Aluminum-containing particles
Aluminum-containing particles with tailored size and density distribution improve fluidity, addressing poor mechanical strength and modeling accuracy in 3D printing by enhancing particle flow and sphericity.
Patent Information
- Application Number
- JP2024055794
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Filing Date
- 2024-03-29
- Publication Date
- 2025-01-10
- Estimated Expiration
- 2044-03-29
AI Technical Summary
Existing aluminum-containing particles exhibit poor fluidity, which affects the mechanical strength and modeling accuracy of 3D printed objects.
Aluminum-containing particles with specific particle size distribution (D50 of 30.0 μm to 60.0 μm, D90/D10 ratio of 1.5 to 3.5, and apparent density of 1.35 g/cm³) are produced to enhance fluidity, using a disk atomization method and sieving processes to achieve desired properties.
The improved fluidity leads to enhanced mechanical strength and modeling accuracy of 3D printed objects, reducing defects and surface irregularities.
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Abstract
Description
Technical Field
[0001] The present invention relates to aluminum-containing particles.
Background Art
[0002] As a technology related to aluminum-containing particles, for example, the technology described in Patent Document 1 is known.
[0003] Patent Document 1 describes particles containing an aluminum alloy, which are substantially spherical in the state of primary particles and have a mixed phase of a phase represented by composition M x Al y and a phase represented by M z Al w where M is a metal other than Al, 0 < x < 1, 0 < y < 1, 0 < z < 1, 0 < w < 1, x / y ≥ 1, z / w < 1, x + y = 1, z + w = 1, and the aluminum content is in the range of 8% by mass to 50% by mass. According to the particles described in Patent Document 1, it is described that particles having a mixed phase of two types of aluminum alloys can be provided in the form of primary particles.
Prior Art Documents
Patent Documents
[0004]
Patent Document 1
Summary of the Invention
Problems to be Solved by the Invention
[0005] The present invention provides aluminum-containing particles with improved fluidity.
Means for Solving the Problems
[0006] According to the present invention, the following aluminum-containing particles are provided.
[0007] [1] D calculated by the following <particle size measurement> 50 The particle size is 30.0 μm or more and 60.0 μm or less, D calculated by the following <particle size measurement> 90 Particle diameter is D 10 The value divided by the particle size is 1.5 or more and 3.5 or less, The apparent density measured in accordance with JIS Z 2504:2020 using a 5.0 mm diameter orifice with a 60° funnel angle is 1.35 g / cm 3 The above is an aluminum-containing particle. <Particle size measurement> 3.0 g of aluminum-containing particles were mixed with 40 mL of water and 10 mL of a 1.3% surfactant, and the mixture was dispersed in an ultrasonic bath for 300 seconds to obtain a measurement sample. The volume-based particle size distribution of the aluminum-containing particles was measured using a laser diffraction / scattering particle size measurement device, and D 10 Particle size, D 50 Particle size and D 90 The particle size values are obtained respectively. [2] D calculated by the above <particle size measurement> 10 The aluminum-containing particles according to [1] above, having a particle diameter of 20.0 μm or more and 40.0 μm or less. [3] D calculated by the above <particle size measurement> 90 The aluminum-containing particles according to [1] or [2], having a particle diameter of 50.0 μm or more and 100.0 μm or less. [4] The aluminum-containing particle according to any one of the above [1] to [3], which has a sphericity of 0.8 or more. [5] The aluminum-containing particles according to any one of [1] to [4], having a fluidity of 15.0 sec / 50 g or less in a hole flow test measured in accordance with JIS Z2502:2020. [6] The aluminum-containing particles according to any one of the above [1] to [5], wherein the aluminum-containing particles include at least one selected from the group consisting of pure aluminum particles and aluminum-based alloy particles. [7] The aluminum-containing particle according to [6], wherein the aluminum-based alloy particle contains at least one element selected from the group consisting of Cu, Mn, Si, Mg, Zn, and Ni. [8] The aluminum-containing particle according to [6] or [7], wherein the aluminum-based alloy particle comprises at least one selected from the group consisting of an Al-Si based alloy, an Al-Cu based alloy, an Al-Mn based alloy, an Al-Mg based alloy, an Al-Si-Mg based alloy, an Al-Si-Cu based alloy, an Al-Zn-Mg based alloy, an Al-Si-Mg-Cu based alloy, an Al-Cu-Ni-Mg based alloy, and an Al-Zn-Mg-Cu based alloy. [9] The aluminum-containing particles according to any one of the above [6] to [8], wherein the aluminum-based alloy particles contain at least one selected from the group consisting of AlSi10Mg and AlSi12.
[10] The aluminum-containing particle according to any one of [1] to [9] above, which can be used as a raw material powder for a 3D printer model. Effect of the Invention
[0008] According to the present invention, it is possible to provide aluminum-containing particles having improved fluidity. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0009] Hereinafter, an embodiment of the present invention will be described. Unless otherwise specified, a numerical range "A to B" indicates A or more and B or less.
[0010] [Aluminum-containing particles] The aluminum-containing particles of this embodiment are D 50 The particle size is 30.0 μm or more and 60.0 μm or less, and D 90 Particle diameter is D 10 The value divided by the particle diameter is 1.5 to 3.5, and the apparent density measured in accordance with JIS Z 2504:2020 using a funnel angle of 60° and an orifice with a diameter of 5.0 mm is 1.35 g / cm3 That's all.
[0011] The aluminum-containing particles are used, for example, as raw material powder for objects made by 3D printers, solder paste powder, etc. There is a demand for raw material powders for 3D printer models that can improve the mechanical strength and modeling precision of the resulting models.
[0012] The present inventors have found that when the fluidity of the powder decreases, the powder does not become dense during modeling using a 3D printer, and there is a concern that the mechanical strength of the resulting model may decrease. The present inventors have also found that when the fluidity of the powder decreases, there is a concern that the modeling accuracy may decrease due to the occurrence of defects inside the resulting model and the manifestation of unevenness on the surface of the resulting model. That is, the inventors considered that by improving the fluidity of the powder, it is possible to improve the mechanical strength and molding accuracy of the molded object.
[0013] The present inventors have conducted extensive research to obtain aluminum-containing particles having improved fluidity. As a result, the present inventors have found that the D 50 Particle size, D 90 Particle diameter is D 10 It has been found that the fluidity of the aluminum-containing particles is improved by setting the value divided by the particle diameter and the apparent density to specific numerical ranges. 50 Particle size, D 90 Particle diameter is D 10 It has been found that the value obtained by dividing the particle diameter and the apparent density are effective design indicators for improving the fluidity of aluminum-containing particles. That is, the aluminum-containing particles of the present invention have improved fluidity. Furthermore, the aluminum-containing particles of the present invention can improve the mechanical strength and modeling accuracy of objects produced by 3D printers.
[0014] D of the aluminum-containing particles of this embodiment50 The particle size is 30.0 μm or more and 60.0 μm or less. D of the aluminum-containing particles of this embodiment 50 From the viewpoint of further improving the flowability, the particle size is preferably 32.0 μm or more and 55.0 μm or less, more preferably 34.0 μm or more and 53.0 μm or less, and even more preferably 36.0 μm or more and 50.0 μm or less.
[0015] D of the aluminum-containing particles of this embodiment 10 From the viewpoint of further improving the flowability, the particle size is preferably 20.0 μm or more and 40.0 μm or less, more preferably 22.0 μm or more and 37.0 μm or less, and even more preferably 25.0 μm or more and 35.0 μm or less.
[0016] D of the aluminum-containing particles of this embodiment 90 From the viewpoint of further improving the flowability, the particle size is preferably 50.0 μm or more and 100.0 μm or less, more preferably 52.0 μm or more and 90.0 μm or less, and even more preferably 54.0 μm or more and 85.0 μm or less.
[0017] D of the aluminum-containing particles of this embodiment 90 Particle diameter is D 10 The value divided by the particle diameter is 1.5 or more and 3.5 or less. D of the aluminum-containing particles of this embodiment 90 Particle diameter is D 10 The value divided by the particle diameter is preferably 1.6 or more and 3.2 or less, more preferably 1.6 or more and 3.0 or less, even more preferably 1.6 or more and 2.9 or less, even more preferably 1.7 or more and 2.8 or less, and even more preferably 1.8 or more and 2.7 or less.
[0018] Here, D of aluminum-containing particles 10 Particle size, D 50 Particle size and D 90 The particle size refers to a value calculated by <Particle Size Measurement> described below.
[0019] <Particle size measurement> 3.0 g of aluminum-containing particles were mixed with 40 mL of water and 10 mL of a 1.3% surfactant, and dispersed in an ultrasonic bath for 300 seconds to obtain a measurement sample. The volume-based particle size distribution of the aluminum-containing particles was measured using a laser diffraction / scattering particle size measurement device, and the D 10 Particle size, D 50 Particle size and D 90 The particle size values are obtained respectively. Here, as the surfactant with a concentration of 1.3%, for example, an aqueous solution obtained by diluting the original solution of Fresh Green Apple with Fruit Acid (manufactured by Rocket Soap Co., Ltd.) by 11 times can be used. In addition, the surfactant is, for example, linear alkylbenzenesulfonate sodium.
[0020] The particle size of the aluminum-containing particles can be adjusted to a desired value, for example, by adjusting the classification conditions when producing the aluminum-containing particles, specifically, by adjusting the opening size of the sieve mesh when classifying the aluminum-containing particles.
[0021] The apparent density of the aluminum-containing particles of this embodiment is 1.35 g / cm 3 That's all. The apparent density of the aluminum-containing particles of the present embodiment is preferably 1.36 g / cm from the viewpoint of further improving the fluidity. 3 More preferably, 1.37 g / cm 3 More preferably, 1.38 g / cm 3 The upper limit is not particularly limited, but is, for example, 1.48 g / cm 3 or less, 1.46 g / cm 3 In addition, the apparent density of the aluminum-containing particles of the present embodiment is preferably 1.36 g / cm or less from the viewpoint of further improving the flowability. 3 More than 1.48g / cm 3 Less than or equal to 1.37 g / cm 3 More than 1.48g / cm 3 More preferably, 1.38 g / cm 3 More than 1.46g / cm 3 The following is the result. The apparent density of the aluminum-containing particles means a value measured in accordance with JIS Z 2504:2020 using an orifice with a diameter of 5.0 mm and a funnel angle of 60°.
[0022] The apparent density of the aluminum-containing particles of this embodiment can be adjusted to a desired value, for example, by adjusting the production conditions when producing the aluminum-containing particles by an atomization method, specifically, by adjusting the amount of molten metal being discharged; by adjusting the oxygen concentration in the atmosphere; by adjusting the opening diameter of the upper screen and the opening diameter of the lower screen in step (C) described below; etc.
[0023] The sphericity of the aluminum-containing particles of this embodiment is preferably 0.8 or more, more preferably 0.85 or more, and even more preferably 0.9 or more. The sphericity of an aluminum-containing particle means a value calculated by image analysis of an image obtained by a scanning electron microscope, and specifically means a value calculated by measuring the short axis length and long axis length of an aluminum-containing particle, determining the sphericity of a single aluminum-containing particle using the formula sphericity = short axis length / long axis length, and then arithmetically averaging the sphericities of 100 or more aluminum-containing particles.
[0024] From the viewpoint of further improving the fluidity, the fluidity of the aluminum-containing particles of this embodiment as measured in a hole flow test in accordance with JIS Z2502:2020 is preferably 15.0 sec / 50 g or less, more preferably 13.0 sec / 50 g or less, and even more preferably 11.0 sec / 50 g or less. The lower limit is not particularly limited, and may be, for example, 5.0 sec / 50 g or more, or 7.0 sec / 50 g or more. The fluidity of aluminum-containing particles as determined by a Hall flow test means the time it takes for 50 g of aluminum-containing particles to flow through an orifice of a calibrated funnel of specified dimensions, as measured in accordance with JIS Z2502:2020. In this specification, the fluidity of the aluminum-containing particles by the Hall Flow test can be determined by measuring the flow time of the aluminum-containing particles twice and averaging the two measured values. In addition, when one of the two measurements is obtained and the other is not obtained, the fluidity of the aluminum-containing particles by the Hall Flow test can be the obtained measured value.
[0025] The aluminum-containing particles of the present embodiment are not particularly limited as long as they contain aluminum (Al) element, but preferably contain at least one type selected from the group consisting of pure aluminum particles and aluminum-based alloy particles, and more preferably contain aluminum-based alloy particles. Here, the pure aluminum particles refer to particles made of aluminum with a purity of 99.00% or more (so-called 1000 series aluminum), and the aluminum alloy particles refer to an aluminum alloy containing Al as a main component.
[0026] The aluminum-based alloy particles of the present embodiment preferably contain at least one element selected from the group consisting of Cu, Mn, Si, Mg, Zn, and Ni, and more preferably contain at least one element selected from the group consisting of Si and Mg. When the aluminum-based alloy particles of this embodiment contain Si, the Si content in the aluminum-based alloy particles is preferably 7.00 mass% or more and 15.00 mass% or less, more preferably 8.00 mass% or more and 14.00 mass% or less, and even more preferably 9.00 mass% or more and 11.00 mass% or less, when the aluminum-based alloy particles are 100.00 mass%. When the aluminum-based alloy particles of this embodiment contain Mg, the Mg content in the aluminum-based alloy particles is preferably 0.10 mass% or more and 0.60 mass% or less, and more preferably 0.20 mass% or more and 0.45 mass% or less, when the aluminum-based alloy particles are taken as 100.00 mass%. The contents of the other elements are not particularly limited and may be set to appropriate amounts. The content of each element can be determined by, for example, elemental analysis using solid-state emission spectrometry.
[0027] The aluminum alloy particles of the present embodiment preferably contain at least one selected from the group consisting of an Al-Si based alloy, an Al-Cu based alloy, an Al-Mn based alloy, an Al-Mg based alloy, an Al-Si-Mg based alloy, an Al-Si-Cu based alloy, an Al-Zn-Mg based alloy, an Al-Si-Mg-Cu based alloy, an Al-Cu-Ni-Mg based alloy, and an Al-Zn-Mg-Cu based alloy, and more preferably contain at least one selected from the group consisting of an Al-Si based alloy and an Al-Si-Mg based alloy.
[0028] The composition of the aluminum-based alloy particles of this embodiment is not particularly limited, and may be any composition selected from the group consisting of, for example, aluminum alloys for rolling, aluminum alloys for casting, and aluminum alloys for die casting, but is preferably an aluminum alloy composition for casting. The composition of the aluminum alloy for casting is, for example, the composition specified in JIS H2211:2010.
[0029] The aluminum-based alloy particles of the present embodiment preferably contain at least one selected from the group consisting of AlSi10Mg and AlSi12, and more preferably contain AlSi10Mg. Here, AlSi10Mg and AlSi12 refer to alloys that satisfy the composition specified in JIS H2211:2010.
[0030] [Uses of aluminum-containing particles] The use of the aluminum-containing particles of the present embodiment is not particularly limited. The aluminum-containing particles of the present embodiment are aluminum-containing particles that can be used for at least one selected from the group consisting of, for example, raw material powders for 3D printer objects and soldering paste powders, and are preferably aluminum-containing particles that can be used for aluminum-containing particles.
[0031] [Method of manufacturing aluminum-containing particles] A preferred embodiment of the method for producing aluminum-containing particles according to the present embodiment will be described.
[0032] The method for producing aluminum-containing particles of the present embodiment preferably includes a step (A) of obtaining aluminum-containing particles (a) by a disk atomization method, a step (B) of classifying the aluminum-containing particles (a) to obtain aluminum-containing particles (b), and, after the step (B), a step (C) of classifying the aluminum-containing particles (b).
[0033] Hereinafter, each step in the method for producing aluminum-containing particles according to the present embodiment will be described.
[0034] <Molten metal preparation process> The method for producing aluminum-containing particles of the present embodiment preferably includes, prior to step (A), a step of preparing a molten metal that is a raw material for the aluminum-containing particles.
[0035] The method for preparing the molten metal is not particularly limited, but examples thereof include a method in which an aluminum alloy ingot is placed in a primary furnace and heated; a method in which an aluminum ingot and each element are placed in a primary furnace and heated so as to obtain the desired composition of aluminum-containing particles; and the like. The molten metal in this embodiment may contain flux. Fluxes include, for example, chlorine compounds (NaCl·KCl) and fluorine compounds (NaF·Na 2 SiF 6 ) and a mixed salt of the above may be used. The content of the flux in the molten metal in this embodiment may be, for example, 0.1 parts by mass or more and 1 part by mass or less, or 0.2 parts by mass or more and 0.3 parts by mass or less, when the aluminum alloy ingot (or the total of the aluminum ingot and each element) is taken as 100 parts by mass.
[0036] The heating temperature when preparing the molten metal is not particularly limited, and may be appropriately adjusted taking into consideration the melting point of aluminum or the melting point of the aluminum-based alloy (or the melting point of the aluminum-based alloy derived from the composition of the target aluminum-containing particles). When the aluminum-containing particles of the present embodiment contain AlSi10Mg, the heating temperature is preferably 700° C. or more and 900° C. or less, more preferably 800° C. or more and 850° C. or less.
[0037] The molten metal obtained in the primary furnace may be transferred to a secondary furnace and held in the secondary furnace. The temperature at which the molten metal is maintained is not particularly limited, and may be appropriately adjusted taking into consideration the melting point of aluminum or the melting point of the aluminum-based alloy (or the melting point of the aluminum-based alloy derived from the composition of the target aluminum-containing particles). When the aluminum-containing particles of the present embodiment contain AlSi10Mg, the holding temperature is preferably 600°C or more and 900°C or less, more preferably 650°C or more and 800°C or less.
[0038] The primary furnace and the secondary furnace are not particularly limited as long as they are melting furnaces that can be used to produce molten metal, and for example, an electric furnace, a high-frequency induction furnace, etc. can be used.
[0039] <Process (A)> The method for producing aluminum-containing particles of the present embodiment preferably includes a step (A) of obtaining aluminum-containing particles (a) by disk atomization.
[0040] In step (A), the diameter of the rotating disk is not particularly limited, but is preferably φ30 mm or more and φ40 mm or less. In step (A), the rotation speed of the rotating disk is preferably 70,000 rpm or more and 90,000 rpm or less, and more preferably 75,000 rpm or more and 85,000 rpm or less.
[0041] In step (A), the rate of tapping of the molten metal is preferably 20 kg / h or more and 50 kg / h or less, more preferably 25 kg / h or more and 40 kg / h or less, and more preferably 25 kg / h or more and 37 kg / h or less. When the amount of the molten metal tapped is equal to or more than the lower limit, the production amount per unit time can be improved. When the amount of the molten metal tapped is equal to or less than the upper limit, the proportion of coarse particles in the aluminum-containing particles (a) can be reduced, and the classification yield can be improved. When the amount of the molten metal tapped is within the above range, the apparent density of the aluminum-containing particles can be further improved. The amount of molten metal discharged can be adjusted, for example, by adjusting the size of the nozzle diameter of the secondary furnace.
[0042] The oxygen concentration in the atmosphere in step (A) is preferably 500 ppm or less, more preferably 100 ppm or less, even more preferably 50 ppm or less, and even more preferably 30 ppm or less, from the viewpoint of further improving the apparent density of the aluminum-containing particles and from the viewpoint of improving the sphericity of the aluminum-containing particles.
[0043] The type of disk atomizer used in step (A) is not particularly limited, but for example, a spherical powder manufacturing device (manufactured by Minerva Machinery Co., Ltd.) can be used.
[0044] <Process (B)> The method for producing aluminum-containing particles of the present embodiment preferably includes a step (B) of classifying the aluminum-containing particles (a) to obtain aluminum-containing particles (b). Step (B) is a step carried out after step (A). An optional step may be provided between step (A) and step (B).
[0045] Step (B) is preferably a step of removing coarse particles from the aluminum-containing particles (a) to obtain the aluminum-containing particles (b), and more specifically, preferably a step of sieving the aluminum-containing particles (a) using a sieve and recovering the aluminum-containing particles (a) that have passed through the sieve to obtain the aluminum-containing particles (b). Here, the opening diameter of the sieve is, for example, 200 μm or more and 300 μm or less, and preferably 250 μm.
[0046] The classifier used in step (B) is not particularly limited, but for example, a vibrating sieve equipped with an ultrasonic oscillator (manufactured by Koei Sangyo Co., Ltd.) can be used.
[0047] <Stirring process> The method for producing aluminum-containing particles of the present embodiment preferably includes a step of stirring the aluminum-containing particles (b) between step (B) and step (C).
[0048] The method of stirring the aluminum-containing particles (b) is not particularly limited, but for example, a method of stirring the aluminum-containing particles (b) using a mixer can be mentioned. As the mixer, for example, an Infinite Mixer (manufactured by Tokuju Kogyosho Co., Ltd.) can be used.
[0049] <Process (C)> The method for producing aluminum-containing particles of the present embodiment preferably includes a step (C) of classifying the aluminum-containing particles (b). Step (C) is a step carried out after step (B). An optional step may be provided between step (B) and step (C).
[0050] In the step (C), the method for classifying the aluminum-containing particles (b) is not particularly limited. Step (C) may be, for example, a step of removing coarse particles and fine powder from the aluminum-containing particles (b), a step of removing only coarse particles from the aluminum-containing particles (b), or a step of removing only fine powder from the aluminum-containing particles (b).
[0051] Step (C) is a step of classifying the aluminum-containing particles (b), for example, by sieving the aluminum-containing particles (b) using an upper screen and a lower screen as sieves and recovering the aluminum-containing particles (b) that passed through the upper screen but not the lower screen. In addition, step (C) may be a step of classifying the aluminum-containing particles (b) by, for example, sieving the aluminum-containing particles (b) using only an upper screen as a sieve and recovering the aluminum-containing particles (b) that have passed through the upper screen, or a step of classifying the aluminum-containing particles (b) by sieving the aluminum-containing particles (b) using only a lower screen as a sieve and recovering the aluminum-containing particles (b) that have not passed through the lower screen.
[0052] The opening diameter of the upper screen is, for example, 40 μm to 180 μm, and preferably 50 μm to 170 μm, while the opening diameter of the lower screen is, for example, 5 μm to 30 μm, and preferably 10 μm to 20 μm. By appropriately adjusting the opening diameter of the upper screen and the opening diameter of the lower screen, the particle diameter of the aluminum-containing particles can be adjusted to a desired value.
[0053] The classifier used in step (C) is not particularly limited, but for example, a Hi-Bolter (blow-through type classifier, manufactured by Toyo Hightec Co., Ltd.) can be used.
[0054] <Other processes> The method for producing aluminum-containing particles of the present embodiment may include other steps as appropriate in addition to the steps described above.
[0055] The aluminum-containing particles of this embodiment may be aluminum-containing particles obtained after step (C) in the method for producing aluminum-containing particles, or may be aluminum-containing particles (a) or aluminum-containing particles (b) prior to step (C). From the viewpoint of adjusting the particle diameter to an appropriate range, however, the aluminum-containing particles are preferably aluminum-containing particles obtained after step (C).
[0056] Although the embodiments of the present invention have been described above, these are merely examples of the present invention, and various configurations other than those described above can also be adopted. Furthermore, the present invention is not limited to the above-described embodiment, and modifications and improvements within the scope of the present invention that can achieve the object of the present invention are included in the present invention. EXAMPLES
[0057] The present embodiment will be described in detail below based on examples and comparative examples. Note that the present embodiment is not limited to the descriptions of these examples.
[0058] [Example 1] <Molten metal preparation process> An aluminum alloy ingot (AlSi10Mg) was placed in a primary furnace (electric furnace, manufactured by Ducor Corporation), and a flux (product name: Tsubasa Flux Smokeless, manufactured by Tokyo Molex Crucible Co., Ltd.) was added in an amount of 0.2 parts by mass per 100 parts by mass of the aluminum alloy ingot. The mixture was then heated to 830°C to prepare a molten metal. The obtained molten metal was transferred from the primary furnace to a secondary furnace (high-frequency induction furnace manufactured by High Frequency Systems Co., Ltd.) The molten metal was maintained at a temperature of 700°C in the secondary furnace.
[0059] <Atomization process (Process (A))> Using the molten metal in the secondary furnace as a raw material, aluminum-containing particles (a) were obtained by disk atomization under the following conditions. Disk atomizer: Spherical powder manufacturing device (Minerva Machinery Co., Ltd.) Rotating disc diameter: φ35mm Revolutions per minute: 82,000 rpm Molten metal output: 34kg / h Secondary furnace nozzle diameter: φ2mm Oxygen concentration: 30ppm or less
[0060] Here, the oxygen concentration refers to the oxygen concentration in the spray chamber, and refers to the value measured by an oxygen concentration meter (product name: zirconia oxygen concentration meter RF-30, manufactured by Toray Engineering Co., Ltd.) The oxygen concentration was adjusted to the target oxygen concentration by appropriately injecting compressed air or nitrogen gas into the spray chamber.
[0061] <1st classification process (process (B))> The aluminum-containing particles (a) were classified using a vibrating sieve machine (manufactured by Koei Sangyo Co., Ltd., product name: vibrating sieve with ultrasonic oscillator UB70UR-3S, sieve mesh opening diameter: 250 μm) to obtain aluminum-containing particles (b). Here, the aluminum-containing particles (a) that passed through the sieve mesh were collected and used as aluminum-containing particles (b).
[0062] <Stirring process> The aluminum-containing particles (b) were stirred using a mixer (manufactured by Tokuju Kogyosho Co., Ltd., product name: Mugen Mixer MM-220) at 29 rpm for 5 minutes.
[0063] Using a solid-state emission spectrometer (Thermo Fischer SCIENTIFIC, product name: ARL-3460), elemental analysis was performed on the aluminum-containing particles (b) after mixing by solid-state emission spectrometry. As a result of the elemental analysis, the composition of the aluminum-containing particles (b) was an alloy represented as AlSi10Mg.
[0064] <Second classification process (process (C))> The aluminum-containing particles (b) were classified using a blow-through classifier (manufactured by Toyo Hightec Co., Ltd., product name: Hi-Bolter NR-600SD type (two-stage)) to obtain the aluminum-containing particles of Example 1. Here, in Example 1, an upper screen was not used, and a lower screen (opening diameter: vertical 10 μm, horizontal 10 μm) was used, and the aluminum-containing particles (b) that did not pass through the lower screen were collected to obtain the aluminum-containing particles of Example 1.
[0065] [Examples 2 to 20 and Comparative Examples 3 to 5] The aluminum-containing particles of Examples 2 to 20 and Comparative Examples 3 to 5 were obtained in the same manner as in Example 1, except that the conditions were as shown in Table 1 and the aluminum-containing particles (b) recovered in the second classification step were as follows.
[0066] In the second classification step in Examples 2 to 20 and Comparative Examples 3 to 5, aluminum-containing particles (b) that passed through the upper screen but not the lower screen were collected and used as aluminum-containing particles. Here, in the case where the upper screen was not used, aluminum-containing particles (b) that did not pass through the lower screen were collected and used as aluminum-containing particles. In the case where the lower screen was not used, aluminum-containing particles (b) that passed through the upper screen were collected and used as aluminum-containing particles.
[0067] [Comparative Examples 1 and 2] The aluminum-containing particles of Comparative Examples 1 and 2 were obtained by the same method as in Example 1, except that the conditions were as shown in Table 1 and the aluminum-containing particles (b) recovered in the second classification step were as follows.
[0068] In the second classification step in Comparative Examples 1 and 2, the aluminum-containing particles (b) that passed through the upper and lower screens were collected and used as the aluminum-containing particles.
[0069] In Table 1, "Flux" indicates whether or not flux was added in the molten metal preparation process. In addition, in Table 1, the values shown under "upper screen" and "lower screen" refer to the opening diameter of the screen of the classifier in the second classification process. The values shown under "upper screen" and "lower screen" with a "-" indicate that the upper screen or lower screen was not used.
[0070] The aluminum-containing particles (b) of Examples 2 to 20 and Comparative Examples 1 to 5 were subjected to elemental analysis in the same manner as in Example 1, and were confirmed to be alloys represented by AlSi10Mg.
[0071] [measurement] The following measurements were carried out on the aluminum-containing particles of Examples 1 to 20 and Comparative Examples 1 to 5. The measurement results are shown in Table 2.
[0072] <Sphericity> First, an observation sample was prepared in which 100 or more aluminum-containing particles were fixed to the surface of a pedestal. Here, the aluminum-containing particles were dispersed in the observation sample so that they did not overlap with each other. Specifically, the observation sample was prepared by placing double-sided tape on the surface of the pedestal, dropping the aluminum-containing particles onto the exposed surface of the double-sided tape, and removing the excess aluminum-containing particles with air. Next, the sample was magnified 500 times using a scanning electron microscope (Hitachi High-Tech Corporation, product name: SU8200) to obtain SEM images. More than 20 SEM images were obtained for each level by shifting the imaging position. The obtained SEM images were subjected to image analysis using ImageJ to determine the sphericity of the aluminum-containing particles of Examples 1 to 20 and Comparative Examples 1 to 5. Specifically, the short axis length and long axis length of the aluminum-containing particle were measured, the sphericity of one aluminum-containing particle was determined according to the formula sphericity = short axis length / long axis length, and the value calculated by arithmetically averaging the sphericities of 100 or more aluminum-containing particles was regarded as the sphericity of the aluminum-containing particle. The sphericity of the aluminum-containing particles of Examples 1 to 20 and Comparative Examples 1 to 5 was all 0.8 or more.
[0073] <Particle size> The measurement sample was prepared by mixing 3.0 g of aluminum-containing particles with 40 mL of water and 10 mL of a 1.3% surfactant, dispersing the mixture in an ultrasonic bath for 300 seconds. The 1.3% surfactant was prepared by diluting the original solution of Fresh Green Apple with Fruit Acid (manufactured by Rocket Soap Co., Ltd., surfactant (sodium linear alkylbenzene sulfonate) 14%) 11 times. Specifically, the 1.3% surfactant was prepared by diluting 50 mL of the original solution of Fresh Green Apple with Fruit Acid with 500 mL of water. The volumetric particle size distribution of aluminum-containing particles was measured using a laser diffraction / scattering particle size analyzer (Microtrac, product name: MT-3300EX II) for the measurement sample, and D 10 Particle size, D 50 Particle size and D 90 The particle size values were obtained. 10 Particle size and D 90 From the particle size value, D 90 Particle diameter is D 10 Divided by particle diameter (D 90 / D 10 ) was calculated.
[0074] <apparent density> The apparent density was measured in accordance with JIS Z 2504:2020 using a funnel angle of 60° and an orifice with a diameter of 5.0 mm.
[0075] <Liquidity> The flowability was measured by the Hall flow test in accordance with JIS Z2502:2020, i.e., the time [sec / 50g] it takes for 50g of aluminum-containing particles to flow through the orifice of a calibrated funnel with specified dimensions was measured. The flow time of the aluminum-containing particles was measured at least twice. In Table 2, "ND" means that the powder did not flow even when the orifice was opened, or the flow stopped during the measurement, i.e., no measured value was obtained. In Table 2, the overall evaluation value is the average of two measured values. 1 and n 2 The values shown indicate the measured values obtained at each time.
[0076] [Table 1]
[0077] [Table 2]
[0078] The 3D printer model using the aluminum-containing particles of the embodiment had better mechanical strength than the 3D printer model using the aluminum-containing particles of the comparative example. Furthermore, the 3D printer model using the aluminum-containing particles of the embodiment had less internal defects and less apparent unevenness on the surface of the model than the 3D printer model using the aluminum-containing particles of the comparative example, and was superior in modeling accuracy.
Claims
1. D calculated by the following <Particle size measurement> 50 The particle size is 30.0 μm or more and 60.0 μm or less, D calculated by the following <Particle size measurement> 90 The particle diameter is D 10 The value divided by the particle size is 1.5 or more and 3.5 or less, The apparent density measured in accordance with JIS Z 2504:2020 using a funnel angle of 60° and an orifice with a diameter of 5.0 mm is 1.35 g / cm 3 or more and 1.48 g / cm 3 or less, Aluminum-containing particles having a fluidity of 5.0 sec / 50 g or more and 15.0 sec / 50 g or less, as measured by a hole flow test in accordance with JIS Z2502:2020. <Particle size measurement> 3.0 g of aluminum-containing particles were mixed with 40 mL of water and 10 mL of a 1.3% surfactant, and the mixture was dispersed in an ultrasonic bath for 300 seconds to obtain a measurement sample. The volume-based particle size distribution of the aluminum-containing particles was measured using a laser diffraction / scattering particle size measurement device. 10 Particle size, D 50 Particle size and D 90 The particle size values are obtained respectively.
2. D calculated by the above <Particle size measurement> 10 The aluminum-containing particle according to claim 1, having a particle diameter of 20.0 μm or more and 40.0 μm or less.
3. D calculated by the above <Particle size measurement> 90 The aluminum-containing particle according to claim 1 or 2, having a particle diameter of 50.0 μm or more and 100.0 μm or less.
4. 3. The aluminum-containing particle according to claim 1, having a sphericity of 0.8 or more.
5. 3. The aluminum-containing particle according to claim 1, wherein the aluminum-containing particle comprises at least one selected from the group consisting of pure aluminum particles and aluminum-based alloy particles.
6. 6. The aluminum-containing particle according to claim 5, wherein the aluminum-based alloy particle contains at least one element selected from the group consisting of Cu, Mn, Si, Mg, Zn, and Ni.
7. 6. The aluminum-containing particle according to claim 5, wherein the aluminum-based alloy particle comprises at least one selected from the group consisting of an Al-Si based alloy, an Al-Cu based alloy, an Al-Mn based alloy, an Al-Mg based alloy, an Al-Si-Mg based alloy, an Al-Si-Cu based alloy, an Al-Zn-Mg based alloy, an Al-Si-Mg-Cu based alloy, an Al-Cu-Ni-Mg based alloy, and an Al-Zn-Mg-Cu based alloy.
8. 6. The aluminum-containing particle according to claim 5, wherein the aluminum-based alloy particle comprises at least one selected from the group consisting of AlSi10Mg and AlSi12.
9. The aluminum-containing particle according to claim 1 or 2, which can be used as a raw material powder for a 3D printer model.
Citation Information
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