CN116786843A - Refractory metal component and method of making the same - Google Patents

Refractory metal component and method of making the same Download PDF

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Publication number
CN116786843A
CN116786843A CN202310703290.5A CN202310703290A CN116786843A CN 116786843 A CN116786843 A CN 116786843A CN 202310703290 A CN202310703290 A CN 202310703290A CN 116786843 A CN116786843 A CN 116786843A
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Prior art keywords
powder
refractory metal
metal component
density
grinding
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Inventor
陈国星
魏少翀
刘成威
覃恩伟
邹扬
邓春银
吴树辉
史一岭
陆壮
陆海峰
潘晨阳
叶林
刘艺武
尹嵩
史经灿
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Suzhou Nuclear Power Research Institute Co Ltd
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Suzhou Nuclear Power Research Institute Co Ltd
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Priority to CN202310703290.5A priority Critical patent/CN116786843A/en
Publication of CN116786843A publication Critical patent/CN116786843A/en
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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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • 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
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/80—Data acquisition or data processing
    • B22F10/85—Data acquisition or data processing for controlling or regulating additive manufacturing processes
    • 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
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • 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
    • B33Y10/00—Processes of additive manufacturing
    • 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
    • B33Y50/00—Data acquisition or data processing for additive manufacturing
    • B33Y50/02—Data acquisition or data processing for additive manufacturing for controlling or regulating additive manufacturing processes
    • 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
    • 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
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/044—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by jet milling

Abstract

The application discloses a preparation method of a refractory metal component, which comprises the following steps: grinding refractory metal raw material powder and then performing plasma spheroidization; creating a three-dimensional model of the component, slicing and layering the three-dimensional model, and slicing according to the three-dimensional modelPlanning a laser selective melting path according to the layered data, and rapidly melting, solidifying and forming powder according to the planned printing melting path to obtain a refractory metal component; the process parameters of the printing are adjusted by a volumetric energy density VED, which is defined as follows: ved=p/(vht); wherein: VED is the energy density (J/mm) 3 ) P is laser power (W), v is scanning speed (mm/s), h is scanning interval (mm), and t is single-layer powder spreading thickness (mm).

Description

Refractory metal component and method of making the same
Technical Field
The application belongs to the technical field of refractory metal additive manufacturing, and particularly relates to a preparation method for preparing an ultra-compact block refractory metal component by selective laser melting and a refractory metal component prepared by the preparation method.
Background
The refractory metal material has the characteristics of high melting point, high hardness, high temperature resistance and corrosion resistance, wherein the typical melting point of tungsten metal is as high as 3410 ℃, and the refractory metal material has high hardness, high density, high thermal shock resistance and excellent high-temperature strength, so that the refractory metal material has wide application in the fields of aerospace, nuclear reactors, weaponry, cutting tools and the like. Due to the excellent mechanical properties of tungsten metal, in recent years, along with the development of technology, the application of tungsten alloy and pure tungsten is gradually increased, and meanwhile, more severe requirements are also put on the performance and manufacturing process of the tungsten alloy and pure tungsten.
The traditional pure tungsten component is usually manufactured by adopting a powder metallurgy method, wherein the main process is to obtain the pure tungsten component by taking powder as a raw material, and performing compression molding and high-temperature sintering. At present, with the deep research, the powder metallurgy technology has been developed from the traditional compression molding technology to the high performance, high densification, low cost and high production efficiency, mainly comprises the molding technologies such as hot isostatic pressing, plasma sintering, vapor deposition and the like, and the technologies are widely applied to production, but the technology process is complicated and high in cost, and because tungsten hardness is high and brittleness is high, mechanical processing is difficult to carry out, so that components with complicated shapes and ultra-dense structures are difficult to prepare, and the problems of limitation are faced, the laser selective melting gradually reaches the corner of the corner, and the advantages of short period, low cost and integrated molding are relied on, so that the technology becomes the most promising technology in refractory metal preparation.
The laser selective melting technology is one of the most development potential technologies in the field of additive manufacturing, and the pre-paved metal powder thin layers are melted layer by layer through high-energy laser to form a plurality of high-performance complex components, so that the technology has the characteristics of short preparation period, high processing precision, low cost, capability of randomly forming the complex components and the like. However, when the pure tungsten block is prepared by melting the laser selective area, the defects of internal pores and the like in the block body reduce the compactness of the pure tungsten block, seriously affect the mechanical property of the pure tungsten component, limit the application of the pure tungsten component, and are one of the important difficulties faced by the additive manufacturing technology for preparing refractory metals, so that the development of a set of laser selective area melting preparation process method for preparing ultra-dense refractory metals is urgently needed.
Disclosure of Invention
In view of the above, in order to overcome the defects of the prior art, the present application aims to provide a method for preparing a refractory metal component, which can prepare an ultra-dense block refractory metal component.
In order to achieve the above purpose, the present application adopts the following technical scheme:
a method of making a refractory metal component comprising the steps of:
grinding refractory metal raw material powder and then performing plasma spheroidization;
creating a three-dimensional model of the component, slicing and layering the three-dimensional model, planning a laser selective melting path according to slicing and layering data of the three-dimensional model, and rapidly melting, solidifying and forming powder according to a planned printing melting path to obtain a refractory metal component;
the process parameters of the printing are adjusted by a volumetric energy density VED, which is defined as follows:
VED＝P/(vht)
wherein: VED is the energy density (J/mm) 3 ) P is laser power (W), v is scanning speed (mm/s), h is scanning interval (mm), and t is single-layer powder spreading thickness (mm).
The bulk density energy is an integrated measure of power, scan speed, scan pitch, and monolayer powder thickness, and the optimal parameters of the printing element are the result of a multi-factor synergy, which is less efficient if adjusted based on only a single factor. Thus, by adjusting four factors simultaneously, the bulk density energy is varied and is brought within a range (400-1100J/mm 3 ) And in addition, single variable factors are integrated, so that the optimization of parameters is more efficient.
According to some preferred embodiments of the application, the refractory metal component produced has a density of 19g/cm or more 3 The density is more than or equal to 99 percent.
According to some preferred embodiments of the application, the grinding is an air-flow mill, and the processing parameters of the air-flow mill are: the rotation speed of the sorting wheel is 4000-6000 rmp, the pressure of the grinding cavity is 0.5-1.0 MPa, the powder feeding rate is 0.5-10 kg/h, and the grinding gas quantity is 8-12 m 3 /min。
According to some preferred embodiments of the application, the refractory metal raw material powder has a powder particle size of 5 to 150 μm after grinding. In order to prepare spherical refractory metal powder with high sphericity, smooth surface, good dispersibility and uniform granularity, optimization treatment is carried out before plasma spheroidization, and raw material powder is subjected to air flow grinding to obtain the spherical refractory metal powder with good dispersibility.
According to some preferred embodiments of the application, the parameters of the plasma spheroidization are: the sheath air flow is 55-75/8-16L/min, the central air flow is 18.5-24.5L/min, the carrier air flow is 4-7L/min, the powder feeding rate is 12-24 g/min, the spheroidizing pressure is 18-30 kPa, and the plasma energy is 40-75 kW.
According to some preferred embodiments of the present application, the powder after the plasma spheroidization has a particle size of 15-65 μm, a sphericity of not less than 98%, an oxygen content of not more than 120ppm, a flowability of 5.25-8.12 s/50g, and a bulk density of 10.54-11.36 g/cm 3 。
According to some preferred embodiments of the application, the sheath gas is Ar/H 2 The method comprises the steps of carrying out a first treatment on the surface of the The central gas is Ar; the carrier gas is Ar.
According to some preferred embodiments of the application, the refractory metal raw material powder is ground and then subjected to plasma spheroidization to a powder particle size in the range of 15 to 65 μm, and more than 85% of the powder particles have a particle size in the range of 25 to 50 μm.
According to some preferred embodiments of the application, the volumetric energy density VED is 400-1100J/mm 3 Preferably 600-800J/mm 3 。
The application also provides the super-compact block refractory metal component prepared by the preparation method.
Due to the adoption of the technical scheme, compared with the prior art, the application has the following advantages: according to the preparation method of the super-compact block refractory metal component, the powder spheroidization technology combining air flow impact dispersion and plasma spheroidization is used, so that the refractory metal powder has the characteristics of narrow particle size distribution, high sphericity, good dispersion and fluidity, low oxygen content and the like; and adjusting the process parameters of the selective laser melting by taking the volumetric energy density VED as a standard, analyzing the influence of each process parameter factor on the compactness of the refractory metal component, qualitatively analyzing the volumetric energy density parameters, and formulating an optimal process parameter scheme to obtain the ultra-compact refractory metal component.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present application, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 shows the microstructure and size distribution of particles after plasma spheroidization in accordance with a preferred embodiment of the present application;
FIG. 2 is a schematic diagram of the macro and micro structure of a refractory metal component prepared by selective laser melting in accordance with a preferred embodiment of the present application;
FIG. 3 illustrates the effect of different volumetric energy densities VEDs on refractory metal component density and densification in accordance with a preferred embodiment of the present application.
Detailed Description
In order to make the technical solution of the present application better understood by those skilled in the art, the technical solution of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present application without making any inventive effort, shall fall within the scope of the present application.
Aiming at the problem of poor compactness of a refractory metal component caused by pores in the selective laser melting preparation of the component, the reason is analyzed, and the method is mainly related to the adopted powder preparation process and the selective laser melting preparation process. Therefore, the technical problem to be solved by the application is to provide a process method for manufacturing an ultra-compact block refractory metal component by laser selective melting, and the compactness of the prepared refractory metal block is improved by selecting a proper powder preparation technology and a proper molding technology, so that the mechanical property of the refractory metal component prepared by the laser selective melting is improved.
On one hand, the application optimizes the physical properties of refractory metal powder by utilizing a plasma spheroidization technology, the melting point of refractory metal is higher, and spherical refractory metal powder cannot be prepared by the traditional gas atomization and water atomization methods. Common techniques for preparing spherical refractory metal powders are the hydrogenation dehydrogenation process, the plasma rotating electrode process and the plasma spheroidization process. The hydrogenation and dehydrogenation method has lower cost, but the process is more complicated, and the content of interstitial elements is higher; the powder obtained by plasma rotary electrode atomization has high sphericity and basically no hollow powder, but the yield of the powder with the granularity smaller than 45 μm is smaller than 10%. The plasma spheroidizing technology is to transmit the energy of plasma to the powder, the powder is melted after obtaining higher energy, spherical liquid drops are formed under the action of surface tension, and the spherical powder is solidified under extremely cold conditions, and the plasma spheroidizing technology has the advantages of controllable process atmosphere, no pollution and high spheroidizing efficiency. The application optimizes the selective laser melting process and improves the compactness of the tissue after selective laser melting.
In order to solve the compactness problem existing in the preparation of refractory metal blocks by laser selective melting, the process method for manufacturing the super-compact block refractory metal component by laser selective melting comprises the following steps:
step (1) spheroidizing pretreatment of refractory metal raw material powder
The refractory metal raw material powder is sent into an air flow mill for grinding, so that powder with good dispersibility, smooth surface and uniform granularity is obtained, the uniformity of the powder is improved, ultrafine-sized particles can be obtained, the subsequent spheroidization treatment is facilitated, and compared with other grinding modes, the air flow mill has the advantages of narrow granularity distribution, high grinding efficiency, small product pollution and the like.
The pretreatment parameters of the jet mill are as follows: the rotation speed of the sorting wheel is 4000-6000 rmp, the pressure of the grinding cavity is 0.5-1.0 MPa, the powder feeding rate is 0.5-10 kg/h, and the grinding gas quantity is 8-12 m 3 And/min. The grain size of the product after air flow grinding is 5-150 mu m.
Step (2) refractory metal powder plasma spheroidization
And (3) performing plasma spheroidization on the powder produced in the step (1), wherein the obtained powder has the characteristics of uniform chemical components, narrow particle size distribution, high sphericity, good fluidity, low oxygen content and the like.
The powder particles obtained after plasma spheroidization have high sphericity, so that the powder has the characteristics of good fluidity and the like in the component preparation process, the compactness of the component can be improved, the powder particles obtained without plasma spheroidization have irregular shapes, poor fluidity and poor compactness of the component prepared later.
Experimental parameters of plasma spheroidization: sheath air flow (Ar/H) 2 ) 55-75/8-16L/min, 18.5-24.5L/min of central gas (Ar), 4-7L/min of carrier gas (Ar), 12-24 g/min of powder feeding rate, 18-30 kPa of spheroidizing pressure and 40-75 kW of plasma energy.
As shown in FIG. 1, the particle size of the product after the plasma spheroidization treatment is 15-65 mu m, the particle size range of more than 85% of powder is 25-50 mu m, the sphericity is more than or equal to 98%, the oxygen content is less than or equal to 120ppm, the fluidity is 5.25-8.12 s/50g, and the bulk density is 10.54-11.36 g/cm 3 。
In the embodiment, the combination of airflow impact dispersion and plasma spheroidization is utilized, the particle size distribution of the obtained spherical refractory metal powder is narrower (15-65 mu m), coarse powder and fine powder are mixed in a proper proportion (namely, more than 85% of powder has the particle size range of 25-50 mu m), and higher powder stacking density can be formed, so that the laser selective melting component achieves the expected molding effect. High bulk density, a continuous melting pool is formed, and the laser selective melting forming piece with smooth surface and stable structure is produced. The bulk density of the powder is controlled by the particle size and shape, so that too many large particles in the powder can reduce the density of the powder, too many small particles can reduce the fluidity of the powder, and only when the proportion of the large particles to the small particles is optimal, the small gaps in the large particles are filled with the small particles, so that the fluidity and the bulk density of the powder are optimal, and a compact laser selective melting refractory metal component is obtained.
Step (3) a three-dimensional model of the component is created, and slicing and layering treatment is carried out
And (3) creating a three-dimensional model of the component by adopting three-dimensional modeling software (such as UG, solidwork, magics and the like), slicing and layering the three-dimensional model, and planning a laser selective melting path according to slicing and layering data of the three-dimensional model.
Step (4) refractory metal component laser selective melting forming
And (3) according to a planned 3D printing melting route, rapidly melting, solidifying and forming the powder to prepare the ultra-compact block refractory metal component, as shown in figure 2.
The density of the laser selective melting refractory metal forming component is closely related to the laser power, the scanning speed, the scanning interval and the single-layer powder spreading thickness in the preparation process, for example, smaller or larger laser power can lead to the density reduction of the component, which is not only influenced by single factor parameters, but also influenced by the interaction of multiple factors such as the laser power, the scanning speed, the scanning interval and the powder spreading thickness, therefore, according to the characteristic of laser selective melting layer-by-layer printing, the printing process parameters in the application are qualitatively measured by Volume Energy Density (VED) and are defined as follows:
VED＝P/(vht)
wherein: VED is the energy density (J/mm) 3 ) P is laser power (W), v is scanning speed (mm/s), h is scanning interval (mm), and t is single-layer powder spreading thickness (mm). By adjusting the process parameters of the volume energy density VED (600-800J/mm) 3 ) Optimizing the preparation process parameters, wherein the density of the prepared refractory metal is more than or equal to 19g/cm 3 The density is equal to or higher than 99 percent, as shown in figure 3. The change of four variables is represented through the comprehensive synergy of one variable of the volume energy density, different influencing factors are regulated simultaneously, and the optimization efficiency is higher.
Example 1:
the process method for manufacturing the super-compact block refractory metal component by selective laser melting in the embodiment comprises the following steps of:
step 1, spheroidizing pretreatment of refractory metal raw material powder
And (3) feeding the refractory metal pure tungsten raw material powder into an air flow mill for grinding to obtain powder with good dispersibility, smooth surface and uniform granularity.
Air flow mill parameters: the rotation speed of the sorting wheel is 5000rmp, the pressure of the grinding cavity is 0.8MPa, the powder feeding rate is 5kg/h, and the grinding gas quantity is 10m 3 The particle size of the obtained powder is 5-150 mu m.
Step 2, refractory metal powder plasma spheroidization
Performing plasma spheroidization on the powder produced in the step 1, wherein the particle size range of the obtained powder is 15-65 mu m, the particle size range of more than 85% of the powder is 25-50 mu m, the sphericity is 99%, the oxygen content is 100ppm, the fluidity is 5.75s/50g, and the apparent density is 11.06g/cm 3 . As shown in fig. 1.
Experimental parameters of plasma spheroidization: sheath air flow (Ar/H) 2 ) 60/12L/min, 21.5L/min of central gas (Ar) flow, 5L/min of carrier gas (Ar) flow, 18g/min of powder feeding rate, 24kPa of spheroidizing pressure and 55kW of plasma energy.
Step 3, creating a component three-dimensional model, and slicing and layering
And a three-dimensional model of the component is created by adopting three-dimensional modeling software UG, slicing and layering processing is carried out on the three-dimensional model, and a laser selective melting path is planned according to slicing and layering data of the three-dimensional model.
Step 4, melting and forming refractory metal components in selective laser mode
And (3) according to a planned 3D printing melting route, rapidly melting, solidifying and forming the powder to prepare the super-compact block refractory metal component.
In the 3D printing process, the volume energy density VED is 650J/mm by adjusting the technological parameters 3 The density of the prepared refractory metal component is 19.2g/cm 3 The density is 99.3%.
Example 2:
the process method for manufacturing the super-compact block refractory metal component by selective laser melting in the embodiment comprises the following steps of:
step 1, spheroidizing pretreatment of refractory metal raw material powder
And (3) feeding the refractory metal tungsten alloy raw material powder into an air flow mill for grinding to obtain powder with good dispersibility, smooth surface and uniform granularity.
Air flow mill parameters: the rotation speed of the sorting wheel is 5000rmp, the pressure of the grinding cavity is 0.8MPa, the powder feeding rate is 5kg/h, and the grinding gas quantity is 10m 3 The particle size of the obtained powder is 5-150 mu m.
Step 2, refractory metal powder plasma spheroidization
Performing plasma spheroidization on the powder produced in the step 1, wherein the particle size range of the obtained powder is 15-55 mu m, the particle size range of more than 85% of the powder is 25-50 mu m, the sphericity is 99%, the oxygen content is 110ppm, the fluidity is 6.32s/50g, and the bulk density is 10.56g/cm 3 。
Experimental parameters of plasma spheroidization: sheath air flow (Ar/H) 2 ) 62/12L/min, 20L/min of central gas (Ar) flow, 6L/min of carrier gas (Ar) flow, 20g/min of powder feeding rate, 24kPa of spheroidizing process pressure and 55kW of plasma energy.
Step 3, creating a component three-dimensional model, and slicing and layering
And a three-dimensional model of the component is created by adopting three-dimensional modeling software UG, slicing and layering processing is carried out on the three-dimensional model, and a laser selective melting path is planned according to slicing and layering data of the three-dimensional model.
Step 4, melting and forming refractory metal components in selective laser mode
And (3) according to a planned 3D printing melting route, rapidly melting, solidifying and forming the powder to prepare the super-compact block refractory metal component. As shown in fig. 2.
In the 3D printing process, the volume energy density VED is 620J/mm by adjusting the technological parameters 3 The density of the prepared refractory metal component is 19.0g/cm 3 The density is 99.1%.
Comparative example 1
The difference between this comparative example and example 1 is that the volumetric energy density VED during 3D printing in this comparative example was 300J/mm 3 Other procedures and parameters were substantially the same as in example 1, producing a refractory metal component having a density of 16.8g/cm 3 The density is 86.4%.
Comparative example 2
The difference between this comparative example and example 1 is that the volumetric energy density VED during 3D printing in this comparative example was 1500J/mm 3 Other procedures and parameters were substantially the same as in example 1, producing a refractory metal component having a density of 17.1g/cm 3 The density is 89.8%.
Comparative example 3
This comparative example differs from example 1 in that the step of air-jet milling, i.e., the direct plasma spheroidization treatment, was eliminated, and other steps and parameters were substantially identical to those of example 1.
Since no jet milling is performed, the particle size distribution is broad, and the particle size distribution is 5 to 500 μm. The density of the refractory metal component obtained by subsequent preparation is 15.2g/cm 3 The density is 82.6%.
Comparative example 4
This comparative example differs from example 1 in that the step of plasma spheroidization, i.e., 3D printing directly according to the laser selective melting path after air-jet milling, was eliminated, and other steps and parameters were substantially identical to example 1.
Since no plasma spheroidization was performed, the sphericity of the powder particles was poor, and the sphericity was 70%. The density of the prepared refractory metal component is 14.8g/cm 3 The density is 81.6%.
Comparative example 5
The comparative example is different from example 1 in that the powder particle size distribution was made wider (10 to 100 μm) during the plasma spheroidization, the ratio between the coarse powder and the fine powder was unsuitable (the ratio of the powder particle size range between 25 to 50 μm was less than 50%) by adjusting the parameters of the plasma spheroidization, and other steps and parameters were substantially identical to those of example 1.
Because the particle size distribution of the powder is wider, the proportion between coarse powder and fine powder is unsuitable, and the powder density is low. The density of the prepared refractory metal component is 15.5g/cm 3 The density is 82.0%.
The technological process package for producing super-compact block refractory metal component by selective laser melting has the following beneficial technical effectsThe method comprises the following steps: (1) The powder spheroidizing process combining air flow impact dispersion and plasma spheroidization is adopted, so that the refractory metal powder has the characteristics of narrow particle size distribution, high sphericity, good dispersion and fluidity, low oxygen content and the like, the obtained powder has the particle size range of 15-65 mu m, more than 85% of powder has the particle size range of 25-50 mu m, the powder accords with the particle size range of laser selective melting three-dimensional printing, and the prepared component has high compactness. (2) Adjusting the melting process parameters of the laser selective regions, analyzing the influence of each process parameter factor on the compactness of the refractory metal component, qualitatively analyzing the volume energy density parameters, and formulating an optimal process parameter scheme to obtain the ultra-compact refractory metal component with the density more than or equal to 19g/cm 3 The density is more than or equal to 99 percent, and provides a process solution for preparing refractory metal materials with ultra-compact structures.
The above embodiments are provided to illustrate the technical concept and features of the present application and are intended to enable those skilled in the art to understand the content of the present application and implement the same, and are not intended to limit the scope of the present application. All equivalent changes or modifications made in accordance with the spirit of the present application should be construed to be included in the scope of the present application.

Claims (10)

1. A method of making a refractory metal component comprising the steps of:
grinding refractory metal raw material powder and then performing plasma spheroidization;
creating a three-dimensional model of the component, slicing and layering the three-dimensional model, planning a laser selective melting path according to slicing and layering data of the three-dimensional model, and rapidly melting, solidifying and forming powder according to a planned printing melting path to obtain a refractory metal component;
the process parameters of the printing are adjusted by a volumetric energy density VED, which is defined as follows:
VED＝P/(vht)
wherein: VED is the energy density (J/mm) 3 ) P is laser power (W), v is scanning speed (mm/s), h is scanning interval (mm), and t is single-layer powder spreading thickness (mm).
2. The method according to claim 1, wherein the refractory metal component produced has a density of 19g/cm or more 3 The density is more than or equal to 99 percent.
3. The method of claim 1, wherein the grinding is an air-jet mill, and the air-jet mill has process parameters of: the rotation speed of the sorting wheel is 4000-6000 rmp, the pressure of the grinding cavity is 0.5-1.0 MPa, the powder feeding rate is 0.5-10 kg/h, and the grinding gas quantity is 8-12 m 3 /min。
4. A method of producing according to claim 3 wherein the refractory metal raw material powder has a powder particle size of 5 to 150 μm after grinding.
5. The method according to claim 1, wherein the parameters of the plasma spheroidization are: the sheath air flow is 55-75/8-16L/min, the central air flow is 18.5-24.5L/min, the carrier air flow is 4-7L/min, the powder feeding rate is 12-24 g/min, the spheroidizing pressure is 18-30 kPa, and the plasma energy is 40-75 kW.
6. The process according to claim 5, wherein the powder after the plasma spheroidization has a particle size of 15 to 65. Mu.m, a sphericity of not less than 98%, an oxygen content of not more than 120ppm, a fluidity of 5.25 to 8.12s/50g and a bulk density of 10.54 to 11.36g/cm 3 。
7. The method according to claim 5, wherein the sheath gas is Ar/H 2 The method comprises the steps of carrying out a first treatment on the surface of the The central gas is Ar; the carrier gas is Ar.
8. The method according to claim 1 or 5, wherein the powder particle size range of the refractory metal raw material powder after grinding is 15 to 65 μm and 85% or more of the powder particle size range is 25 to 50 μm.
9. The process according to claim 1, wherein the volumetric energy density VED is from 400 to 1100J/mm 3 。
10. A refractory metal component prepared according to the preparation method of any one of claims 1-9.
CN202310703290.5A 2023-06-14 2023-06-14 Refractory metal component and method of making the same Pending CN116786843A (en)

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