Composite coating based on textured alpha-alumina and method for its production
By using a hot-wall chemical vapor deposition process, combined with stepwise deposition and a modified layer, the grain size was controlled to be ≤1μm, which solved the problem of grain growth in the strong (006) textured coating and improved the overall performance and service life of the coating.
Patent Information
- Application Number
- CN202511445663.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-11
- Publication Date
- 2026-01-06
- Estimated Expiration
- 2045-10-11
AI Technical Summary
Existing technologies fail to effectively control grain size when preparing strong (006) textured coatings, resulting in reduced coating density and toughness, which can easily become crack sources and weaken the textural strengthening effect.
A hot-wall chemical vapor deposition process was adopted, and a combination of step-by-step deposition and modification layer was used to introduce a temperature gradient decrease and a specific atmosphere ratio to control the grain size ≤1μm and form a strong (006) textured coating.
This achieves stable control of grain size at the submicron level while maintaining high texture, thereby improving the hardness, toughness, and bonding strength of the coating and extending its service life.
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Figure CN120905647B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of surface coating preparation technology, specifically to a texture-based method. Composite coatings and their preparation methods. Background Technology
[0002] MT-TiCN+ based materials were prepared using a hot-wall chemical vapor deposition (CVD) method. The composite coating has excellent wear resistance and high-temperature oxidation resistance, and has been widely used in the field of cemented carbide CNC cutting tools.
[0003] As a key functional layer in the coating system, its crystal structure exhibits significant anisotropy, with multiple crystal plane orientations including (012), (104), (110), (006), (214), (116), and (300). Among these, (012), (104), (110), (006), (214), (116), and (300) are crystal plane indices, used to identify the orientation of different atomic planes in the crystal. Through strict control of the growth process, different textures can be obtained. The coating, in turn, affects its mechanical properties and service behavior. For example, US patents US7455900B2, US7163735B2, and US2006 / 0115662A1 obtained coatings with (116), (012), and (110) textures respectively by controlling the oxidation potential of the oxidation process. Coating; while US Patent 2007 / 0104945A1 uses pulse oxidation technology and controls growth process The proportions obtained have a texture of (006). .
[0004] In recent years, in-depth international research has further revealed that those with strong (006) texture The coating is superior to other textures Coatings exhibit superior wear resistance and crack propagation resistance, making them a hot research topic. To achieve this ideal texture, numerous companies and scholars have explored various technical approaches, such as those employed in US Patent 7923101B2. and Alternating pulse oxidation and control growth process The proportion was used to obtain a texture with (006) Coating; US Patent US2022 / 0274892A1 by controlling the oxidation process The ratio and coating temperature of the main intake duct achieved a strong (006) texture. Coating; US Patent US2016 / 0175940A1 by adopting CO A strong (006) texture was obtained through co-oxidation treatment. Coating; US Patent US2014 / 0287210A1 obtained a strong (006) texture by Ti purging treatment of the bonding layer TiCNO. Coating; Chinese Patent CN118880276A utilizes a bonding layer TiAlCNO with a gradient increase in Al and O elements, forming a coating on top of it. Achieve strong (006) texture Coating. Actual cutting tests show that coatings based on (006) texture prepared through different paths... Composite coatings offer a longer service life than traditional non-woven coatings, whether in continuous high-speed turning or intermittent turning. The coating has been significantly improved, effectively promoting the improvement of product performance and processing efficiency in the machining field.
[0005] Despite the strong (006) texture The coating offers significant performance advantages, but it still faces a long-standing and unresolved technical challenge during the deposition process. During the coating growth process, The grains exhibit grain growth issues. The (006) texture obtained through the aforementioned route... The coating process did not take this issue into account, and there were no specific measures to control it in the process.
[0006] Specifically, most existing texture control processes focus on optimizing crystal orientation through atmospheric composition, pulse programming, or interface modification, but generally neglect the simultaneous fine control of grain size. Grain coarsening reduces the density and toughness of the coating, making it prone to becoming a crack initiation point during service, leading to spalling failure and thus weakening the benefits of texture strengthening. Therefore, how to effectively suppress grain size while ensuring a high-strength (006) texture is a crucial issue. Grain growth, and stabilizing its size at the submicron level (e.g., below 1 μm), is a key challenge to further improve the overall performance of this type of coating and maximize its engineering application value. It is also the core problem that this invention aims to solve. Summary of the Invention
[0007] This invention aims to provide a texture-based The composite coating and its preparation method can achieve a strong (006) texture. While coating, take into account The particle size is adjusted to be ≤1μm to achieve better overall performance.
[0008] To achieve the above objectives, the present invention provides the following basic solution.
[0009] Option 1
[0010] Based on texture The method for preparing the composite coating includes the following steps:
[0011] A hot-wall chemical vapor deposition process was used to sequentially deposit a TiN layer, an MT-TiCN layer, a bonding layer, and a modification layer on the substrate surface. Layer and outermost TiN, where:
[0012] The The layer consists of three sublayers, and its deposition process involves the sequential deposition of the first, second, and third sublayers, while meeting the following conditions: the deposition temperature is in the range of 900–1050℃, gradually decreasing during the deposition process; the deposition pressure is 50–200 mbar; and the introduced mixed gas contains CO and [missing information - likely a specific chemical compound]. And CO and The volume ratio is controlled between 0.5 and 3; in the mixed gas The volume percentage shall not exceed 92% and shall not be less than 80%;
[0013] The modified layer includes an Al purging modified layer and an oxidation modified layer, used to control... Texture and grain size, to ensure The particle size is ≤1μm and has a strong (006) texture.
[0014] Option 2
[0015] Based on texture The composite coating, deposited on the substrate, consists of, from the inside out: a TiN underlayer, an MT-TiCN layer, a bonding layer, and a modified layer. The modified layers consist of an Al-purge modified layer and an oxidation modified layer. The layer has a strong (006) texture, and The particle size is ≤1μm.
[0016] The working principle and advantages of this invention are as follows:
[0017] This invention is based on texture The composite coating and its preparation method can achieve a strong (006) texture. While coating, take into account Particle size, making its particle diameter This achieves superior overall performance. The key points are:
[0018] This solution successfully resolved the current strong (006) texture. A long-standing technical challenge in coating preparation is achieving a highly oriented texture while effectively suppressing abnormal alumina grain growth, thereby obtaining a high-performance coating with excellent texture and fine microstructure. This solution employs a strategy combining stepwise deposition and modification, specifically introducing a modified layer with finely controlled structure, and further... The layer employs a process that combines temperature gradient descent with a specific atmosphere ratio of mixed gas for synergistic control, ensuring high texture while maintaining stable grain size. The following improvements have been achieved in coating hardness, toughness, and bonding strength, resulting in more stable performance and a longer service life under harsh conditions such as high-speed and intermittent cutting.
[0019] Furthermore, compared to the traditional technological development trajectory, as described in the background section, existing technological solutions have all evolved along a path of "single-objective optimization." That is, their improvement strategies consistently revolve around how to further enhance texture strength or improve a single performance indicator of texture, without considering "grain size control" as a related problem that needs to be addressed simultaneously with "texture control." In the field of coating technology, texture formation and grain growth typically involve different physicochemical mechanisms. Therefore, traditional technological thinking usually treats them as independent process objectives that need to be optimized separately. Simultaneously considering both texture and grain size in the same process is quite challenging.
[0020] This solution solves this technical challenge by creatively employing a precise "temperature gradient descent" strategy within the high-temperature deposition range, supplemented by a special modification layer process and simultaneous control of the atmosphere ratio to regulate the gas phase reaction kinetics. This achieves both strong texture and fine grains without significantly sacrificing deposition rate and crystallization quality. Attached Figure Description
[0021] Figure 1 This invention is based on texture A schematic diagram of the coating structure in an embodiment of the composite coating and its preparation method;
[0022] Figure 2 This is a SEM image of the fracture surface of the coating, representing an application example of the present invention.
[0023] Figure 3 Here is a SEM image of the fracture surface of the coating in Comparative Example 1;
[0024] Figure 4 The image shows the SEM morphology of the fracture surface of the coating in Comparative Example 2.
[0025] Figure 5 Coating as an application example of the present invention ;
[0026] Figure 6 Coating as an application example of the present invention Surface SEM morphology image;
[0027] Figure 7 For Comparative Example 1, the coating Surface SEM morphology image;
[0028] Figure 8 Comparative Example 2 Coating Surface SEM morphology image;
[0029] Figure 9 The coating XRD pattern curve is an application example of the present invention;
[0030] Figure 10 The XRD pattern of the coating in Comparative Example 1 is shown.
[0031] Figure 11 The XRD pattern of the coating in Comparative Example 2 is shown.
[0032] Figure 12 The images show the flank wear of the present invention under the same conditions, serving as application examples and comparative examples.
[0033] The markings in the accompanying drawings include: 00-matrix, 11-TiN, 12-MT-TiCN, 13-bonding layer, 14-modified layer, 15- 16-TiN;
[0034] 131-HT-TiCN, 132-TiCNO, 133-TiAlCNO; 141-Al purging modified layer, 142-oxidation modified layer; 151-first sublayer, 152-second sublayer, 153-third sublayer. Detailed Implementation
[0035] The following detailed explanation illustrates the specific implementation methods:
[0036] The basic implementation examples are as follows: Figure 1 As shown: Based on texture The method for preparing the composite coating includes the following steps:
[0037] A hot-wall chemical vapor deposition (CVD) process was used to sequentially deposit a TiN layer, an MT-TiCN layer, a bonding layer, and a modification layer on the substrate surface. Layer and outermost TiN, where:
[0038] The matrix is a WC-based cemented carbide, TiCN-based ceramic, etc. ceramic base Ceramics, silane ceramics, CBN, carbon-based materials (such as graphite, carbon fiber, diamond), high-temperature alloys, or other materials that may be suitable for hot-wall CVD technology.
[0039] The TiN layer is used to ensure the adhesion between the coating and the substrate. The deposition temperature of the TiN layer is 850–1000℃, the coating thickness is 0.3–1.5 μm, the deposition pressure is 100–300 mbar, and the composition of the introduced mixed gas is 0.8–1.8 vol%. 20–40 vol% The margin is .
[0040] The MT-TiCN layer serves as a wear-resistant layer, with a coating thickness of 3-10 μm. The deposition temperature of the MT-TiCN layer is 800–900 °C, the deposition pressure is 50–200 mbar, and the composition of the introduced mixed gas is 1.5–2.5 vol%. 0.5–1.5 vol% 10–25 vol% 1–5 vol% HCl, balance: In this process, reasonable The ratio of MT-TiCN and HCl helps to refine the particle size and increase the hardness of the coating while maintaining its toughness.
[0041] The bonding layer is used to ensure that the MT-TiCN layer and... The bonding strength of the layers. The bonding layer consists of TiCN, TiCNO, and TiAlCNO layers sequentially, allowing MT-TiCN to gradually transition to high temperatures. The coating thickness is 0.5-1.5μm.
[0042] The deposition temperatures of the bonding layers are all 900–1050℃, and the deposition pressures are as follows: TiCN layer, 100–500 mbar; TiCNO layer, 60–300 mbar; TiAlCNO layer, 60–300 mbar.
[0043] The composition of the introduced mixed gas is as follows:
[0044] TiCN layer, 1–2 vol% 2–5 vol% 0–2 vol% HCl, initial volume percentage of 15–35 vol%. The margin is ;
[0045] TiCNO layer, 1-3 vol% 20-30 vol% 0.5-1 vol% 1-2 vol% CO, 0-2 vol% HCl, balance: ;
[0046] TiAlCNO layer, 1.5-2.5 vol%. 20-30 vol% 0.5-4 vol% CO, 1.5-3 vol% The margin is ;
[0047] In the TiCN layer, The volume percentage decreased gradually from 15–35 vol% to 3–5 vol%; in the TiAlCNO layer, the CO volume percentage increased gradually.
[0048] Through a step-by-step design of the bonding layers and precise atmosphere control, MT-TiCN can be gradually transitioned to... At the same time, through Changes in CO flow rate help form "needle-like" structures within the coating, achieving high adhesion of the coating.
[0049] The modified layer includes an Al purging modified layer and an oxidation modified layer, used to control... Texture and grain size, to ensure The particle size is ≤1μm and has a strong (006) texture.
[0050] The deposition temperature of the Al-purged modified layer is 900–1050℃, the deposition pressure is 50–100 mbar, and the composition of the introduced mixed gas is 0.5–0.7 vol%. The margin is .
[0051] The deposition temperature of the oxide-modified layer in the modified layer is 900–1050℃, the deposition pressure is 50–100 mbar, and the composition of the introduced mixed gas is 20–30 vol%. 1.5–3.5 vol% 2.5–3.5 vol% CO, balance: .
[0052] By designing Al-modified and oxide layers, the following can be increased: Nucleation sites, while balancing the oxygen content in the binding layer, to ensure While developing the texture, we also take into account the refinement of the particles.
[0053] The The layer exhibits excellent high-temperature resistance and wear resistance, possesses a strong (006) texture, and has a coating thickness of 1-10 μm. It consists of three sublayers, and its deposition process includes the sequential deposition of the first, second, and third sublayers, while satisfying the following conditions:
[0054] The deposition temperature ranged from 900 to 1050 °C, gradually decreasing during deposition; the deposition pressure was 50–200 mbar; the introduced mixed gas contained CO and... And CO and The volume ratio is controlled between 0.5 and 3; in the mixed gas Its volume percentage is no higher than 92% and no lower than 80%.
[0055] The In the three sub-layers of the layer:
[0056] The gas mixture composition corresponding to the first sublayer is: 4–15 vol% (CO+) ), 1–3 vol%HCl, 0.4–1 vol% 1.5–3 vol% The margin is ;
[0057] The gas mixture composition corresponding to the second sublayer is 2.5–5.5 vol%. , 1.5–10 vol%CO, 1–3 vol%HCl, 0.45–1 vol% 1.5–3 vol% The margin is ;
[0058] The gas mixture composition corresponding to the third sublayer is 2.5–5.5 vol%. , 1.5–5 vol%CO, 3.5–9 vol%HCl, 0.45–1 vol% 1.5–3 vol% The margin is .
[0059] During this process, gradually decreasing the deposition temperature helps to thermodynamically reduce the coating reaction rate, thus controlling the expansion of Al2O3 particles. However, the temperature cannot be too low to avoid... Insufficient response affects The structure may cause Crystallization causes pore blockage. By controlling the CO ratio within a reasonable range, the reaction rate of the coating can be appropriately reduced, while the reaction can be promoted. Growth along the (006) crystal plane. The main issue is the carrier gas in the reaction process; due to the influence of the viscosity coefficient of some reactant gases, Both excessively high and low proportions can cause changes in the uniformity of the distribution of key gases, affecting... The uniformity of texture, through the... The volume ratio limitation helps to ensure The uniformity of the texture leads to better coating quality.
[0060] Notably, this scheme also introduces different proportion ranges in a tiered manner. . exist It plays a remarkable role in the growth process, promoting growth by forming AlO:SH intermediate reactants. It acts as a catalyst for growth, and at the right ratio, it can also promote growth. It grows along the (006) crystal plane, acting as a stabilizer. If A low proportion will have an impact. In terms of growth direction, under extreme conditions, it can even form a (110) texture. ,at the same time The ratio cannot be too high, as it will not only affect... The structure, due to its own viscosity, will adhere to the coating fixture, and when it comes out of the oven, it will be accompanied by a strong "rotten egg" smell, which is not good for the on-site environment. This solution takes both into account.
[0061] The outermost TiN layer is golden yellow and serves as a marker layer to aid in determining the degree of coating wear. Its thickness is 0.5-2 μm, the deposition temperature is 850–1000℃, the deposition pressure is 300–800 mbar, and the composition of the introduced mixed gas is 1–2 vol%. 20–40 vol% The margin is .
[0062] This embodiment also provides a texture-based method. A composite coating is deposited on the substrate and applied as described above based on texture. The composite coating was prepared by a specific method; the coating, from the inside out, comprises: a TiN underlayer, an MT-TiCN layer, a bonding layer, and a modified layer. The layers, and the outermost TiN layer; wherein, the The layer has a strong (006) texture, and The particle size is ≤1μm.
[0063] The The layer consists of three sublayers with a texture coefficient TC(006)≥8, and the texture coefficient TC values of the crystal planes (012), (104), (110), (113), (024), (116), (214), and (300) are all ≤0.5.
[0064] (006), (012), (104), (110), (113), (024), (116), (214), and (300) are all crystal plane indices, used to identify the orientation of different atomic planes in a crystal.
[0065] To verify the effectiveness and superiority of this solution, the following explanation is provided in conjunction with a specific application example and a simplified comparative example, supplemented by multiple test comparisons.
[0066] I. Application Examples:
[0067] WNMG080408-TM CNC inserts (WC-8%Co cemented carbide) were selected as the coating substrate, with a cutting edge passivation value of 35μm. All inserts were sandblasted and cleaned before coating to ensure the cleanliness of the substrate surface.
[0068] In the SCT600TH hot-wall CVD coating furnace, according to Figure 1 Structure (i.e., a texture-based structure provided in this embodiment) (composite coating), applying a texture-based coating provided in this embodiment. The method for preparing the composite coating is described, and the coating is applied.
[0069] The coating components along the growth direction are, in order, TiN (11), MT-TiCN (12), bonding layer (13), and modified layer (14). (15) TiN (16). Figure 2 The SEM image shows the fracture surface morphology of the coating in this application example. The SEM image reveals that the underlying TiN (11) layer is approximately 0.88 μm thick, the MT-TiCN (12) layer is approximately 7.7 μm thick, and the bonding layer + modified layer (13+14) layer is approximately 0.95 μm thick. (15) Thickness is about 5.6 μm, and surface TiN (16) is about 0.6 μm.
[0070] The parameters such as coating temperature, pressure, gas type and ratio are shown in Table 1.
[0071] Table 1. Coating growth process parameters in the implementation case.
[0072]
[0073] II. Comparative Example:
[0074] The comparative examples include two coating schemes. The substrates used are the same batch of WNMG080408-TM CNC inserts (WC-8%Co cemented carbide) as the application examples, with a cutting edge passivation value of 35μm. Before coating, both were sandblasted and cleaned to ensure the cleanliness of the substrate surface.
[0075] The coating process was also carried out in an SCT600TH hot-wall CVD coating oven.
[0076] Figure 3 The SEM morphology of the coating fracture surface in Comparative Example 1 shows the coating composition along the growth direction as follows: TiN, MT-TiCN, bonding layer, ... TiN, where the bottom TiN, MT-TiCN, and top TiN are manufactured using the same process as in the application example. It is a single-layer structure with a non-strong texture, and its total thickness is close to that of the application example.
[0077] The key difference between Comparative Example 1 and the application example is that the modification layer (14) unique to this invention is omitted. The layer is a single-layer deposition, and the process parameters were not optimized for texture and grain size, resulting in a non-strong texture.
[0078] Figure 4 The SEM morphology of the coating fracture surface in Comparative Example 2 shows that the coating composition along the growth direction is, in order, TiN, MT-TiCN, and the bonding layer. TiN, wherein the bottom TiN, MT-TiCN, bonding layer, modified layer and top TiN are processed in the same way as in the application example of this invention.
[0079] The key difference between Comparative Example 2 and the application example is: No gradient cooling or stepwise component control was used during the growth process; the single layer grew continuously.
[0080] Under these conditions, since the bonding layer and the modified layer are consistent with the application example, therefore For a strong (006) texture, however, due to No gradient cooling or stepwise composition control was used during the growth process; instead, a single layer was grown continuously. Therefore, the particles are relatively coarser compared to those in application examples. The thickness is similar to that of the application example, but MT-TiCN is about 4 μm thicker than the application example.
[0081] III. Performance Comparison and Test Results
[0082] 1. Coating adhesion test (scratch test):
[0083] The coating adhesion was tested on the surface of WC carbide cutting tools using the scratch method with a load of 100N.
[0084] Application examples: Figure 5 The image shows the morphology of the coating scratches under a stereomicroscope. The figure shows that the coating did not crack when the loading force reached 100N, proving that the coating adhesion of the application example is excellent.
[0085] 2. Grain morphology and size (SEM analysis):
[0086] Application example: After removing the surface TiN (16) by acid etching, the image was examined using a scanning electron microscope (SEM). Figure 6 ) Observe application examples Morphology and particle size were measured. (Through...) Figure 6 Observations show that, although The nominal size is 2.533 μm, but closer inspection reveals that the large particles are composed of 6 tiny [units / organisms]. It is composed of particles with a typical "pyramid" shape, each The size is only about 0.5μm, successfully achieving the goal of fine grains ≤1μm.
[0087] Comparative Example 1: Using early non-woven materials Coatings prepared by coating process ( Figure 6 Particles larger than 1 μm account for a large proportion, and the grains are obviously coarse.
[0088] Comparative Example 2: Using the same bonding layer and modification layer as the application example, No gradient cooling or stepwise composition control was used during the growth process; the growth was a single-layer continuous process, resulting in a large proportion of particles larger than 1 μm, and some particles larger than 2 μm. Figure 8 ).
[0089] 3. Texture analysis (XRD analysis):
[0090] Calculation method: Determined through XRD The structure was analyzed and the texture factor TC value for each crystal plane was calculated. Because... Both the TiCN peak and the TiCN peak exhibit diffraction peaks around 41.67 degrees. To avoid interference from the TiCN diffraction peak, the parallel peak of (006) around 90.7 degrees, corresponding to the (00 12) peak, was selected for further analysis. The analysis was performed using PDF-10-1073.
[0091] Nine peaks (012), (104), (110), (113), (300), (024), (116), (214), and (00 12) were selected and their texture coefficients (TC) were calculated using the following formula. The maximum TC value was 9.
[0092] ;
[0093] Where I(hkl) represents Measured XRD intensity value of a certain crystal plane; Represents PDF-10-1073 card Standard strength value corresponding to the crystal plane; n=9.
[0094] The calculation results are shown in Table 2:
[0095] Application examples ( Figure 9 (Table 2) Figure 9 The XRD pattern of the coating in the application example shows that the TC value of the (00 12) crystal plane is as high as 8.27, while the TC values of all other crystal planes are <0.5, which proves that it is a strong (006) texture.
[0096] Comparative Example 1 ( Figure 10 (Table 2) Figure 10 The XRD pattern of the coating in Comparative Example 1 shows that the TC value of the (00 12) crystal plane is only 4.4, while the TC values of the other crystal planes are significantly higher (0.37-1.15), proving that it is a non-strong texture or a mixed texture.
[0097] Comparative Example 2 ( Figure 11 (Table 2) Figure 11 The XRD pattern of the coating in Comparative Example 2 shows that the TC value of the (00 12) crystal plane is 8.42, and the TC values of the other crystal planes are all <0.5, indicating a strong (006) texture.
[0098] Table 2 Application Examples and Comparative Examples TC values of different crystal planes
[0099]
[0100] 5. Cutting performance test:
[0101] Test conditions: The cutting performance of the coating was verified through a cutting test. The workpiece was a 45# tempered steel bar with a length of 80mm; dry continuous turning was used with a linear speed of Vc=300m / min, and the cutting speed of each cut was kept consistent by adjusting the spindle speed of the machine tool. The depth of cut was 2mm and the feed rate was 0.3mm / revolution.
[0102] The cutting performance of the coating is judged by the wear of the back face after cutting the same distance.
[0103] Test results:
[0104] Comparative Example 1 (non-strong textured coating): The flank face was worn by 0.43 mm and the cutting edge was damaged, making it impossible to continue cutting.
[0105] Comparative Example 2 (Strong (006) textured coarse grain coating): The wear value on the back face is 0.34 mm, and cutting can still continue.
[0106] Application example (strong (006) textured fine grain coating): the flank wear is only 0.22mm, and cutting can still continue.
[0107] in conclusion: Figure 12For application examples and comparative examples of back face wear comparison, it can be seen from the comparison that, with the same total thickness, the wear resistance of the coating of the present invention is significantly better than that of traditional non-woven coatings, and also significantly improved compared with conventional coarse-particle strong-textured coatings.
[0108] In summary, through detailed process parameter tables and systematic comparative tests (adhesion, microstructure, texture, and machinability), the "modified layer + three-section" provided by this invention has been fully demonstrated. The "deposition + atmosphere control + temperature gradient" process can simultaneously achieve the two key objectives of strong (006) texture and fine grains (≤1μm), thereby significantly improving the overall mechanical properties and cutting life of the coating. The comparative example serves as a counterexample, highlighting the performance gap caused by omitting key technical means.
[0109] This embodiment provides a texture-based method. The composite coating and its preparation method can achieve a strong (006) texture. While coating, take into account The particle size is adjusted to be ≤1μm to achieve better overall performance.
[0110] Specifically, this solution introduces a composite modified layer (Al purging + oxidation modification) to pretreat the bonding layer surface, which can facilitate subsequent... Uniform nucleation and directional growth create favorable conditions; then through a three-stage process... Deposition combined with simultaneous temperature gradient descent and low-hydrogen atmosphere control can respectively dominate nucleation, texture guidance, and grain refinement, forming an optimized dynamic growth environment. This ensures performance optimization from the interface to the bulk phase, guaranteeing the uniformity and stability of the microstructure and structure. This combined strategy cleverly avoids the contradiction between high-temperature strong texture and low-temperature fine grains in traditional processes, and achieves optimization of the overall coating performance.
[0111] The above descriptions are merely embodiments of the present invention. Commonly known structures and characteristics of the solutions are not described in detail here. Those skilled in the art are aware of all common technical knowledge in the field prior to the application date or priority date, are aware of all existing technologies in that field, and have the ability to apply conventional experimental methods prior to that date. Those skilled in the art can, under the guidance of this application, improve and implement this solution in combination with their own capabilities. Some typical known structures or methods should not be obstacles for those skilled in the art to implement this application. It should be noted that those skilled in the art can make several modifications and improvements without departing from the structure of the present invention. These should also be considered within the scope of protection of the present invention, and will not affect the effectiveness of the implementation of the present invention or the practicality of the patent.
Claims
1. A method of making a composite coating based on texture , characterized in that comprising the following steps: The TiN layer, the MT-TiCN layer, the bonding layer, the modification layer, the layer and the outermost TiN layer are sequentially deposited on the surface of the substrate by a hot-wall chemical vapor deposition process, layer and the outermost TiN layer. The layer is composed of three sub-layers, and the deposition process includes sequentially depositing the first sub-layer, the second sub-layer and the third sub-layer, and meets the following conditions: the deposition temperature is in the range of 900-1050℃, and gradually decreases during the deposition process; the deposition pressure is 50-200 mbar; the mixed gas introduced contains CO and , and the volume ratio of CO to is controlled between 0.5-3; the volume ratio of in the mixed gas is not higher than 92% and not lower than 80%. The modification layers include Al purge modification layers and oxidation modification layers for controlling the texture and grain size, ensuring a particle size of ≤1 μm and a strong (006) texture; The Al purge modification layer has a deposition temperature of 900-1050°C, a deposition pressure of 50-100 mbar, and a mixed gas composition of 0.5-0.7 vol% , the balance being ; the oxidation modification layer has a deposition temperature of 900-1050°C, a deposition pressure of 50-100 mbar, and a mixed gas composition of 20-30 vol% , 1.5-3.5 vol% , 2.5-3.5 vol% CO, the balance being .
2. The textured-based composite coating of claim 1, wherein the textured-based composite coating is prepared by a method comprising: The base body is a WC-based cemented carbide, a TiCN-based ceramic, ceramic, ceramic, sialon ceramic, CBN, carbon-based material or high-temperature alloy. 3. The textured based composite coating of claim 1, wherein the textured based composite coating is prepared by a method comprising: The deposition temperature of the TiN layer is 850-1000 °C, the deposition pressure is 100-300 mbar, the composition of the mixed gas introduced is: 0.8-1.8 vol% , 20-40 vol% , and the balance is ; The deposition temperature of the MT-TiCN layer is 800-900 °C, the deposition pressure is 50-200 mbar, the composition of the mixed gas fed in is: 1.5-2.5 vol% , 0.5-1.5 vol% , 10-25 vol% , 1-5 vol% HCI, the balance being .
4. The textured-based composite coating of claim 1, prepared by the method comprising: The binding layer is composed of TiCN layer, TiCNO layer and TiAlCNO layer in turn, the deposition temperature is 900-1050℃, the deposition pressure is 100-500 mbar, 60-300 mbar, 60-300 mbar respectively, the composition of the mixed gas introduced is respectively: 1 - 2 vol% , 2 - 5 vol% , 0 - 2 vol% HCI, initial volume percent 15 - 35 vol% , the balance being ; 1 -3 vol % , 20-30 vol % , 0.5-1 vol % , 1 -2 vol % CO, 0-2 vol % HCI, remainder ; 1.5 - 2.5 vol% , 20 - 30 vol% , 0.5 - 4 vol% CO, 1.5 - 3 vol% , the balance being ; wherein, in the TiCN layer, The volume percentage decreases; in the TiAlCNO layer, the volume percentage of CO changes in a gradient.
5. The textured based composite coating of claim 1, prepared by the method comprising: The In the three-layer sub-layers of the layer: The mixed gas composition corresponding to the first sub-layer is: 4-15 vol% (H2+Ar) + ), 1-3 vol% HCl, 0.4-1 vol% , 1.5-3 vol% , and the balance is ; The mixed gas composition corresponding to the second sub-layer is: 2.5-5.5 vol% , 1.5-10 vol% CO, 1-3 vol% HCl, 0.45-1 vol% , 1.5-3 vol% , and the balance is ; The mixed gas composition corresponding to the third sub-layer is: 2.5-5.5 vol% , 1.5-5 vol% CO, 3.5-9 vol% HCl, 0.45-1 vol% , 1.5-3 vol% , the balance being .
6. The textured-based composite coating of claim 1, prepared by the method comprising: The deposition temperature of the outermost layer TiN is 850-1000℃, the deposition pressure is 300-800 mbar, the composition of the mixed gas introduced is: 1-2 vol% , 20-40 vol% , and the balance is . 7. A composite coating based on a texture deposited on a substrate, characterized in that The application of the texture-based method as described in any one of claims 1-6 The composite coating was prepared by a specific method, and from the inside out, it includes: a TiN base layer, an MT-TiCN layer, a bonding layer, and a modified layer. The modified layers consist of an Al-purge modified layer and an oxidation modified layer. The layer has a strong (006) texture, and The particle size is ≤1μm.
8. The textured based composite coating of claim 7, wherein, The The layer is composed of three sub-layers, the texture coefficient TC(006) is greater than or equal to 8, and the texture coefficients TC of the (012), (104), (110), (113), (024), (116), (214), and (300) crystal planes are all less than or equal to 0.
5.
Citation Information
Patent Citations
Texture-strengthened alpha-Al2O3 coated cutting tool and preparation method thereof
CN118880276A
Enhanced alumina layer with texture
US20060115662A1
Alumina layer with enhanced texture
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Surface-coated cutting tool
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CVD coated cutting tool
US20160175940A1