CN110947976A - Low-oxygen spherical tantalum powder and preparation method thereof - Google Patents
Low-oxygen spherical tantalum powder and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/023—Hydrogen absorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
Abstract
The invention provides low-oxygen spherical tantalum powder and a preparation method thereof. The preparation method of the low-oxygen spherical tantalum powder comprises the following steps: s1: preparing raw material powder; s2: spheroidizing, namely carrying out plasma spheroidizing on the raw material powder prepared in the step S1, wherein the oxygen content of the spheroidized tantalum powder is lower than 500 ppm; s3: screening, namely screening the spheroidized tantalum powder obtained in the step S2 for one or more times according to the target granularity to obtain tantalum powder in the granularity range meeting the additive manufacturing requirement; s4: and (4) classifying, namely performing gas flow classification treatment on the tantalum powder obtained in the step S3 under the protection of gas to remove fine powder with the particle size of below 15 mu m. The tantalum powder prepared by the preparation method has high sphericity, the granularity is concentrated in 15-53 microns, 53-150 microns or 53-175 microns, and the requirement of additive manufacturing technology on materials can be met, so that the technical problem that the tantalum powder prepared by the preparation method in the prior art is low in sphericity is solved.
Description
Technical Field
The invention relates to the technical field of additive manufacturing and powder metallurgy, in particular to low-oxygen spherical tantalum powder and a preparation method thereof.
Background
The metal tantalum is a refractory metal, has good corrosion resistance and excellent biocompatibility, and is often used as a medical material. As a medical material, tantalum oxide is not substantially absorbed and does not exhibit a toxic reaction, and can be used in combination with other metals without damaging the oxide film on the surface thereof. Therefore, metallic tantalum is used as an implant for medical treatment, such as bone substitutes, vascular stents, and the like. To achieve a level similar to the elastic modulus of human bone, a porous structure is used to degrade the elastic modulus of the metal material. The unique porous structure and the rough inner and outer surfaces are favorable for promoting the maximum growth of new bones into pores, so that biological fixation is formed between the implant and human bones, and finally, a whole is formed. The three-dimensional communicated pore structure can transmit body fluid and nutrient substances in the implant, promote tissue regeneration and reconstruction and accelerate the healing process. However, the porous material has a complex structure and is difficult to process.
The additive manufacturing is a rapid manufacturing technology combined with a digital technology, has unique advantages in the aspect of manufacturing porous structural parts, and can rapidly complete design and manufacturing. But the requirement on the material is high, and the material is required to have better sphericity, better fluidity and proper particle size distribution. The powder prepared by the common tantalum powder preparation method, namely hydrogenation dehydrogenation and chemical reduction, is non-spherical and cannot meet the requirements of additive manufacturing on materials. The preparation method of the general spherical powder comprises a mechanical ball milling method, a liquid phase method and an air atomization method. The ball milling method is a method in which hard balls are used to impact and stir a material by using the rotation or vibration of a ball mill, and the edges and corners of the powder are passivated in the process to form nearly spherical powder. The ball milling technology has complex physical process, high uncertainty and poorer sphericity of the prepared powder due to the actions of grinding, deformation, work hardening, fracture, cold welding and the like. The liquid phase method mainly comprises a spray thermal decomposition method, a carbonyl method and a sol-gel method, and spherical powder prepared by the liquid phase method has fine granularity and uniform components, but the powder agglomeration phenomenon is serious. The metal tantalum is a refractory metal, the melting point is more than 2900 ℃, the crucible in the traditional gas atomization method is difficult to keep the original characteristics and functions at the temperature, and the gas atomization method is only suitable for preparing low-melting-point metal powder. The plasma rotating electrode method can prepare spherical tantalum powder, but the particle size of the spherical tantalum powder is concentrated in a coarse powder area with the particle size of more than 50 microns, the selective melting technology in the additive manufacturing technology requires that the particle size of the powder is distributed in a range of 15-53 microns, and the particle size of the tantalum powder prepared by the plasma rotating electrode is coarse.
Therefore, it is necessary to develop a tantalum powder for additive manufacturing and a preparation method thereof.
Disclosure of Invention
The invention mainly aims to provide low-oxygen spherical tantalum powder and a preparation method thereof, the preparation method adopts a plasma spheroidization method, atomization of high-melting-point refractory metal can be realized, the prepared tantalum powder has high sphericity, the yield of target granularity section powder is high, the requirement of additive manufacturing technology on materials can be met, and the technical problem that the tantalum powder prepared by the preparation method in the prior art is not high in sphericity is solved.
In order to achieve the above object, according to a first aspect of the present invention, there is provided a method for preparing low-oxygen spherical tantalum powder.
The preparation method of the low-oxygen spherical tantalum powder comprises the following steps:
s1: preparing raw material powder;
s2: spheroidizing, namely carrying out plasma spheroidizing on the raw material powder prepared in the step S1 to obtain spheroidized tantalum powder, wherein the oxygen content of the spheroidized tantalum powder is lower than 500 ppm;
s3: screening, namely screening the spheroidized tantalum powder obtained in the step S2 for one or more times according to the target granularity to obtain tantalum powder in the granularity range meeting the additive manufacturing requirement;
s4: and (4) classifying, namely performing gas flow classification treatment on the tantalum powder with the particle size of less than or equal to 53 microns obtained in the step S3 under the protection of gas to remove fine powder with the particle size of less than 15 microns.
Further, in the step S3, the particle size of the obtained tantalum powder conforming to additive manufacturing is 15-175 μm.
Further, the step S1 includes:
s1-1: preparing tantalum powder;
s1-2: and (4) screening, namely, carrying out one or more screening treatments on the tantalum powder obtained in the step S1-1.
Further, in the step S1-1, the tantalum powder is prepared by adopting a hydrogenation dehydrogenation method, wherein the hydrogenation dehydrogenation method comprises the technical process of filling hydrogen into a resistance hydrogenation furnace to (1.0-2.0) x 105Pa, carrying out hydrogenation treatment at the temperature of 600-900 ℃, ball milling and crushing, and dehydrogenating at the temperature of 600-900 ℃ to obtain the tantalum powder. The hydrogenation and dehydrogenation method is adopted, no other impurity elements are introduced in the preparation process, and the prepared tantalum powder is high in purity and can better meet the requirements of additive manufacturing technology.
Further, in the step S1-2, the tantalum powder obtained in the step S1-1 is sieved by adopting a vibration sieving device.
Further, in the step S2, the spheroidizing power is 5-80 KW, the flow rate of the working gas is 20-80L/min, the flow rate of the side gas is 50-100L/min, and the system pressure is 80-100 KPa. The spheroidizing power is related to the power of the plasma torch, the higher the spheroidizing power is, the faster the powder is melted, the too low power cannot meet the spheroidizing requirement, and the too high power can cause the instability of the system; the plasma arc can stably operate within the working gas flow and the side gas flow range, and the continuous operation of the spheroidization process is ensured by matching with the system pressure.
Further, in step S2, the plasma torch in the plasma spheroidizing process is a dc plasma torch or a rf plasma torch.
Further, in the step S2, the working gas is at least one of argon, nitrogen, helium and hydrogen.
Further, in the step S3, screening the spheroidized tantalum powder obtained in the step S2 by using a vibration screening device.
Further, in the step S4, a gas classifier is used for classification treatment, and argon is used for protection; wherein the feeding power of the air classifier is 10-20W.
In order to achieve the above object, according to a second aspect of the present invention, there is provided a low-oxygen spherical tantalum powder.
The low-oxygen spherical tantalum powder prepared by the preparation method has the sphericity rate higher than 99%.
In the embodiment of the invention, the atomization of the high-melting-point refractory metal can be realized by adopting a plasma spheroidizing method in the preparation process of the tantalum powder, the prepared tantalum powder has high sphericity, the yield of the powder in the target granularity section is higher, the granularity is concentrated in 15-53 mu m, 53-150 mu m or 53-175 mu m, the requirement of the additive manufacturing technology on materials can be met, and the technical problem of low sphericity of the tantalum powder prepared by the preparation method in the prior art is solved.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a schematic flow chart of a method for preparing low-oxygen spherical tantalum powder according to an embodiment of the present invention;
FIG. 2 is a SEM diagram of low-oxygen spherical tantalum powder prepared in example 1 of the present invention.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
Fig. 1 is a schematic flow chart of a method for preparing low-oxygen spherical tantalum powder according to an embodiment of the present invention, and as shown in fig. 1, the method for preparing low-oxygen spherical tantalum powder mainly includes the following steps:
step S1, preparing raw material powder;
firstly, preparing tantalum powder by adopting a hydrogenation dehydrogenation method, wherein the technological process of the hydrogenation dehydrogenation method is to charge hydrogen into a resistance hydrogenation furnace until the ratio of (1.0-2.0) x 10 is reached5Pa, carrying out hydrogenation treatment at the temperature of 600-900 ℃, ball milling and crushing, and dehydrogenation at the temperature of 600-900 ℃ to obtain tantalum powder; and then, carrying out one or more times of screening treatment on the tantalum powder by adopting vibration screening equipment to mainly remove coarse particles.
S2, spheroidizing, namely carrying out plasma spheroidizing on the tantalum powder prepared in the S1, wherein a plasma torch of plasma spheroidizing equipment is a direct-current plasma torch or a radio-frequency plasma torch, working gas is at least one of argon, nitrogen, helium and hydrogen, plasma spheroidizing power is 5-80 KW, working gas flow is 20-80L/min, side gas flow is 50-100L/min, and system pressure is 80-100 Kpa; and the oxygen content of the spheroidized tantalum powder is lower than 500 ppm.
And S3, screening, namely screening the spheroidized tantalum powder obtained in the S2 for one time or multiple times by adopting vibration screening equipment according to the target granularity to obtain the tantalum powder in the granularity range meeting the additive manufacturing, wherein the granularity range of the tantalum powder is 15-175 microns as required, and the granularity of the tantalum powder is centralized at 15-53 microns, 53-150 microns or 53-175 microns.
Step S4, grading, namely, carrying out gas flow grading treatment on the tantalum powder obtained in the step S3 by adopting a gas flow grader protected by argon gas to remove fine powder with the particle size of below 15 mu m; wherein the feeding power of the air classifier is 10-20W.
In order to more clearly illustrate the method for preparing low-oxygen spherical tantalum powder provided in the embodiments of the present invention, the following embodiments 1 to 3 are described in detail.
Example 1:
s1: 10kg of tantalum powder prepared by a hydrogenation dehydrogenation method is taken, and then the tantalum powder is sieved by a 270-mesh screen on a vibration sieving device to remove coarse particles.
S2: and spheroidizing the tantalum powder by using plasma spheroidizing equipment. Wherein the plasma torch is a direct current plasma torch, the working gas is argon, the plasma spheroidization power is 80KW, the working gas flow is 80L/min, the side gas flow is 60L/min, and the system pressure is 90 Kpa; and the oxygen content of the spheroidized tantalum powder is 300 ppm.
S3: and screening the spheroidized tantalum powder by adopting vibration screening equipment, wherein the mesh number of a screen is 270 meshes, and thus the tantalum powder with the particle size of less than or equal to 53 microns is obtained.
S4: and (3) grading the tantalum powder with the granularity of less than or equal to 53 microns by adopting an argon-protected airflow grader, and removing fine powder with the granularity of less than 15 microns to obtain spherical powder with the granularity distributed in a range of 15-53 microns.
Example 2:
s1: 10kg of tantalum powder prepared by a hydrogenation dehydrogenation method is taken, and then the tantalum powder is sieved by a 100-mesh screen on a vibration sieving device to remove coarse particles.
S2: and spheroidizing the tantalum powder by using plasma spheroidizing equipment. Wherein the plasma torch is a direct current plasma torch, the working gas is argon, the plasma spheroidization power is 5KW, the working gas flow is 20L/min, the side gas flow is 100L/min, and the system pressure is 80 Kpa; and the oxygen content of the spheroidized tantalum powder is 400 ppm.
S3: and screening the spheroidized tantalum powder by adopting vibration screening equipment, wherein the mesh number of a screen is 100 meshes, and the tantalum powder with the granularity of less than or equal to 150 mu m is obtained.
S4: and classifying the tantalum powder with the granularity of less than or equal to 150 microns by adopting an argon-protected airflow classifier to obtain spherical powder with the granularity distribution of 53-150 microns.
Example 3:
s1: 10kg of tantalum powder prepared by a hydrogenation dehydrogenation method is taken, and then the tantalum powder is sieved by a 80-mesh screen on a vibration sieving device to remove coarse particles.
S2: and spheroidizing the tantalum powder by using plasma spheroidizing equipment. Wherein the plasma torch is a radio frequency plasma torch, the working gas is argon, the plasma spheroidization power is 40KW, the working gas flow is 50L/min, the side gas flow is 80L/min, and the system pressure is 100 Kpa; and the oxygen content of the spheroidized tantalum powder is 200 ppm.
S3: and screening the spheroidized tantalum powder by adopting vibration screening equipment, wherein the mesh number of a screen is 80 meshes, and the tantalum powder with the granularity of less than or equal to 180 mu m is obtained.
S4: and classifying the tantalum powder with the granularity of less than or equal to 180 mu m by adopting an argon-protected airflow classifier to obtain spherical powder with the granularity distribution of 53-175 mu m.
FIG. 2 is a SEM schematic diagram of a low-oxygen spherical tantalum powder prepared by the embodiment of the invention, and as can be seen from FIG. 2, the tantalum powder has a regular shape, a high sphericity and a sphericity ratio of 99%; the particle size of the tantalum powder is 15-53 μm.
In order to make the objects and advantages of the present invention more comprehensible, comparative analysis experiments with tantalum powder prepared by a preparation method in the prior art are performed.
First, experimental object
The experimental group adopts the low-oxygen spherical tantalum powder obtained by the preparation method of the embodiment 1-3, and the control group adopts the tantalum powder prepared by the preparation method in the prior art, wherein:
comparative example 1:
the spherical tantalum powder is prepared by adopting a mechanical ball milling method.
Comparative example 2:
and preparing the tantalum powder by adopting plasma rotating electrode powder preparing equipment.
Second, Experimental methods
And (3) determining the sphericity, the powder yield and the oxygen content of the low-oxygen spherical tantalum powder prepared in the examples 1-3 and the tantalum powder prepared in the comparative examples 1-2 by adopting a conventional detection method in the prior art.
Third, experimental results
The results are detailed in table 1.
TABLE 1 comparison of the properties of tantalum powders prepared in examples 1-3 and the prior art preparation method
Group of | Sphericity ratio (%) | Yield of powder (%) | Oxygen content (ppm) |
Example 1 | 99.2 | 85 | 300 |
Example 2 | 99.7 | 87 | 325 |
Example 3 | 99.4 | 85 | 280 |
Comparative example 1 | 80.0 | 30 | 800 |
Comparative example 2 | 99.2 | 30 | 400 |
As can be seen from Table 1, the tantalum powder prepared by the preparation method in the embodiments 1 to 3 of the invention has high sphericity, and meanwhile, the particle size of the tantalum powder can be intensively distributed in 15 to 53 μm, 53 to 150 μm or 53 to 175 μm by screening the particle size of the raw material powder in the early stage; the sphericity of the tantalum powder prepared by the preparation method in the comparative example 1 is not high, and the yield of the powder prepared by the plasma rotating electrode technology in the comparative example 2 in the target particle size section of 15-53 mu m is low; in addition, as can be seen from comparative example 1, the tantalum powder prepared by the method has lower oxygen content and is more suitable for additive manufacturing technology.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. The preparation method of the low-oxygen spherical tantalum powder is characterized by comprising the following steps:
s1: preparing raw material powder;
s2: spheroidizing, namely carrying out plasma spheroidizing on the raw material powder prepared in the step S1 to obtain spheroidized tantalum powder, wherein the oxygen content of the spheroidized tantalum powder is lower than 500 ppm;
s3: screening, namely screening the spheroidized tantalum powder obtained in the step S2 for one or more times according to the target granularity to obtain tantalum powder in the granularity range meeting the additive manufacturing requirement;
s4: and (4) grading, namely carrying out gas flow grading treatment on the tantalum powder obtained in the step S3 under the protection of gas to remove fine powder with the particle size of below 15 mu m.
2. The method for preparing tantalum powder of low oxygen content in spherical form as claimed in claim 1, wherein said step S1 comprises:
s1-1: preparing tantalum powder;
s1-2: and (4) screening, namely, carrying out one or more screening treatments on the tantalum powder obtained in the step S1-1.
3. The method for preparing low-oxygen spherical tantalum powder according to claim 2, wherein in the step S1-1, the tantalum powder is prepared by a hydrogenation dehydrogenation method, wherein the hydrogenation dehydrogenation method comprises the process of filling hydrogen gas into a resistance hydrogenation furnace to (1.0-2.0) x 105Pa, carrying out hydrogenation treatment at the temperature of 600-900 ℃, ball milling and crushing, and dehydrogenating at the temperature of 600-900 ℃ to obtain the tantalum powder.
4. The method of claim 2, wherein in step S1-2, the tantalum powder obtained in step S1-1 is sieved using a vibrating sieving device.
5. The method for preparing low-oxygen spherical tantalum powder according to claim 1, wherein in the step S2, the spheroidizing power is 5-80 KW, the working gas flow is 20-80L/min, the side gas flow is 50-100L/min, and the system pressure is 80-100 KPa.
6. The method for preparing low-oxygen spherical tantalum powder according to claim 1, wherein in the step S2, the plasma torch in the plasma spheroidizing process is a direct current plasma torch or a radio frequency plasma torch.
7. The method for preparing tantalum powder of the low oxygen content in spherical form of claim 1, wherein in step S2, the working gas is at least one of argon, nitrogen, helium and hydrogen.
8. The method for preparing tantalum powder of low oxygen content in spherical form as claimed in claim 1, wherein in step S3, the spheroidized tantalum powder obtained in step S2 is sieved by using a vibrating sieving device.
9. The method for preparing low-oxygen spherical tantalum powder according to claim 1, wherein in the step S4, a gas classifier is adopted for classification treatment, and argon is adopted for protection; wherein the feeding power of the air classifier is 10-20W.
10. The low-oxygen spherical tantalum powder prepared by the method for preparing the low-oxygen spherical tantalum powder according to any one of claims 1 to 9, wherein the sphericity ratio of the low-oxygen spherical tantalum powder is higher than 99%.
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CN111892401A (en) * | 2020-07-28 | 2020-11-06 | 湘潭大学 | Ultrahigh-temperature ceramic coating, composite material thereof and preparation method |
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CN113308671A (en) * | 2021-05-28 | 2021-08-27 | 矿冶科技集团有限公司 | High-purity tantalum rotary target and preparation method thereof |
CN114653959A (en) * | 2022-03-30 | 2022-06-24 | 中南大学 | Spherical tantalum powder, preparation thereof and application thereof in 3D printing |
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