CN108274011B - Preparation method of metal powder with bimodal distribution suitable for 3D printing - Google Patents
Preparation method of metal powder with bimodal distribution suitable for 3D printing Download PDFInfo
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- CN108274011B CN108274011B CN201810181510.1A CN201810181510A CN108274011B CN 108274011 B CN108274011 B CN 108274011B CN 201810181510 A CN201810181510 A CN 201810181510A CN 108274011 B CN108274011 B CN 108274011B
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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
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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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
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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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
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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
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
A preparation method of metal powder with bimodal distribution suitable for 3D printing belongs to the technical field of metal powder materials. Preparing slurry by using metal powder with the average particle size of 0.5-1.5 mu m as an initial raw material; then carrying out agglomeration granulation on the metal powder, and controlling the particle size distribution of the prepared micron-sized metal powder by adjusting the rotating speed of an atomizing disc; finally, carrying out heat treatment on the granulated micron-sized metal powder, and obtaining the metal powder particles with the sphericity, the fluidity and the oxygen content meeting the 3D printing requirements and with the bimodal particle size distribution through degumming, densification and consolidation. Compared with the existing other related metal powder preparation methods, the method has strong controllability on the sphericity, the particle size distribution and the oxygen content of metal powder particles, can prepare and obtain the metal powder with special particle size distribution in the same batch, and has the advantages of simple process and low cost.
Description
Technical Field
The invention relates to a preparation method of metal spherical powder with bimodal particle size distribution, which is suitable for obtaining a high-density printed product through 3D printing, and belongs to the technical field of metal powder materials.
Background
The 3D printing technology is based on the principle of layer-by-layer accumulation, can replace the traditional preparation and processing technology and can prepare three-dimensional workpieces with complex shapes efficiently and precisely, so that the three-dimensional workpieces are widely concerned and researched in hot spots in recent years. However, high quality metallic printing materials are the primary bottleneck problem that restricts the application of 3D printing technology and the acquisition of high performance metallic prints. For the metal-based powder material for 3D printing, it is generally required that the metal powder has a fine (< 50 μm) particle diameter, is uniform, has high sphericity, high fluidity, low oxygen content, and the like. On this basis, high performance metallic printing components place higher demands on the powder material, such as particular particle size distribution metal powders with a bimodal distribution. The bimodal distribution powder can keep high fluidity, and can realize that small-size particles fill pores among large-size particles so as to effectively improve the powder bulk density, so that a high-performance printed part with a smooth surface and a compact tissue structure is obtained under the condition of not changing a printing process. At present, a great deal of researchers are concerned with metal powders with a specific particle size distribution, but studies have reported that bimodal powders are formed by mixing powder particles with two particle sizes. The method is easy to cause poor powder fluidity and uneven density of printed products due to uneven mixing, and introduces metal elements, oxygen, carbon and other impurity elements contained in grinding balls due to long-time ball milling mixing. The powder material obtained by the existing metal powder preparation technology has a unimodal particle size distribution, such as a gas atomization method, a plasma rotating electrode method, a radio frequency plasma spheroidization method and the like. Moreover, the yield of the metal or alloy powder prepared by the existing gas atomization method and the plasma rotating electrode method is lower when the grain diameter is less than 50 μm; the radio frequency plasma spheroidizing method has large energy consumption and high production cost. Therefore, there is an urgent need for a method for preparing metal powder for 3D printing having high purity, low cost, and a specific particle size distribution.
Aiming at the background of the field, the invention provides a preparation method of high-purity spherical metal powder with bimodal special particle size distribution, which is suitable for 3D printing, in order to solve the limitation of the prior art.
Disclosure of Invention
The preparation method provided by the invention comprises the following process flows and principles: preparing slurry by using metal powder with the average particle size of 0.5-1.5 mu m as an initial raw material; then carrying out agglomeration granulation on the metal powder, and controlling the particle size distribution of the prepared micron-sized metal powder by adjusting the rotating speed of an atomizing disc; finally, carrying out heat treatment on the granulated micron-sized metal powder, and obtaining the metal powder particles with the sphericity, the fluidity and the oxygen content meeting the 3D printing requirements and with the bimodal particle size distribution through degumming, densification and consolidation. Compared with other related metal powder preparation methods in the prior art, the method has strong controllability on the sphericity, the particle size distribution and the oxygen content of metal powder particles, can prepare powder with special particle size distribution, and has the advantages of simple process and low cost.
The invention provides a preparation method of metal spherical powder with bimodal distribution, which is suitable for 3D printing and is characterized by comprising the following steps:
(1) mixing initial metal powder with polyvinyl alcohol, polyethylene glycol and deionized water to prepare slurry, and performing ball milling for 1-2 hours to obtain stable slurry, wherein the initial metal powder is one of Fe, Co, Ni, W and the like, the average particle size of the initial metal powder is within the range of 0.5-1.5 microns, the mass of the initial metal powder is 50-78% of the total mass of the slurry, the mass of the polyvinyl alcohol is 0.8-2% of the mass of the initial metal powder, and the mass of the polyethylene glycol is 1-2% of the mass of the initial metal powder;
(2) carrying out centrifugal spray drying on the slurry prepared in the step (1), obtaining spherical metal particles with particle size below 50 microns and bimodal distribution by adjusting the rotating speed of an atomizing disc, and carrying out spray drying in a staged manner, wherein the first stage is used for carrying out spray drying on the slurry with the rotating speed of 12000-13500 rpm, the second stage is used for directly adjusting the rotating speed of the atomizing disc on the residual slurry for carrying out spray drying, and the rotating speed of the atomizing disc in the second stage is 16000-18000 rpm;
(3) carrying out heat treatment on the spherical particles obtained in the step (2) by using a tubular furnace under the protection of argon, and carrying out degumming, densification and consolidation by adopting stage-type heat treatment; the first stage degumming adopts 300 deg.C heat preservation for 120min, and then adopts second stage and third stage heat treatment to complete densification and consolidation, and the second stage heat treatment temperature is Tm/2+120℃～Tm/2+200℃，TmThe temperature is the melting point of the metal, the heat preservation time is 5-10 min, and the temperature of the third stage of heat treatment is directly reduced from the second stage to Tm/2℃～TmAnd at the temperature of 2 plus 120 ℃, preserving the heat for 120-180 min, and finally obtaining the micron-sized spherical metal powder with high compactness and fluidity and bimodal particle size distribution.
The second stage temperature of the step (3) is different from the third stage temperature.
The method of the invention has the following technical characteristics and advantages:
(1) pure metal powder is used as an initial material to prepare suspension solution slurry, the average particle size of the initial powder is within the range of 0.5-1.5 mu m, and compared with a process of granulating by using nano powder, the cost is greatly reduced;
(2) in the preparation process of the slurry, the proportion of the polyvinyl alcohol, the polyethylene glycol and the deionized water is low and is determined by the particle size of the initial powder and the agglomeration degree, if the average particle size is large, the proportion of the polyvinyl alcohol, the polyethylene glycol and the deionized water is reduced;
(3) the preparation of stable and uniform slurry plays a crucial role in the morphology and particle size distribution of the granulated powder, and the ball milling process is adopted in the invention, so that the phenomenon that the adsorption of the organic binder and the dispersing agent on the particle surface is unbalanced due to the fact that heavy large-particle powder sinks to the bottom of the slurry is avoided;
(4) during the centrifugal spray drying process, the control of the rotation speed of the atomizing disc determines whether a satisfactory spherical powder having a bimodal particle size distribution is obtained. For a uniformly dispersed slurry, the feed rate is constant, the centrifugal force is approximately equal to the cohesive force between the slurries, and the radius of the atomized droplets has the following relationship with the rotational speed of the atomizing disk: r is 3 σ/(ρ ω ═ ω)2R), where σ is the surface tension of the slurry and is proportional to the viscosity of the slurry, ρ is the density of the slurry, ω is the rotational speed of the atomizing disk, R is the radius of the atomizing disk, and R is the radius of the atomized droplets (approximately equal to the particle size of the powder particles obtained by atomization). By regulating and controlling various process parameters, the 3D printing metal powder with bimodal particle size distribution, high sphericity and high fluidity can be prepared;
(5) the heat treatment process after granulation is very important for finally ensuring the quality of the metal powder for 3D printing. In the invention, the densification and consolidation are completed by adopting a staged heat treatment mode, the first stage heat treatment has the effect of instantly melting small particles in the granulated powder particles at high temperature to form solid phase bonding, and the whole sintering does not occur among the granulated powder particles; the second stage heat treatment temperature is lower than that of the first stage, the effect is to enable the inside of the granulated powder particles to be densified under the condition of low temperature and long-time heat preservation, and the stage heat treatment method can effectively prevent fine particles in the granulated powder from being overheated and coarser particles from being bonded to form satellite balls or prevent the inside of larger particles from being bonded to be not densified, so that the quality of the powder is improved;
(6) the method realizes the preparation of the metal powder with bimodal particle size distribution in the same batch by simpler process steps, has strong sphericity and particle size distribution controllability of powder particles, and has high production efficiency and obviously reduced cost compared with the prior spherical metal powder preparation process.
Drawings
FIG. 1 is a micrograph and a particle size distribution histogram of a spherical metal powder having a bimodal distribution prepared according to the present invention; wherein, a and b are respectively the micro-morphology and particle size distribution statistical chart of the metal cobalt powder in the embodiment 1, c and d are respectively the micro-morphology and particle size distribution statistical chart of the metal nickel powder in the embodiment 2, and e and f are respectively the micro-morphology and particle size distribution statistical chart of the metal tungsten powder in the embodiment 3.
FIG. 2 is a phase detection spectrum of the micron-sized spherical metal powder prepared by the present invention; wherein a is a phase detection spectrum of the cobalt powder in the embodiment 1, b is a phase detection spectrum of the nickel powder in the embodiment 2, and c is a phase detection spectrum of the tungsten powder in the embodiment 3.
Table 1 sphericity, fluidity and density test results of metallic cobalt, nickel and tungsten powder particles prepared in inventive example 1, example 2 and example 3.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1, preparing a suspension slurry from a pure cobalt powder raw material with an average particle size of 0.5 μm based on 50% of slurry mass, polyvinyl alcohol based on 2% of cobalt powder mass, polyethylene glycol based on 2% of cobalt powder mass, and deionized water, performing ball milling for 1 hour to obtain a uniform and stable suspension slurry, performing agglomeration granulation by using a centrifugal atomization drying device, granulating the slurry of 50% of the total volume of the slurry at an atomizing disc rotating speed of 12000rpm, and granulating the slurry of the remaining 50% of the volume at an atomizing disc rotating speed of 16000rpm to obtain spherical cobalt particles with bimodal distribution; carrying out heat treatment on the granulated cobalt powder by adopting a tube furnace under the protection of argon, wherein the heat treatment temperature in the first stage is 300 ℃, and the heat preservation time is 120 min; the temperature of the second stage heat treatment is 940 ℃, the heat preservation time is 5min, the temperature of the third stage heat treatment is reduced to 870 ℃, and the heat preservation time is 180min, so that the micron-sized spherical cobalt powder for 3D printing with bimodal particle size distribution and high fluidity is obtained. The micro-morphology and particle size distribution statistical diagrams of the prepared cobalt powder are shown as a and b in figure 1, the phase detection spectrum is shown as a in figure 2, the measurement results of sphericity, apparent density and fluidity are shown in table 1, and the density comparison of a printed part prepared by using the cobalt powder and a printed part prepared by using the powder with single-peak particle size distribution is shown in table 2.
Example 2, preparing suspension slurry from a pure nickel powder raw material with an average particle size of 1 μm based on 68% of slurry mass, polyvinyl alcohol based on 1% of nickel powder mass, polyethylene glycol based on 1.5% of nickel powder mass, and deionized water, ball-milling for 1.5h to obtain uniform and stable suspension slurry, granulating slurry 65% of the total slurry volume using an atomizing disk rotating speed of 13000rpm, and granulating slurry of the remaining 35% of the total slurry volume using an atomizing disk rotating speed of 17000rpm to obtain spherical nickel particles with bimodal distribution; carrying out heat treatment on the granulated nickel powder by adopting a tube furnace protected by argon, wherein the heat treatment temperature of the first stage is 300 ℃, and the heat preservation time is 120 min; the temperature of the second stage heat treatment is 870 ℃, the heat preservation time is 8min, the temperature of the third stage heat treatment is reduced to 800 ℃, and the heat preservation time is 150min, so that the micron-sized spherical nickel powder for 3D printing with bimodal particle size distribution and high fluidity is obtained. The micro-morphology and particle size distribution statistical diagrams of the prepared nickel powder are shown as c and d in figure 1, the phase detection spectrum is shown as b in figure 2, the measurement results of sphericity, apparent density and fluidity are shown in table 1, and the density comparison of a printed product prepared by using the nickel powder and a printed product prepared by using the powder with single-peak particle size distribution is shown in table 2.
Example 3, preparing suspension slurry from a pure tungsten powder raw material with an average particle size of 1.5 μm in 78% by mass of the slurry, 0.9% by mass of polyvinyl alcohol, 1.2% by mass of polyethylene glycol and deionized water, ball-milling for 2 hours to obtain uniform and stable suspension slurry, granulating slurry 80% by volume of the total slurry volume using an atomizing disk rotating speed of 13500rpm, and granulating slurry of the remaining 20% by volume using an atomizing disk rotating speed of 18000rpm to obtain spherical tungsten particles with bimodal distribution; carrying out heat treatment on the granulated tungsten powder by adopting a tube furnace protected by argon, wherein the heat treatment temperature of the first stage is 300 ℃, and the heat preservation time is 120 min; the temperature of the second stage heat treatment is 1800 ℃, the heat preservation time is 10min, the temperature of the third stage heat treatment is reduced to 1700 ℃, and the heat preservation time is 180min, so that the micron-sized spherical tungsten powder for 3D printing with bimodal particle size distribution and high fluidity is obtained. The micro-morphology and particle size distribution statistical graphs of the prepared tungsten powder are shown as e and f in figure 1, the phase detection map is shown as c in figure 2, the measurement results of the sphericity, the apparent density and the fluidity are shown in table 1, and the density comparison of a printed part prepared by the tungsten powder and a printed part prepared by the powder with single-peak particle size distribution is shown in table 2.
TABLE 1 physical Properties of the Metal powders obtained in examples 1 to 3 of the present invention
TABLE 2 Density of bimodal particle size distribution metal powder prints and unimodal particle size distribution metal powder prints in inventive examples 1-3
Claims (2)
1. A preparation method of metal spherical powder with bimodal distribution suitable for 3D printing is characterized by comprising the following steps:
(1) mixing initial metal powder with polyvinyl alcohol, polyethylene glycol and deionized water to prepare slurry, and performing ball milling for 1-2 hours to obtain stable slurry, wherein the average particle size of the initial metal powder is within the range of 0.5-1.5 mu m, the mass of the initial metal powder is 50-78% of the total mass of the slurry, the mass of the polyvinyl alcohol is 0.8-2% of the mass of the initial metal powder, and the mass of the polyethylene glycol is 1-2% of the mass of the initial metal powder;
(2) carrying out centrifugal spray drying on the slurry prepared in the step (1), obtaining spherical metal particles with particle size below 50 microns and bimodal distribution by adjusting the rotating speed of an atomizing disc, and carrying out spray drying in a staged manner, wherein the first stage is used for carrying out spray drying on the slurry with the rotating speed of 12000-13500 rpm, the second stage is used for directly adjusting the rotating speed of the atomizing disc on the residual slurry for carrying out spray drying, and the rotating speed of the atomizing disc in the second stage is 16000-18000 rpm;
(3) carrying out heat treatment on the spherical particles obtained in the step (2) by using a tubular furnace under the protection of argon, and carrying out degumming, densification and consolidation by adopting stage-type heat treatment; the first stage degumming adopts 300 deg.C heat preservation for 120min, and then adopts second stage and third stage heat treatment to complete densification and consolidation, and the second stage heat treatment temperature is Tm/2+120℃～Tm/2+200℃，TmThe temperature is the melting point of the metal, the heat preservation time is 5-10 min, and the temperature of the third stage of heat treatment is directly reduced from the second stage to Tm/2℃～TmAt the temperature of 2 plus 120 ℃, then, preserving the heat for 120-180 min, and finally obtaining the micron-sized spherical metal powder with high compactness and fluidity and bimodal particle size distribution;
the second stage temperature of the step (3) is different from the third stage temperature.
2. The method of preparing a metal spherical powder having a bimodal distribution suitable for 3D printing according to claim 1, wherein the starting metal powder is one of Fe, Co, Ni, W.
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| CN109877343A (en) * | 2019-04-04 | 2019-06-14 | 北京工业大学 | A kind of preparation method of the high-quality sized spherical titanium powder suitable for 3D printing |
| CN110614376B (en) * | 2019-09-12 | 2022-05-17 | 北京工业大学 | Preparation method of tungsten-copper composite powder for 3D printing |
| CN112692294B (en) * | 2020-12-22 | 2022-12-09 | 厦门钨业股份有限公司 | High-specific gravity tungsten alloy powder and preparation method thereof |
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