A preparation device for tantalum nitride-coated steel material

Abstract

The present invention relates to a preparation device for tantalum nitride coated steel material, which comprises a reaction chamber, an induction heating system, a liquid collecting tank and a gas pumping and injecting system; the reaction chamber includes a reaction tank, a cover plate, a first cap and a second cap, and the reaction tank is made of an insulating material; the cover plate covers the reaction tank and is hermetically connected, and a large round hole is provided on the cover plate; the first cap and the second cap are not used simultaneously, and both the first cap and the second cap can be hermetically connected to the large round hole; an anode connector and a tantalum electrode are provided on the first cap, the anode connector is connected to the tantalum electrode, and the tantalum electrode can extend into the reaction tank; a cathode connector communicating with the inside of the reaction tank is provided on the cover plate or the reaction tank; a trachea is provided on the second cap, and the trachea communicates with the liquid collecting tank through a condenser tube or communicates with the gas pumping and injecting system through a pipeline; the induction heating system is arranged around the outer periphery of the reaction tank. The device of the present invention has low equipment and raw material costs, is simple to operate, and the tantalum nitride film on the surface of the steel material is uniform, complete and of good quality.

Description

Technical Field

[0001] The present invention relates to the technical field of preparation of tantalum nitride film coating materials, and particularly relates to a preparation device for tantalum nitride coated steel materials. Background Art

[0002] Tantalum nitride thin films have high hardness, good chemical stability, strong corrosion resistance, and excellent heat and impact resistance. Because tantalum nitride thin films have excellent physical and chemical properties, they are widely used in semiconductor sputtering deposition processes, ion implantation processes, and dry etching processes as shielding protective films for components inside the equipment cavity and exposed in the reaction zone.

[0003] In the preparation of tantalum nitride films, magnetron sputtering, physical deposition, chemical deposition, and the recently proposed glow discharge method are mainly used. When depositing tantalum nitride films on large equipment workpieces, the above processes have certain defects. When the size of the equipment workpiece is larger, the requirements for the size of the coating equipment are higher, and the cost increases accordingly. At the same time, the more complex the equipment workpiece is, the higher the coating difficulty is. For example, for some workpieces with drilling positions, the coating cannot be completed in one go on the side. Summary of the Invention

[0004] Aiming at the problems existing in the prior art, the purpose of the present invention is to provide a preparation device for tantalum nitride coated steel materials, which has low equipment cost, low coating difficulty, simple operation, can complete coating on complex equipment workpieces in one go, and the tantalum nitride thin film is completely and evenly covered.

[0005] To achieve the above purpose, the technical solution adopted by the present invention is:

[0006] A preparation device for tantalum nitride coated steel materials, which includes a reaction chamber, an induction heating system, a liquid collecting tank, and a gas pumping and injecting system;

[0007] The reaction chamber includes a reaction tank, a cover plate, a first cap, and a second cap. The reaction tank is made of insulating material; the cover plate covers the reaction tank and is sealedly connected. There is a large round hole on the cover plate; the first cap and the second cap are not used simultaneously, and both the first cap and the second cap can be sealedly connected to the large round hole;

[0008] The first cap is provided with an anode connection head and a tantalum electrode. The anode connection head is connected to the tantalum electrode, and the tantalum electrode can extend into the reaction tank; there is a cathode connection head on the cover plate or the reaction tank that can communicate with the inside of the reaction tank;

[0009] The second cap is provided with an air pipe, and the air pipe is connected to the liquid collecting tank through a condenser pipe or connected to the gas pumping and injecting system through a pipeline;

[0010] The induction heating system is arranged around the outer periphery of the reaction tank.

[0011] Preferably, a metal flange is provided at the notch position of the reaction tank, several first bolt holes are provided on the outer edge of the metal flange, and second bolt holes matching the first bolt holes are provided at the corresponding positions of the cover plate.

[0012] Preferably, a first groove is provided along the inner edge of the metal flange, and a first insulating sealing ring is provided in the first groove.

[0013] Preferably, the cathode connector is arranged outside the metal flange.

[0014] Preferably, a second groove is provided along the outer periphery of the large circular hole, several first threaded holes are provided in the second groove, and third bolt holes corresponding to the first threaded holes are provided at the corresponding positions of the first cap and the second cap; a second insulating sealing ring is also provided in the second groove.

[0015] Preferably, an infrared temperature measuring device is further included and arranged outside the reaction tank.

[0016] Preferably, an explosion-proof air release valve is provided on the cover plate.

[0017] Preferably, several quartz supports are provided at the bottom of the reaction tank.

[0018] Preferably, the reaction tank is made of quartz glass.

[0019] Preferably, several metal wires for connecting the steel material and the cathode connector are provided in the reaction tank.

[0020] After adopting the above scheme, in the present invention, the steel material is placed in the reaction tank and immersed in the conductive liquid. The steel material is connected to the negative electrode of the DC power supply through the cathode connector. First, the first cap is installed so that the tantalum electrode is inserted into the conductive liquid, and the tantalum electrode is connected to the positive electrode of the DC power supply. Through the electrochemical reaction, a tantalum plating layer is accumulated and formed on the surface of the steel material. After the plating layer reaches a certain equivalent amount, the second cap is replaced, and the conductive liquid is distilled and volatilized by heating through the induction heating system. The conductive liquid vapor is condensed and recycled for reuse. Then the second cap is connected to the air extraction and gas injection system. First, the air in the reaction chamber is pumped away and then replaced with a nitrogen / ammonia mixed gas. The induction heating system heats the steel material, and the nitrogen / ammonia mixed gas reacts with the tantalum plating layer to form tantalum nitride. Each equipment component of the present invention is easy to process and purchase, and the equipment cost is low. Electrochemical reaction, distillation separation, and heat treatment are carried out on the same equipment, so that the coating cost efficiency is improved. The tantalum nitride-coated steel material prepared by the device of the present invention has a uniform, complete, and high-quality tantalum nitride film coverage. Especially for coating large and complex workpieces, it has great advantages. Description of the Drawings

[0021] Figure 1 It is a schematic diagram of the present invention during the electrochemical reaction.

[0022] Figure 2 This is a schematic diagram during the distillation separation of the present invention.

[0023] Figure 3 This is a schematic diagram during the heat treatment of the present invention.

[0024] Label description:

[0025] Reaction chamber 10, reaction tank 11, metal flange 12, first bolt hole 121, first groove 122, first insulating seal ring 123, cathode connector 124, cover plate 13, second bolt hole 131, second groove 132, first threaded hole 133, explosion-proof relief valve 134, second insulating seal ring 135, first cap 14, third bolt hole 141, anode connector 142, tantalum electrode 143, second cap 15, gas pipe 151, quartz support 16, metal wire 17;

[0026] Induction heating system 20; infrared temperature measuring device 30; condenser 40; liquid collecting tank 50; air extraction and injection system 60; conductive liquid 70; workpiece 80. Specific implementation mode

[0027] As Figures 1 - 3 shown, the present invention discloses a preparation device for tantalum nitride coated steel material, which includes a reaction chamber 10, an induction heating system 20, a liquid collecting tank 50, an infrared temperature measuring device 30, and an air extraction and injection system 60.

[0028] The reaction chamber 10 includes a reaction tank 11, a metal cover plate 13, a first cap 14 and a second cap 15. The reaction tank 11 is made of an insulating material, preferably quartz glass, which has low cost and is convenient for procurement. The cover plate 13 is made of a metal material, which is more convenient for processing.

[0029] A metal flange 12 is provided at the notch position of the reaction tank 11, and the cover plate 13 covers the metal flange 12. Six to twelve first bolt holes 121 are evenly distributed on the outer circumference of the metal flange 12, and second bolt holes 131 matching the first bolt holes 121 are provided at the corresponding positions of the cover plate 13. The cover plate 13 and the metal flange 12 are fixed by screws and nuts. In addition, a first groove 122 is provided on the inner edge of the metal flange 12, and a first insulating seal ring 123 is provided in the first groove 122. The cover plate 13 and the metal flange 12 press the first insulating seal ring 123 to play a sealing role.

[0030] The first cap 14 and the second cap 15 are not used simultaneously. There is a large round hole on the cover plate 13, and both the first cap 14 and the second cap 15 can be hermetically connected to the large round hole. Specifically, there is a second groove 132 on the outer periphery of the large round hole. There are 6 - 12 first threaded holes 133 in the second groove 132. Corresponding third bolt holes 141 are provided at the relative positions of the first cap 14 and the second cap 15. The first cap 14 or the second cap 15 is fixed on the cover plate 13 by screwing into the first threaded hole 133. In addition, a second insulating sealing ring 135 is also provided in the second groove 132 for sealing the gap.

[0031] An anode connector 142 and a tantalum electrode 143 are provided in the middle of the first cap 14, which are sintered from high - purity tantalum powder. The anode connector 142 is connected to the tantalum electrode 143, and the tantalum electrode 143 can extend into the reaction tank 11. A cathode connector 124 that can communicate with the inside of the reaction tank 11 is provided on the cover plate 13 or the reaction tank 11. Preferably, the cathode connector 124 is provided on the outside of the metal flange 12.

[0032] A trachea 151 is provided in the middle of the second cap 15. The trachea 151 is connected to the liquid collection tank 50 through a condenser tube 40 or connected to the air extraction and injection system 60 through a pipeline.

[0033] The induction heating system 20 is arranged around the outer periphery of the reaction tank 11, and the infrared temperature measuring device 30 is also arranged around the reaction tank 11 to detect the heating temperature for easy control. Since there is a large amount of conductive liquid 70 in the reaction tank 11, in order to prevent the reaction tank 11 from bursting due to heating, an explosion - proof relief valve 134 is provided on the cover plate 13.

[0034] The principle of the present invention is as follows:

[0035] Place the steel material workpiece 80 in the reaction tank 11 and lift it by a plurality of quartz supports 16 to facilitate the bottom surface of the workpiece 80 to fully contact the conductive liquid 70. Add the conductive liquid 70 until the workpiece 80 is completely immersed. The conductive liquid 70 is mixed by diethylamine and alkyl bromide. Fix the first cap 14 so that the tantalum electrode 143 is inserted into the conductive liquid 70, and the other end, the anode connector 142, is connected to the positive electrode of the DC power supply. The workpiece 80 is used as the cathode and is connected to the inside of the metal flange 12 by a metal wire 17, and then connected to the negative electrode of the DC power supply through the cathode connector. When an electrochemical reaction occurs through the current, tantalum is released from the anode and tantalum diethylamide accumulates on the surface of the cathode workpiece 80.

[0036] After reaching one equivalent of the electrochemical reaction, the first cap 14 is replaced with the second cap 15, and it is connected to the condenser 40 through the air pipe 151. At the same time, the induction heating system 20 operates to heat the distilled conductive liquid 70. After the conductive vapor is cooled by the condenser 40, it is recovered by the liquid collection tank 50, and the recovered liquid can be reused. When the induction heating system 20 operates, the workpiece 80 becomes a heating body, and a precursor mixture of tantalum diethylamide / tantalum / tantalum nitride is coated on the surface of the workpiece 80.

[0037] Connect the air pipe 151 to the air extraction and injection system 60. First, evacuate the air in the reaction chamber 10 and then replace it with a nitrogen / ammonia mixed gas. Fill the reaction chamber 10 with the nitrogen / ammonia mixed gas, and then the induction heating system 20 performs heat treatment on the workpiece 80 until the precursor reacts into the finally required tantalum nitride. At the same time, during the heat treatment process of the workpiece 80, some carbon atoms in the precursor will penetrate into the material surface, forming a layer of tantalum carbide on the surface. Tantalum carbide, as an intermediate layer between the workpiece 80 and tantalum nitride, can make the attachment of tantalum nitride more stable.

[0038] The key of the present invention is that the reaction chamber 10 is mainly made of steel and quartz glass, with low material price and easy availability, and the processing technology is mature. The induction heating system 20, the air extraction and injection system 60, the infrared thermometer, etc. are all mature and easy-to-purchase products on the market. The simple design greatly reduces the overall manufacturing cost, and the equipment is easy to obtain. The present invention completes three processes of electrochemical reaction, distillation separation and heat treatment on the same equipment, which also improves the coating cost efficiency.

[0039] Precoat the precursor film by an immersion electrochemical method. The production raw materials are easy to obtain, with lower raw material costs and requirements compared to other processes. At the same time, it can effectively coat the film in all directions at one time, with low design requirements for each workpiece 80 and good overall coating wrapping. The conductive liquid 70 is distilled and recycled for reuse, without causing material waste and environmental protection problems. Heat treatment in a nitrogen / ammonia atmosphere makes the precursor fully react into tantalum nitride. At the same time, high-temperature treatment can change the crystal state of tantalum nitride and improve the quality of the tantalum nitride film. During heat treatment, some carbon atoms in the precursor will penetrate into the material surface, forming a buffer layer of tantalum carbide / tantalum nitride between the workpiece 80 and the tantalum nitride film, making the tantalum nitride thin film have better connection adhesion and reducing the probability of the protective film peeling off during later use.

[0040] The device of the present invention has a simple design and low material cost. The raw materials for film making have low costs and do not cause damage to the environment. At the same time, during the heat treatment reaction to form the film, in addition to improving the crystal state of tantalum nitride, a buffer layer is naturally formed, improving the quality and later service life of the tantalum nitride film.

[0041] As described above, it is only an embodiment of the present invention and does not impose any limitation on the technical scope of the present invention. Therefore, any minor modification, equivalent change, and modification made to the above embodiments based on the technical essence of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. A preparation device for tantalum nitride-coated steel material, characterized in that: It includes a reaction chamber, an induction heating system, a liquid collection tank, and a gas pumping and injection system; The reaction chamber includes a reaction tank, a cover plate, a first cap, and a second cap. The reaction tank is made of an insulating material; the cover plate covers the reaction tank and is hermetically connected. There is a large circular hole on the cover plate; the first cap and the second cap are not used simultaneously, and both the first cap and the second cap can be hermetically connected to the large circular hole; The first cap is provided with an anode connector and a tantalum electrode. The anode connector is connected to the tantalum electrode, and the tantalum electrode can extend into the reaction tank; there is a cathode connector on the cover plate or the reaction tank that can communicate with the inside of the reaction tank; The second cap is provided with an air pipe, and the air pipe is connected to the liquid collection tank through a condenser pipe or connected to the gas pumping and injection system through a pipeline; The induction heating system is arranged around the outer periphery of the reaction tank; When the first cap is hermetically connected to the large circular hole on the cover plate, the reaction tank is used to accommodate a steel material workpiece and a conductive liquid, and the steel material workpiece is completely immersed in the conductive liquid; the tantalum electrode on the first cap is inserted into the conductive liquid; The anode connector is connected to the positive electrode of a DC power supply, and the cathode connector is connected to the negative electrode of the DC power supply. An electrochemical reaction occurs through the current, and the tantalum electrode releases tantalum, which accumulates on the surface of the steel material workpiece to form tantalum diethylamide; When the second cap is hermetically connected to the large circular hole on the cover plate and the air pipe of the second cap is connected to the liquid collection tank through a condenser pipe, the induction heating system starts to heat and distill the conductive liquid, and the steel material workpiece is heated to have a precursor mixture of tantalum diethylamide / tantalum / tantalum nitride on its surface; When the second cap is hermetically connected to the large circular hole on the cover plate and the air pipe of the second cap is connected to the gas pumping and injection system through a pipeline, the gas pumping and injection system first evacuates the air in the reaction chamber, then injects a nitrogen / ammonia mixed gas, and the induction heating system starts to perform heat treatment on the steel material workpiece to form tantalum carbide and tantalum nitride on the surface of the steel material, where tantalum carbide serves as an intermediate layer between the steel material workpiece and tantalum nitride; There are several quartz supports at the bottom of the reaction tank; the reaction tank is made of quartz glass.

2. The preparation device of a tantalum nitride-coated steel material according to claim 1, wherein: There is a metal flange at the mouth position of the reaction tank. There are several first bolt holes on the outer edge of the metal flange, and there are second bolt holes matching the first bolt holes at the corresponding position of the cover plate.

3. The preparation device of a tantalum nitride coated steel material according to claim 2, characterized in that: There is a first groove on the inner edge of the metal flange, and a first insulating sealing ring is arranged in the first groove.

4. The manufacturing apparatus of a tantalum nitride coated steel material according to claim 2, wherein: The cathode connector is arranged on the outside of the metal flange.

5. The preparation device of a tantalum nitride-coated steel material according to claim 1, characterized in that: There is a second groove on the outer periphery of the large circular hole, and several first threaded holes are arranged in the second groove. There are third bolt holes corresponding to the first threaded holes at the corresponding positions of the first cap and the second cap; a second insulating sealing ring is also arranged in the second groove.

6. The preparation device of a tantalum nitride coated steel material according to claim 1, characterized in that: It also includes an infrared temperature measuring device arranged outside the reaction tank.

7. The preparation device of a tantalum nitride coated steel material according to claim 1, characterized in that: There is an explosion-proof air release valve on the cover plate.

8. The preparation device of a tantalum nitride-coated steel material according to claim 1, characterized in that: There are several metal wires in the reaction tank for connecting the steel material and the cathode connector.

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