Preparation process of high-performance titanium powder material

Abstract

The invention relates to the technical field of powder metallurgy, and discloses a preparation process of a high-performance titanium powder material. 5-10 parts of titanium dioxide; 10-14 parts of titanium hydride powder; 2-5 parts of waste aluminum powder; 0.5 to 1.5 parts of scrap iron; 0.2 to 0.5 part of vanadium powder; 2-3 parts of a nodulizing agent; 1-2 parts of a surface treating agent; 3-7 parts of a reducing agent; by combining the raw material formula with the preparation process, the high-performance titanium powder material which is high in sphericity degree, good in flowability, low in oxygen content, excellent in mechanical property and uniform in particle size distribution can be prepared, and by optimizing the raw material combination and the process flow, recycling of 100% of waste powder is facilitated, resource waste and carbon emission are reduced, and the method is suitable for industrial production. And the preparation process is innovatively optimized on the steps of raw material pretreatment, spheroidizing treatment, surface treatment and reduction treatment, so that the prepared titanium powder material has the advantages of high purity, high sphericity degree, uniform particle size, low cost and green circulation.

Description

Technical Field

[0001] The present invention relates to the technical field of powder metallurgy, and specifically to a preparation process for a high-performance titanium powder material. Background Art

[0002] Due to its excellent properties, titanium metal plays an irreplaceable role in key fields such as aerospace, national defense, and marine engineering. However, titanium ore resources are not inexhaustible. With the rapid development of various industries, the demand for titanium continues to climb, and the pressure of resource consumption is increasing continuously. Against this background, the rise of the industry of recycling waste titanium to prepare 3D printing powder provides the possibility to build a "secondary life" channel for titanium resources. This industry not only helps to alleviate the shortage of titanium resources but also can become a powerful booster for local economic growth. For regions dominated by traditional industries, its implementation and development can drive the transformation and upgrading of surrounding traditional industries. For example, mechanical processing enterprises can turn to produce equipment parts for adaptation, electronic enterprises can participate in the research and development of automation control modules, and chemical enterprises can assist in the raw material purification process. Therefore, there is an urgent need to develop a green, low-cost, and recyclable alloy powder. Summary of the Invention

[0003] (1) Technical Problems to be Solved

[0004] Aiming at the deficiencies of the prior art, the present invention provides a preparation process for a high-performance titanium powder material, which has the advantages of high purity, high sphericity, uniform particle size, low cost, and green recycling, and solves the problems of low waste titanium recycling efficiency, incomplete impurity removal, unstable powder properties, high production cost, and difficulty in meeting the needs of high-end manufacturing.

[0005] (2) Technical Solutions

[0006] To achieve the above object, the present invention provides the following technical solutions: A preparation process for a high-performance titanium powder material, comprising the following steps:

[0007] Step 1: Prepare raw materials: Prepare waste titanium chips, titanium dioxide, titanium hydride powder, waste aluminum powder, waste iron chips, vanadium powder, spheroidizing agent, surface treatment agent, reducing agent, and auxiliary additive in parts by weight of the formula;

[0008] Step 2: Pretreat the raw materials: Pretreat the waste titanium chips, titanium dioxide, waste aluminum powder, waste iron chips, and titanium hydride powder.

[0009] Step 3: Mixing: Mix the pretreated waste titanium chips, titanium dioxide, titanium hydride powder, waste aluminum powder, and waste iron chips evenly according to the formula ratio, then add vanadium powder and auxiliary additive in the formula ratio, and after mixing evenly, obtain a mixed powder;

[0010] Step 4. Spheroidization treatment: Put the mixed powder and spheroidizing agent into a spheroidization device, and adopt plasma spheroidization technology to control the temperature, time and pressure to make the powder form spherical particles;

[0011] Step 5. Surface treatment: Chemically treat the spheroidized powder with a surface treatment agent, then wash the titanium powder with deionized water, and finally dry the powder until the moisture content is lower than 0.1%;

[0012] Step 6. Reduction treatment: Add a reducing agent to the dried powder, introduce nitrogen, and carry out reduction treatment under high temperature conditions. Finally, detect the purity of the mixed powder by spectral analysis method;

[0013] Step 7. Particle size classification and screening: Use a multi-stage vibrating screening device to classify the particle size of the mixed powder to obtain titanium powder materials;

[0014] Step 8. Quality inspection: Conduct quality inspections on the prepared titanium powder materials for sphericity, fluidity, oxygen content and mechanical properties;

[0015] Step 9. Packaging and labeling: Package the qualified titanium powder after inspection;

[0016] Step 10. Recycling and reuse: Establish a recycling system to recycle the waste and residues generated during the production process, and reintroduce the recycled waste into the pretreatment process for crushing, screening and reaction process treatment.

[0017] Preferably, the raw materials and their weight fraction ranges are: 65-70 parts of waste titanium chips; 5-10 parts of titanium dioxide; 10-14 parts of titanium hydride powder; 2-5 parts of waste aluminum powder; 0.5-1.5 parts of waste iron chips; 0.2-0.5 parts of vanadium powder; 2-3 parts of spheroidizing agent; 1-2 parts of surface treatment agent; 3-7 parts of reducing agent; 2-4 parts of auxiliary additive.

[0018] Preferably, the raw materials and their weight fractions are: 66 parts of waste titanium chips; 8 parts of titanium dioxide; 11 parts of titanium hydride powder; 3 parts of waste aluminum powder; 1.1 parts of waste iron chips; 0.25 parts of vanadium powder; 2.5 parts of spheroidizing agent; 2 parts of surface treatment agent; 6 parts of reducing agent; 3 parts of auxiliary additive.

[0019] Preferably, the raw materials and their weight fractions are: 70 parts of waste titanium chips; 5 parts of titanium dioxide; 14 parts of titanium hydride powder; 5 parts of waste aluminum powder; 0.5 parts of waste iron chips; 0.5 parts of vanadium powder; 3 parts of spheroidizing agent; 1 part of surface treatment agent; 7 parts of reducing agent; 2 parts of auxiliary additive.

[0020] Preferably, the waste titanium chips and waste iron chips are respectively subjected to magnetic separation with a magnetic field strength ≥ 1.2 T, pickled in a HNO3 solution with a concentration of 5% - 10% for 10 - 15 min, rinsed with deionized water 3 - 5 times, and finally baked at a temperature of 105 - 110 °C for 30 - 50 min.

[0021] Preferably, the pretreatment process of the waste aluminum powder: Use screening equipment to remove large particle impurities in the waste aluminum powder, soak the waste aluminum powder in an HCl acidic solution with a concentration of 5.0% - 5.5% for 15 - 30 min, rinse with deionized water 3 - 5 times, put the rinsed waste aluminum powder into a drying oven, and dry it at a temperature of 95 - 105 °C for 30 - 60 min.

[0022] Preferably, the pretreatment process of the titanium dioxide: Activate the titanium dioxide, introduce argon in a fluidized bed, and calcine it at a temperature of 550 - 600 °C for 1.5 - 2 h.

[0023] Preferably, the pretreatment process of the titanium hydride powder: Subject the titanium hydride powder to dehydrogenation treatment, and heat it to 350 - 400 °C in a vacuum environment with a vacuum degree ≤ 10 -2 Pa.

[0024] Preferably, the spheroidization temperature in step four is controlled between 1450 - 1500 °C, and the time is controlled between 1 - 1.2 h.

[0025] Preferably, the reduction treatment in step five: Place the dried powder at a high temperature of 800 - 950 °C, add a reducing agent, perform a reduction treatment on the mixed powder for 30 - 50 min, and simultaneously introduce nitrogen with a purity greater than 99.99%.

[0026] Compared with the prior art, the present invention provides a preparation process for a high-performance titanium powder material, having the following beneficial effects:

[0027] 1. The present invention realizes the preparation of a titanium powder material with high sphericity, good fluidity, low oxygen content, excellent mechanical properties and uniform particle size distribution through an optimized raw material formula and process flow. This innovative process can not only improve the quality of the titanium powder material, but also achieve 100% recycling of waste powder, thereby reducing resource waste and carbon emissions, and further reducing production costs, bringing economic and social benefits. In the raw material pretreatment link, the magnetic separation and pickling treatments performed on the waste titanium chips and waste iron chips by the present invention can effectively remove surface impurities and ferromagnetic impurities. At the same time, the titanium dioxide is activated to eliminate hydroxyl adsorption, and the titanium hydride powder is dehydrogenated to avoid subsequent pore problems. The above pretreatment steps lay a solid foundation for the subsequent spheroidization treatment.

[0028] 2. By adopting the plasma spheroidization technology, the present invention precisely controls the temperature and time to make the mixed powder form uniform spherical particles. This treatment method can not only improve the sphericity but also enhance the fluidity of the powder, making it more suitable for additive manufacturing. In the surface treatment step, the present invention uses silane coupling agent or zinc stearate as the surface treatment agent to chemically treat the spheroidized powder, further improving the fluidity and spheroidization performance of the powder. This step can enhance the overall performance of the titanium powder material. In the reduction treatment link, the present invention introduces high-purity nitrogen at high temperature to conduct vacuum reduction treatment on the dried powder, effectively reducing the oxygen content to ensure the high purity of the titanium powder material. At the same time, particle size classification is carried out through a multi-stage vibrating screening device to ensure the uniformity of the particle size distribution. The preparation process of the present invention is innovated and optimized at each step, making the prepared titanium powder material not only have the advantages of high purity, high sphericity, and uniform particle size but also achieve the goals of low cost and green recycling. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 It is a flowchart for the preparation of the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0030] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0031] Please refer to Figure 1 , a preparation process of a high-performance titanium powder material, comprising the following steps:

[0032] Step 1. Prepare raw materials: Prepare waste titanium chips, titanium dioxide, titanium hydride powder, waste aluminum powder, waste iron chips, vanadium powder, spheroidizing agent, surface treatment agent, reducing agent, and auxiliary additives in the formula weight parts;

[0033] Step 2. Pretreat the raw materials: Pretreat the waste titanium chips, titanium dioxide, waste aluminum powder, waste iron chips, and titanium hydride powder;

[0034] Step 3. Mixing: Mix the pretreated waste titanium chips, titanium dioxide, titanium hydride powder, waste aluminum powder, and waste iron chips evenly according to the formula ratio, then add the vanadium powder and auxiliary additives in the formula ratio. After mixing evenly, a mixed powder is obtained;

[0035] Step 4. Spheroidization treatment: Put the mixed powder and the spheroidizing agent into the spheroidization equipment, adopt the plasma spheroidization technology, and control the temperature, time, and pressure to make the powder form uniform spherical particles;

[0036] The advantages are as follows: By adopting the plasma spheroidization technology and precisely controlling the temperature and time, the mixed powder forms uniform spherical particles. This treatment method can not only improve the sphericity but also enhance the fluidity of the powder, making it more suitable for additive manufacturing. In the surface treatment step, the present invention uses a silane coupling agent or zinc stearate as a surface treatment agent to chemically treat the spheroidized powder, further improving the fluidity and spheroidization performance of the powder. This step can enhance the overall performance of the titanium powder material. In the reduction treatment link, the present invention introduces high-purity nitrogen at high temperature to perform vacuum reduction treatment on the dried powder, which can effectively reduce the oxygen content to ensure the high purity of the titanium powder material. At the same time, particle size grading is carried out through a multi-stage vibration screening device to ensure the uniformity of the particle size distribution. The preparation process of the present invention is innovated and optimized at each step, making the prepared titanium powder material not only have the advantages of high purity, high sphericity, and uniform particle size, but also achieve the goals of low cost and green recycling.

[0037] Step Five, Surface Treatment: Use a surface treatment agent to chemically treat the spheroidized powder to remove surface impurities, improve fluidity and spheroidization performance, then wash the titanium powder with deionized water to remove the residual chemical treatment agent, and finally dry the powder until the moisture content is lower than 0.1%;

[0038] Step Six, Reduction Treatment: Add a reducing agent to the dried powder, introduce nitrogen, and perform reduction treatment under high-temperature conditions to remove oxygen and nitrogen impurities, ensuring that the oxygen content is lower than 0.13%. Finally, detect the purity of the mixed powder by spectral analysis methods to ensure that it meets the high-performance requirements;

[0039] Step Seven, Particle Size Grading and Screening: Use a multi-stage vibration screening device to perform particle size grading on the mixed powder to ensure uniform particle size distribution and meet the requirements of different additive manufacturing technologies. Then, detect the particle size distribution by a laser particle size analyzer to obtain the titanium powder material and ensure that the particle size distribution meets the requirements;

[0040] Step Eight, Quality Inspection: Perform quality inspections on the prepared titanium powder material for sphericity, fluidity, oxygen content, and mechanical properties;

[0041] Step Nine, Packaging and Labeling: Package the qualified titanium powder, using moisture-proof and anti-oxidation packaging materials, and label the product information, batch number, and quality indicators on the packaging for easy quality traceability;

[0042] Step Ten, Recycling and Circular Utilization: Establish a perfect recycling system to recycle the waste materials and residues generated during the production process, ensure 100% circular recycling, reduce resource waste, re-invest the recycled waste materials into the pretreatment link, and perform crushing, screening, and reaction process treatments to achieve the circular utilization of titanium powder, reduce production costs, and reduce carbon emissions.

[0043] The advantages are as follows: By optimizing the raw material formula and process flow, titanium powder materials with high sphericity, good fluidity, low oxygen content, excellent mechanical properties and uniform particle size distribution are prepared. This innovative process can not only improve the quality of titanium powder materials, but also achieve 100% recycling of waste powder, thus reducing resource waste and carbon emissions, and further reducing production costs, bringing economic and social benefits. In the raw material pretreatment link, the invention conducts magnetic separation and pickling treatment on waste titanium chips and waste iron chips, which can effectively remove surface impurities and ferromagnetic impurities. At the same time, the titanium dioxide is activated to eliminate hydroxyl adsorption, and the titanium hydride powder is dehydrogenated to avoid subsequent pore problems. The above pretreatment steps lay a solid foundation for the subsequent spheroidization treatment.

[0044] Specifically, the raw materials and their weight fraction ranges are as follows: 65 - 70 parts of waste titanium chips; 5 - 10 parts of titanium dioxide; 10 - 14 parts of titanium hydride powder; 2 - 5 parts of waste aluminum powder; 0.5 - 1.5 parts of waste iron chips; 0.2 - 0.5 parts of vanadium powder; 2 - 3 parts of spheroidizing agent; 1 - 2 parts of surface treatment agent; 3 - 7 parts of reducing agent; 2 - 4 parts of auxiliary additive.

[0045] Specifically, the waste titanium chips and waste iron chips are respectively subjected to magnetic separation with a magnetic field strength ≥ 1.2 T to remove surface ferromagnetic impurities, pickled in a HNO3 solution with a concentration of 5% - 10% for 10 - 15 min, then rinsed 3 - 5 times with deionized water, and finally baked at a temperature of 105 - 110 °C for 30 - 50 min and taken out for standby.

[0046] Specifically, the pretreatment process of waste aluminum powder: Use screening equipment to remove large - particle impurities in the waste aluminum powder, soak the waste aluminum powder in an HCl acidic solution with a concentration of 5.0% - 5.5% for 15 - 30 min to remove the surface oxide layer and oil stains, then rinse 3 - 5 times with deionized water to ensure surface cleanliness, and put the rinsed waste aluminum powder into a drying oven and dry it at a temperature of 95 - 105 °C for 30 - 60 min to control the moisture and ensure that the waste aluminum powder is dry and water - free.

[0047] Specifically, the pretreatment process of titanium dioxide: Activate the titanium dioxide, introduce argon in a fluidized bed, and calcine it at a temperature of 550 - 600 °C for 1.5 - 2 h to eliminate hydroxyl adsorption.

[0048] Specifically, the pretreatment process of titanium hydride powder: Dehydrogenate the titanium hydride powder, heat it to 350 - 400 °C in a vacuum environment with a vacuum degree ≤ 10 -2 Pa to release hydrogen and avoid pores in subsequent processes.

[0049] Specifically, in step four, the spheroidization temperature is controlled between 1450 - 1500 °C, and the time is controlled between 1 - 1.2 h.

[0050] Specifically, the reduction treatment in Step 5: Place the dried powder at a high temperature of 800 - 950 °C, add a reducing agent, perform a reduction treatment on the mixed powder for 30 - 50 minutes, and simultaneously introduce nitrogen with a purity greater than 99.99%.

[0051] Example 1

[0052] Specifically, the raw materials and their weight portions are: 66 parts of waste titanium chips; 8 parts of titanium dioxide; 11 parts of titanium hydride powder; 3 parts of waste aluminum powder; 1.1 parts of waste iron chips; 0.25 parts of vanadium powder; 2.5 parts of spheroidizing agent; 2 parts of surface treatment agent; 6 parts of reducing agent; 3 parts of auxiliary additive (prepared by using the method of the present invention).

[0053] Example 2

[0054] Specifically, the raw materials and their weight portions are: 70 parts of waste titanium chips; 5 parts of titanium dioxide; 14 parts of titanium hydride powder; 5 parts of waste aluminum powder; 0.5 parts of waste iron chips; 0.5 parts of vanadium powder; 3 parts of spheroidizing agent; 1 part of surface treatment agent; 7 parts of reducing agent; 2 parts of auxiliary additive (prepared by using the method of the present invention).

[0055] Example 3

[0056] A preparation process of a high-performance titanium powder material, comprising the following steps:

[0057] Step 1. Prepare raw materials: Prepare 66 parts of waste titanium chips; 9 parts of titanium dioxide; 13 parts of titanium hydride powder; 5 parts of waste aluminum powder; 1.4 parts of waste iron chips; 0.4 parts of vanadium powder; 2.5 parts of spheroidizing agent; 1.2 parts of surface treatment agent; 6 parts of reducing agent; 3 parts of auxiliary additive;

[0058] Step 2. Pretreat the raw materials: Pretreat the waste titanium chips, titanium dioxide, waste aluminum powder, waste iron chips and titanium hydride powder;

[0059] Step 3. Mixing: Mix the pretreated waste titanium chips, titanium dioxide, titanium hydride powder, waste aluminum powder and waste iron chips evenly according to the formula ratio, then add the vanadium powder and auxiliary additive in the formula ratio, and after mixing evenly, obtain a mixed powder;

[0060] Step 4. Spheroidizing treatment: Put the mixed powder and the spheroidizing agent into a spheroidizing device, adopt plasma spheroidizing technology, control the temperature, time and pressure to make the powder form spherical particles;

[0061] Step 5. Surface treatment: Chemically treat the spheroidized powder with a surface treatment agent, then wash the titanium powder with deionized water, and finally dry the powder until the water content is lower than 0.1%;

[0062] Step 6. Reduction treatment: Add a reducing agent to the dried powder, introduce nitrogen, perform a reduction treatment under high temperature conditions, and finally detect the purity of the mixed powder by a spectral analysis method;

[0063] Step 7: Particle size classification and screening: Use a multi-stage vibrating screening device to classify the mixed powder by particle size to obtain titanium powder material;

[0064] Step 8: Quality inspection: Conduct quality inspections on the prepared titanium powder material for sphericity, fluidity, oxygen content, and mechanical properties;

[0065] Step 9: Packaging and labeling: Package the qualified titanium powder after inspection;

[0066] Step 10: Recycling and reuse: Establish a recycling system to recycle the waste materials and residues generated during the production process, and reintroduce the recycled waste materials into the pretreatment stage for crushing, screening, and reaction process treatment.

[0067] Comparative Example 1

[0068] Raw materials: Use traditional industrial pure titanium raw materials to replace the complex raw material combination of waste titanium chips, titanium dioxide, titanium hydride powder, waste aluminum powder, waste iron chips, etc. in Example 1. Only use 100 parts of industrial pure titanium, 0.25 parts of vanadium powder, 2.5 parts of spheroidizing agent, 2 parts of surface treatment agent, 6 parts of reducing agent, and 3 parts of auxiliary additive.

[0069] Preparation process: Use mechanical ball milling method to prepare titanium powder. Directly put industrial pure titanium into the ball mill. During the ball milling process, the temperature is controlled at room temperature, and the ball milling time is 6h. During the spheroidizing treatment, use mechanical force to promote powder agglomeration. For surface treatment, use physical polishing method. The reduction treatment is carried out in a heating furnace, nitrogen is introduced, the temperature is controlled at 600°C, and the time is 20min. Particle size classification is carried out using a simple single-layer sieve.

[0070] Comparative Example 2

[0071] Raw materials: Prepare 70 parts of waste titanium chips, the same as in Example 2, but remove other multi-component raw materials such as titanium dioxide, titanium hydride powder, waste aluminum powder, waste iron chips, etc. Additionally, add 5 parts of a traditional single plasticizer to replace the role of the multi-component raw materials, 0.25 parts of vanadium powder, 2.5 parts of spheroidizing agent, 2 parts of surface treatment agent, 6 parts of reducing agent, and 3 parts of auxiliary additive.

[0072] Preparation process: The pretreatment of waste titanium chips is carried out by water washing, without magnetic separation and pickling. During the mixing process, only stir and mix the waste titanium chips, vanadium powder, and auxiliary additive. The spheroidizing treatment is carried out at a relatively low temperature of 1200°C for 0.8h, and the pressure is not precisely controlled. For surface treatment, use a weak alkaline cleaner for cleaning. The reduction treatment is carried out in a reaction kettle, the nitrogen purity is 98%, the temperature is 800°C, and the time is 30min, and then particle size classification is carried out.

[0073] Comparative Example 3

[0074] Raw materials: The raw material formula in Example 3 is adopted, that is, 66 parts of waste titanium chips; 9 parts of titanium dioxide; 13 parts of titanium hydride powder; 5 parts of waste aluminum powder; 1.4 parts of waste iron chips; 0.4 parts of vanadium powder; 2.5 parts of spheroidizing agent; 1.2 parts of surface treatment agent; 6 parts of reducing agent; 3 parts of auxiliary additive.

[0075] Preparation process: The previous technology is used for preparation. All raw materials are not subjected to special pretreatment and are directly mixed. After mixing, traditional flame spraying is used for spheroidization. Surface treatment is carried out by wiping with alcohol with a concentration of 75%. Reduction treatment is carried out in a heating environment of 700 °C, nitrogen is introduced, and the duration is 40 min, and then particle size classification is carried out.

[0076] The titanium powder materials prepared in the examples and comparative examples are subjected to quality inspection, and the inspection data are as follows in the table:

[0077]

[0078] The following information is obtained from the above table:

[0079] Sphericity and fluidity: In Example 1, through the optimization of the plasma spheroidization process (1450 - 1500 °C) and the surface treatment agent (silane coupling agent / zinc stearate), the sphericity is stably ≥0.9, and the fluidity is ≤45 s / 50 g, meeting the requirements of additive manufacturing. In the comparative example, the use of traditional mechanical ball milling and low-temperature spheroidization (Comparative Example 2) results in irregular powder (sphericity ≤0.8) and deteriorated fluidity (≥55 s / 50 g).

[0080] Oxygen content control: In Example 1, through pretreatment (pickling, activation of titanium dioxide, dehydrogenation of titanium hydride) combined with vacuum reduction (1250 °C / 3 h), the oxygen content is stably <0.13%. Defects in the comparative examples: non-dehydrogenation (Comparative Example 3), low-purity nitrogen (Comparative Example 2), and insufficient reduction (Comparative Example 1) lead to excessive oxygen content (>0.15%).

[0081] Mechanical properties: In the examples, through the synergy of multiple raw materials (plasticization with waste aluminum powder, strengthening with vanadium powder) and hot isostatic pressing densification (950 °C / 150 MPa), the tensile strength >1050 MPa and the yield strength >950 MPa. In the comparative examples, the use of a single raw material (Comparative Example 1) and the omission of the auxiliary additive (Comparative Example 2) lead to weakened grain boundaries and a significant decrease in mechanical properties.

[0082] Particle size distribution and recovery rate: In the examples, through multi-stage cyclone classification (D90 / D10 ≤1.6) and a closed-loop recovery system (100% recycling of waste powder), the particle size is uniform and the cost is reduced. In the comparative examples, single-layer screening (Comparative Example 1) and non-classification (Comparative Example 3) lead to uneven particle size distribution and low recovery rate (≤85%).

[0083] The advantages are as follows: The process of the present invention can prepare high-performance titanium powder materials with high sphericity, good fluidity, low oxygen content, excellent mechanical properties and uniform particle size distribution, fully meeting the strict requirements of materials in high-end manufacturing fields such as aerospace, automotive, and medical. By optimizing the raw material combination and process flow, it helps to achieve 100% recycling of waste powder, reduce resource waste and carbon emissions, thereby reducing production costs, and having economic and social benefits. The preparation process of the present invention innovatively optimizes the steps of raw material pretreatment, spheroidization treatment, surface treatment and reduction treatment, enabling the prepared titanium powder materials to have the advantages of high purity, high sphericity, uniform particle size, low cost and green recycling.

[0084] Although the embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the present invention, and the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A preparation process of a high-performance titanium powder material, characterized in that, It includes the following steps: Step 1, Prepare raw materials: Prepare waste titanium chips, titanium dioxide, titanium hydride powder, waste aluminum powder, waste iron chips, vanadium powder, spheroidizing agent, surface treatment agent, reducing agent and auxiliary additive in parts by weight of the formula; Step 2, Pretreat the raw materials: Pretreat the waste titanium chips, titanium dioxide, waste aluminum powder, waste iron chips and titanium hydride powder; Step 3, Mixing: Mix the pretreated waste titanium chips, titanium dioxide, titanium hydride powder, waste aluminum powder and waste iron chips evenly according to the formula ratio, then add vanadium powder and auxiliary additive in the formula ratio, and after mixing evenly, obtain a mixed powder; Step 4, Spheroidizing treatment: Put the mixed powder and spheroidizing agent into a spheroidizing device, adopt plasma spheroidizing technology, control the temperature, time and pressure to make the powder form spherical particles; Step 5, Surface treatment: Chemically treat the spheroidized powder with a surface treatment agent, then wash the titanium powder with deionized water, and finally dry the powder until the moisture content is lower than 0.1%; Step 6, Reduction treatment: Add a reducing agent to the dried powder, introduce nitrogen, carry out reduction treatment under high temperature conditions, and finally detect the purity of the mixed powder by spectral analysis method; Step 7, Particle size classification and screening: Use a multi-stage vibrating screening device to classify the mixed powder by particle size to obtain titanium powder materials; Step 8, Quality inspection: Conduct quality inspections on the prepared titanium powder materials for sphericity, fluidity, oxygen content and mechanical properties; Step 9, Packaging and labeling: Package the qualified titanium powder after inspection; Step 10, Recycling and circular utilization: Establish a recycling system, recycle the waste and residues generated during the production process, and reintroduce the recycled waste into the pretreatment link for crushing, screening and reaction process treatment.

2. The preparation process of a high-performance titanium powder material according to claim 1, characterized in that: The raw materials and their parts by weight range are: 65 - 70 parts of waste titanium chips; 5 - 10 parts of titanium dioxide; 10 - 14 parts of titanium hydride powder; 2 - 5 parts of waste aluminum powder; 0.5 - 1.5 parts of waste iron chips; 0.2 - 0.5 parts of vanadium powder; 2 - 3 parts of spheroidizing agent; 1 - 2 parts of surface treatment agent; 3 - 7 parts of reducing agent; 2 - 4 parts of auxiliary additive.

3. The preparation process of a high-performance titanium powder material according to claim 2, characterized in that: The raw materials and their parts by weight are: 66 parts of waste titanium chips; 8 parts of titanium dioxide; 11 parts of titanium hydride powder; 3 parts of waste aluminum powder; 1.1 parts of waste iron chips; 0.25 parts of vanadium powder; 2.5 parts of spheroidizing agent; 2 parts of surface treatment agent; 6 parts of reducing agent; 3 parts of auxiliary additive.

4. The preparation process of a high-performance titanium powder material according to claim 2, characterized in that: The raw materials and their parts by weight are: 70 parts of waste titanium chips; 5 parts of titanium dioxide; 14 parts of titanium hydride powder; 5 parts of waste aluminum powder; 0.5 parts of waste iron chips; 0.5 parts of vanadium powder; 3 parts of spheroidizing agent; 1 part of surface treatment agent; 7 parts of reducing agent; 2 parts of auxiliary additive.

5. The preparation process of a high-performance titanium powder material according to claim 1, characterized in that: The waste titanium chips and waste iron chips are respectively subjected to magnetic separation with a magnetic field strength ≥ 1.2T, pickled in a HNO3 solution with a concentration of 5% - 10% for 10 - 15 minutes, then rinsed with deionized water 3 - 5 times, and finally baked at a temperature of 105 - 110°C for 30 - 50 minutes.

6. The preparation process of a high-performance titanium powder material according to claim 1, characterized in that: The pre-treatment process of the waste aluminum powder: Use a screening device to remove large particle impurities in the waste aluminum powder, soak the waste aluminum powder in an HCl acidic solution with a concentration of 5.0% - 5.5% for 15 - 30 minutes, then rinse it with deionized water 3 - 5 times, and put the rinsed waste aluminum powder into a drying oven and dry it at a temperature of 95 - 105°C for 30 - 60 minutes.

7. The preparation process of a high-performance titanium powder material according to claim 1, characterized in that: The pre-treatment process of the titanium dioxide: Activate the titanium dioxide, introduce argon gas in a fluidized bed, and calcine it at a temperature of 550 - 600°C for 1.5 - 2 hours.

8. The preparation process of a high-performance titanium powder material according to claim 1, characterized in that: The pretreatment process of the titanium hydride powder: dehydrogenate the titanium hydride powder and heat it to 350 - 400 °C in a vacuum environment with a vacuum degree ≤ 10 -2 Pa.

9. The preparation process of a high-performance titanium powder material according to claim 1, characterized in that: In step 4, the spheroidization temperature is controlled between 1450 - 1500°C and the time is controlled between 1 - 1.2 hours.

10. The preparation process of a high-performance titanium powder material according to claim 1, characterized in that: The reduction treatment in step 5: Place the dried powder at a high temperature of 800 - 950°C, add a reducing agent, perform a reduction treatment on the mixed powder for 30 - 50 minutes, and simultaneously introduce nitrogen gas with a purity greater than 99.99%.

Images