Method for preparing multi-element metalized coating on diamond surface

CN117548673BActive Publication Date: 2026-08-11ZHENGZHOU UNIVERSITY OF AERONAUTICS
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-11-28
Publication Date
2026-08-11

AI Technical Summary

Technical Problem

[0005]本发明为了解决现有技术存在的不足,提供一种金刚石表面多元素金属化镀层制备方法,本方法使用盐浴镀覆的方法来对金刚石进行多元素镀层的处理,制备出的镀覆金刚石,其金刚石基体间不仅有机械把持力,而且基体间形成了C-Ti化合键、Ni-Ti化合键,在金刚石表面形成了多元素金属化镀层,使得金刚石的结合强度及润湿性都得到了极大的提升,更值得一提的是本发明解决了传统工艺镀覆设备复杂、镀层需要多次镀覆、实验污染的难题,更加节能环保

Benefits of technology

本发明实施的金刚石表面多元素金属化镀层制备方法具有工艺简单、制备效率高、节能环保、成本低等优点,适合大规模的生产,相比传统的镀覆技术,本发明通过高温盐浴镀工艺生成C-Ti化合键、Ni-Ti化合键,使得金刚石的结合强度及润湿性都得到了极大的提升,推动了金刚石及其复合材料制品产业的发展。

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Abstract

This invention discloses a method for preparing a multi-element metallized coating on a diamond surface, comprising the following steps: S1: Weighing salt, diamond, titanium powder, and nickel powder according to calculated masses, and grinding and mixing them uniformly for later use; S2: Transferring the mixed powder to a sintering boat, placing the sintering boat in a tube furnace, and obtaining a sample through a high-temperature salt bath plating process; S3: Performing cleaning, ultrasonication, drying, and sieving processes sequentially, and obtaining a Ti-Ni coated diamond powder product after sieving; S4: Characterizing the performance of the diamond powder product. This invention has the advantages of simple process, high preparation efficiency, energy saving and environmental protection, and low cost, and is suitable for large-scale production. Compared with traditional plating technology, this invention generates C-Ti and Ni-Ti bonds through a high-temperature salt bath plating process, which greatly improves the bonding strength and wettability of diamond, promoting the development of the diamond and its composite material products industry.
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Description

Technical Field

[0001] This invention belongs to the field of composite material production technology, specifically relating to a method for preparing a multi-element metallization coating on a diamond surface. Background Technology

[0002] Diamond, known as the king of materials, continues to have its superior properties discovered, ranging from traditional superhardness to ultra-wide bandgap semiconductors, spanning a vast range of industrial applications. As an important functional material in the fields of industry and science and technology, its excellent properties such as light transmission, thermal conductivity, electrical insulation, and high thermal conductivity give it enormous application potential in many high-tech fields, including semiconductors, quantum information, optical devices, heat dissipation, biomedicine, disinfection and sterilization, power generation and energy storage, environmental engineering, functional devices, and aerospace.

[0003] With the continuous development of modern technology, people's demands are constantly increasing, and some traditional technologies can no longer meet current requirements. For example, with the development of precious, hard, and brittle materials such as silicon crystals and ceramics, and the unprecedented increase in their application markets, traditional cutting processes such as steel sheet cutting, band saw cutting, and internal / external circular cutting suffer from defects such as deep surface damage, low yield, and wide kerfs, making it difficult to meet the cutting requirements of hard and brittle materials. Simultaneously, with the continuous development of modern technology, people's demands for electronic products are increasing, not only pursuing faster speeds and better performance but also smaller sizes. The smaller the product, the more prominent the heat dissipation problem becomes, and people hope to find new materials to improve heat dissipation. Diamond, as a reinforcement in novel high thermal conductivity composite materials, directly affects the comprehensive thermophysical properties of the composite material through its interfacial bonding state with the matrix (resin, metal, and ceramic). Interfacial chemical bonding significantly reduces interfacial thermal resistance and enhances mechanical properties. Therefore, improving the multi-element metallization coating technology on the diamond surface is particularly important.

[0004] Modifying diamond surfaces with metals, specifically through metallization coatings, not only meets industrial needs but also improves quality of life. Multi-element metallization coating technology for diamond surfaces improves upon single-element metallization, allowing multiple metal elements to form a coating on the diamond surface. Furthermore, compounds are generated between different metals, enhancing diamond's performance and broadening its applications to meet the demands of various industries. Summary of the Invention

[0005] To address the shortcomings of existing technologies, this invention provides a method for preparing a multi-element metallized coating on the surface of diamond. This method uses salt bath plating to treat diamond with a multi-element coating. The prepared coated diamond not only has mechanical holding force between the diamond matrix but also forms C-Ti and Ni-Ti bonds between the matrix, resulting in a multi-element metallized coating on the diamond surface. This greatly improves the bonding strength and wettability of the diamond. More importantly, this invention solves the problems of complex plating equipment, multiple plating processes, and experimental pollution associated with traditional processes, making it more energy-efficient and environmentally friendly.

[0006] To solve the above-mentioned technical problems, the present invention adopts the following technical solution: a method for preparing a multi-element metallization coating on a diamond surface, comprising the following steps: S1: Weigh the salt, diamond and metal powder according to the calculated mass, grind and mix them evenly for later use. The metal powder includes titanium powder and nickel powder. S2: Transfer the mixed powder to be used in S1 to a sintering boat, then put the sintering boat into a tube furnace, heat it to 600~1000℃, hold it for 20~60min, and obtain the sample through a high-temperature salt bath plating process; S3: The sample obtained in S2 is sequentially cleaned, ultrasonicated, dried and sieved. After sieving, the diamond powder with Ti and Ni multi-element metallized coating is obtained. S4: Performance characterization of multi-element metallized coated diamond powder products.

[0007] A composite salt is formed by combining NaCl (50 g / L, purity greater than 99.5%) and KCl (50 g / L, purity greater than 99.5%).

[0008] The particle size of titanium powder in metal micro powder is 50~80 μm.

[0009] The particle size of nickel powder in metal micro powder is 5~20 μm.

[0010] The mass ratios of salt, diamond, and metal powder are respectively, m 盐 :m 金刚石 :m 金属微粉 =6:3:1; the molar ratio of NaCl to KCl is n NaCl :n KCl =2:1; the mass ratio of titanium powder to nickel powder is m Ti :m Ni =6:4.

[0011] The grinding process in S1 is as follows: salt, diamond and metal powder are manually ground in a grinding bowl for 60 minutes.

[0012] The S2 high-temperature salt bath plating process involves introducing flowing argon gas with a purity greater than 99.99% from the port of the tubular furnace to protect the salt bath plating process throughout.

[0013] The specific cleaning and ultrasonic processes in S3 are as follows: First, use a large amount of deionized water to clean and desalinate the plated product, and then use alcohol for 30 minutes of ultrasonic cleaning.

[0014] The drying process in S3 is as follows: drying is carried out in a drying oven at a constant temperature of 50 ℃ for 30~60 min; the sieving process in S3 is as follows: sieving is carried out using 300 mesh and 600 mesh sieves, and the coated product is manually ground for 10 min before sieving.

[0015] The specific operation process of S4 is as follows: SEM shows that the coating on the diamond surface after multi-element metallization modification is uniform and dense, with no missed areas. XRD can confirm that the diamond matrix contains only C, TiC, Ti, and NiTi.

[0016] Compared with the prior art, the present invention has the following advantages by adopting the above technical solution: The method for preparing a multi-element metallization coating on the diamond surface implemented in this invention has the advantages of simple process, high preparation efficiency, energy saving and environmental protection, and low cost, and is suitable for large-scale production. Compared with traditional coating technology, this invention generates C-Ti and Ni-Ti bonds through a high-temperature salt bath plating process, which greatly improves the bonding strength and wettability of diamond, and promotes the development of the diamond and its composite material products industry. Attached Figure Description

[0017] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0018] Figure 1 This is an SEM image of a diamond surface with a titanium-nickel multi-element metal coating; the image shows that the diamond coating is uniform and dense, with no uncoated areas.

[0019] Figure 2 The image shows the XRD pattern of a titanium-nickel multi-element metal coating on the surface of a diamond. This image shows that the transition zone of the diamond matrix after coating contains only C, TiC, Ti, and NiTi. Detailed Implementation

[0020] The embodiments of the present invention will be further described in detail below with reference to the accompanying drawings and examples. The following detailed description of the embodiments and the accompanying drawings are used to illustrate the principles of the present invention by way of example, but should not be used to limit the scope of the present invention. That is, the present invention is not limited to the described embodiments, and any modifications, substitutions and improvements to the parts, components and connection methods are covered without departing from the spirit of the present invention.

[0021] The present application will be described in detail below with reference to examples.

[0022] Implementation Case 1: A method for preparing a multi-element metallization coating on a diamond surface, comprising the following steps: 1) First, weigh 6.00 g of salt and stir it evenly in a mortar. Then, weigh 3.00 g of diamond and pour it into the mortar containing salt. Next, weigh 0.60 g of titanium powder and 0.40 g of nickel powder and pour them into the mortar containing salt and diamond. Finally, grind and mix all the materials evenly and put them into a mortar for later use.

[0023] 2) Place the burning boat from step 1) into a tube furnace to perform high-temperature coating treatment on the diamond surface. Flowing argon gas is continuously introduced into the tube furnace for protection throughout the process. The tube furnace is heated to 800 ℃ at a heating rate of 30 ℃ / min and held at that temperature for 20 min. After that, the burning boat is allowed to cool to room temperature along with the tube furnace.

[0024] 3) Take out the burning boat that has been cooled to room temperature in step 2) and perform post-plating treatment. First, clean the sample with a large amount of deionized water to completely remove the salt, then clean it with alcohol, and put it in a drying oven at 50 ℃ for 50 min.

[0025] 4) Grind the dried plating product from step 3), and sieve away excess titanium powder with a 300-mesh sieve and excess nickel powder with a 600-mesh sieve to obtain clean finished diamond particles plated with titanium and nickel.

[0026] 5) The diamond particles obtained in step 4) were characterized. SEM showed that the coating on the surface of the titanium-modified diamond was uniform and dense with no uncoated areas. XRD confirmed that the diamond matrix contained only C, TiC, Ti and NiTi.

[0027] Implementation Case 2: A method for preparing a multi-element metallization coating on a diamond surface, comprising the following steps: 1) First, weigh 6.00 g of salt and stir it evenly in a mortar. Then, weigh 3.00 g of diamond and pour it into the mortar containing salt. Next, weigh 0.60 g of titanium powder and 0.40 g of nickel powder and pour them into the mortar containing salt and diamond. Finally, grind and mix all the materials evenly and put them into a mortar for later use.

[0028] 2) Place the burning boat from step 1) into a tube furnace to perform high-temperature coating treatment on the diamond surface. Argon gas is continuously flowing inside the tube furnace for protection throughout the process. The tube furnace is heated to 800 ℃ at a heating rate of 30 ℃ / min and held at that temperature for 40 min. After that, the burning boat is allowed to cool to room temperature along with the tube furnace.

[0029] 3) Take out the burning boat that has been cooled to room temperature in step 2) and perform post-plating treatment. First, clean the sample with a large amount of deionized water to completely remove the salt, then clean it with alcohol, and put it in a drying oven at 50 ℃ for 50 min.

[0030] 4) Grind the dried plating product from step 3), and sieve away excess titanium powder with a 300-mesh sieve and excess nickel powder with a 600-mesh sieve to obtain clean titanium-nickel plated diamond.

[0031] 5) The diamond particles obtained in step 4) were characterized. SEM showed that the coating on the surface of the titanium-modified diamond was uniform and dense with no uncoated areas. XRD confirmed that the diamond matrix contained only C, TiC, Ti and NiTi.

[0032] Implementation Case 3: A method for preparing a multi-element metallization coating on a diamond surface, comprising the following steps: 1) First, weigh 6.00 g of salt and stir it evenly in a mortar. Then, weigh 3.00 g of diamond and pour it into the mortar containing salt. Next, weigh 0.60 g of titanium powder and 0.40 g of nickel powder and pour them into the mortar containing salt and diamond. Finally, grind and mix all the materials evenly and put them into a mortar for later use.

[0033] 2) Place the burning boat from step 1) into a tube furnace to perform high-temperature coating treatment on the diamond surface. Argon gas is continuously flowing inside the tube furnace for protection throughout the process. The tube furnace is heated to 800 ℃ at a heating rate of 30 ℃ / min and held at that temperature for 60 min. After that, the burning boat is allowed to cool to room temperature along with the tube furnace.

[0034] 3) Take out the burning boat that has been cooled to room temperature in step 2) and perform post-plating treatment. First, clean the sample with a large amount of deionized water to completely remove the salt, then clean it with alcohol, and put it in a drying oven at 50 ℃ for 50 min.

[0035] 4) Grind the dried plating product from step 3), and sieve away excess titanium powder with a 300-mesh sieve and excess nickel powder with a 600-mesh sieve to obtain clean titanium-nickel plated diamond.

[0036] 5) The diamond particles obtained in step 4) were characterized. SEM showed that the coating on the surface of the titanium-modified diamond was uniform and dense with no uncoated areas. XRD confirmed that the diamond matrix contained only C, TiC, Ti and NiTi.

[0037] To demonstrate the effectiveness of the experiment, a comparison was made between salt bath titanium plating and electroless nickel plating. The experiment showed that the present invention is simple to operate, produces a uniform coating, and is safe and pollution-free; while electroless nickel plating is complex, generates pollutants, and is dangerous during the experimental operation.

[0038] The above embodiments illustrate the basic principles and features of the present invention, but are merely preferred embodiments and are not limited to these embodiments. Those skilled in the art, inspired by this patent, can make many modifications and improvements without departing from the spirit and scope of the claims, all of which fall within the scope of protection of the present invention. Therefore, the scope of this patent and its protection should be determined by the appended claims.

Claims

1. A method for preparing a multi-element metallization coating on a diamond surface, characterized in that: Includes the following steps: S1: Weigh the salt, diamond and metal powder according to the calculated mass, grind and mix them evenly for later use. The metal powder includes titanium powder and nickel powder. S2: Transfer the mixed powder to be used in S1 to a sintering boat, then put the sintering boat into a tube furnace, heat it to 600~1000℃, hold it for 20~60min, and obtain the sample through a high-temperature salt bath plating process; S3: The sample obtained in S2 is sequentially cleaned, ultrasonicated, dried and sieved. After sieving, the diamond powder with Ti and Ni multi-element metallized coating is obtained. S4: Performance characterization of multi-element metallized diamond powder products; A composite salt is formed by combining NaCl (50 g / L, purity greater than 99.5%) and KCl (50 g / L, purity greater than 99.5%). The particle size of titanium powder in metal micro powder is 50~80 μm; The particle size of nickel powder in metal micro powder is 5~20 μm; The mass ratios of salt, diamond, and metal powder are respectively, m 盐 :m 金刚石 :m 金属微粉 =6:3:1; the molar ratio of NaCl to KCl is n NaCl :n KCl =2:1; the mass ratio of titanium powder to nickel powder is m Ti :m Ni =6:4; The specific operation process of S4 is as follows: SEM shows that the coating on the diamond surface after multi-element metallization modification is uniform and dense, with no missed areas. XRD confirms that the diamond matrix contains only C, TiC, Ti, and NiTi.

2. The method for preparing a multi-element metallization coating on a diamond surface according to claim 1, characterized in that: The grinding process in S1 is as follows: salt, diamond and metal powder are manually ground in a grinding bowl for 60 minutes.

3. The method for preparing a multi-element metallized coating on a diamond surface according to claim 1, characterized in that: The S2 high-temperature salt bath plating process involves introducing flowing argon gas with a purity greater than 99.99% from the port of the tubular furnace to protect the salt bath plating process throughout.

4. The method for preparing a multi-element metallization coating on a diamond surface according to claim 1, characterized in that: The specific cleaning and ultrasonic processes in S3 are as follows: First, use a large amount of deionized water to clean and desalinate the plated product, and then use alcohol for 30 minutes of ultrasonic cleaning.

5. The method for preparing a multi-element metallized coating on a diamond surface according to claim 1, characterized in that: The drying process in S3 is as follows: drying is carried out in a drying oven at a constant temperature of 50 ℃ for 30~60 min; the sieving process in S3 is as follows: sieving is carried out using 300 mesh and 600 mesh sieves, and the coated product is manually ground for 10 min before sieving.

Citation Information

Patent Citations

  • Diamond particle surface salt bath titanium plating method

    CN109930149A

  • Diamond surface titanium coating nickel coating copper coating composite structure and its manufacturing method

    CN1786274A