and is usually located in an evacuated coating chamber, which is also referred to as a reaction chamber. In this reaction chamber, the substrate to be coated is arranged spatially separated from the target.
  • the reaction chamber is filled with an inert process gas which is brought into the ionized state by the energy supply of the DC electric field (plasma formation).
  • the positively charged process gas ions are accelerated by the DC electric field in the direction of the positively charged target and strike by this "bombardment", ie by physical shock pulse transmission, atoms of the target material out of the surface, which subsequently move in the direction of the substrate and its Coat the surface.
  • a permanent current of positively charged ions hits the target, which is why the process is also referred to as DC or DC sputtering.
  • a magnetic field is generated in addition to the DC electric field between the cathode and anode behind the target by one or more electric or permanent magnets, which is why this process is also referred to as "magnetron sputtering".
  • the ions of the process gas do not move parallel to the electric field, but are deflected by the Lorentz force on their spiral path to the target surface, causing the individual ions to travel a longer distance to their impact on the target surface ,
  • This extended path increases the likelihood of further shocks between ionized process gas ions and non-ionized process gas ions.
  • the magnetic field increases the impact ionization and with it the total number of ionized process gas atoms. This results in particular in an increase in the sputtering rate, where the sputtering rate is understood to be the number of atoms of the target material dissolved out.
  • higher coating rates can be realized without increasing the process pressure.
  • An increase in the process pressure also leads to an increase in the ionization rate, since the pulse of the individual process gas ions can be increased by higher pressure conditions inside the reaction chamber.
  • Magnetron sputtering can thus improve the layer growth, the homogeneity and / or the layer properties on the substrate surface in comparison to the simple cathodic sputtering. Increasing the sputtering rate results in less scattering of the material on the way to the substrate and a denser (less porous) surface layer on the substrate surface.
  • the disadvantage of this method is that due to the functional principle, ie the DC field between the target and the anode, only electrically conductive materials can be used as target or coating material. If an electrically insulating material is used as the target material, the formation of an electrically insulating boundary layer on the anode surface occurs when the atoms of this insulating material are deposited.
  • This anode surface may be, for example, the surface of the substrate or the surface of a sacrificial sheet connected as an anode. Through this boundary layer, the otherwise electrically conductive anode loses its electrical conductive property and thus their anode function in the DC field.
  • this phenomenon is also referred to as the "disappearing anode effect", ie, the “disappearance of the anode” and prevents the deposition of many technically interesting materials (eg ceramics such as aluminum oxide).
  • This effect can also destroy a plant or at least lead to a termination of the coating process.
  • a reactive gas is present in the reaction chamber, this phenomenon can occur. If, for example, metals (eg aluminum or zirconium) are processed reactively by oxygen addition in such a reactive PVD process, electrically non-conductive layers are formed, through which the anode can "disappear".
  • electrically nonconductive solids e.g. technical ceramics
  • coating material since these materials have a high hardness, high thermal resistance, good thermal conductivity, high chemical resistance and corrosion resistance.
  • technical ceramics as used herein means an inorganic nonconductive solid.
  • alternating current dual magnetron sputtering A technical possibility of coating substrates with an electrically nonconductive material is provided by so-called alternating current dual magnetron sputtering. Between the two electrodes, for example, between the target and the substrate, an alternating current is switched back and forth, through which the substrate surface is cleaned at each reversal of the current direction, whereby the "disappearing anode effect" can be prevented [Source: http: // /www.semicore.com/news/97-what-is-mf-ac- sputtering; called on 26.04.2018].
  • DE 10 2014 105 947 A1 mentioned at the beginning shows an exemplary DC magnetron sputtering device or a method for depositing a thin piezoelectric film on an acoustic resonator.
  • the target consists of electrically conductive aluminum, which is doped with a likewise electrically conductive rare earth element.
  • This document essentially deals with the object of designing a magnetic field in favor of the piezoelectric properties of the resonator coating. In the document, however, not the above-described technical problem is solved, but it is explicitly mentioned that the target consists of an electrically conductive material.
  • a magnetron sputtering apparatus which is used for the coating of liquid crystal display substrates or semiconductor substrates, this document dealing with the positioning of the magnets within the apparatus and thus illuminating a different technical area.
  • a gas inlet for a vacuum chamber of a magnetron sputtering device is provided, by means of which the distribution of a mixed gas (process gas + reactive gas) after entering the vacuum chamber is to be standardized.
  • the magnetron sputtering apparatus comprises: a substrate; a target which forms a cathode in a DC electric field and has an electrically conductive substance mixture for coating the substrate; an anode in the DC electric field; a reaction chamber in which the target and the substrate are arranged, the target being arranged spatially separated from the substrate; and a voltage source configured to generate the DC electric field between the cathode and the anode; wherein the composition comprises a first material and a second material, and wherein the substrate comprises a third material, wherein the first material is an electrically non-conductive solid, the second material is an electrically conductive solid, and the third material is an electrically conductive solid.
  • the object of the invention is further achieved by a method, the following
  • the substrate can be coated, for example, with a technical ceramic which gives rise to numerous advantageous layer properties.
  • the layer quality and layer properties of the substrate coating are decisively determined according to the invention by the mechanical and thermal properties of the electrically nonconductive material (first material).
  • the second material is only mixed in to produce the electrical conductivity.
  • the mixture of substances provided on the target therefore preferably consists of relatively large proportions of the first material.
  • the proportion of the second material is preferably chosen as small as possible, namely only as large as is necessary for producing the desired electrical conductivity of the target substance mixture. In such a case, the properties of the second material lead only to small, technically tolerable changes in the coating on the substrate.
  • E in a further advantage of the invention is that already in use, conventional Magnetronsputtervoruttervorplatzen - can be used - without the need for an expensive and expensive retrofitting or conversion - because only replaced the target for the device or the method according to the invention must become.
  • the object to be coated is referred to in the most general form.
  • a substrate preferably all types of tools, tool parts, cutting tools, forming tools, tool holders and sections of tool holders are referred to as a substrate.
  • the substrate can be arranged in the reaction chamber, for example, on a substrate holder, or can be fastened in a reversibly detachable manner with it.
  • a target is understood in the present context, a solid, which may in principle have any kind of geometric shape.
  • targets have established themselves in the form of a rectangle or a circle, whereby the target can advantageously be arranged on a target holder within the reaction chamber.
  • a target holder can be used for example as a mounting platform during the coating process, on which the target can be reversibly releasably secured.
  • reaction chamber here the housing or the working space or the working volume of the magnetron sputtering apparatus is referred to, in which the target is arranged spatially separated from the substrate.
  • the reaction chamber for example, a vacuum pump for generating a vacuum in its interior.
  • the reaction chamber additionally has a gas inlet opening, through which after the generation of the vacuum, i. removing the air from the interior of the reaction chamber, a process gas can be introduced.
  • the process gas is a noble gas, i. a gas that behaves chemically inert and thus does not react with one or more reactants.
  • the voltage source provides between its connection points, e.g. Realized by
  • Terminals or electrical outputs an electrical voltage or a potential difference.
  • the voltage depends only slightly on the electric current, which is taken from the voltage source.
  • the delivered electrical voltage is thus ideally independent of the respective connected consumer.
  • the voltage source is a DC electrical source. That is, the electrical output of the DC voltage source, which provides a negative voltage, is connected to the target via a cable connection.
  • the electrical output which provides a positive voltage or zero potential (ground), is connected to the anode via a cable connection. It should be mentioned that, for safety reasons, a grounding of the system is advantageously arranged on the reaction chamber.
  • the target according to the invention comprises a first material and a second material, which means in other words that the target at least from a first and a second material.
  • the target thus has a substance mixture or a material composition consisting of at least the first material and the second material, but may also have further materials, for example carrier materials.
  • a target according to the invention is advantageously sintered or hot-pressed, but can also be produced by other production methods by which it is possible to have two different raw materials or raw materials, preferably in powder form or as granules, ie as solid, prior to preparation. to unite with each other in a solid state.
  • the third material or the substrate material is different from the second material. This means that the chemical composition of the third material differs from that of the second material. Only an altered morphology or crystal lattice structure (e.g., cubic body centered, cubic face centered, or hexagonal packed tight) is not enough to account for the difference between the second material and the third material.
  • the electrical conductivity which is also referred to as conductivity, the physical quantity that indicates the ability of a substance to conduct the electric current.
  • electrical conductivity is often reported as the reciprocal of the resistivity of a substance. This resistance is usually indicated by the SI unit Ohmmeter (Qm).
  • Qm The SI unit of electrical conductivity is given as Siemens per meter (S / m).
  • Conductivity can be divided into four groups. A distinction is made between superconductors, conductors, semiconductors and non-conductors.
  • Superconductors here denote materials in which below a material-dependent transition temperature, the electrical resistance drops to almost 0 and the electrical conductivity is thus almost infinitely large.
  • Conductor or conductive materials have, at an ambient temperature of 25 ° C via an electrical conductivity of> 10 6 S / m. In the group of semiconductors, the electrical conductivity depends on the purity of the material. In the group of non-conductors or insulators, the electrical conductivity is usually given as ⁇ 10 8 S / m. Physically speaking, the electrical conductivity can also be based on the so-called.
  • a solid in the present case, it seems useful to define a solid as electrically conductive, if it has an electrical conductivity speed of> 10 3 S / m at an ambient temperature of 25 ° C. In the present case, however, a solid should be considered to be electrically nonconductive if it has an electrical conductivity of ⁇ 10 3 S / m at an ambient temperature of 25 ° C.
  • the first material comprises a first volumetric fraction AV-i and the second material has a second volumetric fraction AV 2 , where AV-i> AV 2 , preferably AV-i> 1.5 AV 2 .
  • the admixture of the second material takes place only to ensure the electrical conductivity of the coating.
  • the advantageous mechanical and thermal properties of the coating are preferably determined by the material properties of the first material. For this reason, there is the advantage of mixing the second material in a volumetric proportion that is less than the volumetric proportion of the first material.
  • AV-i> 1, 5 AV 2 .
  • a preferred substance mixture is at least at least 60 percent by volume of the first material and at most 40 percent by volume of the second material.
  • the first material is a first inorganic solid.
  • an inorganic solid is understood to mean a substance from the periodic table which is in a solid state up to a temperature of at least 150 ° C.
  • an inorganic material is understood to mean a material that does not have an animated nature.
  • the first inorganic solid is a
  • Carbide, a nitride and / or an oxide Carbide, a nitride and / or an oxide.
  • the high binding energy is represented on the atomic level by a high proportion of covalent and a small proportion of ionic bonds.
  • oxides For oxides, however, dominate the ionic bonds. However, oxides are also distinguished by high hardness, high wear resistance and good heat resistance, but they are more brittle than most conventional hard metals and are therefore preferably used in coatings for coatings. In addition, oxides have a high corrosion resistance up to temperatures of> 1000 ° C.
  • the first inorganic solid is a
  • Metal oxides refer to compounds between a metal and oxygen and are known for their advantageous properties as a coating material. Metal oxides are also dominated by the ionic bonds. In addition, they are characterized (like oxides) high hardness, high wear resistance and good heat resistance.
  • the metal oxide is a zirconia (ZrO 2 )
  • Alumina Al 2 0 3
  • Ti0 2 titanium oxide
  • metal oxides as a coating in the cutting technology are their high hardness and heat resistance and high chemical and thermal resistance. They are also highly resistant to corrosion and can still be used at high temperatures in the operating range up to 1000 ° C.
  • the metal oxide aluminum titanate (Al 2 Ti0 5 ) can also be used as a coating element in the machining industry.
  • the second material is a second inorganic solid.
  • the second inorganic solid is different from the first inorganic solid.
  • the difference is in particular, but preferably not exclusively in the electrical conductivity properties.
  • the second inorganic solid is an elemental metal, a boride, a carbide and / or a nitride.
  • the electrical conductivity of the second material is particularly important, whereby only electrically conductive borides, carbides and / or nitrides can be used as a second material. Elemental metals always have this required electrical conductivity.
  • the second inorganic solid is a
  • carbides denote a substance group whose chemical compound consists of a
  • Element (E) and carbon (C) is given by the general structural formula E x C y .
  • the group includes both salt-like and metallic compounds.
  • the metallic compounds of advantageous importance are characterized by a high mechanical and thermal stability and a high melting point (3000 ° C to 4000 ° C).
  • the carbide is tungsten carbide (WC), niobium carbide (NbC), hafnium carbide (HfC), tantalum carbide (TaC), titanium carbide (TiC), molybdenum carbide (MoC) and / or chromium carbide (Cr 3 C 2 ).
  • Tungsten carbide has a high hardness value and a melting point of 2785 ° C.
  • tungsten carbide is the main constituent of many carbide grades and is mainly used for cutting tools and as a material for heavy-duty components or forming tools.
  • Titanium carbide (TiC) is an inorganic chemical compound consisting of titanium and carbon.
  • the substance has a very good electrical conductivity and is stable in the air up to a temperature of 800 ° C. It is also characterized by a particularly high hardness value of up to 4000 HV (hardness according to Vickers).
  • the material is particularly known as a coating material for indexable inserts, milling tools, broaches, molds, saw blades and the like.
  • Molybdenum carbide like chromium carbide, is an intermetallic compound. Both materials can be used as a basis for corrosion-resistant hardmetal alloys. Niobium carbide (NbC) is of particular advantage as a material for the coating since this carbide has a much lower purchase price compared to tungsten carbide. In addition, it has very similar mechanical properties to WC, but has a lower density. Further advantageous metallic carbides are tantalum carbide (TaC) and hafnium carbide (HfC).
  • the third material is cemented carbide, cermet, cubic
  • Boron nitride or steel These materials find particular use in the manufacture of tool holders and cutting tools for machining e.g. for indexable inserts, turning, milling, drilling, reaming and finishing tools.
  • the voltage source is adapted to generate the electric DC field by energy pulses.
  • Energy pulses are also known under the name "high-energy impulse magnetron sputtering devices" (HiPIMS)
  • HiPIMS high-energy impulse magnetron sputtering devices
  • This embodiment has the advantageous effect that higher power can be applied to the cathode, through which the ionization of the process gas (ie the plasma formation) can be improved.
  • the target material material mixture of first and second material
  • the energy pulses typically have a pulse length between 1 ps and 150 ps and have particularly advantageous powers> 1 MW. Due to these very high powers at the cathode, significantly higher ionization degrees of the target material can be achieved. This high degree of ionization can significantly alter the properties of the growing layer on the substrate via the changed growth mechanisms and can, for example, contribute to an increased adhesive strength of the coating atoms on the substrate surface.
  • the voltage source is adapted to
  • the voltage source is adapted to apply to the substrate with a negative bias voltage.
  • the substrate When biasing the substrate with the bias voltage, the substrate is electrically isolated from the reaction chamber disposed therein.
  • the reaction chamber or a part of the reaction chamber serves as an anode and / or zero potential or ground for the magnetron sputtering device.
  • a negative voltage or a negative potential of -50 to -200 V is applied to the substrate, wherein the bias voltage may in principle also be below or above the aforementioned interval. Due to this substrate bias, the ion energy of the partially ionized plasma, which is generated by the energy input of the DC electric field between the cathode and the anode increases. The bias voltage leads to an ion bombardment of the substrate.
  • the substrate forms the anode.
  • the substrate is connected to the voltage source or is arranged on a substrate holder, which is connected to the voltage source.
  • the reaction chamber has a
  • the term "enclosure” is understood here, for example, a cathode plate that surrounds the cathode at least partially, but is arranged spatially separated from the latter within the reaction chamber.
  • a cathode sheet may, for example, be arranged at a defined distance from the cathode, so that there is a gap between the cathode sheet and the cathode.
  • the process gas plasma necessary for the sputtering process arises in the space between the enclosure and the cathode. In this case, the enclosure is co-coated during the coating process.
  • the advantage is that the geometry of the housing can be freely selected device-specific. For example, a very large surface can be provided which is used as an anode as a whole. HiPIMS in particular requires a large anode surface for a smooth process flow.
  • the term "material” is understood to mean the homogenization or the distribution of the atoms over the substrate surface.
  • An advantageous arrangement of the atoms of the first material relative to the atoms of the second material is, for example, when the respective boundary surfaces between the atoms of the first material and the atoms of the second material ensure an overall electrical conductivity of the substrate surface.
  • the inventive method comprises the following additional step: introducing a reactive gas into the interior of the reaction chamber, wherein the reactive gas methane, acetylene, nitrogen or oxygen, and wherein reactive gas ions of the reactive gas are adapted to, with Atoms of the first material and / or atoms of the second material to react.
  • the inert process gas preferably
  • An advantage of this method is that the layer properties during reactive sputtering can be influenced inter alia via the reactive gas inflow or the reactive gas volume flow.
  • reactive gases such as e.g. Hydrogen, water vapor, ammonia, hydrogen sulfide, methane or Tetraflu- ormethan be used.
  • Fig. 1 is a schematic view of an embodiment of a
  • Fig. 2 is a scanning electron micrograph of an exemplary
  • FIG. 3 is a photomicrograph of the exemplary composition Zr0 2 -WC
  • Fig. 4 is a scanning electron micrograph of an exemplary
  • Fig. 5 is a schematic process flow.
  • Fig. 1 shows a magnetron sputtering apparatus according to an embodiment of the present invention, wherein the magentron sputtering apparatus is generally designated by the reference numeral 100.
  • the magnetron sputtering apparatus 100 has a reaction chamber 10 in which
  • the substrate table 14 is rotatable and can be set in rotation by means of a drive motor not shown here, wherein the rotational speed (in rpm) can be controlled.
  • the substrate table 14 may be, for example, a rotatably mounted circular metal plate.
  • a substrate carrier 18 is arranged, which in the here shown
  • the substrate carrier 18 may be embodied, for example, as a basket-like device and be made of an electrically conductive or electrically non-conductive material, depending on the application.
  • the substrate carrier 18 serves to receive or reversibly fix the substrate 20 during a coating process.
  • four substrates are on the substrate support 18
  • the substrates 20 may be, for example, milling heads to be coated in the magnetron sputtering apparatus 100. According to the invention, however, only one substrate 20 has to be present.
  • Target (s) 16 and substrate (s) 20 are arranged in the interior 12 of the reaction chamber 10 spatially separated from each other.
  • the reaction chamber 10 is connected to a vacuum pump 22, which is set up to generate a vacuum or at least a negative pressure in the interior space 12 of the reaction chamber 10 before the start of the coating process.
  • the vacuum pump 22 may be configured, for example, as a turbo pump. It is used to remove 10 reactive gas molecules, such as nitrogen and / or oxygen or air from the interior 12 of the reaction chamber before the start of the coating process, whereby in the interior 12, a negative pressure.
  • an inert process gas e.g. Argon or another noble gas
  • the gas inlet 24 may be designed, for example, as a gas clutch, in each case ensuring a hermetic sealing of the gas inlet 24.
  • the magnetron sputtering apparatus 100 also has a voltage source 26 which is adapted to generate a DC electric field.
  • the voltage source 26 from FIG. 1 has two electrical outputs 28, 30, wherein in the representation shown here the negative voltage output 28 is connected in each case to the six targets 16 shown, whereby the targets 16 in the example shown in FIG electric DC field form the cathode 30.
  • the target 16 does not necessarily serve as the cathode 30. It is also possible the
  • Substrate table 14 by a corresponding interconnection with the negative voltage output 28 and by the applied voltage as (additional) cathode 30 to use.
  • a target carrier (not shown here) may be used as the cathode 30.
  • the positive voltage output 32 of the voltage source 26 is connected to the reaction chamber 10 by way of example, whereby the reaction chamber 10 forms the anode 34 in the DC electric field.
  • the substrate carrier 18 or a device can be used as the anode 34. tion, such as one or more enclosure (s) for the target (s) 16.
  • a plurality of anodes 34 may be used.
  • at least one anode 34 serves as a ground.
  • the commercially available DC magnetron sputter CemeCon system can be switched, for example, against a "special" anode pair 34, which is referred to as a so-called "booster". These "boosters" have a copper surface.
  • the voltage source (s) 26 may be configured to supply a pulsed electrical power to the cathode 30, these energy pulses (ie, providing the electrical power for a certain pulsed period of time) advantageously having a power> 0.1 MW, preferably > 0.5 MW, more preferably> 1 MW have.
  • the voltage source 26 may have, for example, a pulse generator and / or a pulse width modulator and is advantageously configured to generate a multiplicity of pulse shapes, pulse lengths and / or pulse amplitudes.
  • the substrate 20 to be coated is provided and arranged in the substrate carrier 18 (step S100). This arrangement can be done for example by inserting, threading, skewering, clamping or screwing the substrate 20 into or on the substrate carrier 18.
  • the target 16 (six targets 16 in FIG. 1) is to be provided and arranged in the interior space 12 of the reaction chamber 10 (step S101), which can be arranged, for example, by attaching the target to a target carrier.
  • the substrate carrier 18 is connected to the positive voltage output 32 of the voltage source 26, whereby the target 16 forms the cathode 30 together with the target carrier not shown here.
  • the six targets 16 have an electrically conductive substance mixture 36 for coating the substrate 20, wherein the substance mixture 36 comprises a first material 38 and a second material 40.
  • the first material 38 is an electrically non-conductive solid.
  • the second material 40 is an electrically conductive solid.
  • Step S102 wherein this provision can be made, for example (as in FIG. 1), by connecting the positive voltage output 32 of the voltage source 26 to the reaction chamber 10.
  • the substrate 20 comprises a third material 42, wherein the third material 42 is an electrically conductive solid.
  • the reaction chamber 10 can for example be closed by a hermetically sealable door.
  • a vacuum / vacuum is generated in the interior 12 of the reaction chamber 10 via the vacuum pump 22.
  • an additional heating by a heater take place, through which the interior 12 of the reaction chamber 10 is heated to a process temperature.
  • the process gas is introduced into the interior space 12 of the reaction chamber 10 via the gas inlet 24 (step S103) and a DC electric field is generated by the voltage source 26 between the cathode 30 and the anode 34 (step S104).
  • the DC electric field generated by the power source 26 calls a
  • FIG. 2 shows a scanning electron micrograph of the surface of an exemplary target 16.
  • the target 16 has the electrically conductive substance mixture 36, which in the case shown here is Zr0 2 -WC.
  • FIG. 3 shows a corresponding light microscope image of the substance mixture 36.
  • Substance mixture 36 consists of the first electrically nonconductive material 38 (here zirconium oxide (Zr0 2 )) and the second electrically conductive material 40 (here tungsten carbide (WC)).
  • the first material 38 has a first volumetric proportion AV-i and the second material 40 a second volumetric proportion AV 2, where advantageously applies: AV i> AV 2, preferably AV i> 1, 5 AV. 2
  • the target 16 can be produced for example by hot pressing or a sintering process. Depending on the manufacturing process and manufacturing process, smaller or larger amounts of microstructure in the substance mixture 36 result.
  • the first material 38 may in the most general case be an electrically non-conductive solid. It is advantageous if the first material 38 is a first inorganic solid. It is equally advantageous if the first inorganic solid is a carbide, an oxide and / or a nitride, more preferably a metal oxide. It is particularly advantageous if the metal oxide Zr0 2 , Al 2 0 3 or Ti0 2 .
  • the second material 40 may in the most general case be an electrically conductive solid. It is advantageous if the second material 40 is a second inorganic solid. It is likewise advantageous if the second inorganic solid is an elementary metal, a boride, a carbide, and / or a nitride. ter is a carbide. It is particularly advantageous if the carbide is WC, NbC, HfC, TaC, TiC, MoC and / or Cr 3 C 2 .
  • Fig. 4 shows a scanning electron micrograph after the coating of the
  • Substrate 20 with Zr0 2 -WC was deposited on the surface of the substrate 20, the substrate 20 having the third material 42.
  • the third material 42 is cemented carbide, cermet, cubic boron nitride or steel.
  • Heating phase 1 Start pressure at start of heating 3 mPa
  • Heating phase 2 Heating power Heating 1 9 kW
  • HiPIMS table pulse offset 20 ps
  • Table 2 Variation of the frequency and pulse length of high energy pulses in an exemplary high energy impulse magnetron sputtering process and their influence on the substrate coating.
  • a first heating phase (heating phase 1) was carried out in which the vacuum pump 22 or turbopump was operated at full power to generate the vacuum.
  • This full utilization of the turbopump is necessary because during the heating process, i.
  • the turbopump must remove a larger amount of free molecules from the reaction chamber.
  • the second heating phase (heating phase 2) followed, during which the turbopump was operated at 66% of its capacity. This second heating phase is advantageous in order to ensure a complete heating of the targets 16 and the substrate 20, or to ensure a stabilization of the process temperature.
  • Term “Medium Frequency Etching” is known.
  • the substrate 20 is subjected to a high bias voltage in comparison to the cathode voltage. Due to this high negative bias, more process gas ions impact on the substrate surface than on the target surface. As a result, the surface of the substrate 20 is freed from impurities and additionally roughened for the subsequent coating process, whereby the layer adhesion can be improved.
  • the first etching phase lasted 1200 seconds. Following the first etching phase, the second etching phase followed for a duration of 3600 seconds.
  • argon and krypton were introduced into the reaction chamber 10 and brought into an ionized state (in the form of an ion beam) by an additional plasma booster current.
  • This second etching phase is particularly advantageous for substrates 20 with a large number of edges, since the edges are only slightly cleaned or roughened in the first etching phase.
  • the "argon ion etching" leads to a better adhesion of the layer on the substrate surface, wherein the plurality of edges of the substrate can be cleaned or roughened by the ion beam.
  • the "coating" process step relevant to the invention was carried out, with both the frequency and the pulse length of the high-energy pulses being varied.
  • the layer thickness can be influenced by setting deposition parameters such as HiPIMS frequency, HiPIMS pulse width, temperatures, bias voltage, flow quantities of the gases introduced, and the quantity of the operated targets 16, the respective influence of these process parameters being known from the prior art Technique is known.
  • Cathodes of 40 ps and a coating time of 18000 s produced a substrate coating with a layer thickness of 2.4 pm, a hardness of 22.8 GPa and an E modulus of 380 GPa.
  • a HiPIMS frequency of 2500 Hz a pulse length at the cathodes of 60 ps and a coating time of 10,800 s
  • a substrate coating with a layer thickness of 1.8 ⁇ m a hardness of 21.5 GPa and an E was used Module of 440 GPa generated (see Table 1).
  • the hardness and elastic modulus were determined by nanoindentation in the
  • Unit GPa measured.
  • a diamond specimen having a three-sided pyramidal shape is pressed into the layer and a force-displacement curve is recorded. From this curve, the mechanical characteristics of the layer can be determined according to the Oliver-Pharr method.
  • a NHT1 from CSM, Switzerland was used.
  • a cooling step was performed, wherein the reaction chamber 10 was cooled by aeration.
  • Heating phase 1, heating phase 2, etching phase 1, etching phase 2 and cows are only advantageous, but not necessarily with the Magnetronsputtervor- device 100 according to the invention or in the inventive method must be performed.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

L'invention concerne un dispositif de pulvérisation cathodique à magnétron (100), comprenant : un substrat (20) ; une cible (16) qui forme une cathode (30) dans un champ de tension continue électrique et qui comprend un mélange électroconducteur de matières (36), destiné à revêtir le substrat (20) ; une anode (34) dans le champ de tension continue électrique ; une chambre de réaction (10) dans laquelle sont agencés la cible (16) et le substrat (20), la cible (16) étant agencée de façon à être séparée dans l'espace du substrat (20) ; et une source de tension (26) qui est conçue pour produire un champ de tension continue électrique entre la cathode (30) et l'anode (34) ; le mélange de matières (36) comprenant un premier matériau (38) ainsi qu'un deuxième matériau (40), et le substrat (20) comprenant un troisième matériau (42), le premier matériau (38) étant une matière solide non électroconductrice, le deuxième matériau (40) étant une matière solide électroconductrice et le troisième matériau (42) étant une matière solide électroconductrice.
EP19720848.1A 2018-05-23 2019-04-29 Dispositif de pulvérisation cathodique à magnétron Pending EP3768871A1 (fr)

Applications Claiming Priority (2)

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DE102018112335.3A DE102018112335A1 (de) 2018-05-23 2018-05-23 Magnetronsputtervorrichtung
PCT/EP2019/060913 WO2019223959A1 (fr) 2018-05-23 2019-04-29 Dispositif de pulvérisation cathodique à magnétron

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US (1) US20210050192A1 (fr)
EP (1) EP3768871A1 (fr)
JP (1) JP7168686B2 (fr)
CN (1) CN112154226A (fr)
DE (1) DE102018112335A1 (fr)
MX (1) MX2020012423A (fr)
WO (1) WO2019223959A1 (fr)

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TW202200816A (zh) * 2020-05-28 2022-01-01 日商三菱綜合材料股份有限公司 濺鍍靶材及光學功能膜

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WO2019223959A1 (fr) 2019-11-28
JP2021524884A (ja) 2021-09-16
DE102018112335A1 (de) 2019-11-28
JP7168686B2 (ja) 2022-11-09
CN112154226A (zh) 2020-12-29
US20210050192A1 (en) 2021-02-18

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