CN112647060A - CVD composite coating for trimming die and preparation method thereof - Google Patents
CVD composite coating for trimming die and preparation method thereof Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 58
- 239000011248 coating agent Substances 0.000 title claims abstract description 53
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000009966 trimming Methods 0.000 title claims description 30
- 239000010410 layer Substances 0.000 claims abstract description 102
- 239000000758 substrate Substances 0.000 claims abstract description 29
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 25
- 230000003014 reinforcing effect Effects 0.000 claims abstract description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 16
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000013078 crystal Substances 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 5
- 238000005520 cutting process Methods 0.000 claims abstract description 4
- 229910003074 TiCl4 Inorganic materials 0.000 claims description 12
- 238000000151 deposition Methods 0.000 claims description 12
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 12
- 230000008021 deposition Effects 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- 239000000498 cooling water Substances 0.000 claims description 6
- 230000037452 priming Effects 0.000 claims description 6
- 239000002344 surface layer Substances 0.000 claims description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 3
- 239000007888 film coating Substances 0.000 claims description 3
- 238000009501 film coating Methods 0.000 claims description 3
- 230000002045 lasting effect Effects 0.000 claims description 3
- 230000007704 transition Effects 0.000 claims description 3
- 230000002787 reinforcement Effects 0.000 claims 1
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 16
- 229910000831 Steel Inorganic materials 0.000 abstract description 8
- 239000010959 steel Substances 0.000 abstract description 8
- 239000002346 layers by function Substances 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 2
- 238000005336 cracking Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/34—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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/04—Coating on selected surface areas, e.g. using masks
- C23C16/042—Coating on selected surface areas, e.g. using masks using masks
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/36—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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/403—Oxides of aluminium, magnesium or beryllium
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- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
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- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention relates to the technical field of CVD composite coatings, in particular to a CVD composite coating for an edge cutting die and a preparation method thereof, which solve the defects in the prior art, and comprises a substrate, wherein a TiN layer, a reinforcing layer, an MT-TiCxN1-x layer, an HT-TiCN layer and an Al2O3 layer are deposited on the substrate from inside to outside in sequence by a chemical method, the reinforcing layer comprises a TiC layer and a TiCN layer, the linear expansion coefficients of the TiN layer and the substrate are close, the bonding force between the coating and the surface of the die can be improved, and the MT-TiCxN1-x layer is columnar crystal. According to the invention, the TiN/reinforcing layer/MT-TiCN/HT-TiCN/alpha-Al 2O3 composite coating is prepared by adopting a CVD method, the advantages of each layer of coating are combined, and the problems of poor bonding force between the coating and a substrate, easiness in cracking and peeling caused by the fact that the single functional layer Al2O3 has great difference with the steel substrate in crystal structure, thermal expansion coefficient and elastic modulus are solved.
Description
Technical Field
The invention relates to the technical field of CVD composite coatings, in particular to a CVD composite coating for a trimming die and a preparation method thereof.
Background
With the rapid development of the fields of modern automobiles, electronics, aerospace and the like, the mold industry becomes an important foundation for industrial development. The demand of the trimming die as one of a plurality of dies is increasing, and the requirement on the service life is also increasing. The trimming die plays roles in trimming and shaping in the bolt forming process, the trimming process is a shearing, extruding and tearing process, and the trimming die is required to have high strength, high hardness, high wear resistance, sufficient toughness and certain red hardness. The factors influencing the service life of the trimming die mainly comprise a die structure, a die material, machining, die working conditions and the like, wherein the die material belongs to one of key factors.
At present, most of materials selected by the trimming die are Cr12MoV steel, 7Cr7Mo3V2Si (LD), W6Mo5Cr4V2(M2) steel, W2Mo9Cr4VCo8(M42) and the like, and the application result of practical production shows that the improvement of the service life of the trimming die is limited only by changing the material type or improving the heat treatment process. In recent decades, the material surface modification technology is gradually becoming an important way to improve the quality and service life of the trimming die with its wide functionality, good environmental protection and great synergy. The CVD (chemical vapor deposition) technique, which is an important method for modifying the surface of a material, has been widely used in the field of trimming molds due to its outstanding practicability and effectiveness.
At present, the mainstream coating of the trimming die is a titanium plating coating (TiN series coating), namely a multilayer composite coating formed by coating one or more single coatings of TiN, TiC and TiCN on the surface of the trimming die by a CVD method. But the disadvantage of limited service life of TiN series coating dies also restricts the further development of the series of coatings in the die industry. The Al2O3 series of coatings deposited by CVD methods, typically with cemented carbide as the coating substrate, have limited application on alloy tool steels, especially less on steel substrates for edge trim dies. The Al2O3 coating has the highest mechanical strength, good thermal stability and chemical stability and excellent oxidation wear resistance and diffusion wear resistance at high temperature.
Disclosure of Invention
It is an object of the present invention to apply an Al2O3 series coating to alloy tool steels, especially steel for the shear dies. Another object is to improve the service life of the mould by optimizing the internal structure of the coating.
The invention aims to solve the defects in the prior art and provides a CVD composite coating for an edge cutting die and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a CVD composite coating for an edge cutting die comprises a substrate, wherein a TiN layer, a reinforcing layer, an MT-TiCxN1-x layer, an HT-TiCN layer and an Al2O3 layer are deposited on the substrate from inside to outside in sequence by a chemical method, the reinforcing layer comprises a TiC layer and a TiCN layer, the linear expansion coefficient of the TiN layer and the substrate is close to that of the substrate, the bonding force between the coating and the surface of the die can be improved, and the MT-TiCxN1-x layer is columnar crystal.
Preferably, the TiN layer has a thickness of 0.75 to 1.25 μm.
Preferably, the thickness of the reinforcing layer is 0.75-1.25 μm.
Preferably, the thickness of the MT-TiCxN1-x layer is 2.00-3.00 mu m.
Preferably, the thickness of the HT-TiCN layer is 0.75-1.25 μm.
Preferably, the thickness of the Al2O3 layer is 5.50-6.50 μm.
A preparation method of a CVD composite coating for a trimming die comprises the following steps: s1, loading the pretreated substrate into a graphite boat matched with the pretreated substrate and loading the substrate into a chamber to ensure smooth airflow, and adjusting the rotation speed of a gas conveying pipe to be 2rpm to ensure uniform gas supply;
s2, starting circulating cooling water, a vacuum pump and an H2 valve, setting the pressure in a chamber to be 200-400mba, then starting to heat up, setting the pressure in the chamber to be 160mbar when the temperature rises to 850 ℃, and introducing H2\ N2\ TiCl4 to form a TiN priming layer, wherein the deposition time is 30-60 min;
s3, after the TiN priming layer is finished, keeping the current temperature and the chamber pressure unchanged, shielding the graphite boat part, introducing H2/CH4/TiCl4, forming a TiC layer on the surface layer part, shielding the other part of the graphite boat, and forming a TiCN layer on the surface layer part, wherein the deposition time is 20 min;
s4, after the reinforcing layer is finished, when the temperature is raised to 890 ℃, the pressure of a furnace chamber is set to be 90mbar, H2\ N2\ TiCl4\ CH3CN are respectively introduced to start coating, and an MT-TiCxN1-x layer is formed at the temperature for 220 min;
s5, after the deposition of the MT-TiCxN1-x layer is finished, when the temperature is increased to 1010 ℃, the pressure of a furnace chamber is set to 300mbar, H2\ N2\ TiCl4\ CH4 is respectively introduced to start coating, and a transition layer HT-TiCN layer is formed at the temperature for 15 min;
s6, after finishing the HT-TiCN layer, heating to 1020 ℃, setting the pressure of a furnace chamber to 65mbar, respectively introducing H2\ CO2\ HCl \ H2S \ AlCl3 to start coating, forming an Al2O3 layer at the temperature, and lasting for 280 min;
s7, after deposition is finished, cooling the heating furnace and moving away, simultaneously introducing H2 with the flow rate of 30l/min for cooling for 200min, then changing the cooling flow rate of N2 to be 22l/min, opening the furnace chamber until the temperature of the furnace chamber is reduced to below 50 ℃, taking out a sample, and finishing film coating.
Preferably, in the step S2, the flow rate of the circulating cooling water is 15 l/min.
Preferably, in the step S2, the pressure of the H2 valve is adjusted to be 1.5-2.5bar, and the flow rate is set to be 30 l/min.
The invention has the beneficial effects that:
1. the TiN/reinforcing layer/MT-TiCN/HT-TiCN/alpha-Al 2O3 composite coating is prepared by adopting a CVD method, the advantages of each layer of coating are combined, and the problems that the bonding force between the coating and a substrate is poor and the coating is easy to crack and peel due to the fact that the single functional layer Al2O3 has great difference with the steel substrate in crystal structure, thermal expansion coefficient and elastic modulus are solved.
2. According to the invention, the TiN/reinforcing layer/MT-TiCN/HT-TiCN/alpha-Al 2O3 layers are mutually matched, the coating has better binding force and toughness, the wear resistance and high-temperature oxidation resistance of the whole trimming die are enhanced, and the service life of the trimming die is prolonged.
Drawings
Fig. 1 is a schematic structural diagram of a CVD composite coating for a trimming die according to the present invention.
In the figure: 1 substrate, 2TiN layers, 3 reinforcing layers, 31TiC layers, 32TiCN layers, 4MT-TiCxN1-x layers, 5HT-TiCN layers and 6Al2O3 layers.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1, the CVD composite coating for the trimming die comprises a substrate 1, wherein a TiN layer 2, a reinforcing layer 3, an MT-TiCxN1-x layer 4, an HT-TiCN layer 5 and an Al2O3 layer 6 are deposited on the substrate 1 from inside to outside in sequence by a chemical method, the reinforcing layer comprises a TiC31 layer and a TiCN layer 32, the linear expansion coefficient of the TiN layer 2 and the substrate is approximate, the bonding force between the coating and the die surface can be improved, the MT-TiCxN1-x layer 4 is columnar crystal, the thickness of the TiN layer 2 is 0.75 mu m, the thickness of the reinforcing layer 3 is 0.75 mu m, the thickness of the MT-TiCxN1-x layer 4 is 2.00 mu m, the thickness of the HT-TiCN layer 5 is 0.75 mu m, and the thickness of the Al2O3 layer 6 is 5.50 mu m.
The TiN/MT-TiCN/HT-TiCN/alpha-Al 2O3 composite coating is prepared by a CVD method, the advantages of each coating are combined, the problems that the coating is poor in binding force with a matrix and is easy to crack and peel due to the fact that the single functional layer Al2O3 and the matrix have great difference in crystal structure, thermal expansion coefficient and elastic modulus are solved, interfaces of each TiN/MT-TiCN/HT-TiCN/alpha-Al 2O3 layer are matched with each other, the coating has good binding force and toughness, the wear resistance and high-temperature oxidation resistance of the whole trimming die are enhanced, and the service life of the trimming die is prolonged.
A preparation method of a CVD composite coating for a trimming die comprises the following steps:
s1, loading the pretreated substrate 1 into a graphite boat matched with the substrate and loading the substrate into a chamber to ensure smooth airflow, and adjusting the rotation speed of a gas delivery pipe to be 2rpm to ensure uniform gas supply;
s2, starting circulating cooling water, a vacuum pump and an H2 valve, wherein the flow rate of the circulating cooling water is 15l/min, the pressure of an H2 valve is adjusted to be 2bar, the flow rate is set to be 30l/min, the pressure in a chamber is set to be 300mba, then the temperature is increased, when the temperature is increased to 850 ℃, the pressure in the chamber is set to be 160mbar, H2\ N2\ TiCl4 is introduced, a TiN priming layer is formed, and the deposition time is 45 min;
s3, after the TiN priming coat layer 2 is finished, keeping the current temperature and the chamber pressure unchanged, shielding the graphite boat part, introducing H2/CH4/TiCl4, forming a TiC31 layer on the surface layer part, shielding the other part of the graphite boat, forming a TiCN layer 32 on the surface layer part, and depositing for 20 min;
s4, after the reinforcing layer 3 is finished, when the temperature is raised to 890 ℃, the pressure of a furnace chamber is set to 90mbar, H2\ N2\ TiCl4\ CH3CN are respectively introduced to start coating, and an MT-TiCxN1-x layer 4 is formed at the temperature for 220 min;
s5, after the deposition of the MT-TiCxN1-x layer 4 is finished, when the temperature is increased to 1010 ℃, the pressure of a furnace chamber is set to 300mbar, H2\ N2\ TiCl4\ CH4 is respectively introduced to start coating, and a transition layer HT-TiCN layer 5 is formed at the temperature for 15 min;
s6, after finishing the HT-TiCN layer 5, heating to 1020 ℃, setting the pressure of a furnace chamber to 65mbar, respectively introducing H2\ CO2\ HCl \ H2S \ AlCl3 to start coating, forming an Al2O3 layer 6 at the temperature, and lasting for 280 min;
s7, after deposition is finished, cooling the heating furnace and moving away, simultaneously introducing H2 with the flow rate of 30l/min for cooling for 200min, then changing the cooling flow rate of N2 to be 22l/min, opening the furnace chamber until the temperature of the furnace chamber is reduced to below 50 ℃, taking out a sample, and finishing film coating.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. A CVD composite coating for an edge cutting die comprises a substrate (1), and is characterized in that a TiN layer (2), a reinforcing layer (3), an MT-TiCxN1-x layer (4), an HT-TiCN layer (5) and an Al2O3 layer (6) are deposited on the substrate (1) from inside to outside in sequence by a chemical method, the reinforcing layer comprises a TiC (31) layer and a TiCN layer (32), the linear expansion coefficients of the TiN layer (2) and the substrate are close to each other, the bonding force between the coating and the surface of the die can be improved, and the MT-TiCxN1-x layer (4) is columnar crystal.
2. The CVD composite coating for an edge trimming die according to claim 1, wherein the TiN layer (2) has a thickness of 0.75-1.25 μm.
3. A CVD composite coating for trimming dies according to claim 1, characterized in that the thickness of the reinforcement layer (3) is 0.75 to 1.25 μm.
4. The CVD composite coating for trimming dies according to claim 1, wherein the thickness of the MT-TiCxN1-x layer (4) is 2.00-3.00 μm.
5. The CVD composite coating for trimming dies according to claim 1, wherein the thickness of the HT-TiCN layer (5) is 0.75-1.25 μm.
6. The CVD composite coating for an edge trimming die according to claim 1, wherein the thickness of the Al2O3 layer (6) is 5.50-6.50 μm.
7. A preparation method of a CVD composite coating for a trimming die is characterized by comprising the following steps:
s1, loading the pretreated substrate (1) into a graphite boat matched with the substrate and loading the substrate into a chamber to ensure smooth airflow, and adjusting the rotation speed of a gas delivery pipe to be 2rpm to ensure uniform gas supply;
s2, starting circulating cooling water, a vacuum pump and an H2 valve, setting the pressure in a chamber to be 200-400mba, then starting to heat up, setting the pressure in the chamber to be 160mbar when the temperature rises to 850 ℃, and introducing H2\ N2\ TiCl4 to form a TiN priming layer, wherein the deposition time is 30-60 min;
s3, after the TiN priming layer (2) is finished, keeping the current temperature and the chamber pressure unchanged, shielding the graphite boat part, introducing H2/CH4/TiCl4, forming a TiC (31) layer on the surface layer part, shielding the other part of the graphite boat, forming a TiCN layer (32) on the surface layer part, and depositing for 20 min;
s4, after the reinforcing layer (3) is finished, when the temperature is raised to 890 ℃, the pressure of a furnace chamber is set to 90mbar, H2\ N2\ TiCl4\ CH3CN are respectively introduced to start coating, and an MT-TiCxN1-x layer (4) is formed at the temperature for 220 min;
s5, after the deposition of the MT-TiCxN1-x layer (4) is finished, when the temperature is increased to 1010 ℃, the pressure of a furnace chamber is set to 300mbar, H2\ N2\ TiCl4\ CH4 is respectively introduced to start coating, and a transition layer HT-TiCN layer (5) is formed at the temperature for 15 min;
s6, after finishing the HT-TiCN layer (5), heating to 1020 ℃, setting the pressure of a furnace chamber to 65mbar, respectively introducing H2\ CO2\ HCl \ H2S \ AlCl3 to start coating, forming an Al2O3 layer (6) at the temperature, and lasting for 280 min;
s7, after deposition is finished, cooling the heating furnace and moving away, simultaneously introducing H2 with the flow rate of 30l/min for cooling for 200min, then changing the cooling flow rate of N2 to be 22l/min, opening the furnace chamber until the temperature of the furnace chamber is reduced to below 50 ℃, taking out a sample, and finishing film coating.
8. The method for preparing a CVD composite coating for an edge trimming die according to claim 7, wherein the flow rate of the circulating cooling water in the step S2 is 15 l/min.
9. The method of claim 7, wherein in the step S2, the pressure of the H2 valve is adjusted to 1.5-2.5bar, and the flow rate is set to 30 l/min.
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|---|---|---|---|---|
| CN102392217A (en) * | 2011-11-23 | 2012-03-28 | 西北工业大学 | Blade surface pitting corrosion resistant coating and preparation method thereof |
| CN104085142A (en) * | 2014-05-28 | 2014-10-08 | 厦门金鹭特种合金有限公司 | Coating layer on blade base body |
| CN104099580A (en) * | 2014-05-28 | 2014-10-15 | 厦门金鹭特种合金有限公司 | Cutter coating layer having nanometer columnar crystal for enhancing wear resistance and toughness |
| CN106065448A (en) * | 2015-04-20 | 2016-11-02 | 肯纳金属公司 | Chemical vapour deposition coated cutting insert and manufacture method thereof |
| CN105506622A (en) * | 2015-12-13 | 2016-04-20 | 河南广度超硬材料有限公司 | Composite coating knife and manufacturing method thereof |
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Application publication date: 20210413 |