CN107130213B - Multicomponent alloy laminated film Preparation equipment and preparation method - Google Patents
Multicomponent alloy laminated film Preparation equipment and preparation method Download PDFInfo
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- CN107130213B CN107130213B CN201710305293.8A CN201710305293A CN107130213B CN 107130213 B CN107130213 B CN 107130213B CN 201710305293 A CN201710305293 A CN 201710305293A CN 107130213 B CN107130213 B CN 107130213B
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- 239000000956 alloy Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 52
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 47
- 238000004544 sputter deposition Methods 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 38
- 238000010438 heat treatment Methods 0.000 claims abstract description 32
- 238000001704 evaporation Methods 0.000 claims abstract description 27
- 230000008020 evaporation Effects 0.000 claims abstract description 26
- 238000000151 deposition Methods 0.000 claims abstract description 24
- 230000008021 deposition Effects 0.000 claims abstract description 20
- 230000003028 elevating effect Effects 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 230000007246 mechanism Effects 0.000 claims abstract description 10
- 150000002500 ions Chemical class 0.000 claims description 43
- 239000000758 substrate Substances 0.000 claims description 14
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002131 composite material Substances 0.000 claims description 10
- 230000005672 electromagnetic field Effects 0.000 claims description 10
- 230000001681 protective effect Effects 0.000 claims description 10
- 230000005611 electricity Effects 0.000 claims description 6
- 238000010894 electron beam technology Methods 0.000 claims description 5
- 238000012423 maintenance Methods 0.000 claims description 4
- 230000005855 radiation Effects 0.000 claims description 4
- 229910000765 intermetallic Inorganic materials 0.000 claims description 3
- 239000004744 fabric Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 abstract description 30
- 239000011248 coating agent Substances 0.000 abstract description 27
- 238000005520 cutting process Methods 0.000 abstract description 25
- 238000001755 magnetron sputter deposition Methods 0.000 abstract description 23
- 238000007733 ion plating Methods 0.000 abstract description 15
- 238000005516 engineering process Methods 0.000 abstract description 14
- 238000007738 vacuum evaporation Methods 0.000 abstract description 6
- 239000002103 nanocoating Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 98
- 239000000463 material Substances 0.000 description 18
- 239000007789 gas Substances 0.000 description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- 239000010409 thin film Substances 0.000 description 13
- 229910010037 TiAlN Inorganic materials 0.000 description 12
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 10
- 239000011651 chromium Substances 0.000 description 10
- 229910052718 tin Inorganic materials 0.000 description 10
- 239000010936 titanium Substances 0.000 description 10
- 229910052804 chromium Inorganic materials 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 229910052786 argon Inorganic materials 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000003754 machining Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 229910052726 zirconium Inorganic materials 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 239000004615 ingredient Substances 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 229910052774 Proactinium Inorganic materials 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000010891 electric arc Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910017150 AlTi Inorganic materials 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 229910010038 TiAl Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000012790 confirmation Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000002513 implantation Methods 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 244000144985 peep Species 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 238000005477 sputtering target Methods 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- QFUKUPZJJSMEGE-UHFFFAOYSA-N 5-(hydroxymethyl)-1-(3-methylbutyl)pyrrole-2-carbaldehyde Chemical compound CC(C)CCN1C(CO)=CC=C1C=O QFUKUPZJJSMEGE-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 229910000423 chromium oxide Inorganic materials 0.000 description 2
- 239000012459 cleaning agent Substances 0.000 description 2
- 230000000994 depressogenic effect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000007888 film coating Substances 0.000 description 2
- 238000009501 film coating Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 238000000992 sputter etching Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000013077 target material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- 229910000997 High-speed steel Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- -1 and Al Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
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- 230000004044 response Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
-
- 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
- C23C14/24—Vacuum evaporation
- C23C14/26—Vacuum evaporation by resistance or inductive heating of the source
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B1/00—Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic 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
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/347—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with layers adapted for cutting tools or wear applications
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
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- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Nanotechnology (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The present invention discloses a kind of multicomponent alloy laminated film Preparation equipment and preparation method, especially a kind of multicomponent alloy laminated film Preparation equipment for being related to nano coating technical field and preparation method.The present invention provides a kind of multicomponent alloy laminated film Preparation equipment of cutting tool comprehensive performance for being remarkably improved institute's plated film, including heating system, air supply system, cooling system, vacuum system, vacuum chamber, luggage carrier, elevating mechanism, crucible evaporation source, controlled sputtering source, cathode arc source and electric control system.The group technology of cathodic arc ion plating and magnetron sputtering may be implemented in the equipment of the application, and the binary evaporation source technique that vacuum evaporation coating is combined with magnetron sputtering, carry out the preparation of multicomponent alloy laminated film, accurately control the institutional framework of all kinds of films, to obtain the comprehensive excellent multi-element film such as high hardness, low internal stress, high binding force, low roughness, good wearability, and there is high deposition rate during the preparation process.
Description
Technical field
It is related to nanometer the present invention relates to a kind of multicomponent alloy laminated film Preparation equipment and preparation method, especially one kind to apply
The multicomponent alloy laminated film Preparation equipment and preparation method of layer technical field.
Background technique
Manufacturing develop be unable to do without cutting tool, and modern cutting tools have become the pass for promoting manufacturing industry technical level
One of key factor.At a high speed, efficiently, intelligence and environmental protection become the target that machining is pursued, high-intensitive, high-toughness material and height
The difficult-to-machine materials performance such as temperature alloy, titanium alloy is continuously improved, and proposes requirements at the higher level to cutting tool.Modern cutting technology
Be related to that ambit is wide, wherein modified (coating) technology of tool surface be in response to the market demand and the modern cutting technology that grows up
One of.It is widely used to the industries such as aerospace, automobile, the energy, ship, power generation at present, it has also become manufacturing key skill
One of art.
Cutting tool is in addition to that should have good ambient temperature mechanical properties, outside intensity, toughness, hardness, for high-speed cutting,
For dry cutting, hard machining etc., should also have excellent hot property, such as anti-chemical affinity, diffusion, dissolution, thermal shock resistance properties,
Mechanical behavior under high temperature etc..
The one kind of coating as modern cutting tools process for modifying surface, by method chemically or physically in cutter table
Micro-, nanoscale film is obtained on face, and has the characteristics that hardness is high, lubricity is good, high-temperature behavior is excellent.Table is carried out to cutter
Finishing coat processing is important channel and the means for improving cutting tool comprehensive performance, can tool life, raising processing
Efficiency and machining accuracy facilitate the realization of high-speed cutting, dry cutting, hard machining, precision cutting process.
During High-speed machining or DRY CUTTING, cutting temperature becomes the main original for influencing coated cutting tool service life
Cause, therefore improve the high-temperature behavior of film, guarantee that the red hardness of coated cutting tool becomes PVD (Physical Vapor in recent years
Deposition) the exploitation hot spot of technology.The content for improving Al in TiAlN film is to improve the effective method of coating performance
One of, with the increase of Al content, the hardness and high-temperature behavior of film are all being improved, but bring is stress in thin films therewith
Increase, the decline of toughness and the increase with iron-based material compatibility, so as to cause the generation of built-up edge.Therefore in practical application
In, the comprehensive performance of such coated cutting tool does not obtain the change of essence.From the point of view of the latest development, it is multiple to develop multicomponent alloy
It is very necessary for closing thin film technique.The Basic Ways of ganoine thin film improved combination properties are the diversification of thin film composition, benefit
With the feature of different elements respectively, realize that the matched well of integrated performance index is always polynary, main think of of superhard film development
One of road.By change thin-film material ingredient come solve high speed, high-temperature machining processing problems, such as routine TiN, TiAlN,
Cr and Y is added in AlCrN can be improved inoxidizability；Zr, V, B and Hf, which is added, can be improved abrasion resistance；Si, which is added, can be improved hardness
With anti-chemical diffusivity.
The most common technology of PVD can be divided into three categories: vacuum evaporation coating VE (Vacuum Evaporating), magnetic control splash
Penetrate MS (Magnetron Sputtering), cathodic arc ion plating AIP (Arc Ion Plating).
In vacuum evaporation coating evaporation process, evaporation rate and its influence factor of membrane material etc. and the close phase of its saturated vapour pressure
It closes.Therefore it is evaporated in vacuo restriction of the coating technology by material properties, will lead to the segregation of ingredient for the evaporation of alloy material.
For magnetron sputtering technique compared with cathodic arc ion plating technology, deposition efficiency is lower, and the ionization level of atom also compares
Low, stress present in the Thin Film Tissue of preparation is also larger, and magnetron sputtering is poor around plating property and binding force.
Cathodic arc ion plating, in membrane-film preparation process, some metallic particles, the big molten drop generated by cathode arc source is easy
The surface for pressing from both sides in the film or depositing to film, on the one hand will affect the compactness of film, reduces the service life of film, another
It is coarse that aspect will lead to film surface；Thin film composition is relatively single.
Therefore, the single equipment technology of the prior art is difficult to meet a variety of requirements, bad adaptability, prepared film
Comprehensive performance is not high, cannot achieve the preparation of the multicomponent alloy laminated film of high-quality.
Summary of the invention
The cutting tool that institute's plated film can be significantly improved technical problem to be solved by the invention is to provide one kind is comprehensive
The multicomponent alloy laminated film Preparation equipment of energy.
The present invention solves multicomponent alloy laminated film Preparation equipment used by its technical problem, including heating system, confession
Gas system, cooling system, vacuum system, vacuum chamber, luggage carrier, elevating mechanism, crucible evaporation source, controlled sputtering source, cathode electricity
Arc source, electromagnetic field generator and electric control system, the vacuum system and vacuum chamber, the elevating mechanism and loading
Frame transmission connection, the air supply system and vacuum chamber, the electric control system and crucible evaporation source, controlled sputtering source,
Cathode arc source, electromagnetic field generator, heating system electrical connection, the crucible evaporation source, controlled sputtering source, cathode arc source
In vacuum chamber, the target-substrate distance of the cathode arc source is 160mm to 230mm, and the target-substrate distance of the controlled sputtering source is
50mm to 75mm.
Further, further including heated filament ion source, the heated filament ion source is arranged in a vacuum chamber, the heated filament ion
Source is electrically connected with electric control system.
Further, the electric control system includes ion source current, argon-arc plasma field maintenance power supply, sputtering source electricity
Source, cathode arc power supply, grid bias power supply, the argon-arc plasma field maintain power supply and ion source current to connect with heated filament ion source, institute
It states sputtering source current to connect with controlled sputtering source, the cathode arc power supply is connect with cathode arc source.
Further, the heating system includes being located at heating system inside the electron beam in the middle part of vacuum chamber and being located at true
The external radiation heating system of empty room furnace wall surrounding.
Further, the controlled sputtering source is symmetrically distributed in the inner wall of vacuum chamber, the cathode arc source is with vacuum
The centre of gyration of room is symmetry axis, is spirally distributed the inner wall in vacuum chamber.
Further, the vacuum system includes molecular pump, lobe pump, mechanical pump, maintains pump, the molecular pump and true
Empty room connection, the exhaust outlet for maintaining pump to be connected to molecular pump are connect, the exhaust outlet connection of the lobe pump and molecular pump, institute
The exhaust outlet for stating mechanical pump and lobe pump connects.
Further, further including protective case, the protective case is mounted on side of the cathode arc source towards luggage carrier, institute
It states protective case and is additionally provided with baffle far from the side of cathode arc source.
It is comprehensive that another technical problem solved by the invention is to provide a kind of cutting tool that can significantly improve institute's plated film
The method for closing the multicomponent alloy laminated film preparation of performance.
The present invention solves the preparation method of multicomponent alloy laminated film used by its technical problem, utilizes cathode arc source
While carrying out multicomponent alloy material ions deposition, single metallic elements are mixed using controlled sputtering source, it is compound to form multicomponent alloy
Film layer.
Further, depositing to form metallic compound in workpiece surface by crucible evaporation source evaporated metal element
Other elements are implanted by controlled sputtering source simultaneously, form multicomponent alloy laminated film in workpiece surface.
The beneficial effects of the present invention are: AIP (yin may be implemented using the multicomponent alloy laminated film Preparation equipment of the application
Pole electrical arc ion plating) with the group technology of MS (magnetron sputtering) and VE (vacuum evaporation coating) and MS (magnetic controlled sputtering ion plating)
The binary evaporation source technique combined carries out the preparation of multicomponent alloy laminated film, flexibly realizes the in due course variation of coating composition,
The institutional framework for accurately controlling all kinds of films, by mixing single metallic elements, significantly improving thin while AIP ion deposition
The performance of film, to obtain high rigidity, the comprehensive performances such as low internal stress, high-bond, low roughness, good wearability are excellent
Different multiple elements design film, and there is very high deposition rate during the preparation process.
Detailed description of the invention
Fig. 1 is the general assembly drawing of the application；
Fig. 2 is the structural schematic diagram of the vacuum chamber of the application；
Fig. 3 is the plane outspread drawing of vacuum chamber；
Fig. 4 is the structural schematic diagram of heated filament ion source；
Fig. 5 is the structural schematic diagram of luggage carrier；
Fig. 6 is the XRD spectrum of the AlCrN film prepared using single cathode arc；
Fig. 7 is that the XRD spectrum of AlCrN film is prepared using AMS technique using equipment of the invention；
Fig. 8 is the hardness image of the AlCrN film prepared using single cathode arc；
Fig. 9 is that the hardness image of AlCrN film is prepared using AMS technique using equipment of the invention；
Figure 10 is the XRD spectrum of the TiAlN film prepared using single cathode arc；
Figure 11 is, using AMS technique by addition element, to adjust Al using equipment of the invention67Ti33After N structure
The XRD spectrum of TiAlN film；
Figure 12 is the hardness image of the TiAlN film prepared using single cathode arc；
Figure 13 is, using AMS technique by addition element, to adjust Al using equipment of the invention67Ti33After N structure
The hardness image of TiAlN film；
Figure 14 is the voice signal figure using the slight crack experiment of the AlCrN film of prior art preparation；
Figure 15 is the present invention using while AIP carries out AlCrN compound deposition, is just implanted into simple substance elements Mo by MS
The voice signal figure of the slight crack experiment of film obtained；
Figure 16 is the structural schematic diagram of cathode arc source of the present invention；
Figure 17 is individually using film microstructure figure made from AIP；
Figure 18 is to utilize MS to be implanted into film microstructure figure prepared by Me element simultaneously using AIP.
Main parts size and number in figure: loading vehicle motor 1, carrier 2, luggage carrier 3, vacuum chamber bracket 4, elevating screw
5, coil 6, peep hole 7, cathode arc source 8, controlled sputtering source 9, heated filament ion source 10, gas flow interface 11, vacuum cavity
12, high vacuum valve 13, molecular pump 14, forevacuum valve 15, pre- pumping valve 16, by-passing valve 17, lobe pump 18, maintenance pump 19, machinery
Pump 20, vacuum system bracket 21, impressed current anode 22, crucible evaporation source 23, substrate 24, protective case 25, baffle 26, workpiece 27, in
Interbed 28, AlCrMeN composition 29, MeNx composition 30, AlCrN ingredient 31.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings.
As shown in Figures 1 and 2, multicomponent alloy laminated film Preparation equipment of the invention, including heating system, gas supply system
System, cooling system, vacuum system, vacuum chamber, luggage carrier 3, elevating mechanism, crucible evaporation source 23, controlled sputtering source 9, cathode electricity
Arc source (i.e. the source CAE), electromagnetic field generator and electric control system, the vacuum acquiring system and vacuum chamber, it is described
Elevating mechanism and luggage carrier 3 are sequentially connected, the air supply system and vacuum chamber, and the electric control system and crucible evaporate
Source 23, controlled sputtering source 9, cathode arc source 8, electromagnetic field generator, heating system electrical connection, the crucible evaporation source 23,
Controlled sputtering source 9, cathode arc source 8 are located in vacuum chamber, and the target-substrate distance of the cathode arc source 8 is 160mm to 230mm, institute
The target-substrate distance for stating controlled sputtering source 9 is 50mm to 75mm.
Vacuum chamber is evacuated by vacuum system, forms vacuum cavity 12, makes the preparation process of multicomponent alloy laminated film,
It is completed in the vacuum environment for meeting preparation process standard.As shown in figure 5, wherein luggage carrier 3 is for the fixed knife for needing plated film
Has and realizes the two-dimensional surface movement of cutter, elevating mechanism is used to move luggage carrier 3.The wherein two-dimensional surface movement of luggage carrier 3
Elevating movement with elevating mechanism can be by the way of mechanically widely applied worm drive.Specific implementation is can also to add
Load vehicle motor 1, carrier 2, elevating mechanism use elevating screw 5, and provide the vacuum chamber bracket 4 of support vacuum chambers,
Coil 6 is additionally provided with above vacuum chamber.
Crucible evaporation source 23 for completing the coating of composite Ti N, CrN, ZrN in membrane-film preparation process, and as auxiliary from
The reception anode in change source realizes that gas ion etches purpose.And crucible evaporation source 23 can play vacuum chamber by evaporation
Cleaning effect, operating cost is low, diffractive good, the consistency of continuous work can be ensured, particularly with non-conductive film
It prepares for a long time particularly critical.
Cathode arc source 8 is used in multicomponent alloy laminated film preparation process, with cathodic arc ion plating (AIP) deposition
Based on technique and the addition for carrying out the polynary element of multicomponent alloy material technical process.
Controlled sputtering source 9 is used in the implantation technique of multicomponent alloy laminated film preparation process microelement.
Heating system is for heating vacuum chamber in multicomponent alloy laminated film preparation process, to maintain polynary conjunction
Stable environment temperature required for golden composite film preparation technology.
Cooling system is used to meet the requirement of cooling technique in multicomponent alloy laminated film preparation process, carries out to vacuum chamber
Timely and effectively cool down.
Air supply system is mainly used for being passed through Ar, N into vacuum chamber2、H2、O2Equal gases, and the amount for the gas being passed through is carried out
Accurate regulation.The application preferably uses six road mass flow control systems, and maximum stream flow is 300~1000sccm.
The electromagnetic field generator of this equipment makes the drive in electric arc arc spot variable electromagnetic field for generating variable electromagnetic field
Under dynamic, not only along target surface annulus fast run, and radially move back and forth so that arc spot run faster, it is more；
(under the driving of variable magnetic field, arc spot movement speed can be made compared to not using 30% or more raising, the number of arc spot when variable magnetic field
Amount, which is compared not use, improves 30% or more when variable magnetic field) in addition, the plasma generated near evaporation material surface, passes through
Variable electromagnetic field can be pushed to coating film area (distance can be greater than 300mm), greatly strengthen the indoor plasma density of vacuum,
The environment and condition of reactive ion plated film are improved, so as to significantly improve reactive ion coating quality.
Following coating process may be implemented to enhance by plated film using the multicomponent alloy laminated film Preparation equipment of the application
The comprehensive performance of workpiece 27:
In the prior art employed in film preparation be vacuum evaporation coating, magnetron sputtering, cathodic arc ion plating its
A kind of middle monotechnics, or bottom film is made first with cathodic arc ion plating, recycle magnetron sputtering to do top film,
That is the method that carries out respectively of cathodic arc ion plating and magnetron sputtering.There is no phase using the material between each film of the above method
Mutually fusion, but layered coverage, on 27 surface of workpiece, the performance of each layer is single, is unable to fully realize to various material excellent properties
Comprehensive utilization, keep the comprehensive performance of final obtained film relatively low.
And equipment of the invention, it in a vacuum chamber will be to cathode arc source 8, controlled sputtering source 9 combines, and to its space bit
It sets and optimizes arrangement, make the target-substrate distance 160mm to 230mm of cathode arc source 8, the target-substrate distance of controlled sputtering source 9 is 50mm
To 75mm.Wherein target-substrate distance refer to the targets source such as cathode arc source 8 or controlled sputtering source 9 to the surface of workpiece 27 to be coated away from
From.In this way using equipment of the invention may be implemented cathodic arc ion plating and magnetron sputtering and meanwhile carry out technique, AIP into
While row deposition, microelement is implanted by MS, final film obtained is made closely to have merged a variety of alloys within the same layer
Material and single metallic elements further increase the performance of film by the incorporation of single metallic elements, to make using aforementioned side
Legal system obtains film while having high rigidity, low internal stress, high-bond, low roughness, high-wearing feature performance, and have very
High deposition.
Based on depositing using the equipment of the application with AIP, using multicomponent alloy material means, pass through cathode arc source 8
(CAE), the synthesis of polynary element thin film is realized；The implantation of microelement then uses the MS technical solution (combination abbreviation of AIP and MS
AMS), relative components content is less than 1%.The accurate control to film phase structure may be implemented, can achieve most preferably with obtaining
Mechanical property film phase structure.Figure 17 is when Me target current is 0A, i.e., merely using film knot made from AIP method
Structure, bottom is substrate 24 in figure, and be close to substrate 24 be middle layer 28 against middle layer 28 is AlCrN ingredient 31.Figure 18 is
When Me target current improves, i.e., using membrane structure obtained when MS implantation Me element, the characteristics of obtained film, is: short
Column structure form.Bottom is substrate 24 in figure, be close to substrate 24 be middle layer 28 against middle layer 28 be AlCrMeN at
Divide 29 and MeNx ingredient 30.It can be seen that coating is when Me target current is 0A with typical column by the comparison of Figure 17 and Figure 18
The growth of shape crystalline form state, when Me target current improves, a part of Me atom enters MeNx crystal lattice replacement Cr atom, plays to coating
Solution strengthening effect, another part Me form Me and form tiny MeNx crystal grain inhibition AlCrN crystal in the presence of with AlCrN intergranular
Invigoration effect is played in further growth.
The binary evaporation source that vacuum evaporation coating is combined with magnetic controlled sputtering ion plating may be implemented using equipment of the invention
Technology；Passed through while workpiece surface deposits to form metallic compound by crucible evaporation source evaporated metal element
Controlled sputtering source is implanted into other elements, can be in N in workpiece surface formation multicomponent alloy laminated film, specific implementation2With Ar's
Under mixed atmosphere, Ti element is evaporated by electron beam evaporation source 23, forms traditional TiAlN thin film, forms the same of TiN film in deposition
When by controlled sputtering source 9 be implanted into X element, be coated with (Ti on tool and mould surfaceX, Me1-X) N layers；The X is in Al, Cr, Si
It is at least one.Since TiN is a kind of ideal thin film system, there is extensive preparation basis, such as the methods of AIP, MS, VE
Industrialization production requirements can all be met.TiN has excellent physics, chemical property, as hardness is high, coefficient of friction is low, good
Chemical compatibility etc. is the desired coating material of slow cutting process tool, it can mitigate cutting edge portion and processed material
Adherency increases cutting-tool's used life and improves processing efficiency, is still at present using more one of thin-film material.But it is traditional
TiN hardness is relatively low, wearability is short of, thermal stability is poor, limits its and widely applies.The improvement of TiAlN thin film is main
In terms of being embodied in novel TiN based alloy and multiple elements design layer.In addition, the binary nitride of magnesium-yttrium-transition metal, carbide are often
It can dissolve each other each other, by adding certain elements into TiN film, nitride type compound can be formed and close object, and then can be from basic
The upper performance for changing TiAlN thin film, improves its abrasion resistance and thermal stability.Using TiN as base, multi-element alloyed changeable control is thin
The phase structure of film obtains so-called (TiX, Me1-X) N membrane system.Polynary element can be related to C, Si, Cr, Al, Mo, W, V, Zr, Y,
La etc..
Using the equipment of the application with AIP deposit based on the preparation of insulation oxide film may be implemented.Although AIP is helped
It is higher in the deposition of the generation of ionization, plated film, but in O2When excessive or original electric field changes, O2It is easier in yin
It reacts on the target surface of pole, required element cannot normally be exported by generating oxide to cause the failure of cathodic discharge.
The oxide of PVD is mainly aluminium oxide at present, and Al, AlTi material are easier to relatively and O2It reacts, therefore conventional way exists
The Cr of certain content is added in Al material, can effectively prevent the oxidation of target surface, but chromium oxide stability is relatively poor, will lead to
The change of film performance.Although therefore the prior art thinks that AIP deposition is high, the insulation met the requirements can not be prepared with it
Sull.And the variable electromagnetic for using the device, method of the application to generate by control system and electromagnetic field generator,
It can guide and drive O2It is mobile towards 27 direction of workpiece of plated film, to effectively prevent O far from target body2On cathode target surface
It reacts, generates oxide, prepare high performance sull, overcoming cannot be prepared in the prior art using AIP
The technology prejudice of insulation oxide.
As shown in figure 4, further including heated filament ion source, the heated filament ion source is arranged in a vacuum chamber, the heated filament ion
Source is electrically connected with electric control system.The heated filament ion source that the application adds can significantly increase gas etching effect.For knife
Have for coating, vacuum etching, activation are most important.Give up traditional high bias of CAE metal using equipment of the invention to bang
Blow mode, and gas ion low bias etching method is used, more uniform, whole clean effect can be obtained, and guarantee
The integrality of cutting edge.Furthermore the heated filament ion source that the application adds can also play internal heating, increase ionization intensity, auxiliary
The effect for helping deposition is played the role of increasing plasma when being individually evaporated ion plating.
The electric control system includes ion source current, plasma maintenance power supply, sputtering source current, cathode arc electricity
Source, grid bias power supply, the argon-arc plasma field maintain power supply and ion source current to connect with heated filament ion source, the sputtering source current and
Controlled sputtering source 9 connects, and the cathode arc power supply connect with cathode arc source 8, grid bias power supply and workpiece to be plated 27 when work
Connection.Wherein ion source current is heated filament ion source by power supply, and plasma maintains power supply to provide arc for heated filament ion source
Power supply, sputtering source current are controlled sputtering source 9 by power supply, and cathode arc power supply is that cathode arc source 8 provides power supply.Bias plasma
Source provides the electric field of control charged ion movement.Electric control system is mainly that the electric component of this equipment provides corresponding parameter
Adjustable power supply, wherein the parameters such as voltage and current of aforementioned each power supply can require to use existing electric-controlled according to technique
Technology processed is controlled to adjust, and makes this equipment by controlling the parameter of each power supply to control technical process, to power parameter
Adjusting can be realized using hardware circuit, can also be by the way of software and hardware combination.
The heating system includes being located at heating system inside the electron beam in the middle part of vacuum chamber and being located at vacuum chamber furnace wall four
The external radiation heating system in week.The application keeps the globality of heating more perfect using the structure that interior external heat combines, and
And in AMS system running, the uniformity in temperature field can be effectively maintained, depositing operation requirement is met.Specific implementation is this
Equipment increases external radiation heating using heated filament ion source as internal heat, then on the basis of heated filament ion source heating
System.
As shown in figure 3, the controlled sputtering source 9 is symmetrically distributed in the inner wall of vacuum chamber, the cathode arc source 8 is with vacuum
The centre of gyration of room is symmetry axis, is spirally distributed the inner wall in vacuum chamber.Using Spiral distribution scheme, sky is made full use of
Between, the target source of such cathode arc can increase to eight or more, significantly enhance adjustment and control of this equipment to film composition
Ability, producing this equipment, composition is more complicated, the more excellent film of comprehensive performance.
The vacuum system includes that the vacuum system includes molecular pump 14, lobe pump 18, mechanical pump 20, maintains pump 19,
The molecular pump 14 and vacuum chamber, the exhaust outlet for maintaining pump 19 to be connected to molecular pump 14 are connect, the lobe pump 18
It is connect with the exhaust outlet of molecular pump 14, the mechanical pump 20 is connect with the exhaust outlet of lobe pump 18.May be used also on vacuum system pipeline
Forevacuum valve 15, pre- pumping valve 16, by-passing valve 17 are set.The limiting pressure of vacuum chamber, work pressure are wherein determined with molecular pump 14
Power, the pumpdown time of high vacuum plate the stability of film pressure, it is desirable that it does not return oil, no switching on and shutting down non-cutting time.Mechanical pump 20 is used
In vacuum chamber being extracted into the pressure value for meeting 14 air inlet of molecular pump, exhaust outlet.Which determine the pumpdown times of low vacuum.It maintains
Pump 19 makes vacuum chamber main pump when opening that can also run well work, dimension for maintaining the pressures at expulsion of 14 exhaust outlet of molecular pump
Hold 19 optional sliding vane rotary pumps of pump.Vacuum system is fixedly mounted on vacuum system bracket 21.
Peep hole 7 is provided on the vacuum chamber.It adds peep hole 7 and understands vacuum chamber inside information in real time convenient for operator
Condition.Gas flow interface 11 is additionally provided on vacuum chamber, to be passed through associated gas during the work time.
It as shown in figure 16, further include protective case 25, the protective case 25 is mounted on cathode arc source 8 towards luggage carrier (3)
Side, the protective case 25 is additionally provided with baffle 26 far from the side of cathode arc source 8.Although AIP facilitates the hair of ionization
Raw, the deposition of plated film is higher, but in O2When excessive or original electric field changes, O2It is easier to send out on cathode target surface
Raw reaction, required element cannot normally be exported by generating oxide to cause the failure of cathodic discharge.The oxygen of PVD at present
Compound is mainly aluminium oxide, and Al, AlTi material are easier to relatively and O2It reacts, therefore conventional way is added in Al material
The Cr of certain content, can effectively prevent the oxidation of target surface, but chromium oxide stability is relatively poor, will lead to changing for film performance
Become.Although therefore the prior art thinks that AIP deposition is high, the sull met the requirements can not be prepared with it.This Shen
Effective protection please be carried out to target surface using aforementioned structure, prevent O2Into cathode target surface, and it can guide and flow through around target surface
O2, it is mobile towards the direction of film-coating workpiece 27, to effectively prevent O far from target surface2It reacts on cathode target surface, generates institute
The oxide of meaning prepares high performance sull, overcomes the skill that cannot prepare oxide using AIP in the prior art
Art prejudice.
Temperature measuring device and vacuum measuring device are provided on the vacuum chamber.By the temperature measuring device added and
Vacuum measuring device can measure temperature and vacuum degree in vacuum chamber, so as in coating process to both the above parameter into
Row accurately controls.
The cooling system is multichannel water circulation type cooling system.Using multichannel water circulation type cooling system, cooling effect
It is good, and resource and cost can be saved.
It is heavy to carry out multicomponent alloy material ions using cathode arc source 8 for the method for multicomponent alloy laminated film of the invention
While product, single metallic elements are mixed using controlled sputtering source 9, form multicomponent alloy composite film layer.Due in the prior art
The technique that coating process uses cathodic arc ion plating or magnetron sputtering to carry out respectively, therefore cannot effectively combine two kinds of techniques
The advantages of, prevent film obtained from being provided simultaneously with a variety of excellent performances.And the application carried out with cathode arc source 8 it is polynary
While alloy material ion depositions, single metallic elements are mixed using controlled sputtering source 9, form multicomponent alloy composite film layer,
The metallurgical structure that film can accurately be controlled in this way, optimizes adjustment to the performance of film coating according to the needs of use,
And can guarantee higher deposition during the preparation process, to make film obtained, performance is higher compared with prior art.
The technical process of multicomponent alloy laminated film is prepared using multicomponent alloy laminated film Preparation equipment of the invention:
A, AIP and MS
(1) pre-treatment:
Before plated film, cutter is dry after conventional alkalescent cleaning agent and absolute alcohol ultrasonic cleaning, is placed in coating chamber；
(2) preparation before coating:
1. vacuum chamber is inflated, fire door is opened；
2. replacement electric arc, sputter target material as needed replaces sight glass；
3. cleaning each position of furnace body, pressure 0.6MPa with high pressure air rifle；
4. selecting fixture appropriate, it is packed into workpiece 27 (cutter), confirmation clamp movement is reliably errorless；
5. the insulation shape of confirmation heated filament ion source, cathode arc source 8, controlled sputtering source, impressed current anode 22,27 fixture of workpiece
Condition, resistance value should be greater than 100K Ω；
6. closing deposited chamber, closing vent valve.
(3) it vacuumizes (to 5 × 10-2Pa it) and preheats
1. starting water cooler；
2. mechanical pump (20), lobe pump (18) open pre- pumping valve 16；
3. starting compound vacuum gauge, thermocouple rule 1 are opened, test fore line vacuum, vacuum is less than 5Pa
4. starting molecular pump 14；
5. when molecular pump 14 enters normal operating conditions, and vacuum degree in vacuum chamber meets less than after 5Pa, closes and takes out valve in advance
16, step valve 15, high vacuum valve 13 before opening；
6. when vacuum values are less than 5 × 10-2When Pa, it is sent into the Ar gas of 40~60sccm, and opens auxiliary heating (5KW)；
7. opening workpiece 27 to rotate, frequency modulation 15Hz；
8. being prepared to enter into the composite heating stage after 40min.
(4) electron beam heats
1. pressure in vacuum tank is adjusted to 2.5 × 10-190~120sccm of Pa, Ar throughput；
2. opening heated filament ion source current, electric current is slowly risen to 170~230A；
3. opening field supply is adjusted to 12~20A；
4. opening argon-arc plasma field maintains power supply, switch goes to heating gear；
5. causing electric arc, electric current is gradually added in 180A；
6. 40~70min of composite heating period.
(5) gas plasma etches
1. heater current maintains 170~230A；
2. argon-arc plasma field maintains source current to reduce to 100~120A；
3. field supply reduces to 6~8A；
4. pressure in vacuum tank is adjusted to 2 × 10-1Pa, Ar throughput 50~65sccm, H212~20sccm of throughput；
5. breakdown grid bias power supply, gradually power-up is depressed into 0~200V of DC voltage, 300~500V of pulse voltage；
6. the ion etching period is about 80~150min.
(6) coating
1. Ti, Cr, Zr layers: nitrogen (Ar) 80~140sccm of flow, bias are adjusted to 800~1000V, open 2 cathode electricity
Arc source 8 (Ti, Cr, Zr), arc 70~100A of target current, 180~600sec of period；
2. TiN, CrN, ZrN layers: 480~680sccm of nitrogen flow, bias are adjusted to 150V, open 2 cathode arc sources 8
Source (Ti, Cr, Zr), arc 100~120A of target current, 180~600sec of period；
3. TiAl layers: 540~900sccm of nitrogen flow, bias are adjusted to 100~120V, open 4 cathode arc sources 8
(TiAl), 100~120A of arc target current, 3600~7200sec of period；
4. opening 2 controlled sputtering sources 9,1~3A of sputtering current, 3600~7200sec of period: nitrogen flow 540~
900sccm, bias are adjusted to 80~100V；
5. 48 sources of cathode arc source (TiAl) are closed, unlatching (2) a cathode arc source 8 (AlTi), arc target current 100~
120A, 1800~3600sec of period, nitrogen flow 540~900sccm, O230~100sccm of flow；
6. closing cathode arc, magnetic controlled sputtering target source, grid bias power supply；
7. closing heating source, N2、O214 startup power supply of molecular pump is closed in source, is opened and is maintained pump (19)；Send nitrogen 80~
120sccm；
8. sending argon gas to 30Pa；
(7) cooling: 60~120min of process time.
B, VE and MS
(1) pre-treatment:
Before plated film, high-speed steel or hard alloy cutter (being not necessarily to special polishing treatment) are through conventional alkalescent cleaning agent and anhydrous
It is dry after alcohol ultrasonic cleaning, it is placed in coating chamber；
(2) equipment inspection:
1. vacuum chamber is inflated, fire door is opened；
2. replacement sputter target material as needed replaces sight glass；
3. evaporation source return, and add new 20~30g of evaporation material (Ti)；
4. cleaning each position of furnace body, pressure 0.6MPa with high pressure air rifle；
5. selecting fixture appropriate, it is packed into workpiece 27 (cutter), confirmation clamp movement is reliably errorless；
6. confirming the insulation status of electron gun, evaporation source 23, sputtering source, impressed current anode 22,27 fixture of workpiece, resistance value is answered
Greater than 100K Ω；
7. rising chassis, closes deposited chamber, closes vent valve.
(3) it vacuumizes and preheats
1. starting water cooler；
2. mechanical pump (20), lobe pump (18) open pre- pumping valve 16；
3. starting compound vacuum gauge, thermocouple rule 1 are opened, test fore line vacuum, vacuum is less than 5Pa
4. starting molecular pump 14；
5. when molecular pump 14 enters normal operating conditions, and vacuum degree in vacuum chamber meets less than after 5Pa, closes and takes out valve in advance
16, step valve, high vacuum valve 13 before opening；
6. when vacuum values are less than 1 × 10-1When Pa, the Ar gas for the 40~60sccm that makes a gift to someone, and open auxiliary heating；
7. opening workpiece 27 to rotate, frequency modulation 20Hz；
8. being prepared to enter into the composite heating stage after 40min.
(4) electron beam heats
1. pressure in vacuum tank is adjusted to 2.5 × 10-190~110sccm of Pa, Ar throughput；
2. opening heated filament ion source current, electric current is slowly risen to 170~230A；
3. opening field supply is adjusted to 12~20A；
4. opening argon-arc plasma field maintains power supply, switch goes to heating gear；
5. causing electric arc, electric current is gradually added in 180A；
6. 40~100min of composite heating period.
(5) gas plasma etches
1. heated filament ion ource electric current maintains 170~230A；
2. argon-arc plasma field maintains source current to reduce to 100~120A；
3. field supply reduces to 6~8A；
4. pressure in vacuum tank is adjusted to 2 × 10-150~65sccm of Pa, Ar throughput；
5. breakdown grid bias power supply, gradually power-up is depressed into 0~200V of DC voltage, 300~500V of pulse voltage；
6. the ion etching period is about 50~90min.
(6) coating
1. heated filament ion ource electric current maintains 170~230A；
2. argon gas is adjusted to 23~35sccm,
3. field supply is adjusted to 25~35A；
4. bias is adjusted to 0~200V of voltage DC, 300~500V of pulse；
5. plus argon-arc plasma field maintains source current to 200A (5min)；
6. coating 5~20min of Ti intermediate metal；
7. sending nitrogen 80~120sccm；
8. bias is adjusted to 180V (10min)；
9. opening magnetic controlled sputtering target source, 1.0~2.0A (AlTiCr, C, Cr, Zr, Si etc.)
10. bias is adjusted to 100~150V (10min)；
(11) 20~50min of plated film period；
(12) magnetic controlled sputtering target source is closed；
(13) close argon-arc plasma field and maintain power supply, filament supply, magnetic field power supply, heating source, N2The starting of molecular pump 14 is closed in source
Power supply is opened and maintains pump (19)；
(14) send argon gas to 30Pa；
(7) cooling: 60~120min of process time.
Measured data comparison:
As shown in Figure 6 and Figure 7, AlCrN coating is prepared and using equipment benefit of the invention using single cathode arc
It is compared with AMS technique preparation AlCrN coating.The two has differences in (111), (200) diffraction maximum, is added by micro Mo,
Cause the enhancing of AlCrN (200) diffracted intensity.As shown in Figure 8 and Figure 9, it is prepared using equipment utilization AMS technique of the invention
For AlCrN coating after adding Mo, film hardness improves about 10% or so.
As shown in fig. 10 and fig. 12, the TiAlN coating prepared using single cathode arc, TiN (200) diffracted intensity compared with
By force, TiAlN (200) diffracted intensity is relatively weak, and film hardness is about 2400~3000HV.
As illustrated in figures 11 and 13, Al is adjusted by addition element using equipment utilization AMS technique of the invention67Ti33N
Structure, TiAlN (200) diffracted intensity significantly change, and film hardness is promoted to 3500~4000HV.
As shown in FIG. 14 and 15, to film made from the use prior art and using the present invention in the same of AIP ion deposition
When incorporation single metallic elements method made from film carry out scratch experiment, the sound during generating to scratch can be carried out and detect
To voice signal figure.As can be seen from the figure the sound during being generated using film scratch produced by the present invention can compare existing skill
Art is substantially reduced, and is indicated above film hardness prepared by the present invention and is increased significantly compared with prior art.
Claims (9)
1. multicomponent alloy laminated film Preparation equipment, it is characterised in that: including heating system, air supply system, cooling system, vacuum
System, vacuum chamber, luggage carrier (3), elevating mechanism, crucible evaporation source (23), controlled sputtering source (9), cathode arc source (8), electricity
Field generator for magnetic and electric control system, the vacuum system and vacuum chamber, the elevating mechanism and luggage carrier (3) pass
Dynamic connection, the air supply system and vacuum chamber, the electric control system and crucible evaporation source (23), controlled sputtering source
(9), cathode arc source (8), electromagnetic field generator, heating system electrical connection, the crucible evaporation source (23), controlled sputtering source
(9), cathode arc source (8) is located in vacuum chamber, and the target-substrate distance of the cathode arc source (8) is 160mm to 230mm, the magnetic
The target-substrate distance for controlling sputtering source (9) is 50mm to 75mm.
2. multicomponent alloy laminated film Preparation equipment as described in claim 1, it is characterised in that: further include heated filament ion source
(10), in a vacuum chamber, the heated filament ion source (10) is electrically connected with electric control system for heated filament ion source (10) setting.
3. multicomponent alloy laminated film Preparation equipment as claimed in claim 2, it is characterised in that: the electric control system is also
Power supply, sputtering source current, cathode arc power supply, grid bias power supply, the plasma are maintained including ion source current, plasma
Power supply and ion source current is maintained to connect with heated filament ion source (10), the sputtering source current is connect with controlled sputtering source (9), institute
Cathode arc power supply is stated to connect with cathode arc source (8).
4. multicomponent alloy laminated film Preparation equipment as described in claim 1, it is characterised in that: the heating system includes position
Heating system and the external radiation heating system positioned at vacuum chamber furnace wall surrounding inside electron beam in the middle part of vacuum chamber.
5. multicomponent alloy laminated film Preparation equipment as described in claim 1, it is characterised in that: the controlled sputtering source (9)
It is symmetrically distributed in the inner wall of vacuum chamber, the cathode arc source (8) is divided in the shape of a spiral using the centre of gyration of vacuum chamber as symmetry axis
Inner wall of the cloth in vacuum chamber.
6. multicomponent alloy laminated film Preparation equipment as described in claim 1, it is characterised in that: the vacuum system includes point
Son pump (14), mechanical pump (20), maintains pump (19), the molecular pump (14) and vacuum chamber, the maintenance at lobe pump (18)
Pump (19) is connect with the exhaust outlet that molecular pump (14) is connected to, and the lobe pump (18) connect with the exhaust outlet of molecular pump (14), institute
Mechanical pump (20) is stated to connect with the exhaust outlet of lobe pump (18).
7. multicomponent alloy laminated film Preparation equipment as described in claim 1, it is characterised in that: it further include protective case, it is described
Protective case is mounted on side of the cathode arc source (8) towards luggage carrier (3), the protective case far from cathode arc source (8) one
Side is additionally provided with baffle (26).
8. the method that multicomponent alloy laminated film is prepared using multicomponent alloy laminated film Preparation equipment described in claim 1,
It is characterized by: being utilized controlled sputtering source (9) while carrying out multicomponent alloy material ions deposition using cathode arc source (8)
Single metallic elements are mixed, multicomponent alloy composite film layer is formed.
9. multicomponent alloy preparation method of composite film as claimed in claim 8, it is characterised in that: evaporated by crucible evaporation source
Metallic element is implanted into other elements by controlled sputtering source while workpiece surface deposits to form metallic compound, in workpiece
Surface forms multicomponent alloy laminated film.
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| CN201710305293.8A CN107130213B (en) | 2017-05-03 | 2017-05-03 | Multicomponent alloy laminated film Preparation equipment and preparation method |
| RU2017133149A RU2678492C1 (en) | 2017-05-03 | 2017-09-22 | Device for producing a composite film of multi-element alloy |
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| CN108330452A (en) * | 2018-01-12 | 2018-07-27 | 中国科学院宁波材料技术与工程研究所 | The preparation method of MAX phase coatings |
| CN108359937B (en) * | 2018-02-27 | 2023-08-22 | 温州驰诚真空机械有限公司 | Conversion type physical vapor deposition particle source |
| CN108441828B (en) * | 2018-05-03 | 2020-10-09 | 宁波正元铜合金有限公司 | Plating equipment and plating method for copper-lead self-lubricating film on dynamic sealing element |
| CN110804725A (en) * | 2019-11-19 | 2020-02-18 | 成都四盛科技有限公司 | Sublimation magnetron sputtering coating all-in-one |
| CN113604789A (en) * | 2021-07-16 | 2021-11-05 | 山东宏旺实业有限公司 | Stainless steel band vacuum coating device |
| CN114164405B (en) * | 2021-12-07 | 2023-12-29 | 四川真锐晶甲科技有限公司 | Tool thick film nitride coating and preparation method thereof |
| CN114481071B (en) * | 2022-02-11 | 2023-10-27 | 松山湖材料实验室 | Coating device and DLC coating process |
| CN114481017B (en) * | 2022-02-11 | 2023-10-27 | 松山湖材料实验室 | Coating device and cleaning process |
| CN116590662B (en) * | 2023-05-09 | 2024-01-23 | 东莞市普拉提纳米科技有限公司 | Boron-containing high-entropy alloy cutter coating for cutting titanium alloy and preparation process thereof |
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| RU2678492C1 (en) | 2019-01-30 |
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