CN117089804A - Composite coating, preparation method thereof and coated tap - Google Patents
Composite coating, preparation method thereof and coated tap Download PDFInfo
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- CN117089804A CN117089804A CN202310891796.3A CN202310891796A CN117089804A CN 117089804 A CN117089804 A CN 117089804A CN 202310891796 A CN202310891796 A CN 202310891796A CN 117089804 A CN117089804 A CN 117089804A
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- coating
- nitriding
- substrate
- composite coating
- arc discharge
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- 238000000576 coating method Methods 0.000 title claims abstract description 179
- 239000011248 coating agent Substances 0.000 title claims abstract description 172
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000005121 nitriding Methods 0.000 claims abstract description 110
- 239000000758 substrate Substances 0.000 claims abstract description 98
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 75
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 72
- 238000001020 plasma etching Methods 0.000 claims abstract description 52
- 150000004767 nitrides Chemical class 0.000 claims abstract description 47
- 239000000463 material Substances 0.000 claims abstract description 44
- 238000010891 electric arc Methods 0.000 claims abstract description 43
- 229910052786 argon Inorganic materials 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 37
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 239000001257 hydrogen Substances 0.000 claims abstract description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000008021 deposition Effects 0.000 claims description 15
- 229910010037 TiAlN Inorganic materials 0.000 claims description 5
- 238000005530 etching Methods 0.000 claims description 5
- 229910008482 TiSiN Inorganic materials 0.000 claims description 3
- QRXWMOHMRWLFEY-UHFFFAOYSA-N isoniazide Chemical compound NNC(=O)C1=CC=NC=C1 QRXWMOHMRWLFEY-UHFFFAOYSA-N 0.000 claims description 3
- 239000010410 layer Substances 0.000 abstract description 57
- 238000005520 cutting process Methods 0.000 abstract description 16
- 239000011247 coating layer Substances 0.000 abstract description 3
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 description 35
- 239000002585 base Substances 0.000 description 33
- 210000002381 plasma Anatomy 0.000 description 31
- 229910000997 High-speed steel Inorganic materials 0.000 description 20
- 238000010438 heat treatment Methods 0.000 description 13
- 238000000151 deposition Methods 0.000 description 12
- 238000005498 polishing Methods 0.000 description 12
- 230000008569 process Effects 0.000 description 12
- 229910045601 alloy Inorganic materials 0.000 description 9
- 239000000956 alloy Substances 0.000 description 9
- -1 hydrogen ions Chemical class 0.000 description 9
- 238000012545 processing Methods 0.000 description 9
- 238000001816 cooling Methods 0.000 description 8
- 239000011651 chromium Substances 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 230000003746 surface roughness Effects 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000003513 alkali Substances 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 238000010079 rubber tapping Methods 0.000 description 5
- 238000002791 soaking Methods 0.000 description 5
- 238000004506 ultrasonic cleaning Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 229910052804 chromium Inorganic materials 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000005012 migration Effects 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- 230000001603 reducing effect Effects 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 229910001315 Tool steel Inorganic materials 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000005496 tempering Methods 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical group [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910010038 TiAl Inorganic materials 0.000 description 1
- 229910008484 TiSi Inorganic materials 0.000 description 1
- QJCMRMSRJIYGEG-UHFFFAOYSA-N [Co].[Ta].[Ti].[W] Chemical compound [Co].[Ta].[Ti].[W] QJCMRMSRJIYGEG-UHFFFAOYSA-N 0.000 description 1
- UUJDYXCAZMFYTK-UHFFFAOYSA-N [Co].[Ta].[W] Chemical compound [Co].[Ta].[W] UUJDYXCAZMFYTK-UHFFFAOYSA-N 0.000 description 1
- YWJQGSHYTRHJJH-UHFFFAOYSA-N [Co].[Ti].[W] Chemical compound [Co].[Ti].[W] YWJQGSHYTRHJJH-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- JPNWDVUTVSTKMV-UHFFFAOYSA-N cobalt tungsten Chemical compound [Co].[W] JPNWDVUTVSTKMV-UHFFFAOYSA-N 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000002173 cutting fluid Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- MGRWKWACZDFZJT-UHFFFAOYSA-N molybdenum tungsten Chemical compound [Mo].[W] MGRWKWACZDFZJT-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
- 239000011885 synergistic combination Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052720 vanadium 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23G—THREAD CUTTING; WORKING OF SCREWS, BOLT HEADS, OR NUTS, IN CONJUNCTION THEREWITH
- B23G5/00—Thread-cutting tools; Die-heads
- B23G5/02—Thread-cutting tools; Die-heads without means for adjustment
- B23G5/06—Taps
-
- 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
-
- 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
- C23C14/0664—Carbonitrides
-
- 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/02—Pretreatment of the material to be coated
-
- 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding
- C23C8/38—Treatment of ferrous surfaces
-
- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F4/00—Processes for removing metallic material from surfaces, not provided for in group C23F1/00 or C23F3/00
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
Abstract
The invention relates to a composite coating, a preparation method thereof and a coated tap. The preparation method of the composite coating comprises the following steps: arranging a substrate in a reaction cavity, vacuumizing, and preheating the substrate; argon and hydrogen are introduced into the reaction cavity, first plasma etching is carried out under the condition of arc discharge, and the temperature of the base material is increased to nitriding temperature; argon and nitrogen are introduced into the reaction cavity, and plasma nitriding is carried out under the conditions of arc discharge and glow discharge, so that a nitriding layer is formed on the surface of the base material; forming a nitride coating layer on the nitriding layer; wherein the method further comprises the following steps before and/or after plasma nitriding: argon is introduced into the reaction cavity, and the second plasma etching is performed under the arc discharge condition. The preparation method enables the base material, the nitriding layer and the nitride coating to form proper hardness gradient, and effectively improves the nanometer hardness, the elastic modulus and the binding force of the composite coating, thereby enhancing the cutting performance of the composite coating.
Description
Technical Field
The invention relates to the technical field of coating preparation, in particular to a composite coating, a preparation method thereof and a coating tap.
Background
A tap is a tool that processes internal threads (i.e., tapping). In the tapping process, the working part of the tap is buried in the workpiece for drilling, the cutting edge of the tap is extruded by the workpiece while being subjected to axial and radial cutting forces, and the cutter also bears a large bending moment. In order to overcome complex and severe working conditions and meet the modern processing requirements of high efficiency and high precision, the tap is generally required to be subjected to surface treatment to improve the comprehensive performance of the tap.
As coating technology has matured, coated taps made by coating processes have become increasingly popular in the tap field. The coating tap has the advantages of high surface hardness, good wear resistance, low friction coefficient, oxidation resistance and the like, and can effectively improve the processing precision and the service life of the tap. However, the cutting performance of the current coating tap is still not ideal enough, and the processing requirements of high efficiency and high precision cannot be met.
Disclosure of Invention
Based on this, there is a need to provide a composite coating, a method of preparing the same, and a coated tap to overcome the problem that the cutting performance of the current coated tap is not ideal enough.
The above object of the present invention is achieved by the following technical solutions:
in a first aspect of the present invention, a method for preparing a composite coating is provided, comprising the steps of:
arranging a substrate in a reaction cavity, vacuumizing, and preheating the substrate;
argon and hydrogen are introduced into the reaction cavity, first plasma etching is carried out under the condition of arc discharge, and the temperature of the base material is increased to nitriding temperature;
argon and nitrogen are introduced into the reaction cavity, and plasma nitriding is carried out under the conditions of arc discharge and glow discharge, so that a nitriding layer is formed on the surface of the base material;
forming a nitride coating on the nitrided layer;
wherein the method further comprises the following steps before and/or after plasma nitriding: argon is introduced into the reaction cavity, and second plasma etching is performed under the condition of arc discharge.
In one embodiment, the nitride coating includes one or more of a TiAlN coating, a TiSiN coating, a CrAlN coating, a CrAlCN coating, a CrAlBN coating, and a craaltisin coating.
In one embodiment, the nitriding temperature is 440 ℃ to 480 ℃.
In one embodiment, the first plasma etching under the condition of arc discharge comprises the following steps:
and (3) turning on an ion source to generate arc discharge, applying a negative bias voltage of 30-100V to the substrate, and then performing first plasma etching on the surface of the substrate for 30-60 min.
In one embodiment, the second plasma etching under the condition of arc discharge comprises the following steps:
and (3) turning on an ion source to generate arc discharge, applying a negative bias voltage of 150-200V to the substrate, and then carrying out argon etching for 90-150 min on the surface of the substrate or the surface of the nitriding layer.
In one embodiment, the plasma nitriding is performed under the conditions of arc discharge and glow discharge, comprising the steps of:
and (3) turning on an ion source to generate arc discharge, applying a negative bias voltage of 300-600V to the substrate, and then carrying out plasma nitriding on the surface of the substrate for 30-90 min.
In one embodiment, one or more of the following conditions are met:
1) The flow ratio of the argon to the nitrogen is 1: (1-3);
2) The pressure of the reaction cavity is 0.5 Pa-1.5 Pa;
3) The thickness of the nitriding layer is 15-30 mu m.
In one embodiment, the method of forming the nitride coating on the nitrided layer is arc ion deposition.
In one embodiment, the arc ion deposition includes the steps of:
and (3) introducing nitrogen, starting an arc target to generate arc discharge, applying a negative bias voltage of 60-120V to the base material, and then performing arc ion deposition on the nitriding layer for 120-180 min.
In one embodiment, one or more of the following conditions are met:
1) The pressure of the reaction cavity is 3.8 Pa-4.2 Pa;
2) The target current of the coating target is 100A-150A;
3) The thickness of the nitride coating is 2-2.5 mu m.
In one embodiment, one or more of the following conditions are met:
1) The pressure of the reaction cavity after being vacuumized is 1 multiplied by 10 -3 Pa～1×10 -2 Pa；
2) The preheating temperature is 300-350 ℃.
In a second aspect of the present invention, there is provided a composite coating layer prepared by the above-described method for preparing a composite coating layer.
In a third aspect of the present invention, a coated tap is provided comprising the composite coating described above.
The invention has the following beneficial effects:
according to the invention, the steps of preheating, first plasma etching, second plasma etching, plasma nitriding, coating treatment and the like are adopted, and the nitriding layer and the nitride coating are sequentially formed on the surface of the base material, so that a proper hardness gradient is obtained among the base material, the nitriding layer and the nitride coating, the nano hardness, the elastic modulus and the binding force of the composite coating are effectively improved, and the cutting performance of the composite coating is enhanced.
Wherein, the preheating can remove the gas in the substrate, prevents the problems of rupture membrane, falling off and the like in the subsequent coating treatment. The first plasma etching is carried out under the condition of arc discharge, so that the oxide on the surface of the substrate can be removed by utilizing hydrogen ions with reactivity, and ion energy can be transferred to the substrate through collision, thereby playing a role in heating and reducing the energy consumption required by heating to nitriding temperature. And the second plasma etching is carried out under the arc discharge condition, so that the roughness and the surface energy of the surface of the substrate or the surface of the nitriding layer can be increased, the migration of nitrogen element and the growth of the nitride coating are promoted, and the film base binding force, compactness and uniformity of the coating are improved. By utilizing the cooperation of arc discharge and glow discharge, the ionization rate and ion energy of plasma in the nitriding process can be increased, the nitriding temperature is reduced, the nitriding time is shortened, and the nitriding efficiency and the thickness of the nitriding layer are improved. In addition, the nitriding layer can reduce the hardness difference between the base material and the nitride coating, has good affinity with the nitride coating, is beneficial to the growth of the nitride coating, and effectively improves the film-based binding force of the coating.
Drawings
FIG. 1 is a cross-sectional profile view of the coated tap of example 1;
FIG. 2 is a cross-sectional nitrogen profile of the coated tap shown in FIG. 1;
FIG. 3 is a metallographic section view of the coated tap of example 1;
FIG. 4 is a metallographic section view of the coated tap of example 2;
FIG. 5 is a metallographic section view of the coated tap of example 3;
FIG. 6 is a graph comparing the nano hardness and elastic modulus of the nitride coating of each coated tap;
FIG. 7 is a schematic illustration of the bonding force of the nitride coating for each coated tap;
FIG. 8 is a graph of wear profile of the flank face of the first row of teeth of each coated tap;
FIG. 9 is a graph of the wear profile of the second row of tooth flank of each coated tap;
FIG. 10 is a graph of wear profile of the third row of tooth flank of each coated tap;
FIG. 11 is a graph of wear profile at the root of each coated tap.
Detailed Description
In order that the above objects, features and advantages of the invention will be readily understood, a more particular description of the invention will be rendered by reference to the appended drawings. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. The present invention may be embodied in many other forms than described herein and similarly modified by those skilled in the art without departing from the spirit of the invention, whereby the invention is not limited to the specific embodiments disclosed below.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
In the present invention, the cutting performance means the wear resistance and the service life of a tool such as a tap.
In order to overcome complex and severe working conditions and meet the modern processing requirements of high efficiency and high precision, taps generally need surface treatment, mainly comprising surface nitriding, coating treatment and the like. As coating technology matures, coated taps are increasingly dominant in the tap field. The coating tap has the advantages of high surface hardness, good wear resistance, low friction coefficient, oxidation resistance and the like, and can effectively improve the processing precision and the service life of the tap.
Tap materials mainly include tool steel, high-speed steel, cemented carbide, etc., wherein high-speed steel is the most widely used tap material. The coating in the coated tap mainly comprises TiN, tiCN, tiAlN and AlCrN nitride coatings. The TiN coating is the earliest nitride coating, has good mechanical property, good bonding property between high-speed steel and good anti-adhesion abrasion property, and is a common coating for low-speed processing taps; the TiCN coating has higher hardness and low friction coefficient, can effectively prolong the service life of the screw tap, has poorer oxidation resistance, is easy to damage and peel after the processing temperature exceeds 30 ℃, and is only suitable for low-speed tapping; the TiAlN coating has good hardness, wear resistance and better oxidation resistance, is one of the most widely applied coatings in tool coatings, but the TiAlN coating has poor adaptation degree between high-speed steels and has the problem of insufficient binding force, and the coating is easy to peel off in the tapping process; the AlCrN coating has better binding force with high-speed steel, better oxidation resistance and can meet the requirement of high-speed tapping with the assistance of certain cutting fluid, so that the AlCrN coating is widely applied to high-speed processing taps at present. However, the overall hardness of the high-speed steel is lower than that of various coatings, so that the binding force between the high-speed steel and the coatings is insufficient, and the wear resistance and cutting performance of the coating tap are seriously affected.
Based on the above, the first aspect of the present invention provides a method for preparing a composite coating, comprising the following steps:
arranging a substrate in a reaction cavity, vacuumizing, and preheating the substrate;
argon and hydrogen are introduced into the reaction cavity, first plasma etching is carried out under the condition of arc discharge, and the temperature of the base material is increased to nitriding temperature;
argon and nitrogen are introduced into the reaction cavity, and plasma nitriding is carried out under the conditions of arc discharge and glow discharge, so that a nitriding layer is formed on the surface of the base material;
forming a nitride coating on the nitrided layer;
wherein the method further comprises the following steps before and/or after plasma nitriding: argon is introduced into the reaction cavity, and second plasma etching is performed under the condition of arc discharge.
According to the invention, the steps of preheating, first plasma etching, second plasma etching, plasma nitriding, coating treatment and the like are adopted, and the nitriding layer and the nitride coating are sequentially formed on the surface of the base material, so that a proper hardness gradient is obtained among the base material, the nitriding layer and the nitride coating, the nano hardness, the elastic modulus and the binding force of the composite coating are effectively improved, and the cutting performance of the composite coating is enhanced.
Wherein, the preheating can remove the gas in the substrate, prevents the problems of rupture membrane, falling off and the like in the subsequent coating treatment. The first plasma etching is carried out under the condition of arc discharge, so that the oxide on the surface of the substrate can be removed by utilizing hydrogen ions with reactivity, and ion energy can be transferred to the substrate through collision, thereby playing a role in heating and reducing the energy consumption required by heating to nitriding temperature. And the second plasma etching is carried out under the arc discharge condition, so that the roughness and the surface energy of the surface of the substrate or the surface of the nitriding layer can be increased, the migration of nitrogen element and the growth of the nitride coating are promoted, and the film base binding force, compactness and uniformity of the coating are improved. By utilizing the cooperation of arc discharge and glow discharge, the ionization rate and ion energy of plasma in the nitriding process can be increased, the nitriding temperature is reduced, the nitriding time is shortened, and the nitriding efficiency and the thickness of the nitriding layer are improved. In addition, the nitriding layer can reduce the hardness difference between the base material and the nitride coating, has good affinity with the nitride coating, is beneficial to the growth of the nitride coating, and effectively improves the film-based binding force of the coating.
Optionally, before the step of disposing the substrate in the reaction chamber, the method further comprises the steps of polishing, cleaning and drying the substrate.
Further optionally, the polishing, cleaning and drying the substrate comprises the steps of: polishing the surface of the base material to a mirror surface after polishing, so that the surface roughness of the base material is lower than 50nm; soaking a substrate in hot alkali solution to remove oil, then placing the substrate in alcohol solution to carry out ultrasonic cleaning, and then placing the substrate in deionized water to soak and clean; and (5) drying after cleaning, and wrapping with dust-free paper for standby.
Optionally, the material of the substrate is cemented carbide and/or high-speed steel.
The main component of the hard alloy is tungsten carbide (WC), and the tungsten carbide comprises one or more of tungsten cobalt hard alloy (WC+Co), tungsten titanium cobalt hard alloy (WC+TiC+Co), tungsten tantalum cobalt hard alloy (WC+TaC+Co) and tungsten titanium tantalum cobalt hard alloy (WC+TiC+TaC+Co). The high-speed steel (High Speed Steels, HSS) is also called high-speed tool steel, high-speed steel or white steel, is high-carbon high-alloy steel containing alloy elements such as tungsten (W), molybdenum (Mo), chromium (Cr), cobalt (Co), vanadium (V) and the like, has a carbon content of 0.70-1.65%, and the total content of the alloy elements of 10-25%, and can be classified into tungsten high-speed steel, tungsten molybdenum high-speed steel, high-molybdenum high-speed steel, vanadium high-speed steel and cobalt high-speed steel according to the types and the content of the alloy elements.
Further alternatively, the material of the workpiece is high-speed steel.
The high-speed steel has good technological properties, hardness, strength, toughness, wear resistance and the like, can be used for manufacturing complex thin-blade and impact-resistant cutting tools, and can also be used for manufacturing cold working dies, hot working dies, rollers, high-temperature bearings, high-temperature springs and the like.
Optionally, the composition of the nitride coating includes one or more of titanium (Ti), chromium (Cr), aluminum (Al), silicon (Si), carbon (C), and boron (B).
By the synergistic combination of metal elements such as titanium (Ti), chromium (Cr) and aluminum (Al) and nonmetallic elements such as silicon (Si), carbon (C) and boron (B), the nitride coating has higher hardness and better film-based bonding property, and the cutting performance of the nitride coating is obviously improved.
In some embodiments, the nitride coating includes one or more of a TiAlN coating, a TiSiN coating, a CrAlN coating, a CrAlCN coating, a CrAlBN coating, and a craaltisin coating.
Preferably, the nitride coating is a CrAlBN coating.
In some embodiments, the nitriding temperature is 440 ℃ to 480 ℃.
In the plasma nitriding process, nitrogen is taken as a gas with reactivity, so that the nitrogen is easy to react with elements such as Fe, cr, mo and the like in the base material, and meanwhile, the kinetic energy of particles such as nitrogen ions and the like can be converted into the heat energy of the base material through energy exchange, so that the temperature of the base material is increased. Therefore, the nitriding temperature is controlled to be 440-480 ℃, the actual nitriding temperature can be prevented from being increased to be higher than the tempering temperature of the base material, the integral nitriding temperature is ensured to be lower than 500 ℃, and the risk of tempering and softening the base material in the nitriding process is effectively avoided. In addition, the lower nitriding temperature can prevent precipitation of chromium-containing compounds, which deteriorates corrosion resistance of the substrate.
Preferably, the nitriding temperature is 450 ℃.
In some embodiments, the first plasma etching under the condition of arc discharge comprises the following steps:
and (3) turning on an ion source to generate arc discharge, applying a negative bias voltage of 30-100V to the substrate, and then performing first plasma etching on the surface of the substrate for 30-60 min.
The argon and hydrogen are ionized by an arc discharge of an ion source to form a plasma containing argon ions and hydrogen ions, and the oxide and organic contaminants on the surface of the substrate are removed by the hydrogen ions having a reducing property. Because the negative bias applied to the substrate is low, the argon ions and the hydrogen ions are mostly not bounced after contacting the surface of the substrate, but the ion energy is transferred to the substrate, thereby playing a role in heating. The time of the first plasma etching is controlled within the range of 30-60 min, so that the nitriding temperature is reasonably controlled, and the method is suitable for nitriding treatment of base materials of different materials. When the material of the base material is hard alloy, the hydrogen etching time is usually 40-60 min; when the material of the substrate is high-speed steel, the hydrogen etching time is about 30 minutes.
Optionally, the ion source is a hollow cathode gun.
Compared with arc sources such as a column arc source or a rectangular plane large arc source, the hollow cathode gun is used as an auxiliary ion source, a cathode target and a baffle plate for filtering target ions are not required to be additionally arranged, so that the pollution of the target ions to the surface of a workpiece can be avoided, and meanwhile, a large number of electrons are prevented from being blocked by the baffle plate, so that enough electrons can be obtained under lower current and voltage, the treatment time of the steps such as first plasma etching, second plasma etching, plasma nitriding and the like can be shortened, and a better surface treatment effect can be obtained.
In some embodiments, the performing a second plasma etch under arc discharge conditions includes the steps of:
and (3) turning on an ion source to generate arc discharge, applying a negative bias voltage of 150-200V to the substrate, and then carrying out argon etching for 90-150 min on the surface of the substrate or the surface of the nitriding layer.
The arc discharge of the ion source is used for emitting arc electron flow to ionize argon, and under the action of higher bias voltage of 150-200V, the argon ion can effectively etch the surface of the substrate, so that the surface roughness, the surface energy and the interatomic gaps of the surface of the substrate or the surface of the nitriding layer are obviously increased, on one hand, the migration of nitrogen element in the nitriding process is facilitated, on the other hand, the nitriding layer is rapidly formed at relatively low temperature and pressure, the nitriding efficiency is increased, on the other hand, the growth of the coating can be promoted, the binding force between the substrate and the coating is increased, and the cutting performance of the composite coating is improved.
In some embodiments, the plasma nitriding is performed under arc discharge and glow discharge conditions, comprising the steps of:
and (3) turning on an ion source to generate arc discharge, applying a negative bias voltage of 300-600V to the substrate, and then carrying out plasma nitriding on the surface of the substrate for 30-90 min.
The arc discharge of the ion source is utilized to ionize argon and nitrogen near the ion source, and high bias voltage of 300V-600V is applied to the base material to generate glow discharge to ionize the argon and the nitrogen near the base material, so that plasmas with high ionization rate and high ion energy can be obtained, the rapid nitriding treatment is realized at a lower nitriding temperature, the nitriding efficiency is high, and the thickness of the nitriding layer is larger.
In some embodiments, one or more of the following conditions are met:
1) The flow ratio of the argon to the nitrogen is 1: (1-3);
2) The pressure of the reaction cavity is 0.5 Pa-1.5 Pa;
3) The thickness of the nitriding layer is 15-30 mu m.
By adjusting the flow ratio of argon to nitrogen and keeping the pressure of the reaction cavity within the range of 0.5 Pa-1.5 Pa, different nitriding layer thicknesses can be obtained while better nitriding efficiency is obtained, so that the requirements of the coating tap in different processing scenes can be met.
Preferably, the flow ratio of the argon to the nitrogen is 1:1.
preferably, the pressure of the reaction chamber is 1.2Pa.
Preferably, the thickness of the nitriding layer is 15 μm to 25 μm.
In some embodiments, the method of forming a nitride coating on the nitrided layer is arc ion deposition.
Compared with other ion plating techniques, the ionization rate of arc ion deposition is highest, the ion energy is also high, the ion energy is easy to combine with reactive gases such as nitrogen and the like to generate a nitride coating, and the film base binding force of the coating is enhanced.
In some embodiments, the arc ion deposition comprises the steps of:
and (3) introducing nitrogen, starting an arc target to generate arc discharge, applying a negative bias voltage of 60-120V to the base material, and then performing arc ion deposition on the nitriding layer for 120-180 min.
The arc target material is used as an evaporation source and an ionization source for arc ion deposition, and emits high-density arc plasma through cold field arc discharge, and has the advantages of high ionization rate and high ion energy.
Optionally, the arc target comprises one or more of a TiAl target, a TiSi target, a CrAl target, and a CrAlB target. .
In some embodiments, one or more of the following conditions are met:
1) The pressure of the reaction cavity is 3.8 Pa-4.2 Pa;
2) The target current of the coating target is 100A-150A;
3) The thickness of the nitride coating is 2-2.5 mu m.
In some embodiments, one or more of the following conditions are met:
1) The pressure of the reaction cavity after being vacuumized is 1 multiplied by 10 -3 Pa～1×10 -2 Pa；
2) The preheating temperature is 300-350 ℃.
Preferably, the pressure of the reaction cavity after being vacuumized is 2 multiplied by 10 -3 Pa。
Preferably, the preheating temperature is 300 ℃.
In a second aspect, the invention provides a composite coating, which is characterized in that the composite coating is prepared by the preparation method.
In a third aspect, the present invention provides a coated tap comprising a composite coating as described above.
The present invention will be described in further detail with reference to specific examples. The raw materials used in the following examples are all commercially available products unless otherwise specified.
Example 1
The base material of the embodiment is a three-row tooth cutting tap made of M35 high-speed steel, and the second plasma etching is carried out before the plasma nitriding, and the specific steps are as follows:
(1) Polishing the surface of the substrate to a mirror surface after polishing, so that the surface roughness of the substrate is less than 50nm; soaking a substrate in hot alkali solution to remove oil, then placing the substrate in alcohol solution to carry out ultrasonic cleaning, and then placing the substrate in deionized water to soak and clean; and (5) drying after cleaning, and wrapping with dust-free paper for standby.
(2) Placing the substrate on a workpiece frame in a coating furnace, vacuumizing until the cavity pressure in the coating furnace is 2×10 -3 Pa, the resistance heating module is started to heat to 300 ℃.
(3) Argon is introduced at the flow of 300sccm until the atmosphere in the coating furnace is stable; starting a hollow cathode gun, applying a negative bias voltage of 60V to a workpiece, then introducing hydrogen at a flow rate of 150sccm, and then performing first plasma etching on the surface of the substrate for 30 min; in the first plasma etching process, the resistance heating module is kept on, so that the temperature of the base material is heated to 450 ℃; after the first plasma etching is finished, the hollow cathode gun is closed.
(4) Argon is introduced at the flow of 350sccm, a hollow cathode gun is started, 180V negative bias is applied to the substrate, and then the surface of the substrate is subjected to 90min of second plasma etching; and after the second plasma etching is finished, closing the hollow cathode gun.
(5) Argon is introduced at a flow of 210sccm, and nitrogen is introduced at a flow of 210sccm, so that the cavity pressure in the coating furnace is kept at 1.2Pa; starting a hollow cathode gun, applying a negative bias voltage of 500V to the substrate, and then carrying out plasma nitriding on the surface of the substrate for 60min, so as to form a nitriding layer with the thickness of 25 mu m on the surface of the substrate; after the plasma nitriding is finished, the hollow cathode gun is closed.
(6) Introducing nitrogen at a flow of 1200sccm, and keeping the cavity pressure in the coating furnace at 4.2Pa; starting the CrAlB target, applying a negative bias voltage of 100V to the workpiece, and then performing arc ion deposition on the nitriding layer for 120min, so as to form a CrAlBN coating with the thickness of 2.4 mu m on the nitriding layer.
(7) After the coating treatment is finished, closing the CrAlB target, cooling to 350 ℃ along with a furnace, and introducing nitrogen until the cavity pressure is 5 multiplied by 10 4 Pa, continuously cooling to 150 ℃, and then opening the furnace for sampling to obtain the coating tap.
Example 2
The preparation method of this example is basically the same as that of example 1, except that: the second plasma etching is carried out after the plasma nitriding, and the specific steps are as follows:
(1) Polishing the surface of the substrate to a mirror surface after polishing, so that the surface roughness of the substrate is less than 50nm; soaking a substrate in hot alkali solution to remove oil, then placing the substrate in alcohol solution to carry out ultrasonic cleaning, and then placing the substrate in deionized water to soak and clean; and (5) drying after cleaning, and wrapping with dust-free paper for standby.
(2) Placing the substrate on a workpiece frame in a coating furnace, vacuumizing until the cavity pressure in the coating furnace is 2×10 -3 Pa, the resistance heating module is started to heat to 300 ℃.
(3) Argon is introduced at the flow of 300sccm until the atmosphere in the coating furnace is stable; starting a hollow cathode gun, applying a negative bias voltage of 60V to a workpiece, then introducing hydrogen at a flow rate of 150sccm, and then performing first plasma etching on the surface of the substrate for 30 min; in the first plasma etching process, the resistance heating module is kept on, so that the temperature of the base material is heated to 450 ℃; after the first plasma etching is finished, the hollow cathode gun is closed.
(4) Argon is introduced at a flow of 210sccm, and nitrogen is introduced at a flow of 210sccm, so that the cavity pressure in the coating furnace is kept at 1.2Pa; starting a hollow cathode gun, applying a negative bias voltage of 500V to the substrate, and then carrying out plasma nitriding on the surface of the substrate for 60min, so as to form a nitriding layer with the thickness of 15 mu m on the surface of the substrate; after the plasma nitriding is finished, the hollow cathode gun is closed.
(5) Argon is introduced at the flow of 350sccm, a hollow cathode gun is started, 180V negative bias is applied to the base material, and then second plasma etching is carried out on the surface of the nitriding layer for 90 min; and after the second plasma etching is finished, closing the hollow cathode gun.
(6) Continuously introducing nitrogen at the flow of 1200sccm, and keeping the cavity pressure in the coating furnace at 4.2Pa; starting the CrAlB target, applying a negative bias voltage of 100V to the workpiece, and then performing arc ion deposition on the nitriding layer for 120min, so as to form a CrAlBN coating with the thickness of 2.4 mu m on the nitriding layer.
(7) After the coating treatment is finished, closing the CrAlB target, cooling to 350 ℃ along with a furnace, and introducing nitrogen until the cavity pressure is 5 multiplied by 10 4 Pa, continuously cooling to 150 ℃, and then opening the furnace for sampling to obtain the coating tap.
Example 3
The preparation method of this example is basically the same as that of example 1, except that: the second plasma etching is carried out both before and after the plasma nitriding, and the specific steps are as follows:
(1) Polishing the surface of the substrate to a mirror surface after polishing, so that the surface roughness of the substrate is less than 50nm; soaking a substrate in hot alkali solution to remove oil, then placing the substrate in alcohol solution to carry out ultrasonic cleaning, and then placing the substrate in deionized water to soak and clean; and (5) drying after cleaning, and wrapping with dust-free paper for standby.
(2) Placing the substrate on a workpiece frame in a coating furnace, vacuumizing until the cavity pressure in the coating furnace is 2×10 -3 Pa, the resistance heating module is started to heat to 300 ℃.
(3) Argon is introduced at the flow of 300sccm until the atmosphere in the coating furnace is stable; starting a hollow cathode gun, applying a negative bias voltage of 60V to a workpiece, then introducing hydrogen at a flow rate of 150sccm, and then performing first plasma etching on the surface of the substrate for 30 min; in the first plasma etching process, the resistance heating module is kept on, so that the temperature of the base material is heated to 450 ℃; after the first plasma etching is finished, the hollow cathode gun is closed.
(4) Argon is introduced at the flow of 350sccm, a hollow cathode gun is started, 180V negative bias is applied to the substrate, and then the surface of the substrate is subjected to 90min of second plasma etching; and after the second plasma etching is finished, closing the hollow cathode gun.
(5) Argon is introduced at a flow of 210sccm, and nitrogen is introduced at a flow of 210sccm, so that the cavity pressure in the coating furnace is kept at 1.2Pa; starting a hollow cathode gun, applying a negative bias voltage of 500V to the substrate, and then carrying out plasma nitriding on the surface of the substrate for 60min, so as to form a nitriding layer with the thickness of 25 mu m on the surface of the substrate; after the plasma nitriding is finished, the hollow cathode gun is closed.
(6) Argon is introduced at the flow of 350sccm, a hollow cathode gun is started, 180V negative bias is applied to the base material, and then second plasma etching is carried out on the surface of the nitriding layer for 60min; and after the second plasma etching is finished, closing the hollow cathode gun.
(7) Continuously introducing nitrogen at the flow of 1200sccm, and keeping the cavity pressure in the coating furnace at 4.2Pa; starting the CrAlB target, applying a negative bias voltage of 100V to the workpiece, and then performing arc ion deposition on the nitriding layer for 120min, so as to form a CrAlBN coating with the thickness of 2.4 mu m on the nitriding layer.
(8) After the coating treatment is finished, closing the CrAlB target, cooling to 350 ℃ along with a furnace, and introducing nitrogen until the cavity pressure is 5 multiplied by 10 4 Pa, continuously cooling to 150 ℃, and then opening the furnace for sampling to obtain the coating tap.
Comparative example 1
This comparative example was prepared in substantially the same manner as in example 1 except that: the comparative example was not subjected to plasma nitriding, and the specific steps are as follows:
(1) Polishing the surface of the substrate to a mirror surface after polishing, so that the surface roughness of the substrate is less than 50nm; soaking a substrate in hot alkali solution to remove oil, then placing the substrate in alcohol solution to carry out ultrasonic cleaning, and then placing the substrate in deionized water to soak and clean; and (5) drying after cleaning, and wrapping with dust-free paper for standby.
(2) Placing the substrate on a workpiece frame in a coating furnace, vacuumizing until the cavity pressure in the coating furnace is 2×10 -3 Pa, the resistance heating module is started to heat to 300 ℃.
(3) Argon is introduced at the flow of 300sccm until the atmosphere in the coating furnace is stable; starting a hollow cathode gun, applying a negative bias voltage of 60V to a workpiece, then introducing hydrogen at a flow rate of 150sccm, and then performing first plasma etching on the surface of the substrate for 30 min; in the first plasma etching process, the resistance heating module is kept on, so that the temperature of the base material is heated to 450 ℃; after the first plasma etching is finished, the hollow cathode gun is closed.
(4) Argon is introduced at the flow of 350sccm, a hollow cathode gun is started, 180V negative bias is applied to the substrate, and then the surface of the substrate is subjected to 90min of second plasma etching; and after the second plasma etching is finished, closing the hollow cathode gun.
(5) Continuously introducing nitrogen at the flow of 1200sccm, and keeping the cavity pressure in the coating furnace at 4.2Pa; starting the CrAlB target, applying a negative bias voltage of 100V to the workpiece, and then performing arc ion deposition on the nitriding layer for 120min, so as to form a CrAlBN coating with the thickness of 2.4 mu m on the nitriding layer.
(6) After the coating treatment is finished, closing the CrAlB target, cooling to 350 ℃ along with a furnace, and introducing nitrogen into the cavityThe pressure is 5 multiplied by 10 4 Pa, continuously cooling to 150 ℃, and then opening the furnace for sampling to obtain the coating tap.
Test case
(1) Morphology characterization and elemental analysis: the elemental analysis of the coated tap of example 1 was performed using a Scanning Electron Microscope (SEM) of Zeiss Gemini Sigma and an Oxford spectroscopy probe, and the results are shown in fig. 1-2. FIG. 1 is a cross-sectional morphology of the coated tap of example 1, in which a distinct white bright layer was formed at the interface between the coating and the substrate, which was observed in the Inlens mode of SEM, and the thickness of the white bright layer was about 0.5. Mu.m, indicating that the surface of the substrate was significantly modified after plasma nitriding treatment, forming a more fine-grained dense compound layer (typically the nitrided layer was a nitrogen element diffusion layer, and the thickness was greater than that of the white bright layer or compound layer), and laterally reflecting the improvement in hardness and adhesion of the nitriding treatment. Fig. 2 is a cross-sectional nitrogen profile of the coated tap of fig. 1, from which it can be seen that the nitrogen signal is concentrated in the interfacial layer of the coating and the substrate, and the surface of the substrate is a nitrogen-rich region.
(2) Metallographic analysis: the coated taps of examples 1 to 3 were respectively prepared into metallographic sections according to ASTM E3-11, and the metallographic sections were observed under 500-fold magnification using a Leica DMI 8C metallographic microscope, and the results are shown in FIGS. 3 to 5.
FIG. 3 is a metallographic section of the coated tap of example 1 with a nitrided layer depth of about 25 μm; FIG. 4 is a metallographic section of the coated tap of example 2 with a nitrided layer depth of about 15 μm; FIG. 5 is a metallographic section of the coated tap of example 3 with a nitrided layer depth of about 25 μm.
(3) Nano hardness, elastic modulus and stress strain curve: according to the instrument indentation test of hardness and material parameters of ISO 14577:2015, the stress-strain curve of the nitride coating of each coating tap was obtained by using an Anton Paar NHT3 nanoindentation instrument, and the nano hardness and elastic modulus of the nitride coating of each coating tap were calculated from the stress-strain curve, and the results are shown in FIG. 6.
FIG. 6 is a graph comparing the nano hardness and elastic modulus of the nitride coating of each coating tap, and it can be seen that the nitride coating is better supported by the nitriding layer after plasma nitriding treatment, so that the nano hardness and elastic modulus of the nitride coating are improved; among them, the nitride coating of example 2 was optimal in nano hardness and elastic modulus, and was greatly improved as compared with comparative example 1 without nitriding layer.
(4) Binding force: the binding force of the nitride coating of each coating tap was measured using an Anton Paar RST3 scratch meter according to ASTM C1624-05, test method for adhesion strength and mechanical failure type of ceramic coating with quantitative single point allergy test, and the results are shown in fig. 7.
The load of complete peeling of the coating is the high critical load LC2, the larger the value of LC2, the higher the film-based bonding force of the coating. As can be seen from fig. 7, LC2 of the nitride of comparative example 1 was 56N, and LC2 of the nitrides of examples 1 to 3 were 72N, 75N and 73N, respectively; the bonding force of the nitride coatings of examples 1-3 is significantly improved, demonstrating that the presence of the nitriding layer can reduce the hardness gap between the substrate and the nitride coating, thereby improving the film-based bonding force of the nitride coating.
(4) Wear profile: after 300 holes were formed in steel No. 45 with the coating tap, the wear profile of the coating tap was observed with a KEYENCE VHX-7000N digital microscope system, and the results are shown in FIGS. 8 to 11.
The coating taps of examples 1-3 and comparative example 1 were three rows of tooth cutting taps, fig. 8 is a graph of wear profile of the first row of tooth flank of each coating tap, fig. 9 is a graph of wear profile of the second row of tooth flank of each coating tap, fig. 10 is a graph of wear profile of the third row of tooth flank of each coating tap, and fig. 11 is a graph of wear profile at the root of each coating tap. As is clear from fig. 8 to 11, the coated tap after plasma nitriding treatment had less wear on the cutting face and the tooth root and the cutting edge was more complete than comparative example 1.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. The scope of the invention is therefore intended to be covered by the appended claims, and the description and drawings may be interpreted in accordance with the contents of the claims.
Claims (13)
1. The preparation method of the composite coating is characterized by comprising the following steps of:
arranging a substrate in a reaction cavity, vacuumizing, and preheating the substrate;
argon and hydrogen are introduced into the reaction cavity, first plasma etching is carried out under the condition of arc discharge, and the temperature of the base material is increased to nitriding temperature;
argon and nitrogen are introduced into the reaction cavity, and plasma nitriding is carried out under the conditions of arc discharge and glow discharge, so that a nitriding layer is formed on the surface of the base material;
forming a nitride coating on the nitrided layer;
wherein the method further comprises the following steps before and/or after plasma nitriding: argon is introduced into the reaction cavity, and second plasma etching is performed under the condition of arc discharge.
2. The method of preparing a composite coating according to claim 1, wherein the nitride coating comprises one or more of a TiAlN coating, a TiSiN coating, a CrAlN coating, a cracn coating, a crabn coating, and a craaltisin coating.
3. The method of producing a composite coating according to claim 1, wherein the nitriding temperature is 440 ℃ to 480 ℃.
4. A method of producing a composite coating according to any one of claims 1 to 3, wherein the first plasma etching is performed under the condition of arc discharge, comprising the steps of:
and (3) turning on an ion source to generate arc discharge, applying a negative bias voltage of 30-100V to the substrate, and then performing first plasma etching on the surface of the substrate for 30-60 min.
5. A method of producing a composite coating according to any one of claims 1 to 3, wherein the second plasma etching is performed under the condition of arc discharge, comprising the steps of:
and (3) turning on an ion source to generate arc discharge, applying a negative bias voltage of 150-200V to the substrate, and then carrying out argon etching for 90-150 min on the surface of the substrate or the surface of the nitriding layer.
6. A method of producing a composite coating according to any one of claims 1 to 3, wherein the plasma nitriding is performed under the conditions of arc discharge and glow discharge, comprising the steps of:
and (3) turning on an ion source to generate arc discharge, applying a negative bias voltage of 300-600V to the substrate, and then carrying out plasma nitriding on the surface of the substrate for 30-90 min.
7. The method of preparing a composite coating according to claim 6, wherein one or more of the following conditions are satisfied:
1) The flow ratio of the argon to the nitrogen is 1: (1-3);
2) The pressure of the reaction cavity is 0.5 Pa-1.5 Pa;
3) The thickness of the nitriding layer is 15-30 mu m.
8. A method of producing a composite coating according to any one of claims 1 to 3, wherein the method of forming a nitride coating on the nitrided layer is arc ion deposition.
9. The method of preparing a composite coating according to claim 8, wherein the arc ion deposition comprises the steps of:
and (3) introducing nitrogen, starting an arc target to generate arc discharge, applying a negative bias voltage of 60-120V to the base material, and then performing arc ion deposition on the nitriding layer for 120-180 min.
10. The method of preparing a composite coating according to claim 9, wherein one or more of the following conditions are satisfied:
1) The pressure of the reaction cavity is 3.8 Pa-4.2 Pa;
2) The target current of the coating target is 100A-150A;
3) The thickness of the nitride coating is 2-2.5 mu m.
11. A method of producing a composite coating according to any one of claims 1 to 3, wherein one or more of the following conditions are satisfied:
1) The pressure of the reaction cavity after being vacuumized is 1 multiplied by 10 -3 Pa～1×10 -2 Pa；
2) The preheating temperature is 300-350 ℃.
12. A composite coating prepared by the method of any one of claims 1 to 11.
13. A coated tap comprising the composite coating of claim 12.
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| CN202310891796.3A CN117089804A (en) | 2023-07-20 | 2023-07-20 | Composite coating, preparation method thereof and coated tap |
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| CN202310891796.3A CN117089804A (en) | 2023-07-20 | 2023-07-20 | Composite coating, preparation method thereof and coated tap |
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