A multi-layer alternating coating tool and preparation method thereof
Multi-layer alternating coating tools were prepared by chemical vapor deposition method. The alternating deposition technology of Zr1-aSiaN and ZrBx was used to solve the problems of chip accumulation and bond wear during the processing of titanium alloy and nickel-based high-temperature alloy cutting tools, achieving higher wear resistance and service life.
Patent Information
- Application Number
- CN202411382970.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-30
- Publication Date
- 2025-04-29
- Estimated Expiration
- 2044-09-30
AI Technical Summary
Existing titanium alloy and nickel-based high-temperature alloy cutting tools are prone to chip accumulation and severe bonding wear during processing, and the bonding strength of high-hardness coatings is low, resulting in a short service life.
A multi-layer alternating coating tool was prepared by chemical vapor deposition method, including two coatings, Zr1-aSiaN and ZrBx. By alternately deposition and controlling the thickness and crystal structure of each layer, the wear resistance, toughness and bond strength of the coating were improved.
It achieves higher wear resistance, toughness and oxidation resistance, while reducing the friction coefficient and extending the service life of the tool.
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Figure CN118880275B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of coated tool technology, and specifically relates to a multi-layer alternating coating tool and a preparation method thereof. Background Art
[0002] Materials such as titanium alloys and nickel-based high-temperature alloys are high in strength. During cutting, the tool surface is prone to built-up edge and tool adhesion and wear are serious. Preparing a coating on the surface of the cutting tool can effectively extend the tool life. To solve these processing problems, the tool coating surface is required to be smooth, have a low friction coefficient, high coating bonding strength, good wear resistance, and good oxidation resistance. At present, most of the cutting of titanium alloys, nickel-based high-temperature alloys and other materials uses physical vapor deposition coating tools, commonly used TiAlN, NbN, TiB 2 , ZrB 2 Single-layer or multi-layer PVD coatings have the advantages of high hardness, high wear resistance and low friction coefficient, but when the coating hardness is high (such as >35GPa), the compressive stress of the PVD coating is large, resulting in low coating bonding strength, thereby reducing the service life of the cutting tool. The deposition temperature of CVD coatings for cemented carbide cutting tools is usually between 700~1050℃, which is generally higher than the deposition temperature of PVD coatings (<700℃). During the deposition process of CVD coatings, elements between the coating and the substrate and between the coatings can diffuse with each other to form a metallurgical bond. Therefore, CVD coatings usually have higher bonding strength than PVD coatings. CVD multilayer coatings TiN / TiBN / TiB 2 It is suitable for cutting materials such as titanium alloys and nickel-based high-temperature alloys. However, in the titanium alloy cutting process, CVD TiB 2 Since the Ti element has a high affinity with titanium alloy, element diffusion is likely to occur, which intensifies wear. Summary of the invention
[0003] In order to solve the problems existing in the prior art, the main purpose of the present invention is to provide a multi-layer alternating coating tool and a preparation method thereof.
[0004] To solve the above technical problems, according to one aspect of the present invention, the present invention provides the following technical solutions:
[0005] A multi-layer alternating coating tool comprises a substrate and a multi-layer coating sequentially arranged on the surface of the substrate, wherein the multi-layer coating is prepared by a chemical vapor deposition method and comprises a first sub-coating and a second sub-coating adjacent to each other; the first sub-coating is Zr 1-a Si a N layer, 0.05≤a≤0.2; the second sub-coating is ZrB x layer, 1.8≤x≤2.5; the first sub-coating and the second sub-coating are deposited alternately, and with the alternating deposition of the coatings, the thickness of the first sub-coating gradually decreases, and the thickness of the second sub-coating gradually increases.
[0006] As a preferred embodiment of a multi-layer alternating coating tool described in the present invention, the multi-layer coating further comprises a bonding layer deposited between the substrate surface and the first sub-coating, wherein the bonding layer is any one of TiN, Ti, ZrN, and Zr, preferably ZrN, and the thickness of the bonding layer is 0.5 to 2.0 μm.
[0007] As a preferred solution of a multi-layer alternating coating tool described in the present invention, wherein: the first sub-coating Zr 1-a Si a The grains of the N layer are equiaxed grains <35 nm. x The layer has a columnar crystal structure.
[0008] As a preferred solution of a multi-layer alternating coating tool described in the present invention, wherein: the ZrB x The micro-Vickers hardness of the layer reaches above 35 GPa.
[0009] As a preferred solution of the multi-layer alternating coating tool described in the present invention, the total thickness of the multi-layer coating is 4.0-12.0 μm, and the first sub-coating and the second sub-coating are alternately deposited at least once.
[0010] As a preferred solution of the multi-layer alternating coating tool described in the present invention, a surface layer is deposited on the surface of the second sub-coating.
[0011] As a preferred solution of the multi-layer alternating coating tool described in the present invention, wherein: the surface layer is any one of ZrN and ZrCN, and the total thickness of the surface layer is 0.2-2.0 μm.
[0012] As a preferred solution of the multi-layer alternating coating tool described in the present invention, the substrate is any one of cemented carbide, high-speed steel, metal ceramic, polycrystalline diamond, and cubic boron nitride.
[0013] As a preferred embodiment of the multi-layer alternating coating tool described in the present invention, the base body is a cutting tool, a forming tool, a stamping tool, or a component or part of a vehicle, or a component or part used in the automotive industry or the aerospace industry.
[0014] To solve the above technical problem, according to another aspect of the present invention, the present invention provides the following technical solution:
[0015] A method for preparing a multi-layer alternating coating tool comprises: depositing a coating on a substrate by a chemical vapor deposition method;
[0016] Zr 1-a Si aThe N layer is heated at 800-950℃ and 20-100 mbar with H 2 、ZrCl 4 、SiCl 4 NH 3 、N 2 (The purity of each gas is greater than 99.99%) is formed by the deposition of raw materials;
[0017] ZGar x The layer was heated at 800-950℃ and 50-200 mbar with H 2 、ZrCl 4 , BCl 3 , Ar (the purity of each gas is greater than 99.99%) as raw materials.
[0018] As a preferred embodiment of the method for preparing a multi-layer alternating coating tool according to the present invention, the ZrN bonding layer is prepared under the conditions of 800-950°C and 50-200 mbar with ZrCl 4 、N 2 , H 2 (The purity of each gas is greater than 99.99%) as raw materials and is obtained by chemical reaction on the surface of the substrate.
[0019] The beneficial effects of the present invention are as follows:
[0020] The present invention provides a multi-layer alternating coating tool and a preparation method thereof. The multi-layer alternating coating tool comprises a substrate and a multi-layer coating sequentially arranged on the surface of the substrate. The multi-layer coating is prepared by a chemical vapor deposition method and comprises a first sub-coating and a second sub-coating adjacent to each other. The first sub-coating is Zr 1-a Si a N layer, 0.05≤a≤0.2; the second sub-coating is ZrB x The multilayer coating tool provided by the present invention has better wear resistance, toughness, oxidation resistance and bonding strength as well as low friction coefficient, and can be applied to cutting of materials such as titanium alloy and nickel-based high-temperature alloy. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the structures shown in these drawings without paying creative work.
[0022] Figure 1 It is a schematic cross-sectional view of a multi-layer alternating coating tool of the present invention.
[0023] The realization of the purpose, functional features and advantages of the present invention will be further explained in conjunction with embodiments and with reference to the accompanying drawings. DETAILED DESCRIPTION
[0024] The following will be described clearly and completely in conjunction with the technical solutions in the embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0025] The present invention provides a multi-layer alternating coating tool and a preparation method thereof. The preparation of a boride coating without titanium element is more suitable for cutting titanium alloy. The CVD method prepares the boride coating at a high temperature, usually greater than 700°C, and the boron atom radius is small, making it easier for the boron atom to diffuse into the WC-Co based cemented carbide matrix to form W 3 CoB 3 In order to minimize the diffusion of boron into the substrate, one or more coatings of TiN, ZrN, Ti, and Zr may be deposited before depositing the boride. In addition, the anti-oxidation temperature of the boride coating is relatively low (usually <500°C). 1-a Si a N, has a higher oxidation resistance temperature, and the second sub-coating ZrB x There is a high bonding strength between them. x High hardness, good wear resistance, suitable for turning, while equiaxed Zr 1-a Si a N has high toughness and is suitable for milling. The first sub-coating Zr 1-a Si a N (0.05≤a≤0.2) and the second sub-coating ZrB x (1.8≤x≤2.5) Alternating deposition can bring into play the synergistic effect of the high wear resistance and low friction coefficient of the second sub-coating and the high toughness and high oxidation resistance of the first sub-coating. As the coating is deposited, the thickness of the first sub-coating (equiaxed crystals) decreases and the thickness of the second sub-coating (columnar crystals) increases, which can make the coating have good internal toughness and good external wear resistance. The coating has good overall strength and toughness, and is suitable for turning and milling of titanium alloys and nickel-based high-temperature alloys. The first sub-coating Zr 1-a Si a The Si atomic percentage content of N is controlled at 5~20% (0.05≤a≤0.2): When a<0.05, the Si content is low, and Zr 1-a Si aThe grain size of N coating is larger, the coating hardness is lower, and the oxidation resistance is poor; when a>20%, the Si content is higher, and the Zr 1-a Si a The grain size of the N coating is small, and although it has good oxidation resistance, the amorphous Si 3 N 4 The higher the content, the lower the hardness of the coating. x The B / Zr atomic ratio is controlled at 1.8≤x≤2.5: when x<1.8, ZrB x There are vacancies in the coating lattice, and the coating hardness is low; when x>2.5, ZrB x Excessive free B element in the coating will reduce the hardness of the coating.
[0026] like Figure 1 As shown, the multi-layer alternating coating tool of the present invention comprises a substrate 100 and a multi-layer coating 200 sequentially arranged on the surface of the substrate 100. The substrate 100 can be one of materials such as cemented carbide, high-speed steel, and metal ceramics. The bonding layer 201 can be one or more of Ti, TiN, Zr, and ZrN, preferably ZrN. The first sub-coating 202 is Zr 1-a Si a N (0.05≤a≤0.2) layer, the second sub-coating 203 is ZrB x (1.8≤x≤2.5) layers, the first sub-coating 202 and the second sub-coating 203 are deposited alternately, and there is at least one alternating layer. As the deposition proceeds, the thickness of the first sub-coating 202 decreases and the thickness of the second sub-coating 203 increases. The coating 204 is a surface layer, and the surface coating is one or more materials such as ZrN and ZrCN.
[0027] The technical solution of the present invention is further described below in conjunction with specific embodiments.
[0028] Example 1
[0029] A method for preparing a multi-layer alternating coating tool, wherein the substrate is a WC-Co based cemented carbide, the bonding layer is ZrN, and the first sub-coating is Zr 0.9 Si 0.1 N, the second sub-coating is ZrB 2 , the coatings are deposited on the substrate surface in sequence, the total coating thickness is 8 μm, and the preparation method of each layer is as follows:
[0030] (1) Bonding layer ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm;
[0031] (2) First sub-coating Zr 0.9 Si 0.1 N layer, deposition temperature 850 °C, deposition pressure 30 mbar, reaction gas H 2 、ZrCl 4 、SiCl 4 NH 3 、N 2 , the purity of each gas is greater than 99.99%, the deposition time is 120 min, and the coating thickness is 2.5 μm;
[0032] (3) Second sub-coating ZrB 2 , deposition temperature 850 °C, deposition pressure 100 mbar, reaction gas H 2 、ZrCl 4 , BCl 3 , Ar, the purity of each gas is greater than 99.99%, the deposition time is 120 min, and the coating thickness is 1.0 μm;
[0033] (4) First sub-coating Zr 0.9 Si 0.1 N layer, deposition temperature 850 °C, deposition pressure 30 mbar, reaction gas H 2 、ZrCl 4 、SiCl 4 NH 3 、N 2 , the purity of each gas is greater than 99.99%, the deposition time is 90 min, and the coating thickness is 1.5 μm;
[0034] (5) Second sub-coating ZrB 2 , deposition temperature 850 °C, deposition pressure 100 mbar, reaction gas H 2 、ZrCl 4 , BCl 3 , Ar, the purity of each gas is greater than 99.99%, the deposition time is 240 min, and the coating thickness is 2.0 μm;
[0035] (6) Surface ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm.
[0036] Example 2
[0037] A method for preparing a multi-layer alternating coating tool, wherein the substrate is a WC-Co based cemented carbide, the bonding layer is ZrN, and the first sub-coating is Zr0.9 Si 0.1 N, the second sub-coating is ZrB 2 , the coatings are deposited on the substrate surface in sequence, the total coating thickness is 8 μm, and the preparation method of each layer is as follows:
[0038] (1) Bonding layer ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm;
[0039] (2) First sub-coating Zr 0.9 Si 0.1 N layer, deposition temperature 850 °C, deposition pressure 30 mbar, reaction gas H 2 、ZrCl 4 、SiCl 4 NH 3 、N 2 , the purity of each gas is greater than 99.99%, the deposition time is 240 min, and the coating thickness is 5.0 μm;
[0040] (3) Second sub-coating ZrB 2 , deposition temperature 850 °C, deposition pressure 100 mbar, reaction gas H 2 、ZrCl 4 , BCl 3 , Ar, the purity of each gas is greater than 99.99%, the deposition time is 240 min, and the coating thickness is 2.0 μm;
[0041] (4) Surface ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm.
[0042] Example 3
[0043] A method for preparing a multi-layer alternating coating tool, wherein the substrate is a WC-Co based cemented carbide, the bonding layer is ZrN, and the first sub-coating is Zr 0.95 Si 0.05 N, the second sub-coating is ZrB 1.8 , the coatings are deposited on the substrate surface in sequence, the total coating thickness is 8 μm, and the preparation method of each layer is as follows:
[0044] (1) Bonding layer ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm;
[0045] (2) First sub-coating Zr 0.95 Si 0.05 N layer, deposition temperature 850 °C, deposition pressure 30 mbar, reaction gas H 2 、ZrCl 4 、SiCl 4 NH 3 、N 2 , the purity of each gas is greater than 99.99%, the deposition time is 120 min, and the coating thickness is 2.5 μm;
[0046] (3) Second sub-coating ZrB 1.8 , deposition temperature 850 °C, deposition pressure 100 mbar, reaction gas H 2 、ZrCl 4 , BCl 3 , Ar, the purity of each gas is greater than 99.99%, the deposition time is 120 min, and the coating thickness is 1.0 μm;
[0047] (4) First sub-coating Zr 0.95 Si 0.05 N layer, deposition temperature 850 °C, deposition pressure 30 mbar, reaction gas H 2 、ZrCl 4 、SiCl 4 NH 3 、N 2 , the purity of each gas is greater than 99.99%, the deposition time is 90 min, and the coating thickness is 1.5 μm;
[0048] (5) Second sub-coating ZrB 1.8 , deposition temperature 850 °C, deposition pressure 100 mbar, reaction gas H 2 、ZrCl 4 , BCl 3 , Ar, the purity of each gas is greater than 99.99%, the deposition time is 240 min, and the coating thickness is 2.0 μm;
[0049] (6) Surface ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2, the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm.
[0050] Example 4
[0051] A method for preparing a multi-layer alternating coating tool, wherein the substrate is a WC-Co based cemented carbide, the bonding layer is ZrN, and the first sub-coating is Zr 0.95 Si 0.05 N, the second sub-coating is ZrB 1.8 , the coatings are deposited on the substrate surface in sequence, the total coating thickness is 8 μm, and the preparation method of each layer is as follows:
[0052] (1) Bonding layer ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm;
[0053] (2) First sub-coating Zr 0.95 Si 0.05 N layer, deposition temperature 850 °C, deposition pressure 30 mbar, reaction gas H 2 、ZrCl 4 、SiCl 4 NH 3 、N 2 , the purity of each gas is greater than 99.99%, the deposition time is 240 min, and the coating thickness is 5.0 μm;
[0054] (3) Second sub-coating ZrB 1.8 , deposition temperature 850 °C, deposition pressure 100 mbar, reaction gas H 2 、ZrCl 4 , BCl 3 , Ar, the purity of each gas is greater than 99.99%, the deposition time is 240 min, and the coating thickness is 2.0 μm;
[0055] (4) Surface ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm.
[0056] Example 5
[0057] A method for preparing a multi-layer alternating coating tool, wherein the substrate is a WC-Co based cemented carbide, the bonding layer is ZrN, and the first sub-coating is Zr 0.8 Si 0.2 N, the second sub-coating is ZrB 2.5 , the coatings are deposited on the substrate surface in sequence, the total coating thickness is 8 μm, and the preparation method of each layer is as follows:
[0058] (1) Bonding layer ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm;
[0059] (2) First sub-coating Zr 0.8 Si 0.2 N layer, deposition temperature 850 °C, deposition pressure 30 mbar, reaction gas H 2 、ZrCl 4 、SiCl 4 NH 3 、N 2 , the purity of each gas is greater than 99.99%, the deposition time is 120 min, and the coating thickness is 2.5 μm;
[0060] (3) Second sub-coating ZrB 2.5 , deposition temperature 850 °C, deposition pressure 100 mbar, reaction gas H 2 、ZrCl 4 , BCl 3 , Ar, the purity of each gas is greater than 99.99%, the deposition time is 120 min, and the coating thickness is 1.0 μm;
[0061] (4) First sub-coating Zr 0.8 Si 0.2 N layer, deposition temperature 850 °C, deposition pressure 30 mbar, reaction gas H 2 、ZrCl 4 、SiCl 4 NH 3 、N 2 , the purity of each gas is greater than 99.99%, the deposition time is 90 min, and the coating thickness is 1.5 μm;
[0062] (5) Second sub-coating ZrB 2.5 , deposition temperature 850 °C, deposition pressure 100 mbar, reaction gas H 2 、ZrCl 4 , BCl 3, Ar, the purity of each gas is greater than 99.99%, the deposition time is 240 min, and the coating thickness is 2.0 μm;
[0063] (6) Surface ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm.
[0064] Example 6
[0065] A method for preparing a multi-layer alternating coating tool, wherein the substrate is a WC-Co based cemented carbide, the bonding layer is ZrN, and the first sub-coating is Zr 0.8 Si 0.2 N, the second sub-coating is ZrB 2.5 , the coatings are deposited on the substrate surface in sequence, the total coating thickness is 8 μm, and the preparation method of each layer is as follows:
[0066] (1) Bonding layer ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm;
[0067] (2) First sub-coating Zr 0.8 Si 0.2 N layer, deposition temperature 850 °C, deposition pressure 30 mbar, reaction gas H 2 、ZrCl 4 、SiCl 4 NH 3 、N 2 , the purity of each gas is greater than 99.99%, the deposition time is 240 min, and the coating thickness is 5.0 μm;
[0068] (3) Second sub-coating ZrB 2.5 , deposition temperature 850 °C, deposition pressure 100 mbar, reaction gas H 2 、ZrCl 4 , BCl 3 , Ar, the purity of each gas is greater than 99.99%, the deposition time is 240 min, and the coating thickness is 2.0 μm;
[0069] (4) Surface ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2, H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm.
[0070] Example 7
[0071] A method for preparing a multi-layer alternating coating tool, wherein the substrate is a WC-Co based cemented carbide, the bonding layer is ZrN, and the first sub-coating is Zr 0.95 Si 0.05 N, the second sub-coating is ZrB 2.5 , the coatings are deposited on the substrate surface in sequence, the total coating thickness is 8 μm, and the preparation method of each layer is as follows:
[0072] (1) Bonding layer ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm;
[0073] (2) First sub-coating Zr 0.95 Si 0.05 N layer, deposition temperature 850 °C, deposition pressure 30 mbar, reaction gas H 2 、ZrCl 4 、SiCl 4 NH 3 、N 2 , the purity of each gas is greater than 99.99%, the deposition time is 120 min, and the coating thickness is 2.5 μm;
[0074] (3) Second sub-coating ZrB 2.5 , deposition temperature 850 °C, deposition pressure 100 mbar, reaction gas H 2 、ZrCl 4 , BCl 3 , Ar, the purity of each gas is greater than 99.99%, the deposition time is 120 min, and the coating thickness is 1.0 μm;
[0075] (4) First sub-coating Zr 0.95 Si 0.05 N layer, deposition temperature 850 °C, deposition pressure 30 mbar, reaction gas H 2 、ZrCl 4 、SiCl 4 NH 3 、N 2 , the purity of each gas is greater than 99.99%, the deposition time is 90 min, and the coating thickness is 1.5 μm;
[0076] (5) Second sub-coating ZrB 2.5 , deposition temperature 850 °C, deposition pressure 100 mbar, reaction gas H 2 、ZrCl 4 , BCl 3 , Ar, the purity of each gas is greater than 99.99%, the deposition time is 240 min, and the coating thickness is 2.0 μm;
[0077] (6) Surface ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm.
[0078] Example 8
[0079] A method for preparing a multi-layer alternating coating tool, wherein the substrate is a WC-Co based cemented carbide, the bonding layer is ZrN, and the first sub-coating is Zr 0.95 Si 0.05 N, the second sub-coating is ZrB 2.5 , the coatings are deposited on the substrate surface in sequence, the total coating thickness is 8 μm, and the preparation method of each layer is as follows:
[0080] (1) Bonding layer ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm;
[0081] (2) First sub-coating Zr 0.95 Si 0.05 N layer, deposition temperature 850 °C, deposition pressure 30 mbar, reaction gas H 2 、ZrCl 4 、SiCl 4 NH 3 、N 2 , the purity of each gas is greater than 99.99%, the deposition time is 240 min, and the coating thickness is 5.0 μm;
[0082] (3) Second sub-coating ZrB 2.5 , deposition temperature 850 °C, deposition pressure 100 mbar, reaction gas H 2 、ZrCl 4 , BCl 3, Ar, the purity of each gas is greater than 99.99%, the deposition time is 240 min, and the coating thickness is 2.0 μm;
[0083] (4) Surface ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm.
[0084] Example 9
[0085] A method for preparing a multi-layer alternating coating tool, wherein the substrate is a WC-Co based cemented carbide, the bonding layer is ZrN, and the first sub-coating is Zr 0.8 Si 0.2 N, the second sub-coating is ZrB 1.8 , the coatings are deposited on the substrate surface in sequence, the total coating thickness is 8 μm, and the preparation method of each layer is as follows:
[0086] (1) Bonding layer ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm;
[0087] (2) First sub-coating Zr 0.8 Si 0.2 N layer, deposition temperature 850 °C, deposition pressure 30 mbar, reaction gas H 2 、ZrCl 4 、SiCl 4 NH 3 、N 2 , the purity of each gas is greater than 99.99%, the deposition time is 120 min, and the coating thickness is 2.5 μm;
[0088] (3) Second sub-coating ZrB 1.8 , deposition temperature 850 °C, deposition pressure 100 mbar, reaction gas H 2 、ZrCl 4 , BCl 3 , Ar, the purity of each gas is greater than 99.99%, the deposition time is 120 min, and the coating thickness is 1.0 μm;
[0089] (4) First sub-coating Zr 0.8 Si 0.2 N layer, deposition temperature 850 °C, deposition pressure 30 mbar, reaction gas H2 、ZrCl 4 、SiCl 4 NH 3 、N 2 , the purity of each gas is greater than 99.99%, the deposition time is 90 min, and the coating thickness is 1.5 μm;
[0090] (5) Second sub-coating ZrB 1.8 , deposition temperature 850 °C, deposition pressure 100 mbar, reaction gas H 2 、ZrCl 4 , BCl 3 , Ar, the purity of each gas is greater than 99.99%, the deposition time is 240 min, and the coating thickness is 2.0 μm;
[0091] (6) Surface ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm.
[0092] Example 10
[0093] A method for preparing a multi-layer alternating coating tool, wherein the substrate is a WC-Co based cemented carbide, the bonding layer is ZrN, and the first sub-coating is Zr 0.8 Si 0.2 N, the second sub-coating is ZrB 1.8 , the coatings are deposited on the substrate surface in sequence, the total coating thickness is 8 μm, and the preparation method of each layer is as follows:
[0094] (1) Bonding layer ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm;
[0095] (2) First sub-coating Zr 0.8 Si 0.2 N layer, deposition temperature 850 °C, deposition pressure 30 mbar, reaction gas H 2 、ZrCl 4 、SiCl 4 NH 3 、N 2 , the purity of each gas is greater than 99.99%, the deposition time is 240 min, and the coating thickness is 5.0 μm;
[0096] (3) Second sub-coating ZrB 1.8 , deposition temperature 850 °C, deposition pressure 100 mbar, reaction gas H 2 、ZrCl 4 , BCl 3 , Ar, the purity of each gas is greater than 99.99%, the deposition time is 240 min, and the coating thickness is 2.0 μm;
[0097] (4) Surface ZrN, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas ZrCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 0.5 μm.
[0098] Comparative Example 1
[0099] A method for preparing a multi-layer alternating coating tool, wherein the substrate is a WC-Co based cemented carbide and the coating is a CVD TiN / TiBN / TiB 2 Multilayer coating, total thickness 8μm, the preparation method of each layer is as follows:
[0100] (1) TiN layer, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas TiCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 100 min, and the coating thickness is 2.0 μm;
[0101] (2) TiBN layer, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas H 2 、TiCl 4 , BCl 3 、N 2 , the purity of each gas is greater than 99.99%, the deposition time is 120 min, and the coating thickness is 3.0 μm;
[0102] (3) TiB 2 layer, deposition temperature 900 °C, deposition pressure 100 mbar, reaction gas H 2 , BCl 3 , the purity of each gas is greater than 99.99%, the deposition time is 120 min, and the coating thickness is 3.0 μm.
[0103] Comparative Example 2
[0104] A method for preparing a multi-layer alternating coating tool, wherein the substrate is a WC-Co based cemented carbide and the coating is a CVD TiN / MT-Ti(C,N) / TiAlOCN / Al 2 O 3 / TiN multilayer coating, with a total thickness of 8μm, the preparation method of each layer is as follows:
[0105] (1) TiN layer, deposition temperature 900 °C, deposition pressure 120 mbar, reaction gas TiCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 1.0 μm;
[0106] (2) MT-TiCN layer, deposition temperature 880 °C, deposition pressure 80 mbar, reaction gas TiCl 4 , CH 3 CN、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 90 min, and the coating thickness is 2.0 μm;
[0107] (3) TiAlOCN layer, deposition temperature 950 °C, deposition pressure 100 mbar, reaction gas TiCl 4 、AlCl 3 ,CO,N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 60 min, and the coating thickness is 1.0 μm;
[0108] (4) Al 2 O 3 layer, deposition temperature 1000 ℃, deposition pressure 80 mbar, reaction gas AlCl 3 , CO 2 , H 2 S.H. 2 , the purity of each gas is greater than 99.99%, the deposition time is 120 min, and the coating thickness is 3.0 μm;
[0109] (5) TiN layer, deposition temperature 1000 °C, deposition pressure 120 mbar, reaction gas TiCl 4 、N 2 , H 2 , the purity of each gas is greater than 99.99%, the deposition time is 40 min, and the coating thickness is 1.0 μm.
[0110] The performance of the cutting tools prepared in the embodiments and comparative examples was tested, and the results are shown in Table 1.
[0111] Table 1
[0112]
[0113] The following tests were conducted on the processing performance of the cutting tools prepared by the embodiments of the present invention and the comparative examples, wherein:
[0114] Test condition 1 is as follows:
[0115] Processing method: rough milling
[0116] Workpiece: Titanium alloy blade
[0117] Material: Ti6Al4V
[0118] Tool type: RPHT120408E-MM3
[0119] Cutting conditions: cutting speed 30 m / min, feed 0.1 mm / z, cutting depth 1.5 mm, cutting width ae 60 mm, wet cutting
[0120] On the premise of no chipping, the number of tool parts processed is calculated after the tool face wear reaches 0.3 mm. The results are shown in Table 2.
[0121] Table 2
[0122]
[0123] Test condition 2 is as follows:
[0124] Processing method: continuous turning
[0125] Material: GH4169
[0126] Tool type: WNMG080408-SC3
[0127] Cutting conditions: cutting speed 60 m / min, feed 0.25 mm, cutting depth 1 mm, dry cutting
[0128] Under the condition of no chipping, the cutting time after the tool life is up to 0.3 mm is calculated. The test results are shown in Table 3. The wear of the tool face after the tool is empty is measured by an OLYMPUS SZ61 optical super-depth microscope with a scale.
[0129] Table 3
[0130]
[0131] It can be seen from Tables 1-3 above that the service life of the cutting tools in the embodiments of the present invention is significantly better than that in the comparative example, and the wear resistance of the cutting tools in the embodiments of the present invention is greatly improved.
[0132] The above description is only a preferred embodiment of the present invention, and does not limit the patent scope of the present invention. All equivalent structural changes made by using the contents of the present invention specification under the inventive concept of the present invention, or directly / indirectly applied in other related technical fields are included in the patent protection scope of the present invention.
Claims
1. A multi-layer alternating coating tool, characterized in that: The invention comprises a substrate and a multilayer coating sequentially arranged on the surface of the substrate, wherein the multilayer coating is prepared by a chemical vapor deposition method, and comprises a first sub-coating and a second sub-coating sequentially deposited from the inside to the outside; the first sub-coating is Zr 1-a Si a N layer, 0.05≤a≤0.2; the second sub-coating is ZrB x layer, 1.8≤x≤2.5; the Zr 1-a Si a The grains of the N layer are equiaxed crystals <35nm. x The layer is a columnar crystal structure; The first sub-coating and the second sub-coating are deposited alternately at least twice, and as the coatings are deposited alternately, the thickness of the first sub-coating gradually decreases, while the thickness of the second sub-coating gradually increases.
2. The multi-layer alternating coating tool according to claim 1, characterized in that: The multi-layer coating further comprises a bonding layer deposited between the substrate surface and the first sub-coating, wherein the bonding layer is any one of TiN, Ti, ZrN and Zr, and the thickness of the bonding layer is 0.5-2.0 μm.
3. The multi-layer alternating coating tool according to claim 1, characterized in that: The ZrB x The micro-Vickers hardness of the layer reaches above 35 GPa.
4. The multi-layer alternating coating tool according to claim 1, characterized in that: The total thickness of the multilayer coating is 4.0~12.0μm.
5. The multi-layer alternating coating tool according to claim 1, characterized in that: A surface layer is deposited on the surface of the second sub-coating layer. The surface layer is any one of ZrN and ZrCN, and the total thickness of the surface layer is 0.2-2.0 μm.
6. The multi-layer alternating coating tool according to claim 1, characterized in that: The substrate is any one of cemented carbide, high speed steel, metal ceramic, polycrystalline diamond and cubic boron nitride.
7. A method for preparing a multi-layer alternating coating tool according to any one of claims 1 to 6, characterized in that: include: depositing a coating on a substrate by chemical vapor deposition; Zr 1-a Si a The N layer is deposited at 800-950°C and 20-100 mbar using H2, ZrCl4, SiCl4, NH3, and N2 as raw materials; ZGar x The layer is deposited at 800~950℃ and 50~200mbar using H2, ZrCl4, BCl3 and Ar as raw materials.
8. The method for preparing a multi-layer alternating coating tool according to claim 7, characterized in that: The ZrN bonding layer is obtained by chemical reaction on the substrate surface at 800~950℃ and 50~200mbar using ZrCl4, N2 and H2 as raw materials.
Citation Information
Patent Citations
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CN112805109A
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CN116162917A