Preparation device and preparation method of titanium-carbon composite powder and titanium-carbon composite powder
By using a combination of a vibrating conveyor, a limiting scraper, an atomizer, a vacuum drying oven, and an argon-protected treatment furnace, titanium-carbon composite powder was prepared, solving the problem of uneven carbon distribution in titanium alloys and improving the quality and performance of the material.
Patent Information
- Application Number
- CN202511809108.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-03
- Publication Date
- 2026-02-27
AI Technical Summary
Existing technologies make it difficult to achieve uniform distribution and controllable addition of carbon in titanium alloys, which leads to the easy agglomeration of titanium carbide, affecting the material's microstructure and properties.
A combination of a vibrating conveyor, a limiting scraper, an atomizer, a vacuum drying oven, and an argon-protected furnace is used to achieve in-situ generation and uniform distribution of carbon on the surface of titanium powder through atomized spraying of tannic acid solution, low-temperature drying, and high-temperature calcination.
It achieves uniform distribution and precise control of carbon elements on the surface of titanium powder, avoids the agglomeration of titanium carbide, improves the quality and performance of composite powder, and is suitable for continuous and batch production.
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Figure CN121571644A_ABST
Abstract
Description
Technical Field
[0001] This disclosure relates to the field of composite powder technology, and more specifically, to an apparatus for preparing titanium-carbon composite powder, a method for preparing titanium-carbon composite powder, and titanium-carbon composite powder. Background Technology
[0002] Titanium alloys are widely used in aerospace, shipbuilding, and biomedical fields due to their excellent specific strength, corrosion resistance, and high-temperature performance.
[0003] In the actual production process of titanium alloys, carbon is often introduced into the titanium alloy by directly mixing graphite powder with other raw materials, followed by pressing and smelting. However, due to the small amount of graphite added and its large density difference with other metal raw materials, it is difficult to achieve uniform distribution of graphite powder in the raw materials during the mixing process. In addition, graphite dust is easily generated during the batching, mixing, and pressing processes, resulting in uncontrolled carbon content and dust pollution.
[0004] To address this issue, related technologies employ mechanical alloying and powder metallurgy to prepare titanium-carbon master alloys, which are then mixed with other raw materials in appropriate proportions to prepare titanium alloys. Mechanical alloying typically involves high-energy ball milling of graphite powder and titanium powder to prepare the titanium-carbon master alloy; powder metallurgy involves mixing titanium powder and carbon powder and then sintering to prepare the titanium-carbon master alloy. However, in both of these methods, when using the titanium-carbon master alloy as a raw material to smelt titanium alloys, titanium carbide is prone to agglomeration, ultimately leading to a deterioration in the material's microstructure and properties. Therefore, achieving controllable addition and uniform distribution of carbon is a fundamental and critical problem that urgently needs to be solved in the manufacturing of high-end titanium alloys. Summary of the Invention
[0005] The purpose of this disclosure is to provide an apparatus for preparing titanium-carbon composite powder, a method for preparing titanium-carbon composite powder, and titanium-carbon composite powder, thereby overcoming, to at least a certain extent, the problem of easy agglomeration of titanium carbide caused by the limitations and defects of related technologies.
[0006] According to one aspect of this disclosure, an apparatus for preparing titanium-carbon composite powder is provided, the apparatus comprising: Vibrating conveyor, on which titanium powder is laid, is used to convey the titanium powder; A limiting scraper, positioned above the vibrating conveyor, is used to control the thickness of the titanium powder spread. The atomizer, located on the upper side of the vibrating conveyor, is used to atomize the tannic acid solution and spray it evenly onto the titanium powder; A vacuum drying oven is used to dry titanium powder with a uniformly sprayed tannic acid solution on its surface at low temperature. An argon-protected furnace, connected to a vacuum drying oven, is used to calcine titanium powder dried at low temperature at high temperature to obtain titanium-carbon composite powder.
[0007] In one exemplary embodiment of this disclosure, the vibration conveyor consists of an electric drive belt and a vibrator.
[0008] In one exemplary embodiment of this disclosure, the vibrator, the limiting scraper, the atomizer, the vacuum drying oven, and the argon-protected treatment furnace are arranged sequentially along the electric conveyor belt in the vibratory conveyor.
[0009] In one exemplary embodiment of this disclosure, the atomizer includes an air compressor, an air tank, an electrical control box, a water circuit, an air circuit, and an atomizing nozzle; the vacuum drying chamber includes a vacuum pump, a motor, blades, an electric heating wire, a thermometer, and a pressure gauge; the argon-protected treatment furnace includes a vacuum pump, an argon storage tank, a heating element, and an electrical control system; the vacuum drying chamber and the argon-protected treatment furnace are connected by a transition chamber.
[0010] According to one aspect of this disclosure, a method for preparing titanium-carbon composite powder is provided. The method utilizes the aforementioned apparatus for preparing titanium-carbon composite powder, and the method includes: Tannic acid is dissolved in water to prepare a tannic acid solution, and the resulting tannic acid solution is placed in the atomizer; Titanium powder is spread on a vibrating conveyor for conveying. The thickness of the titanium powder is controlled by a limiting scraper above the vibrating conveyor. Tannic acid solution is atomized and evenly sprayed onto the titanium powder by an atomizer placed above the vibrating conveyor. Titanium powder with tannic acid solution uniformly sprayed on its surface is sequentially transferred to a vacuum drying oven and an argon-protected furnace for low-temperature drying and high-temperature calcination, respectively, to obtain titanium-carbon composite powder.
[0011] In one exemplary embodiment of this disclosure, the titanium-carbon composite powder comprises carbon, titanium, and impurities, with a carbon mass fraction of 0.1% to 2.0%.
[0012] In one exemplary embodiment of this disclosure, the concentration of the tannic acid solution is 0.1% to 0.5%.
[0013] In one exemplary embodiment of this disclosure, the powder thickness is 0.2~0.5mm, and the conveying speed of the vibrating conveyor is 0.05~0.2m / s.
[0014] In one exemplary embodiment of this disclosure, the first temperature for low-temperature drying is 50°C to 60°C, and the drying time for low-temperature drying is 1.5 to 2 hours; the second temperature for high-temperature calcination is 300°C to 400°C, and the calcination time for high-temperature calcination is 0.5 to 1 hour.
[0015] According to one aspect of this disclosure, a titanium-carbon composite powder is provided, which is prepared according to the above-described titanium-carbon composite powder preparation apparatus.
[0016] In the technical solution provided in this disclosure, on the one hand, the tannic acid solution is uniformly sprayed onto the surface of titanium powder on a vibrating conveyor by an atomizer in the titanium-carbon composite powder preparation device. Through vacuum drying and argon-protected calcination, in-situ generation, uniform distribution, and precise control of carbon content on the titanium powder surface are achieved. Furthermore, by controlling the calcination temperature, the problem of refractory titanium carbide in related technologies is avoided, solving the difficulty of accurate addition and uniform distribution of carbon in existing titanium alloys, thereby improving the quality of the composite powder. On the other hand, the titanium-carbon composite powder preparation device has a simple structure, is suitable for continuous and batch production, and is easy to implement for industrial application.
[0017] It should be understood that the above general description and the following detailed description are exemplary and explanatory only, and are not intended to limit this disclosure. Attached Figure Description
[0018] The accompanying drawings, which are incorporated in and form part of this specification, illustrate embodiments consistent with this disclosure and, together with the description, serve to explain the principles of this disclosure. It is obvious that the drawings described below are merely some embodiments of this disclosure, and those skilled in the art can obtain other drawings based on these drawings without any inventive effort.
[0019] Figure 1 The diagram schematically illustrates the structure of the apparatus for preparing titanium-carbon composite powder in an embodiment of this disclosure.
[0020] Figure 2 The diagram illustrates the specific structure of the apparatus for preparing titanium-carbon composite powder in an embodiment of this disclosure.
[0021] Figure 3 The flowchart illustrating a method for preparing a titanium-carbon composite powder according to an embodiment of the present disclosure is shown.
[0022] Figure 4 The chemical composition analysis results of the titanium-carbon composite powder prepared according to Example 1 are illustrated schematically.
[0023] Figure 5 The image shows a secondary electron scanning electron microscope image of the titanium-carbon composite powder prepared according to Example 1.
[0024] Figure 6 The diagram illustrates the Ti elemental distribution of the titanium-carbon composite powder prepared according to Example 1.
[0025] Figure 7The C elemental distribution of the titanium-carbon composite powder prepared according to Example 1 is shown schematically.
[0026] Figure 8 The XRD pattern of the titanium-carbon composite powder prepared according to Example 1 is shown schematically. Detailed Implementation
[0027] Example embodiments will now be described more fully with reference to the accompanying drawings. However, example embodiments can be implemented in many forms and should not be construed as limited to the examples set forth herein; rather, these embodiments are provided to make this disclosure more comprehensive and complete, and to fully convey the concept of the example embodiments to those skilled in the art. The described features, structures, or characteristics can be combined in any suitable manner in one or more embodiments. In the following description, numerous specific details are provided to give a full understanding of embodiments of this disclosure. However, those skilled in the art will recognize that the technical solutions of this disclosure can be practiced with one or more of the specific details omitted, or other methods, components, apparatus, steps, etc., can be employed. In other instances, well-known technical solutions are not shown or described in detail to avoid obscuring various aspects of this disclosure.
[0028] The terms “a,” “an,” “the,” and “the” are used in this specification to indicate the presence of one or more elements / components, etc.; the terms “including” and “having” are used to indicate an open-ended inclusion and to mean that there may be other elements / components, etc., in addition to those listed; the terms “first” and “second” are used only as markings and are not a limitation on the number of objects.
[0029] Titanium alloys are widely used in aerospace, shipbuilding, and biomedical fields due to their excellent specific strength, corrosion resistance, and high-temperature performance. However, the insufficient strength and wear resistance of pure titanium limit its application in extreme environments. To improve the performance of titanium alloys, carbon, a lightweight and high-strength non-metallic element, is introduced into the titanium matrix to form titanium carbide, which can refine grains, improve mechanical properties, and enhance wear resistance. During the smelting process of titanium alloys, titanium and carbon can form stable titanium carbide particles, which have a high melting point (approximately 3140℃) and high hardness (Vickers hardness approximately 3000 HV), making them an important strengthening phase in titanium alloys. By controlling the carbon content, the size and distribution of titanium carbide particles can be optimized, thereby significantly improving the strength, rigidity, and high-temperature stability of the alloy. In addition, titanium carbide particles can also inhibit grain boundary migration, refine the α / β phase structure, and improve the fatigue performance of titanium alloys. However, in the actual production process of titanium alloys, the method of directly mixing graphite powder with other raw materials, then pressing and smelting, is often used to introduce carbon into the titanium alloy. However, due to the small amount of graphite added and its large density difference with other metal raw materials, it is difficult to achieve a uniform distribution of graphite powder in the raw materials during the powder mixing process. Furthermore, graphite dust is easily generated during batching, mixing, and pressing, leading to uncontrolled carbon content and dust pollution. To solve this problem, researchers have attempted to use mechanical alloying and powder metallurgy to prepare titanium-carbon master alloys, and then mix these master alloys with other raw materials in appropriate proportions to prepare titanium alloys. Mechanical alloying typically involves high-energy ball milling of graphite powder and titanium powder to prepare titanium-carbon master alloys; powder metallurgy involves mixing titanium powder and carbon powder and then sintering to prepare titanium-carbon master alloys. Both methods can achieve uniform distribution and content control of carbon, but the formation of titanium carbide is unavoidable during the preparation of titanium-carbon master alloys. Due to the high melting point of titanium carbide, it easily agglomerates when the titanium-carbon master alloy is used as a raw material to smelt titanium alloys, ultimately causing deterioration of the material's microstructure and properties. Therefore, how to achieve the controllable addition and uniform distribution of carbon is a fundamental and critical issue that urgently needs to be addressed in the manufacturing of high-end titanium alloys.
[0030] To address the aforementioned issues, this disclosure provides an apparatus for preparing titanium-carbon composite powder. This apparatus integrates powder vibration transmission, tannic acid atomization spraying, composite powder precursor preparation, vacuum drying, and high-temperature carbonization under a protective atmosphere into the preparation of titanium-carbon composite powder.
[0031] In this embodiment of the disclosure, in order to achieve efficient and environmentally friendly preparation of titanium-carbon composite powder, a method for preparing titanium-carbon composite powder can be performed based on a titanium-carbon composite powder preparation apparatus. (Reference) Figure 1 As shown, the titanium-carbon composite powder preparation apparatus 100 may include a vibrating conveyor 1, a limiting scraper 2, an atomizer 3, a vacuum drying oven 4, and an argon-protected treatment furnace 6.
[0032] Titanium powder is spread on the vibrating conveyor 1 for conveying the titanium powder. The titanium powder can be spread on the vibrating conveyor for conveying, and the conveying speed of the vibrating conveyor is 0.05~0.2m / s.
[0033] A limiting scraper 2 is positioned above the vibrating conveyor to control the thickness of the titanium powder spread. The limiting scraper can be positioned above the vibrating conveyor, specifically vertically or obliquely, to control the thickness of the titanium powder spread on the vibrating conveyor belt. This spread thickness can be 0.2~0.5mm. For example, the gap between the bottom of the limiting scraper and the surface of the vibrating conveyor belt can be determined so that the titanium powder is flattened as it passes through the gap; the height of the gap is the spread thickness. It should be noted that the position of the limiting scraper can be adjusted according to the required spread thickness, either manually or automatically by the system; no specific limitation is made here.
[0034] Atomizer 3, located on the upper side of the vibrating conveyor, is used to atomize the tannic acid solution and spray it evenly onto the titanium powder. The atomizer can be an atomizing sprayer, which may include multiple atomizing nozzles to achieve uniform spraying of the tannic acid solution onto the titanium powder. The tannic acid solution is prepared by dissolving tannic acid in water, and its concentration is 0.1%~0.5%. By controlling the concentration of the tannic acid solution, excessively high local concentrations of tannic acid molecules on the surface of the titanium powder can be avoided, thereby ensuring effective carbonization of the tannic acid molecules after calcination, while simultaneously suppressing the phenomenon of an excessively thick carbon layer on the surface of the titanium powder after calcination.
[0035] Vacuum drying oven 4 is used to dry titanium powder with a tannic acid solution uniformly sprayed on its surface at a low temperature. Exemplarily, the first temperature for low-temperature drying is 50°C to 60°C, and the drying time is 1.5 to 2 hours. Low-temperature drying yields dried titanium powder.
[0036] Argon-protected furnace 6, connected to a vacuum drying oven, is used to calcine titanium powder dried at low temperature at high temperature to obtain titanium-carbon composite powder. The titanium powder dried in the vacuum drying oven can be transferred to the argon-protected furnace for high-temperature calcination. The second high-temperature calcination temperature is 300℃~400℃, and the calcination time is 0.5~1h. The prepared titanium-carbon composite powder consists of carbon, titanium, and impurities, with a carbon content of 0.1%~2.0%.
[0037] By controlling the low-temperature drying in a vacuum drying oven at 50℃~60℃ and the drying time at 1.5~2h, the moisture in the tannic acid solution is completely removed, avoiding an increase in the hydrogen and oxygen content in the composite powder. By controlling the high-temperature calcination in an argon-protected furnace at 300℃~400℃ and the calcination time at 0.5~1h, the tannic acid molecules are fully carbonized. Furthermore, controlling the calcination temperature not to exceed 400℃ effectively prevents the reaction between titanium and carbon to produce refractory titanium carbide.
[0038] In this embodiment of the invention, the titanium-carbon composite powder preparation device uniformly sprays tannic acid solution onto the surface of titanium powder, and achieves in-situ generation, uniform distribution and precise control of carbon content on the surface of titanium powder through vacuum drying and argon-protected calcination. Furthermore, by controlling the calcination temperature, the problem of refractory titanium carbide that cannot be avoided in the prior art is avoided.
[0039] refer to Figure 2 As shown, the preparation apparatus for titanium-carbon composite powder includes a vibrating conveyor, a limiting scraper, an atomizer, a vacuum drying oven, and an argon-protected treatment furnace. Specifically, the apparatus includes a vibrating conveyor 1, a limiting scraper 2, an atomizer 3, a vacuum drying oven 4, and an argon-protected treatment furnace 6. Exemplarily, the vibrating conveyor 1 consists of an electric drive belt 11 connected to a vibrator 12, enabling vibration transmission. The limiting scraper 2 allows for powder thickness control. The atomizer 3 comprises an air compressor 31, an air tank 32, an electrical control box 33, a water path 34, an air path 35, and an atomizing nozzle 36, enabling uniform spraying of tannic acid solution onto the titanium powder. The vacuum drying oven 4 comprises a vacuum pump 41, a motor 42, blades 43, an electric heating wire 44, a thermometer 45, and a pressure gauge 46, enabling moisture removal. The argon-protected treatment furnace 6 consists of a vacuum pump 61, an argon storage tank 62, a heating element 63, and an electrical control system 64, enabling the pyrolysis of tannic acid into carbon under a protective atmosphere. A transition chamber 5 connects the vacuum drying oven 4 to the argon-protected treatment furnace 6. The vibrator 12, limiting scraper 2, atomizer 3, vacuum drying oven 4, and argon-protected treatment furnace 6 are arranged sequentially along the electric conveyor belt 11, enabling continuous and batch production of titanium-carbon composite powder. Depending on different process requirements, this titanium-carbon composite powder preparation device can be used for the pyrolysis of tannic acid or other organic substances to produce carbon, as well as for the synthesis of metal-carbon composite powders with titanium powder or other metal powders.
[0040] In some embodiments, reference Figure 2 As shown, the vibrating conveyor 1 serves as a conveying device for titanium powder. Vibration causes the titanium powder to move along a predetermined path, achieving continuous transport of the titanium powder. An electric drive belt 11 provides power to the vibrating conveyor, driving its vibration to transport the titanium powder. A vibrator 12 assists in enhancing the vibration effect of the vibrating conveyor, ensuring that the tannic acid solution is uniformly adhered to the surface of the titanium powder, while simultaneously enabling the titanium powder to be transported smoothly and uniformly.
[0041] The limiting scraper 2 is used to limit the position of titanium powder on the vibrating conveyor, so as to achieve precise control of the powder thickness.
[0042] The atomizer 3 can be an atomizing sprayer used to atomize the conveyed titanium powder. Exemplarily, an air compressor 31 provides compressed air to power the atomization process. An air tank 32 stores compressed air to ensure the stability of the air supply from the air compressor. An electrical control box 33 controls the atomization parameters of the atomizer 3, such as atomization time and atomization flow rate. A water path 34 delivers the liquid medium for atomization. An air path 35 delivers compressed air, which works in conjunction with the water path to achieve liquid atomization. An atomizing nozzle 36 mixes the liquid and compressed air to form atomized particles and sprays them onto the titanium powder.
[0043] The vacuum drying oven 4 dries the atomized titanium powder in a vacuum environment, improving drying efficiency and preventing oxidation. A vacuum pump 41 extracts air from the drying oven to create a vacuum environment. A motor 42 powers the blades within the drying oven. The blades 43 stir the titanium powder during drying, ensuring uniform heating and accelerating the drying process. An electric heating wire 44 provides a heat source to the drying oven, causing the moisture in the titanium powder to evaporate. A temperature gauge 45 monitors the temperature inside the drying oven to ensure it remains within a suitable range. A pressure gauge 46 monitors the vacuum level inside the drying oven to ensure a stable vacuum environment.
[0044] The transition chamber 5 is used to connect the vacuum drying oven and the argon protection furnace, serving as a buffer and transition, allowing the titanium powder to smoothly enter the subsequent argon protection process from the drying stage, while preventing air from entering the argon protection furnace and disrupting its protective atmosphere.
[0045] The argon-protected treatment furnace 6 is used to process titanium powder in an inert environment protected by argon gas, preventing the titanium powder from reacting with oxygen in the air. A vacuum pump 61 evacuates air from the furnace before introducing argon gas, creating the conditions for argon protection. An argon storage tank 62 stores argon gas and provides the inert protective gas to the furnace. A heating element 63 provides a heat source to the furnace for heating treatment. An electrical control system 64 controls parameters such as temperature, argon flow rate, and treatment time within the argon-protected treatment furnace 6 to ensure the accuracy of the treatment process.
[0046] In this embodiment, tannic acid solution is uniformly sprayed onto the surface of titanium powder on a vibrating conveyor using an atomizer. Through vacuum drying and argon-protected calcination, the in-situ generation, uniform distribution, and precise control of carbon content on the surface of titanium powder are achieved. Furthermore, by controlling the calcination temperature, the problem of refractory titanium carbide in related technologies is avoided, and the problem of accurate addition and uniform distribution of carbon in existing titanium alloys is solved, thereby improving the quality of the composite powder.
[0047] In the aforementioned titanium-carbon composite powder preparation apparatus, titanium powder is conveyed by a vibrating conveyor, limited by a limiting scraper, and then atomized by an atomizer using a tannic acid solution. The treated titanium powder then enters a vacuum dryer for drying. The dried titanium powder is then transferred through a transition chamber into an argon-protected treatment furnace for final processing under argon protection. The equipment in each stage works collaboratively through an electrical control system to achieve continuous and automated processing of the titanium powder.
[0048] In this titanium-carbon composite powder preparation device, a vibrating conveyor and a limiting scraper are combined. The vibrating conveyor not only performs the basic function of conveying titanium powder, but its unique vibration action also keeps the titanium powder in a continuous micro-tumbling state during the conveying process, effectively breaking the tendency of powder to agglomerate when stationary, and creating a dynamic and loose powder bed for subsequent uniform coating. The limiting scraper, working in tandem with the conveyor, ensures, through precise control of the powder thickness (0.2-0.5 mm), that the powder bed has a uniform and extremely thin cross-section from a physical structure perspective. This uniformity is the basis for the uniform penetration and adhesion of the subsequent atomized tannic acid solution, avoiding localized solution enrichment or loss due to uneven thickness.
[0049] The combined functions of the two components—the limiting scraper, which creates the ideal static powder geometry, and the vibrating conveyor, which imparts dynamic activation properties to the powder—solve the industry problem of uneven carbon source distribution in traditional powder mixing processes. This lays a crucial technological foundation for achieving in-situ generation and nanoscale uniform coating of carbon elements on the surface of titanium powder, and enables continuous, batch production of high-quality titanium-carbon composite powder. The preparation device for this titanium-carbon composite powder is simple in structure, highly reliable, safe, environmentally friendly, and easy to operate. It is suitable for continuous, batch production and readily applicable to industrial applications.
[0050] Figure 3 The flowchart of a method for preparing titanium-carbon composite powder is illustrated in the figure. Figure 3 As shown, the preparation method mainly includes the following steps: In step S310, tannic acid is dissolved in water to prepare a tannic acid solution, and the obtained tannic acid solution is placed in an atomizer; In step S320, titanium powder is spread on a vibrating conveyor for conveying. The thickness of the titanium powder is controlled by the limiting scraper above the vibrating conveyor. The tannic acid solution is atomized and evenly sprayed onto the titanium powder by an atomizer placed above the vibrating conveyor. In step S330, titanium powder with tannic acid solution uniformly sprayed on its surface is sequentially transferred to a vacuum drying oven and an argon-protected furnace for low-temperature drying and high-temperature calcination treatment, respectively, to obtain titanium-carbon composite powder.
[0051] Next, the preparation method of titanium-carbon composite powder in the embodiments of this disclosure will be described in detail with reference to the accompanying drawings.
[0052] Step S310: Dissolve tannic acid in water to prepare a tannic acid solution, and place the obtained tannic acid solution in an atomizer.
[0053] In this embodiment, the tannic acid solution prepared by dissolving tannic acid in water has a concentration of 0.1% to 0.5%. By controlling the concentration of the tannic acid solution, excessively high local concentrations of tannic acid molecules on the surface of titanium powder can be avoided, thereby ensuring effective carbonization of tannic acid molecules after calcination and suppressing the phenomenon of excessively thick carbon layer on the surface of titanium powder after calcination.
[0054] After obtaining the tannic acid solution, it can be placed in an atomizer. The atomizer can be an atomizing sprayer, which may include multiple atomizing nozzles to achieve uniform spraying of the tannic acid solution onto the titanium powder.
[0055] In step S320, titanium powder is spread on a vibrating conveyor for conveying. The thickness of the titanium powder is controlled by a limiting scraper above the vibrating conveyor. Tannic acid solution is atomized and evenly sprayed onto the titanium powder by an atomizer placed above the vibrating conveyor.
[0056] In this embodiment, titanium powder can be spread on a vibrating conveyor for conveying, and the conveying speed of the vibrating conveyor is 0.05~0.2m / s. During the conveying process, the thickness of the titanium powder is controlled by a limiting scraper set above the vibrating conveyor, and the tannic acid solution is atomized and evenly sprayed onto the titanium powder by an atomizer placed above the vibrating conveyor.
[0057] Furthermore, the tannic acid solution in the atomizer can be atomized and uniformly sprayed onto the titanium powder using an atomizer installed above the vibrating conveyor. In this embodiment, the tannic acid solution is uniformly sprayed onto the surface of the titanium powder, and by adjusting the powder thickness and the conveying speed of the vibrating conveyor, the uniform distribution of the tannic acid solution on the surface of the titanium powder and the control of the tannic acid loading can be achieved. By atomizing a tannic acid solution of a specific concentration using an atomizer, and by adjusting the conveying speed of the vibrating conveyor to control the titanium powder conveying, the content of tannic acid molecules uniformly loaded on the surface of the titanium powder can be controlled. In this embodiment, by controlling the powder thickness and the conveying speed of the vibrating conveyor, the uniform loading of tannic acid molecules on the surface of the titanium powder can be achieved, thereby ensuring the uniform distribution of the carbon layer on the surface of the titanium powder after calcination.
[0058] In step S330, titanium powder with tannic acid solution uniformly sprayed on its surface is sequentially transferred to a vacuum drying oven and an argon-protected furnace for low-temperature drying and high-temperature calcination, respectively, to obtain titanium-carbon composite powder.
[0059] In this embodiment, after obtaining titanium powder with a uniformly coated surface of tannic acid solution, the titanium powder with the uniformly coated surface of tannic acid solution can be transferred to a vacuum drying oven for low-temperature drying to obtain dried titanium powder. Exemplarily, the first temperature for low-temperature drying is 50°C to 60°C, and the drying time is 1.5 to 2 hours. Further, the dried titanium powder can be transferred to an argon-protected furnace for high-temperature calcination. The second temperature for high-temperature calcination is 300°C to 400°C, and the calcination time is 0.5 to 1 hour. The prepared titanium-carbon composite powder comprises carbon, titanium, and impurities, wherein the carbon content is 0.1% to 2.0%.
[0060] By controlling the low-temperature drying in a vacuum drying oven at 50℃~60℃ and the drying time at 1.5~2h, the moisture in the tannic acid solution is completely removed, avoiding an increase in the hydrogen and oxygen content in the composite powder. By controlling the high-temperature calcination in an argon-protected furnace at 300℃~400℃ and the calcination time at 0.5~1h, the tannic acid molecules are fully carbonized. Furthermore, controlling the calcination temperature not to exceed 400℃ effectively prevents the reaction between titanium and carbon to produce refractory titanium carbide.
[0061] In this embodiment of the disclosure, by uniformly spraying tannic acid solution onto the surface of titanium powder, and then drying it under vacuum and calcining it under argon protection, the in-situ generation, uniform distribution, and precise control of carbon content on the surface of titanium powder are achieved. Furthermore, by controlling the calcination temperature, the problem of unavoidable refractory titanium carbide in related technologies is avoided.
[0062] The method for preparing titanium-carbon composite powder in this embodiment includes processes such as powder vibration transmission, tannic acid atomization spraying, composite powder precursor preparation, vacuum drying, and high-temperature carbonization under a protective atmosphere. Tannic acid solution is uniformly sprayed onto the surface of titanium powder. By adjusting the powder thickness and transmission speed of the vibrating conveyor, the uniform distribution of the tannic acid solution on the titanium powder surface and the control of the tannic acid loading can be achieved. Subsequently, the titanium powder with the tannic acid solution loaded on its surface is vacuum dried to fully remove the moisture from the tannic acid solution. Finally, high-temperature calcination under a nitrogen atmosphere achieves effective carbonization of the tannic acid molecules. In the preparation process of the titanium-carbon composite powder, in-situ generation, uniform distribution, and precise control of carbon content on the titanium powder surface are achieved. Because the carbon is generated in situ, a strong bond between carbon and titanium powder is achieved, while avoiding the formation of titanium carbide. This solves the problem of accurate addition and uniform distribution of carbon in titanium alloys, improving the material's microstructure and properties. The preparation device for titanium-carbon composite powder has a simple structure, and the preparation method for titanium-carbon composite powder is highly reliable, safe, environmentally friendly, and easy to operate. It is suitable for continuous and batch production and is easy to implement in industrial applications.
[0063] Next, the preparation method of titanium-carbon composite powder will be described in detail with reference to the embodiments.
[0064] Example 1
[0065] In this embodiment, the mass fraction of carbon in the titanium-carbon composite powder is 0.35%, with the remainder being titanium and other unavoidable impurities.
[0066] The preparation method of titanium-carbon composite powder includes the following steps: Step 1: Dissolve tannic acid in water to prepare a tannic acid solution with a mass concentration of 0.2%, and place the obtained tannic acid solution in an atomizer; Step 2: Spread titanium powder on a vibrating conveyor for conveying. Use the limiting scraper above the vibrating conveyor to control the thickness of the titanium powder to 0.3mm. Use an atomizer placed above the vibrating conveyor to atomize the tannic acid solution and spray it evenly onto the titanium powder. Set the conveying speed of the vibrating conveyor to 0.1m / s. Step 3: The titanium powder with tannic acid solution uniformly sprayed on its surface is transferred to a vacuum drying oven for low-temperature drying at 55°C for 2 hours. Then, the dried titanium powder is transferred to an argon-protected furnace for high-temperature calcination at 350°C for 1 hour to obtain titanium-carbon composite powder with a carbon content of 0.35%.
[0067] The chemical composition of the titanium-carbon composite powder prepared in Example 1 was analyzed, and the results are as follows: Figure 4 As shown. Figure 4 The test results showed that the titanium-carbon composite powder prepared according to Example 1 can achieve precise control of carbon content. The titanium-carbon composite powder prepared in Example 1 was subjected to secondary electron scanning and elemental analysis using scanning electron microscopy, such as... Figure 5 As shown. By Figure 5 It can be seen that the titanium-carbon composite powder retains the original morphology of the titanium powder. For example... Figure 6 Ti element distribution map and Figure 7 As shown in the carbon element distribution diagram, the titanium and carbon elements are evenly distributed with a high degree of overlap, and the carbon element is evenly distributed, indicating that the carbon element obtained by using tannic acid as a carbon source is evenly distributed on the surface of the titanium powder. Figure 8 The XRD pattern of the titanium-carbon composite powder prepared in Example 1 shows only the characteristic peaks of α-Ti and not the characteristic peaks of TiC. This result indicates that the preparation of titanium-carbon composite powder using the method disclosed herein avoids the formation of refractory titanium carbide.
[0068] Example 2
[0069] In this embodiment, the mass fraction of carbon in the titanium-carbon composite powder is 0.1%, with the remainder being titanium and other unavoidable impurities.
[0070] The preparation method of titanium-carbon composite powder includes the following steps: Step 1: Dissolve tannic acid in water to prepare a tannic acid solution with a mass concentration of 0.1%, and place the obtained tannic acid solution in an atomizer; Step 2: Spread titanium powder on a vibrating conveyor for conveying. Use the limiting scraper above the vibrating conveyor to control the thickness of the titanium powder to 0.2mm. Use an atomizer placed above the vibrating conveyor to atomize the tannic acid solution and spray it evenly on the titanium powder. Set the conveying speed of the vibrating conveyor to 0.05m / s. Step 3: The titanium powder with tannic acid solution uniformly sprayed on its surface is transferred to a vacuum drying oven for low-temperature drying at 50°C for 1.5 hours to obtain dried titanium powder. The dried titanium powder is then transferred to an argon-protected furnace for high-temperature calcination at 300°C for 0.5 hours to obtain titanium-carbon composite powder with a carbon content of 0.1% by mass.
[0071] Example 3
[0072] In this embodiment, the mass fraction of carbon in the titanium-carbon composite powder is 2.0%, with the remainder being titanium and other unavoidable impurities.
[0073] The preparation method of titanium-carbon composite powder includes the following steps: Step 1: Dissolve tannic acid in water to prepare a tannic acid solution with a mass concentration of 0.5%, and place the obtained tannic acid solution in an atomizer; Step 2: Spread titanium powder on a vibrating conveyor for conveying. Use the limiting scraper above the vibrating conveyor to control the thickness of the titanium powder to 0.5mm. Use an atomizer placed above the vibrating conveyor to atomize the tannic acid solution and spray it evenly onto the titanium powder. Set the conveying speed of the vibrating conveyor to 0.2m / s. Step 3: The titanium powder with tannic acid solution uniformly sprayed on its surface is transferred to a vacuum drying oven for low-temperature drying at 60°C for 2 hours to obtain dried titanium powder. Further, the dried titanium powder is transferred to an argon-protected furnace for high-temperature calcination at 400°C for 1 hour to obtain titanium-carbon composite powder with a carbon content of 2.0% by mass.
[0074] In this embodiment, tannic acid solution is uniformly sprayed onto the surface of titanium powder using an atomizer. Through vacuum drying and argon-protected calcination, the in-situ generation, uniform distribution, and precise control of carbon content on the surface of titanium powder are achieved. Furthermore, by controlling the calcination temperature, the problem of refractory titanium carbide that cannot be avoided in related technologies is avoided.
[0075] In this embodiment, a titanium-carbon composite powder is also provided, which is prepared according to the above-described method for preparing titanium-carbon composite powder. This titanium-carbon composite powder has a controllable carbon content.
[0076] Furthermore, the above figures are merely illustrative of the processes included in the method according to exemplary embodiments of this disclosure and are not intended to be limiting. It is readily understood that the processes shown in the above figures do not indicate or limit the temporal order of these processes. Additionally, it is readily understood that these processes may be executed synchronously or asynchronously, for example, in multiple modules.
[0077] Other embodiments of this disclosure will readily occur to those skilled in the art upon consideration of the specification and practice of the invention disclosed herein. This application is intended to cover any variations, uses, or adaptations of this disclosure that follow the general principles of this disclosure and include common knowledge or customary techniques in the art not disclosed herein. The specification and examples are to be considered exemplary only, and the true scope and spirit of this disclosure are indicated by the appended claims.
[0078] It should be understood that this disclosure is not limited to the precise structures described above and shown in the accompanying drawings, and various modifications and changes can be made without departing from its scope. The scope of this disclosure is limited only by the appended claims.
Claims
1. An apparatus for preparing titanium-carbon composite powder, characterized in that, An apparatus for preparing titanium-carbon composite powder includes: A vibrating conveyor, wherein titanium powder is spread on the vibrating conveyor for conveying the titanium powder; A limiting scraper is positioned above the vibrating conveyor to control the thickness of the titanium powder layer. An atomizer, located on the upper side of the vibrating conveyor, is used to atomize the tannic acid solution and spray it evenly onto the titanium powder; A vacuum drying oven is used to dry titanium powder with a uniformly sprayed tannic acid solution on its surface at low temperature. An argon-protected furnace, connected to the vacuum drying oven, is used to calcine titanium powder dried at low temperature at high temperature to obtain titanium-carbon composite powder.
2. The apparatus for preparing titanium-carbon composite powder according to claim 1, characterized in that, The vibration conveyor consists of an electric drive belt and a vibrator.
3. The apparatus for preparing titanium-carbon composite powder according to claim 2, characterized in that, The vibrator, limiting scraper, atomizer, vacuum drying oven, and argon-protected treatment furnace are arranged sequentially along the electric conveyor belt in the vibratory conveyor.
4. The apparatus for preparing titanium-carbon composite powder according to claim 3, characterized in that, The atomizer includes an air compressor, a gas storage tank, an electrical control box, a water circuit, a gas circuit, and an atomizing nozzle; the vacuum drying chamber includes a vacuum pump, a motor, blades, an electric heating wire, a thermometer, and a pressure gauge; the argon protection furnace includes a vacuum pump, an argon storage tank, a heating element, and an electrical control system; the vacuum drying chamber and the argon protection furnace are connected by a transition chamber.
5. A method for preparing titanium-carbon composite powder, characterized in that, The method for preparing the titanium-carbon composite powder utilizes the titanium-carbon composite powder preparation apparatus according to any one of claims 1-4, and the method for preparing the titanium-carbon composite powder includes: Tannic acid is dissolved in water to prepare a tannic acid solution, and the resulting tannic acid solution is placed in an atomizer; Titanium powder is spread on a vibrating conveyor for conveying. The thickness of the titanium powder is controlled by a limiting scraper above the vibrating conveyor. The tannic acid solution is atomized and evenly sprayed onto the titanium powder by an atomizer placed above the vibrating conveyor. Titanium powder with tannic acid solution uniformly sprayed on its surface is sequentially transferred to a vacuum drying oven and an argon-protected furnace for low-temperature drying and high-temperature calcination, respectively, to obtain titanium-carbon composite powder.
6. The method according to claim 5, characterized in that, The titanium-carbon composite powder comprises carbon, titanium, and impurities, wherein the mass fraction of carbon is 0.1% to 2.0%.
7. The method according to claim 5, characterized in that, The concentration of the tannic acid solution is 0.1% to 0.5%.
8. The method according to claim 5, characterized in that, The powder coating thickness is 0.2~0.5mm, and the conveying speed of the vibrating conveyor is 0.05~0.2m / s.
9. The method according to claim 5, characterized in that, The first temperature for low-temperature drying is 50℃~60℃, and the drying time is 1.5~2h; the second temperature for high-temperature calcination is 300℃~400℃, and the calcination time is 0.5~1h.
10. A titanium-carbon composite powder, characterized in that, The titanium-carbon composite powder is prepared by the titanium-carbon composite powder preparation apparatus according to any one of claims 1-4.