CN114632910A - Preparation method of nano-composite multi-element oxycarbide coating on surface of die-casting aluminum die - Google Patents
Preparation method of nano-composite multi-element oxycarbide coating on surface of die-casting aluminum die Download PDFInfo
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- 239000011248 coating agent Substances 0.000 title claims abstract description 37
- 238000000576 coating method Methods 0.000 title claims abstract description 37
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 31
- 238000004512 die casting Methods 0.000 title claims abstract description 30
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 24
- 229910002090 carbon oxide Inorganic materials 0.000 claims abstract description 22
- 239000002052 molecular layer Substances 0.000 claims abstract description 17
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 14
- 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
- 238000004140 cleaning Methods 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 32
- 229910052786 argon Inorganic materials 0.000 claims description 23
- 229910052757 nitrogen Inorganic materials 0.000 claims description 20
- 238000000151 deposition Methods 0.000 claims description 18
- 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
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- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
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- 239000002356 single layer Substances 0.000 claims description 6
- 238000010891 electric arc Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 238000001771 vacuum deposition Methods 0.000 claims description 3
- 238000007747 plating Methods 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 5
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- 210000002381 plasma Anatomy 0.000 description 19
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- 150000004767 nitrides Chemical class 0.000 description 4
- 239000013077 target material Substances 0.000 description 4
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
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- 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
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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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- Condensed Matter Physics & Semiconductors (AREA)
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Abstract
The invention relates to the field of die coatings, in particular to a preparation method of a nano composite multi-component carbon oxide coating on the surface of a die-casting aluminum die, wherein the coating is respectively a base layer, a composite transition layer and a multi-layer circulating nano layer from inside to outside; wherein the base layer is AlCrN, the composite transition layer is a TiSiN/AlCrN composite layer, and the multi-layer circulating nano layer is a TiSiAlCrCN/TiSiAlCrCON alternating layer. Because the basic layer is AlCrN and the composite layer AlCrN/TiSiN, hardness gradient is naturally formed by the material properties of the AlCrN and AlCrN/TiSiN layers without changing bias voltage, air pressure and other parameters intentionally; 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.
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 when metal flows into a cavity at low speed or high speed, a certain pressure can be applied to forge and press the aluminum alloy in the casting process. The die-casting die is high in manufacturing cost, and can realize large-batch and large-quantity product molding.
In the aluminum alloy die-casting process, on one hand, the die is repeatedly cooled and heated alternately, and the surface and the inside of the die are subjected to repeated and cyclic thermal stress to generate microcracks. Meanwhile, in the process of die casting of the aluminum alloy, the aluminum alloy is easy to be compatible with the surface material of the die, and the material adhesion and the demoulding are difficult.
On the premise of not changing the die material, surface treatment is the main technical means for prolonging the service life of the die-casting aluminum die. The traditional nitriding, metal infiltration, cladding and other processes can realize the surface strengthening of the die-casting die, but the nitriding has little effect on improving the hardness; the metal infiltration requires higher temperature to easily cause the deformation of the die; cladding is suitable for the surface of a die with a simpler shape, and is difficult to be applied to dies such as a porous die.
PVD is a more advantageous technical means for carrying out surface treatment on a die-casting aluminum die at the present stage, and on one hand, the surface hardness of the die can be improved through depositing a coating, and on the other hand, the machining temperature is lower, so that the die cannot be deformed. The prior art finds that the main technical principle for prolonging the service life of the die is that for a die-casting aluminum die; 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 corrosion 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, the more stable the surface structure of the die and the longer the service life of the die.
At present, the conventional die-casting aluminum die coating prepared by PVD mainly comprises pure metal, unit nitride, a unit and multi-nitride composite supporting layer, a multi-nitride and nitrogen oxide composite hardening layer and an anti-adhesion layer, and because the ion energy of the traditional magnetron sputtering or arc ion plating is low, a multi-gradient and progressive coating deposition mode is adopted to realize the transition deposition from soft to hard, and then the deposition of functional layers (high hardness, anti-adhesion and corrosion resistance) is carried out; however, the technology is not only complicated in deposition process, but also low in ion energy in magnetic control process, insufficient in reaction of formed coating and large in particle in arc ion plating, so that the surface of the coating is not uniform enough, the quality of finished products formed by die casting of the die is affected, and the service life of the die is affected.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of a nano composite multi-component carbon oxide coating on the surface of a die-casting aluminum die.
The technical scheme adopted by the invention is as follows: a preparation method of a nano composite multi-element carbon oxide coating on the surface of a die-casting aluminum die comprises the following steps that the coating is respectively a base layer, a composite transition layer and a multi-layer circulating nano layer from inside to outside; wherein the base layer is AlCrN, the composite transition layer is a TiSiN/AlCrN composite layer, and the multi-layer circulating nano layer is a TiSiAlCrCN/TiSiAlCrCON alternating layer;
the preparation method is carried out in a pulse arc source vacuum coating device, and the pulse arc source and the ion cleaning device are configured, wherein 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 arranged oppositely, the AlCr targets and the TiSi targets arranged oppositely are respectively positioned at two sides of a mould 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 arranged adjacently;
the preparation method comprises the following steps:
1) placing the die to be plated in a vacuum film plating device for preheating;
2) carrying out plasma cleaning on the surface of the die by adopting an ion cleaning source;
3) introducing nitrogen, starting at least one row of AlCr targets, and depositing an AlCrN layer;
4) introducing nitrogen, simultaneously starting a group of oppositely arranged TiSi targets and AlCr targets, and depositing an AlCrN/TiSiN composite layer;
5) introducing acetylene, nitrogen and argon, simultaneously starting a group of adjacent TiSi targets and AlCr targets, and depositing a TiSiAlCrCN layer;
6) introducing oxygen, acetylene, nitrogen and argon, simultaneously starting a group of adjacent TiSi targets and AlCr targets, and depositing a TiSiAlCrCON layer;
7) and (5) alternately repeating the step 5) and the step 6) to form a plurality of layers of circulating nano-layers.
The thickness of the base layer is 300-1500 nm, the thickness of the composite transition layer is 100-800 nm, and the thickness of the multilayer circulating nano layer is 100-1000 nm; the thickness of the TiSiAlCrCON layer accounts for not more than 30% of the thickness of the multilayer circulating nano layer.
The two rows of metal AlCr targets and the two rows of TiSi targets are distributed in a clockwise direction and are sequentially 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 on two sides of the die to be plated; and (3) alternately using gaps in at least partial processes in the steps 4) to 6) in a group of adjacently arranged TiSi targets and AlCr targets formed by the first AlCr targets and the first TiSi targets, a group of adjacently arranged TiSi targets and AlCr targets formed by the first TiSi targets and the second AlCr targets, and a group of adjacently arranged TiSi targets and AlCr targets formed by the second AlCr targets and the second TiSi targets.
In the step 3) and the step 4), the pulse arc discharge of the pulse arc target adopts a mode of stacking basic value current and pulse arc current discharge, wherein the basic 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%.
And in the step 5), mixing acetylene, nitrogen and argon to form mixed gas, wherein the atomic ratio of argon is not less than 30%, the atomic ratio of nitrogen is not more than 60%, and the atomic ratio of acetylene is not more than 20%.
And 6), mixing oxygen, acetylene, nitrogen and argon to form mixed gas, and introducing the mixed gas, wherein the atomic ratio of the argon is not lower than 30%, the atomic ratio of the nitrogen is not higher than 60%, the atomic ratio of the acetylene is not higher than 20%, and the atomic ratio of the oxygen is not higher than 20%.
The time of the single layer deposited in the steps 5) and 6) is 1-5min, wherein the time of the single layer deposited in the step 5) is at least 3 times of the time of the single layer deposited in the step 6).
The cycle 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: setting the bias voltage at 20-300V, duty ratio at 60-80% and frequency at 15-30khz, introducing argon and hydrogen, and controlling the pressure at 2-5Pa for 10-140 min. The plasma cleaning in step 2) includes but is not limited to ion source, bias glow cleaning, hot wire cleaning, and arc-excited electron ionization source.
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 2-5 Pa; and 5) controlling the air pressure to be 1-3Pa, setting the bias voltage to be 20-200V, setting the duty ratio to be 60-80% and setting the frequency to be 15-30khz in the steps and 6).
The invention has the following beneficial effects:
1. according to the invention, the binary nitride layer is directly deposited on the surface of the die to be used as a basic layer, and the complex deposition process of gradient layers of metal, nitride and polynary nitride at the present stage is abandoned, on one hand, the invention adopts the technical advantage of pulse arcs, and on the other hand, the invention also has the effect of deep plasma cleaning on the surface of the die; the invention greatly simplifies the process steps of the coating;
2. the invention adopts the basic layer of AlCrN and the composite layer of AlCrN/TiSiN, and does not need to deliberately change the parameters of bias voltage, air pressure and the like, so that the material properties of the AlCrN and AlCrN/TiSiN layers naturally form hardness gradient; 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, the carbon nitride of AlCr and TiSi metals is generated by introducing acetylene, so that on one hand, the addition of acetylene can effectively form carbide to form a dispersion strengthening effect and effectively increase a grain refining effect, and on the other hand, the existence of the carbide also improves the wear resistance of the coating and reduces the friction coefficient;
4. according to the invention, oxygen is intermittently introduced, so that the carbon-oxygen nitride is effectively formed in the carbon nitride, on one hand, a nano-scale gap is formed in the coating, the surface energy of the coating surface can be effectively reduced, on the other hand, the oxidation speed of the mold in a high-temperature state in the use process is inhibited due to the existence of the oxide, and the service life of the mold is effectively prolonged;
5. the pulse arc source is used as a current source for depositing the carbon oxide of the die-casting aluminum die, so that the ion ionization rate of the traditional direct current arc source can be further improved, and the surface structure of the coating is fine and smooth. The mode of low-base-value arc stabilization and high pulse current can effectively reduce the generation of large particles, further provides the fineness of the surface structure of the coating, and is favorable for prolonging the service life of the die.
In conclusion, the nano composite multi-element oxycarbide coating on the surface of the die-casting aluminum die provided by the invention has good bonding force, wear resistance and temperature resistance, and good surface 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 present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is within the scope of the present invention for those skilled in the art to obtain other drawings based on the drawings without inventive exercise.
FIG. 1 is a schematic structural diagram of a nanocomposite multi-element oxycarbide layer on a die cast aluminum mold surface;
FIG. 2 is a schematic view of an apparatus for producing a carbon oxide coating in accordance with the present invention;
FIG. 3 is a schematic diagram of a 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
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings.
Referring to FIG. 1: a nanometer composite multi-component carbon oxide layer 2 on the surface of a die-casting aluminum die 1 comprises a base layer 21, a composite transition layer 22 and a multilayer circulating nano layer 23, wherein the base layer 21 is AlCrN, the composite transition layer 22 is a TiSiN/AlCrN composite layer, and the multilayer circulating nano layer 23 is a TiSiAlCrCN/TiSiAlCrCON alternating layer; and no less than 4 circulating layers are arranged between carbonitrides and carbonitrides in the multi-layer circulating nano-layer 23. Wherein: the thickness of the base layer 21 is 300-1500 nm, the thickness of the composite transition layer 22 is 100-800 nm, the thickness of the multi-layer circulating nano layer 23 is 100-1000 nm, and the total thickness of the nano composite multi-component carbon oxide layer 2 is 2000-3500 nm.
The multilayer circulating nano layer is an alternating layer of carbonitride and carbooxynitride formed by intermittently introducing oxygen, and the thickness of the carbooxynitride layer accounts for no more than 30% of the thickness of the multilayer circulating nano layer.
Referring to fig. 2: the equipment used for preparing the nano composite multi-element carbon oxide layer is pulse arc source vacuum coating equipment which is provided with 4 rows of arc sources, wherein 01 row and 04 row are respectively provided with metal AlCr targets, 02 row and 03 row are respectively provided with TiSi targets, and an ion cleaning device is arranged at the position 05. In the invention, 01 rows of arcs are adopted when the base layer 21AlCrN layer is deposited, 01 and 02 rows of arcs are adopted for the composite transition layer 22 TiSiN/AlCrN composite layer, and 01 and 03 are arranged as a group and 02 and 04 are arranged as a group when the multilayer circulating nano layer 23TiSiAlCrCN/TiSiAlCrCON alternating layer is deposited, so that the target surface carbonization phenomenon in the carbon oxide deposition process can be reduced and the target surface carbonization device can be alternately and intermittently used; and 05, an ion cleaning device.
The preparation method of the nano composite multi-component oxycarbide layer of the die-casting aluminum die is as described in the following embodiments:
example hot filament plasma cleaning of deposited oxycarbide layers
Referring to fig. 2 and 4, the ion cleaning device 05 is a hot wire plasma cleaning device, and the principle of the hot wire plasma cleaning device is that the hot wire plasma cleaning device comprises a hot wire assembly and a hot wire anode, wherein a heating power supply and a cathode of the anode power supply are applied to a filament, an anode of the anode power supply is loaded to the filament, the filament is heated, electrons overflow, under the action of an electric field of the anode power supply, the electrons move to the anode, and in the moving process, the electrons collide with argon gas to ionize more plasmas; and (3) bombarding the to-be-plated die on the rotating frame by a large amount of argon ions by the plasma under the action of the biasing electric field of the rotating frame.
Referring to FIG. 3: adopt the pulse arc to mean taking certain background value electric current as steady arc current, peak current is the pulse high current, can exert the high current in the twinkling of an eye on the target surface, the application of high current has increased the magnetic field intensity of target surface on the one hand, thereby cause the branching of arc spot on the target surface, form the split arc, the production of big granule has been reduced, the stack of on the other hand strong current in the twinkling of an eye, can greatly reduced steady arc background value electric current's size (DC power supply steady arc current more than 45A, pulse arc current 20A also can normally work), thereby can reduce the production of big granule, the stack of strong current simultaneously, can promote the plasma intensity of arc discharge in-process, improve the ionization rate of negative pole.
As shown in table 1, the main processes of this example are as follows:
1. vacuumizing, heating to 450 ℃, and keeping the temperature for 50min, wherein the rotating speed is set to 1 r/min;
2. introducing mixed gas of argon and hydrogen, argon 300 and hydrogen 300, adjusting the pressure of a throttling valve to be controlled at 2Pa, controlling filament current at 150A, controlling filament anode constant current mode and anode current at 50A, applying linear bias voltage at 30-100V (10min) on a substrate to be plated, then cleaning for 10min at 100V, wherein the duty ratio of a bias power supply is 70%, and the frequency is 20 khz;
3. then hydrogen is closed, argon 450 is introduced, the pressure of a throttle valve is adjusted to be controlled at 2.5Pa, filament parameters are unchanged, linear bias voltage of 100V-200V (10min) is applied to the substrate to be plated, then cleaning is carried out for 30min at 200V, the duty ratio of a bias power supply is 70%, and the frequency is 20 khz;
4. then, opening 01 rows of AlCr targets, introducing 300 parts of nitrogen, adjusting a throttle valve to control the air pressure to be 3.5Pa, adjusting the pulse arc base value current to be 30A, adjusting the peak current to be 800A, adjusting the frequency to be 120hz, and adjusting the duty ratio to be 10%; setting the bias voltage to 40V, depositing for 40min, then closing the arc target, and controlling the duty ratio of the bias power supply to be 70% and the frequency to be 20 khz;
5.01 rows of AlCr targets continue to work, 02 rows of TiSi targets are started, the nitrogen flow is unchanged, the air pressure is 3.5Pa, the pulse arc base value current of the AlCr targets is 30A, the peak current is 800A, the frequency is 120hz, and the duty ratio is 10 percent; the TiSi target pulse arc base value current is 33A, the peak current is 600A, the frequency is 120hz, and the duty ratio is 10%; setting the bias voltage to be 40V, depositing for 25min, setting the duty ratio of a bias power supply to be 70%, and closing 01 and 02 column arcs after the frequency is 20 khz;
6. argon 160, nitrogen 220 and acetylene 50 are introduced, the air pressure is regulated to be 2Pa, two rows of arcs (01 and 03) are started, the pulse arc base value current of the AlCr target 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 is 33A, the peak current is 600A, the frequency is 120hz, and the duty ratio is 10%; setting the bias voltage to be 40V, depositing for 5min, setting the duty ratio of a bias power supply to be 70%, and setting the frequency to be 20 khz;
7. argon 160, nitrogen 220 and acetylene 50 are introduced, the air pressure is regulated to be 2Pa, two rows of arcs (01 and 03) are started, the pulse arc base value current of the AlCr target 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 is 33A, the peak current is 600A, the frequency is 120hz, and the duty ratio is 10%; the bias voltage was increased from 40V to 80V in a linear increasing manner, deposited for 5 min;
8. and introducing oxygen 65, adjusting the air pressure of a throttle valve to be 2Pa, keeping the arc parameters of the 01 and 03 columns unchanged, biasing by 80v, keeping the duty ratio of a bias power supply to be 70%, controlling the frequency to be 20khz, and depositing for 70 s. Then closing 01, 03 column arcs;
9. starting 02 and 04 rows of arcs, keeping parameters of the AlCr target and the TiSi target unchanged, and performing 80v bias deposition for 5 min;
10. repeat step 8 with 02.04 column arcs, then close 02, 04 column arcs;
and repeating the steps 9 and 10, and periodically using 01 and 03 column arcs and 02 and 04 column arcs in each cycle.
Example two arc excited Electron ionization Source cleaning of deposited oxycarbide layers
The main difference between this embodiment and the first embodiment is that an arc electron excitation plasma cleaning device is adopted, that is, the arc 05 in fig. 2 is provided with an arc electron excitation plasma cleaning device, the arc 05 adopts a conventional direct current arc power supply, and the target material is a Ti target.
Referring to FIG. 5: the arc electron excitation plasma cleaning device loads the anode of an arc ion plating arc power supply on an anode independent of the suspension potential of the whole vacuum chamber, loads the cathode of the arc power supply on a cathode arc source, and is characterized in that a circular shielding plate with the area about 2 times that of the surface of a target material and the distance of 70-200mm from the target material is arranged in front of the cathode arc source target material, and the shielding plate is in potential suspension. The arc striking device is used for inducing the cathode arc source to generate arc discharge, at the moment, the anode of the cathode arc power supply is loaded on the anode, and electrons in the discharge process flow back to the cathode arc power supply through the anode. In the process that electrons move to the anode, a large amount of plasmas are excited by the electrons of large beam current, and the plasmas can bombard the mould transferred on the rotating frame under the action of the bias voltage on the rotating frame, so that the mould is cleaned, etched and activated.
Compared with the conventional atmospheric glow discharge (bias current is below 1A) and ion source discharge (bias current is 2-4A), the bias current of the arc-excited plasma can reach 6-10A, although the cleaning bias current of the arc discharge can reach 10A, a very large bias voltage of 400-800V is needed in the cleaning process, meanwhile, the cleaning source is metal ions, the energy is large, the surface of the mold is easy to be roughened, and the cleaning source of the arc-excited plasma is inert gas ions, so that a very high cleaning effect can be realized below 300V of the lower bias voltage.
The cleaning process comprises the following steps:
(1) argon 300 and hydrogen 300 were pumped in, the throttle valve was adjusted to control the gas pressure at 3Pa, the bias voltage was set at 40V, the Ti target was turned on, the arc current was 100A, the bias voltage was linearly increased from 40 to 80V (10min), and then etching was performed at 80V for 10 min.
Then hydrogen is closed, argon is set to be 450, the pressure of the throttle valve is adjusted to be 3Pa, the bias voltage is linearly increased to 200v (10min), the arc current is kept unchanged, 200v is cleaned for 30min, and the arc target is closed.
It will be understood by those skilled in the art that all or part of the steps in the method for implementing the above embodiments may be implemented by relevant hardware instructed by a program, and the program may be stored in a computer-readable storage medium, such as ROM/RAM, magnetic disk, optical disk, etc.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention, and it is therefore to be understood that the invention is not limited by the scope of 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 provided with a base layer, a composite transition layer and a multi-layer circulating nano layer from inside to outside; wherein the base layer is AlCrN, the composite transition layer is a TiSiN/AlCrN composite layer, and the multi-layer circulating nano layer is a TiSiAlCrCN/TiSiAlCrCON alternating layer;
the preparation method is carried out in a pulse arc source vacuum coating device, and the pulse arc source and the ion cleaning device are configured, wherein 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 arranged oppositely, the AlCr targets and the TiSi targets arranged oppositely are respectively positioned at two sides of a mould 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 arranged adjacently;
the preparation method comprises the following steps:
1) placing the die to be plated in a vacuum film plating device for preheating;
2) carrying out plasma cleaning on the surface of the die by adopting an ion cleaning source;
3) introducing nitrogen, starting 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 oppositely arranged, 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 a TiSiAlCrCN layer;
6) introducing oxygen, acetylene, nitrogen and argon, simultaneously starting a group of adjacent TiSi targets and AlCr targets, and depositing a TiSiAlCrCON layer;
7) and (5) alternately repeating the step 5) and the step 6) to form a plurality of layers of circulating nano-layers.
2. The method for preparing a nano composite multi-carbon oxide coating on the surface of a die-casting aluminum die as claimed in claim 1, wherein the method comprises the following steps: the thickness of the base layer is 300-1500 nm, the thickness of the composite transition layer is 100-800 nm, and the thickness of the multilayer circulating nano layer is 100-1000 nm; the thickness of the TiSiAlCrCON layer accounts for not more than 30% of the thickness of the multilayer circulating nano layer.
3. The method for preparing a nano composite multi-carbon oxide coating on the surface of a die-casting aluminum die as claimed in claim 1, wherein the method comprises the following steps: the two rows of metal AlCr targets and the two rows of TiSi targets are distributed in a clockwise direction and are sequentially 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 on two sides of the die to be plated; and (3) alternately using gaps in at least partial processes in the steps 4) to 6) in a group of adjacently arranged TiSi targets and AlCr targets formed by the first AlCr targets and the first TiSi targets, a group of adjacently arranged TiSi targets and AlCr targets formed by the first TiSi targets and the second AlCr targets, and a group of adjacently arranged TiSi targets and AlCr targets formed by the second AlCr targets and the second TiSi targets.
4. The method for preparing the nanocomposite multi-carbon oxide coating on the surface of the die-casting aluminum die as claimed in claim 1, wherein: in the step 3) and the step 4), the pulse arc discharge of the pulse arc target adopts a mode of stacking basic value current and pulse arc current discharge, wherein the basic 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 a nano composite multi-carbon oxide coating on the surface of a die-casting aluminum die as claimed in claim 1, wherein the method comprises the following steps: and in the step 5), mixing acetylene, nitrogen and argon to form mixed gas, wherein the atomic ratio of argon is not less than 30%, the atomic ratio of nitrogen is not more than 60%, and the atomic ratio of acetylene is not more than 20%.
6. The method for preparing a nano composite multi-carbon oxide coating on the surface of a die-casting aluminum die as claimed in claim 1, wherein the method comprises the following steps: and 6), mixing oxygen, acetylene, nitrogen and argon to form mixed gas, and introducing the mixed gas, wherein the atomic ratio of the argon is not lower than 30%, the atomic ratio of the nitrogen is not higher than 60%, the atomic ratio of the acetylene is not higher than 20%, and the atomic ratio of the oxygen is not higher than 20%.
7. The method for preparing a nano composite multi-carbon oxide coating on the surface of a die-casting aluminum die as claimed in claim 1, wherein the method comprises the following steps: the time of the single layer deposited in the steps 5) and 6) is 1-5min, wherein the time of the single layer deposited in the step 5) is at least 3 times of the time of the single layer deposited in the step 6).
8. The method for preparing a nanocomposite poly-carbon oxide coating on the surface of a die-cast aluminum die according to claim 7, wherein: and 5) circulating for not less than 4 times, wherein the carbon oxide layer is the outermost layer of the coating.
9. The method for preparing a nano composite multi-carbon oxide coating on the surface of a die-casting aluminum die as claimed in claim 1, wherein the method comprises the following steps: in step 2), the plasma cleaning setting parameters are as follows: setting the bias voltage at 20-300V, duty ratio at 60-80% and frequency at 15-30khz, introducing argon and hydrogen, and controlling the pressure at 2-5Pa for 10-140 min.
10. The method for preparing a nano composite multi-carbon oxide coating on the surface of a die-casting aluminum die as claimed in 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 2-5 Pa; and 5) controlling the air pressure to be 1-3Pa, setting the bias voltage to be 20-200V, the duty ratio to be 60-80% and the frequency to be 15-30khz in step 5) and step 6).
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