CN114632910B - Preparation method of nano composite multi-element carbon oxide coating on surface of die-casting aluminum die - Google Patents
Preparation method of nano composite multi-element carbon oxide coating on surface of die-casting aluminum die Download PDFInfo
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- 239000011248 coating agent Substances 0.000 title claims abstract description 36
- 238000000576 coating method Methods 0.000 title claims abstract description 36
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 31
- 238000004512 die casting Methods 0.000 title claims abstract description 31
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 29
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910002090 carbon oxide Inorganic materials 0.000 title claims abstract description 29
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 23
- 239000002052 molecular layer Substances 0.000 claims abstract description 13
- 230000007704 transition Effects 0.000 claims abstract description 13
- 229910008482 TiSiN Inorganic materials 0.000 claims abstract description 11
- QRXWMOHMRWLFEY-UHFFFAOYSA-N isoniazide Chemical group NNC(=O)C1=CC=NC=C1 QRXWMOHMRWLFEY-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000010410 layer Substances 0.000 claims description 73
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 45
- 229910008484 TiSi Inorganic materials 0.000 claims description 41
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 40
- 238000000034 method Methods 0.000 claims description 34
- 238000004140 cleaning Methods 0.000 claims description 32
- 229910052786 argon Inorganic materials 0.000 claims description 23
- 238000000151 deposition Methods 0.000 claims description 21
- 229910052757 nitrogen Inorganic materials 0.000 claims description 20
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 16
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 14
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- 150000002500 ions Chemical class 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- 239000002356 single layer Substances 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 238000010891 electric arc Methods 0.000 claims description 5
- 238000001771 vacuum deposition Methods 0.000 claims description 5
- 239000000758 substrate Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 4
- 238000007607 die coating method Methods 0.000 abstract description 3
- 210000002381 plasma Anatomy 0.000 description 18
- 230000001105 regulatory effect Effects 0.000 description 8
- 229910000838 Al alloy Inorganic materials 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000007733 ion plating Methods 0.000 description 4
- 150000004767 nitrides Chemical class 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 238000005137 deposition process Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000003491 array Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- -1 argon ions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 238000011086 high cleaning Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000002346 layers by function Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C3/00—Selection of compositions for coating the surfaces of moulds, cores, or patterns
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D17/00—Pressure die casting or injection die casting, i.e. casting in which the metal is forced into a mould under high pressure
- B22D17/20—Accessories: Details
- B22D17/22—Dies; Die plates; Die supports; Cooling equipment for dies; Accessories for loosening and ejecting castings from dies
- B22D17/2209—Selection of die materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C23C14/0021—Reactive sputtering or 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
- C23C14/06—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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention relates to the field of die coating, in particular to a preparation method of a nano composite multi-element carbon oxide coating on the surface of a die-casting aluminum die, wherein the coating is respectively a basic layer, a composite transition layer and a multi-layer circulating nano layer from inside to outside; wherein the basic layer is AlCrN, the composite transition layer is TiSiN/AlCrN composite layer, and the multilayer circulating nano layer is TISIALCRCN/TiSiAlCrCON alternating layer. Because the base layer is AlCrN and the composite layer is AlCrN/TiSiN, the hardness gradient is naturally formed by the material properties of AlCrN and AlCrN/TiSiN layers without deliberately changing parameters such as bias voltage, air pressure and the like; meanwhile, the existence of Al, cr, si and the like in the coating optimizes the surface energy of the die surface on one hand and effectively improves the red hardness of the coating from the substrate layer on the other hand.
Description
Technical Field
The invention relates to the technical field of die coating preparation, in particular to a preparation method of a nano composite multi-element carbon oxide coating on the surface of a die casting aluminum die.
Background
The die-casting aluminum die is an important tool in aluminum alloy forming processing, and can apply certain pressure to realize forging and pressing in the aluminum alloy casting process when metal flows into a cavity at a low speed or a high speed. The die casting die has high manufacturing cost, and can realize the molding of large-batch and large-quantity products.
In the die casting process of the aluminum alloy, the surface and the inside of the die are subjected to repeated and circulated thermal stress to generate microcracks on the one hand, and the cold and the hot are repeatedly alternated. Meanwhile, in the die casting process of the aluminum alloy, the aluminum alloy is easy to be compatible with the surface material of the die, and the sticking and demolding are difficult.
On the premise of not changing the die material, the surface treatment is a main technical means for prolonging the service life of the die-casting aluminum die. Although the traditional nitriding, metal infiltration, cladding and other processes can realize the surface strengthening of the die casting die, the nitriding has little effect on improving the hardness; the mold is easy to deform due to the higher temperature required by metal infiltration; and cladding is suitable for the surface of a die with a simpler shape, and is difficult to apply to dies with multiple holes and the like.
PVD is a technical means for carrying out surface treatment on a die-casting aluminum die at present, on one hand, the surface hardness of the die can be improved by depositing a coating, and on the other hand, the processing temperature is lower, and the die cannot be deformed. The prior art finds that for a die-casting aluminum die, the main technical principle of prolonging the service life of the die is as follows; the hardness of the surface of the die is improved, the surface energy of the surface of the die is reduced, and the high-temperature oxidation resistance of the surface of the die is improved. The hardness of the surface of the die is improved, so that the surface of the die can be effectively protected, the erosion of liquid aluminum is prevented, and the resistance to thermal cracking is improved; the surface energy of the surface of the die is reduced, so that the adhesive force between the liquid aluminum and the die is reduced, and the die is convenient to demould; the better the high-temperature oxidation resistance of the surface of the die is, the more stable the surface structure is, and the longer the service life is.
At present, a die-casting aluminum die coating prepared by conventional PVD mainly comprises a pure metal, a unit nitride, a unit and multi-nitride composite supporting layer, a multi-nitride and oxynitride composite hardening layer and an anti-adhesion layer, and a multi-gradient and progressive coating deposition mode is adopted to realize soft-to-hard transition deposition due to low ion plating energy of traditional magnetron sputtering or arc ion plating, and then functional layer (high hardness, anti-adhesion and corrosion resistance) deposition is carried out; however, the technology is complex in deposition process, low in ion energy in the magnetic control process, insufficient in reaction of the formed coating and large in quantity of large particles in arc ion plating, so that the surface of the coating is uneven, the quality of a finished product formed by die casting of a die is affected, and the service life of the die is also affected.
Disclosure of Invention
The invention aims to overcome the defects and the shortcomings in the prior art and provides a preparation method of a nano composite multi-element carbon oxide coating on the surface of a die-casting aluminum die.
The technical scheme adopted by the invention is as follows: the preparation method of the nano composite multi-element carbon oxide coating on the surface of the die-casting aluminum die comprises the steps of respectively forming a base layer, a composite transition layer and a plurality of circulating nano layers from inside to outside; wherein the basic layer is AlCrN, the composite transition layer is TiSiN/AlCrN composite layer, and the multilayer circulating nano layer is TISIALCRCN/TiSiAlCrCON alternating layers;
the preparation method is carried out in pulse arc source vacuum coating equipment, the pulse arc source comprises at least one row of metal AlCr targets and two rows of TiSi targets, the pulse arc source is provided with at least one group of pulse arc sources which are AlCr targets and TiSi targets which are arranged in opposite directions, the AlCr targets and the TiSi targets which are arranged in opposite directions are respectively positioned at two sides of a die to be coated, and the pulse arc source is provided with at least one group of pulse arc sources which are AlCr targets and TiSi targets which are arranged adjacently;
The preparation method comprises the following steps:
1) Placing a die to be plated into a vacuum coating device for preheating;
2) Carrying out plasma cleaning on the surface of the die by adopting an ion cleaning source;
3) Introducing nitrogen, opening at least one row of AlCr targets, and depositing an AlCrN layer;
4) Introducing nitrogen, simultaneously starting a group of TiSi targets and AlCr targets which are arranged in opposite directions, and depositing an AlCrN/TiSiN composite layer;
5) Introducing acetylene, nitrogen and argon, simultaneously starting a group of TiSi targets and AlCr targets which are adjacently arranged, and depositing TISIALCRCN layers;
6) Introducing oxygen, acetylene, nitrogen and argon, simultaneously starting a group of TiSi targets and AlCr targets which are adjacently arranged, and depositing TiSiAlCrCON layers;
7) And alternately repeating the step 5) and the step 6) to form a plurality of circulating nano layers.
The thickness of the base layer is 300-1500 nanometers, the thickness of the composite transition layer is 100-800 nanometers, and the thickness of the multi-layer circulating nano layer is 100-1000 nanometers; the TiSiAlCrCON layers have a thickness that is no greater than 30% of the thickness of the multilayer circulating nanolayer.
The two rows of metal AlCr targets and the two rows of TiSi targets are sequentially distributed in a clockwise direction into a first AlCr target, a first TiSi target, a second AlCr target and a second TiSi target, wherein the first AlCr target and the second TiSi target are oppositely arranged and are respectively positioned at two sides of a die to be plated; and (2) alternately using two or three of the adjacent TiSi targets and AlCr targets formed by the first AlCr target and the first TiSi target, the adjacent TiSi targets and AlCr targets formed by the first TiSi target and the second AlCr target, and the adjacent TiSi targets and AlCr targets formed by the second AlCr target and the second TiSi target in the process of at least part of the steps 4) -6).
In the step 3) and the step 4), the pulse arc discharge of the pulse arc target adopts a mode of superposition of base value current and pulse arc current discharge, wherein the base value current is 20-40A, the high value pulse current is 300-1500A, the frequency is 30-150Hz, and the duty ratio is 10-40%.
In the step 5), acetylene, nitrogen and argon are mixed into mixed gas, wherein the atomic ratio of the argon is not less than 30%, the atomic ratio of the nitrogen is not more than 60%, and the atomic ratio of the acetylene is not more than 20%.
In the step 6), oxygen, acetylene, nitrogen and argon are mixed into mixed gas and are introduced, wherein the atomic ratio of the argon is not less than 30%, the atomic ratio of the nitrogen is not more than 60%, the atomic ratio of the acetylene is not more than 20%, and the atomic ratio of the oxygen is not more than 20%.
The monolayer time deposited in step 5) and step 6) is 1-5min, wherein the monolayer time deposited in step 5) is at least 3 times greater than the monolayer time deposited in step 6).
The circulation times of the steps 5) and 6) are not less than 4, and the carbon oxide layer is the outermost layer of the coating.
In step 2), the plasma cleaning setting parameters are as follows: the bias voltage is set to 20-300V, the duty ratio is 60-80%, the frequency is 15-30khz, argon and hydrogen are introduced, the air pressure is controlled to be 2-5Pa, and the time is 10-140min. The plasma cleaning in step 2) includes, but is not limited to, ion sources, bias glow cleaning, hot wire cleaning, arc excited electron ionization sources.
In the steps 3) and 4), the bias voltage is set to be 20-200V, the duty ratio is 60-80%, the frequency is 15-30khz, and the air pressure is controlled to be 2-5Pa; in the steps 5) and 6), the air pressure is controlled to be 1-3Pa, the bias voltage is set to be 20-200V, the duty ratio is 60-80%, and the frequency is 15-30khz.
The beneficial effects of the invention are as follows:
1. The binary nitride layer is directly deposited on the surface of the die as a base layer, and the complex deposition process of the gradient layers of metal, nitride and multi-element nitride in the current stage is abandoned, on the one hand, because the invention adopts the technical advantage of pulse arc, and on the other hand, the invention has the effect of cleaning the depth plasma of the surface of the die; the invention greatly simplifies the process steps of the coating;
2. According to the invention, the base layer is AlCrN, the composite layer is AlCrN/TiSiN, and the hardness gradient is naturally formed by the material properties of AlCrN and AlCrN/TiSiN layers without deliberately changing parameters such as bias voltage, air pressure and the like; meanwhile, the existence of Al, cr, si and the like in the coating optimizes the surface energy of the surface of the die on one hand and effectively improves the red hardness of the coating from the substrate layer on the other hand;
3. According to the invention, acetylene is introduced to generate carbonitrides of AlCr and TiSi metals, so that carbide can be effectively formed by adding acetylene on one hand, a dispersion strengthening effect is formed, a grain refinement effect can be effectively improved, and on the other hand, the wear resistance of a coating is improved and the friction coefficient is reduced due to the existence of carbide;
4. According to the invention, oxygen is intermittently introduced to effectively form the carbo-oxynitride in the carbo-nitride, on one hand, a nano-scale gap is formed in the coating, so that the surface energy of the surface of the coating can be effectively reduced, and on the other hand, the existence of the oxide inhibits the oxidation speed of the die in a high-temperature state in the use process, and the service life of the die is effectively prolonged;
5. The pulse arc source is used as a current source for depositing the carbon oxide of the die-casting aluminum, so that the ionization rate of the traditional direct current arc source can be further improved, and the surface structure of the coating is fine. The mode of stable arc with low base value and high pulse current can effectively reduce the generation of large particles, further provide the fineness of the surface structure of the coating, and be favorable for prolonging the service life of the die.
In conclusion, the nano composite multi-element carbon oxide coating on the surface of the die-casting aluminum die has good binding force, wear resistance and temperature resistance, and meanwhile, the surface has good smoothness, so that the die-casting aluminum die can work stably for a long time.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are required in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that it is within the scope of the invention to one skilled in the art to obtain other drawings from these drawings without inventive faculty.
FIG. 1 is a schematic diagram of the structure of a nanocomposite multi-element carbon oxide layer on the surface of a die-cast aluminum die;
FIG. 2 is a schematic diagram of an apparatus for preparing a carbon oxide coating according to the present invention;
FIG. 3 is a schematic diagram of pulsed arc current output;
FIG. 4 illustrates hot wire plasma cleaning in accordance with the present invention;
FIG. 5 is a schematic view of an arc-excited electron ionization source cleaning apparatus according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings, for the purpose of making the objects, technical solutions and advantages of the present invention more apparent.
See fig. 1: the nano composite multi-element carbon oxide layer 2 on the surface of the die-casting aluminum die 1 comprises a base layer 21, a composite transition layer 22 and a plurality of circulating nano layers 23, wherein the base layer 21 is AlCrN, the composite transition layer 22 is a TiSiN/AlCrN composite layer, and the plurality of circulating nano layers 23 are TISIALCRCN/TiSiAlCrCON alternating layers; and not less than 4 circulating layers between the carbonitride and the oxycarbonitride in the multilayer circulating nano-layer 23. Wherein: the thickness of the base layer 21 is 300-1500 nanometers, the thickness of the composite transition layer 22 is 100-800 nanometers, the thickness of the multi-layer circulating nano layer 23 is 100-1000 nanometers, and the total thickness of the nano composite multi-element carbon oxide layer 2 is 2000-3500 nanometers.
The multilayer circulating nano-layer is an alternating layer of carbon nitride and carbon oxynitride formed by intermittently introducing oxygen, and the thickness of the carbon oxynitride layer accounts for not more than 30% of the thickness of the multilayer circulating nano-layer.
See fig. 2: the invention relates to equipment for preparing a nano composite multi-element carbon oxide layer, which is pulse arc source vacuum coating equipment, wherein 4 rows of arc sources are configured, 01 rows and 04 rows of metal AlCr targets are respectively arranged, 02 rows and 03 rows of TiSi targets are respectively arranged, and an ion cleaning device is arranged at 05 positions. In the invention, 01 columns of arcs are adopted when the base layer 21AlCrN layer is deposited, 01 and 02 columns of arcs are adopted for the composite transition layer 22 TiSiN/AlCrN composite layer, and 01 and 03 columns are one group and 02 and 04 are one group when the multi-layer circulating nano layer 23TISIALCRCN/TiSiAlCrCON alternate layer is deposited, so that the target surface carbonization phenomenon in the carbon oxide deposition process can be reduced, and the method can be alternatively and intermittently used; 05 is an ion cleaning device.
The preparation method of the die-casting aluminum die nano composite multi-element carbon oxide layer is as follows:
Example one hot filament plasma cleaning deposition of carbon oxide layers
Referring to fig. 2 and 4, the ion cleaning device 05 is a hot filament plasma cleaning device, and the principle of the ion cleaning device is that the hot filament plasma cleaning device comprises a hot filament component and a hot filament anode, wherein a heating power supply and a negative electrode of an anode power supply are applied to a filament, the anode of the filament is loaded with a positive electrode of the anode power supply, heated electrons of the filament overflow, and under the action of an electric field of the anode power supply, the electrons move to the anode, and collide with argon gas in the moving process of the electrons, so that more plasmas are ionized; the plasma bombards the die to be plated on the rotating frame with a large amount of argon ions under the action of the rotating frame bias electric field.
See fig. 3: the pulse arc is used as an arc stabilizing current, the peak current is a pulse strong current, and strong current can be instantaneously applied to the target surface, so that the magnetic field intensity of the target surface is increased due to the application of the strong current, on the one hand, the arc spots on the target surface are branched to form split arcs, the generation of large particles is reduced, on the other hand, the superposition of the instantaneous strong current is reduced, the magnitude of the arc stabilizing base current (more than 45A of a direct current power supply and the normal operation of the pulse arc current 20A) can be greatly reduced, the generation of the large particles can be reduced, meanwhile, the superposition of the strong current can improve the plasma intensity in the arc discharge process, and the ionization rate of a cathode can be improved.
As shown in table 1, the main processes of this example are as follows:
1. Vacuum pumping, heating to 450 ℃, preserving heat for 50min, and setting the rotating speed to be 1 revolution/min;
2. Introducing mixed gas of argon and hydrogen, wherein the pressure of the argon 300 and the hydrogen 300, regulating the throttle valve to be 2Pa, controlling the filament current to be 150A, applying linear bias voltage to a substrate to be plated to be 30V-100V (10 min) in a filament anode constant current mode, then cleaning the substrate with 100V for 10min, wherein the duty ratio of a bias power supply is 70%, and the frequency is 20khz;
3. then closing hydrogen, introducing argon 450, regulating the pressure of a throttle valve to be 2.5Pa, controlling filament parameters unchanged, applying linear bias voltage to a substrate to be plated to be 100V-200V (10 min), and then cleaning the substrate for 30min at 200V, wherein the duty ratio of a bias power supply is 70%, and the frequency is 20khz;
4. Then opening 01 AlCr targets, introducing nitrogen 300, regulating the control air pressure of a throttle valve to 3.5Pa, and controlling the pulse arc base value current to 30A, the peak current to 800A, the frequency to 120hz and the duty ratio to 10%; setting the bias voltage to 40V, depositing for 40min, then closing the arc target, and setting the bias power supply duty ratio to 70% and the frequency to 20khz;
5.01 AlCr targets continue to work, 02 TiSi targets are started, the nitrogen flow is unchanged, the air pressure is 3.5Pa, the AlCr target pulse arc base value current is 30A, the peak current is 800A, the frequency is 120hz, and the duty ratio is 10%; the TiSi target pulse arc base value current 33A, peak current 600A, frequency 120hz and duty ratio 10%; setting the bias voltage to 40V, depositing for 25min, setting the bias power supply duty ratio to 70%, and closing 01 and 02 columns of arcs at the frequency of 20 khz;
6. Argon 160, nitrogen 220 and acetylene 50 are introduced, the control pressure of a throttle valve is regulated to be 2Pa, two arrays of arcs of 01 and 03 are opened, alCr target pulse arc base value current is 30A, peak current is 800A, the frequency is 120hz, and the duty ratio is 10%; the TiSi target pulse arc base value current 33A, peak current 600A, frequency 120hz and duty ratio 10%; setting the bias voltage to 40V, depositing for 5min, and setting the bias power supply duty ratio to 70% and the frequency to 20khz;
7. Argon 160, nitrogen 220 and acetylene 50 are introduced, the control pressure of a throttle valve is regulated to be 2Pa, two arrays of arcs of 01 and 03 are opened, alCr target pulse arc base value current is 30A, peak current is 800A, the frequency is 120hz, and the duty ratio is 10%; the TiSi target pulse arc base value current 33A, peak current 600A, frequency 120hz and duty ratio 10%; the bias voltage increased from 40V to 80V in a linear increase, depositing for 5min;
8. introducing oxygen 65, regulating the control air pressure of a throttle valve to 2Pa, keeping the arc parameters of 01 and 03 unchanged, biasing 80v, and depositing for 70s at the frequency of 20khz with the duty ratio of a biasing power supply of 70%. Then closing the 01 and 03 columns of arcs;
9. starting 02 and 04 columns of arcs, keeping the parameters of AlCr targets and TiSi targets unchanged, and depositing for 5min at 80v bias voltage;
10. repeating step 8 with 02.04 columns of arcs, and then closing 02 and 04 columns of arcs;
The steps 9 and 10 are repeated, and each cycle uses 01 and 03 columns of arcs and 02 and 04 columns of arcs periodically.
Example two arc-excited Electron ionization Source cleaning deposition of carbon oxide layers
The main difference between the present embodiment and the first embodiment is that an arc electron excited plasma cleaning device is adopted, that is, the plasma cleaning device with arc electron excited at the position 05 in fig. 2, the arc at the position 05 adopts a conventional dc arc power supply, and the target material is a Ti target.
See fig. 5: the arc electron excited plasma cleaning device is characterized in that the anode of an arc ion plating power supply is loaded on an anode independent of the suspension potential of the whole vacuum chamber, the cathode of the arc power supply is loaded on a cathode arc source, a circular shielding plate with the area about 2 times of the surface of the target and 70-200mm away from the target is arranged in front of the target of the cathode arc source, and the potential of the shielding plate is suspended. The arc striking device is utilized to induce the cathode arc source to generate arc discharge, at the moment, the anode of the cathode arc source is loaded on the anode, and electrons in the discharge process flow back to the cathode arc source through the anode. In the process of moving the electrons to the anode, a large amount of plasmas are excited by the electrons with large beam current, and the plasmas can bombard the die transferred on the rotating frame under the action of the bias voltage on the rotating frame, so that the cleaning, etching and activation of the die are realized.
Compared with the conventional atmospheric glow discharge (bias current below 1A) and ion source discharge (bias current 2-4A), the bias current of the arc light excited plasma can reach 6-10A, and the cleaning bias current of the arc discharge can reach 10A, but the cleaning process needs a large bias voltage of 400-800V, meanwhile, the cleaning source is metal ions, the energy is large, the surface of the mold is easy to coarsen, the cleaning source of the arc light excited plasma is inert gas ions, and a high cleaning effect can be realized under a lower bias voltage of 300V.
The cleaning process comprises the following steps:
(1) Argon 300 and hydrogen 300 are pumped in, the control air pressure of a throttle valve is regulated to be 3Pa, the bias voltage is set to be 40V, a Ti target is started, the arc current is 100A, the bias voltage is linearly increased from 40V to 80V (10 min), and then etching and cleaning are carried out for 10min at 80V.
Then hydrogen is closed, argon is set to 450, the control air pressure of a throttle valve is regulated to 3Pa, the bias voltage is linearly increased to 200v (10 min), the arc current is kept unchanged, the arc target is cleaned for 30min at 200v, and the arc target is closed.
Those of ordinary skill in the art will appreciate that all or a portion of the steps in implementing the methods of the above embodiments may be implemented by a program to instruct related hardware, where the program may be stored in a computer readable storage medium, such as ROM/RAM, a magnetic disk, an optical disk, etc.
The foregoing disclosure is illustrative of the present invention and is not to be construed as limiting the scope of the invention, which is defined by the appended claims.
Claims (10)
1. A preparation method of a nano composite multi-element carbon oxide coating on the surface of a die-casting aluminum die is characterized by comprising the following steps: the coating is respectively a basic layer, a composite transition layer and a plurality of circulating nano layers from inside to outside; wherein the basic layer is AlCrN, the composite transition layer is TiSiN/AlCrN composite layer, and the multilayer circulating nano layer is TISIALCRCN/TiSiAlCrCON alternating layers;
the preparation method is carried out in pulse arc source vacuum coating equipment, the pulse arc source comprises at least one row of metal AlCr targets and two rows of TiSi targets, the pulse arc source is provided with at least one group of pulse arc sources which are AlCr targets and TiSi targets which are arranged in opposite directions, the AlCr targets and the TiSi targets which are arranged in opposite directions are respectively positioned at two sides of a die to be coated, and the pulse arc source is provided with at least one group of pulse arc sources which are AlCr targets and TiSi targets which are arranged adjacently;
The preparation method comprises the following steps:
1) Placing a die to be plated into a vacuum coating device for preheating;
2) Carrying out plasma cleaning on the surface of the die by adopting an ion cleaning source;
3) Introducing nitrogen, opening at least one row of AlCr targets, and depositing an AlCrN layer;
4) Introducing nitrogen, simultaneously starting a group of TiSi targets and AlCr targets which are arranged in opposite directions, and depositing an AlCrN/TiSiN composite layer;
5) Introducing acetylene, nitrogen and argon, simultaneously starting a group of TiSi targets and AlCr targets which are adjacently arranged, and depositing TISIALCRCN layers;
6) Introducing oxygen, acetylene, nitrogen and argon, simultaneously starting a group of TiSi targets and AlCr targets which are adjacently arranged, and depositing TiSiAlCrCON layers;
7) And alternately repeating the step 5) and the step 6) to form a plurality of circulating nano layers.
2. The method for preparing the nanocomposite multi-element carbon oxide coating on the surface of the die-casting aluminum die according to claim 1, wherein the method comprises the following steps: the thickness of the base layer is 300-1500 nanometers, the thickness of the composite transition layer is 100-800 nanometers, and the thickness of the multi-layer circulating nano layer is 100-1000 nanometers; the TiSiAlCrCON layers have a thickness that is no greater than 30% of the thickness of the multilayer circulating nanolayer.
3. The method for preparing the nanocomposite multi-element carbon oxide coating on the surface of the die-casting aluminum die according to claim 1, wherein the method comprises the following steps: the two rows of metal AlCr targets and the two rows of TiSi targets are sequentially distributed in a clockwise direction into a first AlCr target, a first TiSi target, a second AlCr target and a second TiSi target, wherein the first AlCr target and the second TiSi target are oppositely arranged and are respectively positioned at two sides of a die to be plated; and (2) alternately using two or three of the adjacent TiSi targets and AlCr targets formed by the first AlCr target and the first TiSi target, the adjacent TiSi targets and AlCr targets formed by the first TiSi target and the second AlCr target, and the adjacent TiSi targets and AlCr targets formed by the second AlCr target and the second TiSi target in the process of at least part of the steps 4) -6).
4. The method for preparing the nanocomposite multi-element carbon oxide coating on the surface of the die-casting aluminum die according to claim 1, wherein the method comprises the following steps: in the step 3) and the step 4), the pulse arc discharge of the pulse arc target adopts a mode of superposition of base value current and pulse arc current discharge, wherein the base value current is 20-40A, the high value pulse current is 300-1500A, the frequency is 30-150Hz, and the duty ratio is 10-40%.
5. The method for preparing the nanocomposite multi-element carbon oxide coating on the surface of the die-casting aluminum die according to claim 1, wherein the method comprises the following steps: in the step 5), acetylene, nitrogen and argon are mixed into mixed gas, wherein the atomic ratio of the argon is not less than 30%, the atomic ratio of the nitrogen is not more than 60%, and the atomic ratio of the acetylene is not more than 20%.
6. The method for preparing the nanocomposite multi-element carbon oxide coating on the surface of the die-casting aluminum die according to claim 1, wherein the method comprises the following steps: in the step 6), oxygen, acetylene, nitrogen and argon are mixed into mixed gas and are introduced, wherein the atomic ratio of the argon is not less than 30%, the atomic ratio of the nitrogen is not more than 60%, the atomic ratio of the acetylene is not more than 20%, and the atomic ratio of the oxygen is not more than 20%.
7. The method for preparing the nanocomposite multi-element carbon oxide coating on the surface of the die-casting aluminum die according to claim 1, wherein the method comprises the following steps: the monolayer time of the step 5) and the step 6) is 1-5min, wherein the monolayer time of the step 5) is more than 3 times of the monolayer time of the step 6).
8. The method for preparing the nanocomposite, multi-element carbon oxide coating on the surface of the die-casting aluminum die according to claim 7, wherein: the circulation times of the steps 5) and 6) are not less than 4, and the carbon oxide layer is the outermost layer of the coating.
9. The method for preparing the nanocomposite multi-element carbon oxide coating on the surface of the die-casting aluminum die according to claim 1, wherein the method comprises the following steps: in step 2), the plasma cleaning setting parameters are as follows: the bias voltage is set to 20-300V, the duty ratio is 60-80%, the frequency is 15-30kHz, argon and hydrogen are introduced, the air pressure is controlled to be 2-5Pa, and the time is 10-140min.
10. The method for preparing the nanocomposite multi-element carbon oxide coating on the surface of the die-casting aluminum die according to claim 1, wherein the method comprises the following steps: in the steps 3) and 4), the bias voltage is set to be 20-200V, the duty ratio is 60-80%, the frequency is 15-30kHz, and the air pressure is controlled to be 2-5Pa; in the steps 5) and 6), the air pressure is controlled to be 1-3Pa, the bias voltage is set to be 20-200V, the duty ratio is 60-80%, and the frequency is 15-30kHz.
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