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WO2017163834A1 - Matériau en poudre et procédé de production d'un modèle tridimensionnel - Google Patents

Matériau en poudre et procédé de production d'un modèle tridimensionnel Download PDF

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Publication number
WO2017163834A1
WO2017163834A1 PCT/JP2017/008708 JP2017008708W WO2017163834A1 WO 2017163834 A1 WO2017163834 A1 WO 2017163834A1 JP 2017008708 W JP2017008708 W JP 2017008708W WO 2017163834 A1 WO2017163834 A1 WO 2017163834A1
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Prior art keywords
resin
coated particles
powder material
temperature
thin layer
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English (en)
Japanese (ja)
Inventor
和也 磯部
雅晴 白石
一史 山▲崎▼
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Konica Minolta Inc
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Konica Minolta Inc
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Priority to JP2018507183A priority Critical patent/JPWO2017163834A1/ja
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C67/00—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00
    • 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

Definitions

  • the present invention relates to a powder material and a method for manufacturing a three-dimensional structure.
  • a powder bed fusion bonding method is known.
  • a thin layer is formed by laying flat a powder material including particles made of a resin material or a metal material. Then, a desired position of the thin layer is irradiated with a laser beam to selectively sinter or melt bond the adjacent coated particles (hereinafter also simply referred to as “melt bonding”).
  • modeled object layer a layer obtained by finely dividing the three-dimensional modeled object in the thickness direction is formed.
  • a three-dimensionally shaped object having a desired shape is manufactured by further spreading a powder material on the shaped object layer thus formed and repeating laser light irradiation.
  • the powder bed fusion bonding method has an advantage that a three-dimensional molded article having high strength is easily obtained because of high modeling accuracy and high adhesion strength between the layered molded article layers.
  • resin types used in the powder bed fusion bonding method are limited to polystyrene, polyamide 11, polyamide 12, and the like, and it is required to form a three-dimensional model using more versatile resins.
  • a thin layer made of a powder material may be preheated before the laser beam irradiation for the purpose of reducing the amount of laser energy to be used.
  • the particles may aggregate during preheating, and it is difficult to sufficiently increase the preheating temperature. Therefore, in order to sufficiently melt and bond the particles, a large amount of laser energy is still necessary, and further reduction in the amount of laser energy is required from the viewpoint of improving productivity and expanding applications.
  • the particles used in the powder bed fusion bonding method are core-shell type coated particles (see, for example, Patent Document 1).
  • the melt bonding force between particles is enhanced by including a fine-grained material that can be sintered or glass-formed at a temperature lower than the core particles in the shell.
  • toner made of resin or the like
  • various particles have been developed.
  • Such toners are required to be capable of being fused onto a substrate at a low energy amount, that is, at a low temperature (low-temperature fusibility), and not to be fused during storage (storage stability).
  • Such toner for electrophotography is generally formed by a melt-kneading pulverization method or the like.
  • a chemical polymerization method such as a suspension polymerization method or an emulsion aggregation method is used. In many cases, it is also manufactured by a conventional method.
  • Patent Documents 2 and 3 describe coated particles (electrophotographic toner) in which particle surfaces made of a polyester resin or the like are crosslinked with an oxazoline compound to modify the particle surfaces.
  • the storage stability is enhanced by crosslinking the particle surface.
  • Patent Document 4 proposes core-shell type coated particles (electrophotographic toner) having a core made of a polyester resin and a shell made of an amorphous polyester resin.
  • the difference in SP between the core resin and the shell resin is provided to enhance the low-temperature fixability and storage stability of the coated particles.
  • the powder material used in the powder bed fusion bonding method is required to sufficiently melt and bond particles with a small amount of laser energy while the particles do not aggregate during preheating.
  • an object of the present invention is to provide a powder material and a three-dimensional modeling method in which particles are less likely to aggregate during preheating and can sufficiently sinter coated particles with a small amount of laser energy.
  • the first of the present invention is the following powder material. [1] The formation of a thin layer of a powder material containing coated particles, preheating of the thin layer, and selective laser light irradiation to the thin layer are repeated, and a plurality of shaped product layers in which the coated particles are melt-bonded are formed.
  • a powder material used in a method for producing a three-dimensional structure by layering wherein the coated particles include a core resin and a shell resin that coats the core resin, and the SP value of the core resin and the The absolute value of the difference in SP value of the shell resin is 2.5 (J / cm 3 ) 1/2 to 7.0 (J / cm 3 ) 1/2 , and the storage elastic modulus G ′ of the shell resin is 10 6.5 becomes Pa temperature TS (65) has a storage modulus G of the core resin 'is higher than the temperature TC (65) to become 10 6.5 Pa, the powder material.
  • the storage modulus G of the core resin' is 10 6.5 Pa Temperature TS (65), the storage modulus G of the core resin' [2]
  • the storage elastic modulus of the shell resin G temperature is 10 6.5 Pa TC and (65)
  • the powder material according to [1] or [2], wherein in the coated particles, the thickness of the layer containing the shell resin that coats the core resin is 10 to 500 nm.
  • the manufacturing method of a three-dimensional molded item which repeats an irradiation process in this order several times and forms a three-dimensional molded item by laminating
  • the preheating temperature is a temperature at which the storage elastic modulus G′c of the core resin of the coated particles is 10 6 Pa or less and the storage elastic modulus G ′s of the shell resin is 10 8 Pa or more.
  • the coated particles it is difficult for the coated particles to aggregate during preheating, and it is possible to provide a method and powder material capable of sufficiently sintering the coated particles with a small amount of laser energy.
  • FIG. 1A is a schematic cross-sectional view of coated particles in one embodiment of the present invention.
  • FIG. 1B is a schematic cross-sectional view of a coated particle in another embodiment of the present invention.
  • FIG. 2 is a side view schematically showing the configuration of the three-dimensional modeling apparatus in one embodiment of the present invention.
  • FIG. 3 is a diagram showing the main part of the control system of the three-dimensional modeling apparatus in one embodiment of the present invention.
  • the present inventors have conducted intensive studies and experiments on powder materials for powder bed fusion bonding.
  • the present inventors have a core resin and a shell resin that coats the core resin as the coated particles for the powder bed fusion bonding method, and the storage elastic modulus G ′ of the shell resin is 10 6.5 Pa.
  • TS (65) is capable of melting and bonding the coated particles with a low laser energy amount by adopting coated particles higher than the temperature TC (65) at which the storage elastic modulus G ′ of the core resin becomes 10 6.5 Pa. I found.
  • the coated particles satisfying the above relationship by making the powder material containing coated particles in which the absolute value of the difference between the SP value of the core resin and the SP value of the shell resin is within a specific range, Regardless of the combination, it was further found that the strength of the three-dimensional modeled product was reduced and the particles were prevented from agglomerating during preheating, and a three-dimensional molded product having high strength was obtained, and the present invention was achieved.
  • core-shell type coated particles comprising a core resin having a relatively low storage modulus at a preheating temperature and a shell resin having a relatively high storage modulus at a preheating temperature are used in the powder bed melt bonding method.
  • the shell resin can maintain an appropriate rigidity, it is difficult for the coated particles to bind to each other at the time of preheating, and deformation of the coated particles hardly occurs.
  • the laser beam is irradiated, the shell resin softens, dissolves, or disappears, and the coated particles are melt-bonded.
  • the core resin since the core resin has already been softened or melted, it is not necessary to soften or melt all the core resin by laser light irradiation. That is, it is possible to bind the coated particles with a relatively small amount of laser energy.
  • the particles are aggregated due to deformation of the coated particles during the preheating or disappearance of the layer made of the shell resin. May end up.
  • the reason is considered that the core resin and the shell resin are easily compatible with each other.
  • the compatibility of the core resin and the shell resin is excessive, when the core resin is softened or melted by preheating, the shell resin is dissolved in the core resin. Therefore, it is considered that the layer made of the shell resin becomes thin or the layer made of the shell resin disappears and the particles are aggregated during the preheating.
  • the strength of the three-dimensional model may not be sufficiently increased.
  • the reason may be that the compatibility between the core resin and the shell resin is excessively low. If the compatibility between the core resin and the shell resin is excessively low, the softened or melted shell resin and the core resin are likely to be separated after the laser light irradiation. Therefore, it is thought that the area
  • the absolute value of the difference between the SP value of the core resin and the SP value of the shell resin (hereinafter also referred to as “ ⁇ SP”) is determined as described below. Range.
  • ⁇ SP the absolute value of the difference between the SP value of the core resin and the SP value of the shell resin
  • Range the absolute value of the difference between the SP value of the core resin and the SP value of the shell resin.
  • preliminary heating can be performed without agglomerating the coated particles. Since the preliminary heating can be sufficiently performed, the coated particles can be sufficiently melt-bonded even with a small amount of laser energy.
  • ⁇ SP is not too large, the core resin and the shell resin are compatible with each other after the laser light irradiation, and are difficult to separate. Therefore, according to this embodiment, there also exists an advantage that the intensity
  • Patent Document 1 shows the core-shell type particle
  • Patent Documents 2 to 4 described above relate to an electrophotographic toner, and preheating is not performed when an electrophotographic image is produced. Therefore, the techniques of Patent Documents 2 to 4 do not give sufficient consideration to the problems caused by the preheating as described above. From the viewpoint of heat resistance, etc., the electrophotographic toners described therein are powder bed melt bonded. It is difficult to obtain coated particles for the method.
  • Powder material The powder material of this embodiment is used for manufacturing a three-dimensional structure by a powder bed fusion bonding method. More specifically, repeated preheating of the thin layer of the powder material containing the coated particles and selective laser light irradiation to the thin layer are performed to laminate a plurality of layers of the modeled object in which the coated particles are melt-bonded. And used in a method of manufacturing a three-dimensional model.
  • the powder material only needs to contain at least coated particles, and may be composed only of coated particles.
  • the powder material may further include a material other than the coated particles including the laser absorber and the flow agent as long as the melt bonding by laser light irradiation is not hindered.
  • the coated particle has a core resin and a structure in which this is coated with a shell resin (hereinafter, this structure is also referred to as “core-shell structure”).
  • the core-shell structure means that the ratio of the area of the portion covered with the shell resin in the surface of the core particles basically composed of the core resin is 90% or more.
  • TEM transmission electron microscope
  • the ratio of the coated area of the shell resin to the surface area of the core particles is calculated for 10 arbitrarily selected coated particles. And if those average values are 90% or more, it will be considered that those coated particles have a core-shell structure.
  • the coated particles having a core-shell structure may be coated particles 100 in which a core particle 101 is coated with a sheet-like shell resin 102 as shown in FIG. 1A, which is a schematic cross-sectional view showing one embodiment. Further, as shown in FIG. 1B, which is a schematic cross-sectional view showing another embodiment, coated particle 100 in which core particle 101 is coated with particulate shell resin 102 may be used.
  • the coated particles preferably have a storage elastic modulus G′c of the core resin lower than a storage elastic modulus G ′s of the shell resin at the preheating temperature in the manufacturing method of the three-dimensional structure to be described later.
  • the core resin can be preferentially softened by preheating. Whether the storage elastic modulus (G′c and G ′s) of the core resin and the shell resin satisfies the above relationship at the preheating temperature depends on the temperature TS (the storage elastic modulus G ′ of the shell resin becomes 10 6.5 Pa ). 65) and the temperature TC (65) at which the storage elastic modulus G ′ of the core resin becomes 10 6.5 Pa can be estimated to some extent. In this embodiment, TS (65) is more than TC (65) . High.
  • the storage elastic modulus G′c of the core resin at the preheating temperature in the method for manufacturing a three-dimensional model to be described later is specifically preferably 10 6 Pa or less, and preferably 10 1 Pa to 10 6 Pa. Is more preferably 10 2 Pa to 10 6 Pa.
  • the storage elastic modulus G′c of the core resin at the preheating temperature is 10 6 Pa or less, it is possible to reduce the amount of laser energy required for softening or melting the core resin at the time of laser light irradiation.
  • the storage elastic modulus G ′s of the shell resin at the preheating temperature is specifically preferably 10 8 Pa or more, more preferably 10 8 Pa to 10 9.5 Pa, and more preferably 10 8.
  • the preheating temperature is appropriately set according to the type of the coated particles and the like, and can be set similarly to a general powder bed fusion bonding method.
  • the preheating temperature is preferably 50 ° C or higher and 300 ° C or lower, more preferably 100 ° C or higher and 300 ° C or lower, further preferably 100 ° C or higher and 250 ° C or lower, and 140 ° C or higher and 250 ° C or lower. More preferably it is.
  • the absolute value ⁇ SP of the difference between the SP value of the shell resin of the coated particles and the SP value of the shell resin is 2.5 (J / cm 3 ) 1/2 to 7.0 (J / cm 3 ) 1/2 , and preferably 2.6 (J / cm 3 ) 1/2 to 6.7 (J / cm 3 ) 1/2 .
  • ⁇ SP is 2.5 (J / cm 3 ) 1/2 or more, the compatibility between the core resin and the shell resin is moderately suppressed, and the shell resin is difficult to dissolve in the core resin softened by the preheating. . That is, it is difficult for the layer made of the shell resin to be thinned or disappeared by the preheating, and the coated particles are hardly melt-bonded.
  • the shell resin and the core resin are difficult to separate after laser light irradiation. It is easy to sufficiently increase the strength of the three-dimensional structure to be obtained.
  • the SP value of the core resin and the shell resin may be high.
  • the SP value of the shell resin is higher than that of the core resin, it is considered that when the shell resin is melted, the shell resin attempts to lower the surface tension, and fusion bonding between particles is promoted.
  • the SP value of the shell resin is lower than that of the core resin, it is considered that the shell resin is likely to move inside the particles when the particles are melted, and it is considered that fusion bonding between the core resins is promoted.
  • the unit of the SP value (solubility parameter) in this specification is (J / cm 3 ) 1/2 , and in this specification, the value at 25 ° C. is expressed unless otherwise specified.
  • the SP value is a value ⁇ determined based on the following equation by the Fedors method [Robert F. Fedors, Polymer Engineering and Science, 14, 47-154 (1974)].
  • Fedors equation: ⁇ ( ⁇ ei / ⁇ vi) 1/2 [Where ⁇ ei is the evaporation energy (J / mol) of atoms and atomic groups, and ⁇ vi is the molar volume (cm 3 / mol).
  • each SP value of core resin and shell resin can be measured, for example using a cloud point titration method.
  • a polymer solution in which only the core resin or only the shell resin is dissolved is prepared.
  • a poor solvent is dripped at the said polymer solution, and the quantity of the poor solvent required until it produces turbidity is calculated
  • measurement is performed for a poor solvent (eg, water) having a high SP value and a poor solvent (eg, n-hexane) having a low SP value. It can be calculated based on the method described in KWSuh, JMCorbett; J. Apply Polym. Sci., 12 (10), p2359-2370 (1968).
  • the coated particles are melt-bonded due to softening, melting, or disappearance of the shell resin. Therefore, the temperature at which the shell resin softens, melts, or disappears from the viewpoint of making the shell resin soften, melt, or disappear easily by laser light irradiation, and the three-dimensional structure is manufactured in a shorter time, and the core resin
  • the softening or melting temperature is preferably a close value.
  • the temperature difference is preferably small in order to melt-bond the coated particles while the volume change of the core resin is small.
  • the temperature difference is not too small from the viewpoint of suppressing deformation of the coated particles during preheating, that is, suppressing softening of the shell resin.
  • the difference between the above TS (65) and TC (65) is preferably 5 ° C. or higher and 75 ° C. or lower, more preferably 5 ° C. or higher and 70 ° C. or lower, and more preferably 10 ° C. or higher and 70 ° C. or lower. More preferably, it is more preferably 10 ° C. or more and 60 ° C. or less, and further preferably 30 ° C. or more and 60 ° C. or less.
  • the temperature TC (65) at which the storage elastic modulus G ′ of the core resin becomes 10 6.5 Pa is preferably included in the range of the general preheating temperature in the powder bed fusion bonding method. Therefore, TC (65) is preferably 50 ° C. or higher and 300 ° C. or lower, more preferably 100 ° C. or higher and 300 ° C. or lower, further preferably 100 ° C. or higher and 250 ° C. or lower, and 140 ° C. or higher and 250 ° C. or lower. More preferably, it is not higher than ° C.
  • the temperature TS (65) at which the storage elastic modulus G ′ of the shell resin becomes 10 6.5 Pa is a temperature at which the core resin can be easily melted by irradiation with laser light while ensuring the freedom of selection of the core resin. It is preferable to be in the range. Therefore, TS (65) is preferably 100 ° C. or higher and 350 ° C. or lower, more preferably 150 ° C. or higher and 350 ° C. or lower, further preferably 150 ° C. or higher and 330 ° C. or lower, and 170 ° C. or higher and 330 ° C. or lower. It is more preferable that the temperature is not higher than 170C, and it is more preferable that the temperature is not lower than 170C and not higher than 300C.
  • the core resin is preferably solidified in a shorter time during cooling after the laser light irradiation.
  • the temperature at which the core resin softens (temperature TC (65) at which the storage elastic modulus G ′ becomes 10 6.5 Pa) and the temperature at which the core resin becomes hard enough to be deformed (storage elastic modulus G ′)
  • the temperature difference with the temperature (TC (70) ) at which 10 7.0 Pa is reached is small, specifically,
  • each storage elastic modulus can be a value measured by a known method.
  • a value obtained by measurement by a method using a storage elastic modulus measuring apparatus is defined as the storage elastic modulus.
  • viscoelasticity data may be measured according to the following procedure with the coated particles having the core-shell structure.
  • the core resin is removed by immersing the coated particles in a solvent that dissolves only the core resin and dissolving the core resin. And viscoelasticity data is measured with respect to the remaining shell resin according to the following procedures.
  • the core resin or shell resin that constitutes the coated particles is separated and extracted with a solvent that dissolves only one of the core resin and the shell resin, and dried to form a powder.
  • a pressure molding machine (NT-100H manufactured by NP System Co., Ltd.)
  • the obtained powder is pressed at 30 kN for 1 minute at room temperature to form a cylindrical sample having a diameter of about 8 mm and a height of about 2 mm. .
  • Measurement frequency 6.28 radians / second Measurement distortion setting: The initial value is set to 0.1%, and measurement is performed in the automatic measurement mode.
  • Sample extension correction Adjust in automatic measurement mode.
  • Measurement temperature Slow cooling from 250 ° C. to 100 ° C. at a rate of 5 ° C. per minute.
  • Measurement interval Viscoelasticity data is measured every 1 ° C.
  • the average particle diameter of the coated particles is preferably 2 ⁇ m or more and 210 ⁇ m or less, and more preferably 10 ⁇ m or more and 80 ⁇ m or less.
  • the average particle diameter of the coated particles is 2 ⁇ m or more, the thickness of each modeled object layer produced by the method for manufacturing a three-dimensional modeled object described later tends to be sufficiently thick, and a three-dimensional modeled object can be manufactured efficiently.
  • the average particle diameter of the coated particles is 210 ⁇ m or less, a three-dimensionally shaped object having a complicated shape can be produced.
  • the average particle size of the core is preferably 1 ⁇ m or more and 200 ⁇ m or less, more preferably 2 ⁇ m or more and 150 ⁇ m or less, further preferably 5 ⁇ m or more and 100 ⁇ m or less, and 5 ⁇ m or more and 70 ⁇ m or less. Is more preferably 10 ⁇ m or more and 60 ⁇ m or less.
  • the average particle diameter of the core is 1 ⁇ m or more, the powder material has sufficient fluidity, so that it becomes easy to handle the powder material when manufacturing the three-dimensional structure. Further, when the average particle diameter is 1 ⁇ m or more, the core resin can be easily produced, and the production cost of the powder material does not increase.
  • the average particle diameter is 200 ⁇ m or less, it becomes possible to produce a higher-definition three-dimensional modeled object.
  • the thickness of the shell is preferably 10 to 500 nm, more preferably 20 to 500 nm, further preferably 40 to 500 nm, and more preferably 40 to 450 nm. More preferably.
  • the average particle diameter of the particles constituting the shell resin is preferably smaller than the average particle diameter of the core resin particles, and the average particle diameter of the core resin is More preferably, it is half or less.
  • the thickness of the layer made of the core resin is 10 nm or more, it is difficult for the coated particles to aggregate during preheating.
  • the thickness is 500 nm or less, deformation such as warpage hardly occurs in the obtained molded article.
  • the average particle diameter of the coated particles is a volume average particle diameter measured by a dynamic light scattering method.
  • the volume average particle diameter can be measured with a laser diffraction particle size distribution measuring apparatus (manufactured by SYMPATEC, HELOS) equipped with a wet disperser.
  • the average particle diameter of the core and the thickness of the shell are the thickness of the layer made of the shell resin for 10 randomly selected coated particles in an image obtained by imaging a cross section of a large number of coated particles with a TEM. Ten points are actually measured, and an average value thereof can be adopted.
  • the amount of the core resin and the shell resin in the coated particles may be an amount that allows the core-shell structure to be formed.
  • the amount of the shell resin with respect to 100 parts by mass of the core resin is preferably 0.1 parts by mass or more and 20 parts by mass or less, more preferably 0.5 parts by mass or more and 20 parts by mass or less. More preferably, they are 1 mass part or more and 15 mass parts or less, More preferably, they are 1 mass part or more and 15 mass parts or less, More preferably, they are 1 mass part or more and 10 mass parts or less.
  • the circularity of the coated particles is preferably 0.95 or more, more preferably 0.96 or more, and further preferably 0.97 or more.
  • the degree of circularity of the coated particles is 0.95 or more, the volume of each coated particle tends to be uniform, and it becomes easy to form a shaped article layer in a desired shape.
  • the circularity indicates the average circularity of the coated particles, and is a value measured using “FPIA-2100” (manufactured by Sysmex).
  • the coated particles are wetted with an aqueous surfactant solution, and ultrasonic dispersion is performed for 1 minute. Then, using “FPIA-2100”, measurement is performed at an appropriate density of 3000 to 10,000 HPF detections in a measurement condition HPF (high magnification imaging) mode. Within this range, reproducible measurement values can be obtained.
  • the average circularity is an arithmetic average value obtained by adding the circularity of each particle and dividing by the total number of particles measured.
  • the core resin and the shell resin of the above-described coated particles are not particularly limited as long as they are resins that are softened or melted by heating, and the above-described ⁇ SP, TS (65) , TC (65) , storage elastic modulus, etc. Each can be selected in consideration.
  • a resin that disappears by heating can be selected as the shell resin.
  • resins applicable to the core resin and the shell resin include crystalline resins such as polyethylene, polypropylene, nylon, polyacetal, polyethylene terephthalate (PET), polyphenyl sulfide, polyether ether ketone (PEEK), and crystalline polyester.
  • Polystyrene polyurethane, polyvinyl chloride, acrylonitrile-butadiene-styrene copolymer (ABS), acrylic polymer, polycarbonate, ethylene-vinyl acetate copolymer (EVA), styrene-acrylonitrile copolymer (SAN), polyarylate, polyethersulfone (PES) ), Non-crystalline resins such as polyphenylene ether and polycaprolactone.
  • ABS acrylonitrile-butadiene-styrene copolymer
  • EVA ethylene-vinyl acetate copolymer
  • SAN styrene-acrylonitrile copolymer
  • PES polyarylate
  • PES polyethersulfone
  • Non-crystalline resins such as polyphenylene ether and polycaprolactone.
  • the powder material may contain components other than the above-described coated particles, and examples thereof include a laser absorber and a flow agent.
  • the powder material may further include a laser absorber.
  • the laser absorber may be a material that absorbs a laser having a wavelength to be used and generates heat. Examples of such laser absorbers include carbon powder, nylon resin powder, pigments, and dyes. These laser absorbers may be used alone or in combination of two types.
  • the amount of the laser absorber can be appropriately set within a range that facilitates the melt bonding of the coated particles. For example, it can be more than 0 mass% and less than 3 mass% with respect to the total mass of the powder material.
  • the powder material may further include a flow agent.
  • the flow agent may be a material having a small coefficient of friction and self-lubricating properties. Examples of such flow agents include silicon dioxide and boron nitride. These flow agents may be used alone or in combination.
  • the amount of the flow agent can be appropriately set within a range in which the fluidity of the powder material is improved and the melt-bonding of the coated particles having the core-shell structure is sufficiently generated, for example, with respect to the total mass of the powder material, It can be more than 0% by mass and less than 2% by mass.
  • the manufacturing method of the said powder material is not restrict
  • the coated particles can be used as the powder material as they are.
  • the powder material includes coated particles and other materials, the powdered other materials and the coated particles can be manufactured by stirring and mixing.
  • a method for preparing the coated particles will be described.
  • the aforementioned coated particles can be produced by a known method.
  • Examples of the method for preparing the coated particles include a wet coating method in which a coating solution in which a shell resin is dissolved in particles made of a core resin is applied, or a mixture of particles made of a core resin and particles made of a shell resin. And a dry coating method in which bonding is performed by mechanical impact, and a combination of these methods.
  • the coating solution may be spray-coated on the surface of the core resin, or the core resin may be immersed in the coating solution.
  • coated particles in which a core particle is coated with a sheet-like shell resin as shown in FIG. 1A can be obtained.
  • coated particles in which the core particles are coated with the particulate shell resin as shown in FIG. 1B can be obtained.
  • the wet coating method it is easy to form a layer made of a shell resin having a uniform thickness. Since the dry coating method does not require a drying step, the manufacturing process can be simplified.
  • the core resin and the shell resin are selected in consideration of ⁇ SP and the storage elastic modulus.
  • Commercially available core resins and shell resins may be used.
  • ⁇ SP of each resin may be calculated by the method described in the above-mentioned literature, or may be specified by a cloud point titration method.
  • TC (65) and TS (65) can be easily satisfied.
  • the core resin is selected from polyethylene, polypropylene, and polystyrene that tend to have a low Tg
  • the polyether ether ketone (PEEK), polycarbonate, and acrylic polymer that tend to have a high Tg are selected as the shell resin
  • the above-mentioned TC It becomes possible to easily satisfy the relationship between (65) and TS (65) .
  • Tg of commercially available resin is often announced by each manufacturer.
  • the SP value of the resin can be adjusted by the structure of the resin (for example, the functional group and the number of carbons in the main chain). Depending on the type of monomer or prepolymer used, It is possible to adjust.
  • the storage elastic modulus G ′ of the resin to be prepared can be controlled within a desired range by changing the average molecular weight of the resin. Specifically, if the average molecular weight of the prepared resin is increased, the storage elastic modulus G ′ of the resin is increased, and if the average molecular weight of the prepared resin is decreased, the storage elastic modulus G ′ of the resin is decreased.
  • the relationship between the molecular weight and the storage elastic modulus G ′ at the preheating temperature is examined in advance, and the molecular weight of the resin to be prepared is determined by referring to the above relationship at the next resin production. Also good.
  • the manufacturing method of the three-dimensional molded item of this embodiment it can carry out similarly to the normal powder bed fusion
  • Thin layer formation process (process (1)) In this step, a thin layer of the powder material is formed.
  • the powder material supplied from the powder supply unit is laid flat on a modeling stage by a recoater.
  • the thin layer may be formed directly on the modeling stage, or may be formed so as to be in contact with the already spread powder material or the already formed modeling layer.
  • the thickness of the thin layer is the same as the thickness of the desired object layer.
  • the thickness of a thin layer can be arbitrarily set according to the precision of the three-dimensional molded item to manufacture, it is 0.01 mm or more and 0.30 mm or less normally.
  • the thickness of the thin layer is 0.01 mm or more, it is possible to spread a uniform powder.
  • the thickness of the thin layer is more preferably 0.01 mm or more and 0.10 mm or less.
  • the thickness of the thin layer is determined by the beam spot diameter of the laser beam described later. It is preferable to set the difference of 0.10 mm or less.
  • Preheating process (process (2)) In this step, the thin layer of the formed powder material is preheated.
  • the preheating temperature is determined by the surface temperature of the thin layer after the preheating from the viewpoint of suppressing the pre-heated powder material from re-dissolving and distorting the modeling layer and reducing the modeling accuracy.
  • the storage elastic modulus G ′ is preferably set so as to be higher by 5 ° C. or more and 50 ° C. or less than the temperature TC (65) at which 10 6.5 Pa is obtained. Further, it is preferable to set the temperature so that the storage elastic modulus G′c of the core resin of the coated particles is 10 6 Pa or less and the storage elastic modulus G ′s of the shell resin is 10 8 Pa or more.
  • the preheating temperature is preferably 50 ° C or higher and 300 ° C or lower, more preferably 100 ° C or higher and 300 ° C or lower, further preferably 100 ° C or higher and 250 ° C or lower, and 140 ° C or higher and 250 ° C or lower. More preferably it is.
  • the heating time is preferably 1 to 30 seconds, more preferably 5 to 20 seconds.
  • Laser light irradiation process (process (3)) In this step, laser light is selectively irradiated to a position where a shaped article layer is to be formed in the preheated thin layer, and the coated particles at the irradiated position are melt-bonded. The melt-bonded coated particles are melted together with adjacent powders to form a melt-bonded body, which becomes a shaped article layer. At this time, since the coated particles that have received the energy of the laser beam are also melt-bonded to the already formed object layer, adhesion between adjacent layers also occurs.
  • the wavelength of a laser beam can be, for example, not less than 0.8 ⁇ m and not more than 12 ⁇ m.
  • the output condition of the laser beam may be set so that the storage elastic modulus G ′ of the core resin is 10 6 (Pa) or less.
  • the power at the time of laser beam output may be set within a range in which the shell resin is sufficiently melt-bonded at the laser beam scanning speed described later. Specifically, it can be set to 5.0 W or more and 60 W or less. From the viewpoint of reducing the energy of the laser beam, reducing the manufacturing cost, and simplifying the configuration of the manufacturing apparatus, the power at the output of the laser beam is preferably 30 W or less, preferably 20 W or less. More preferably.
  • the scanning speed of the laser beam may be set within a range that does not increase the manufacturing cost and does not excessively complicate the apparatus configuration. Specifically, it is preferably 1 mm / second to 100 mm / second, more preferably 1 mm / second to 80 mm / second, further preferably 2 mm / second to 80 mm / second, and more preferably 3 mm. / Mm or more and 80 mm / second or less is more preferable, and 3 mm / second or more and 50 mm / second or less is further preferable.
  • the beam diameter of the laser beam can be appropriately set according to the accuracy of the three-dimensional structure to be manufactured.
  • Step (1) to Step (3) When manufacturing a three-dimensional structure, the above steps (1) to (3) are repeated an arbitrary number of times in this order. Thereby, a modeling object layer is laminated
  • At least step (3) is preferably performed under reduced pressure or in an inert gas atmosphere.
  • the pressure at which the pressure is reduced is preferably 10 ⁇ 2 Pa or less, and more preferably 10 ⁇ 3 Pa or less.
  • the inert gas that can be used in the present embodiment include nitrogen gas and rare gas. Among these inert gases, nitrogen (N 2 ) gas, helium (He) gas, or argon (Ar) gas is preferable from the viewpoint of availability. From the viewpoint of simplifying the production process, it is preferable to perform all of the steps (1) to (3) under reduced pressure or in an inert gas atmosphere.
  • the three-dimensional modeling apparatus 200 which can be used for the manufacturing method of the said three-dimensional molded item is demonstrated.
  • the three-dimensional modeling apparatus that can be used in the present embodiment can have the same configuration as a known three-dimensional modeling apparatus.
  • the three-dimensional modeling apparatus 200 according to the present embodiment includes a modeling stage 210 located in the opening, and a thin film forming unit 220 for forming a thin film made of a powder material.
  • the base 290 is provided.
  • the three-dimensional modeling apparatus 200 controls the thin film forming unit 220, the preheating unit 230, the laser irradiation unit 240, and the stage support unit 250 to form and stack a modeled object, Display unit 270 for displaying various types of information, operation unit 275 including a pointing device for receiving instructions from the user, storage unit 280 for storing various types of information including control programs executed by control unit 260, and external You may provide the data input part 285 containing the interface etc. for transmitting / receiving various information, such as three-dimensional modeling data, between apparatuses.
  • the three-dimensional modeling apparatus 200 may include a temperature measuring device 235 that measures the surface temperature of the thin layer formed on the modeling stage 210.
  • the three-dimensional modeling apparatus 200 may be connected to a computer device 300 for generating three-dimensional modeling data.
  • the modeling stage 210 is controlled to be movable up and down, and on the modeling stage 210, a thin layer is formed by the thin film forming unit 220, a thin layer is preheated by the preheating unit 230, and a laser beam is irradiated by the laser irradiation unit 240. Done. And the modeling thing formed by these is laminated
  • the thin film forming unit 220 includes a powder material storage unit 221a that stores a powder material, a powder supply unit 221 that is provided at the bottom of the powder material storage unit 221a, and a supply piston 221b that moves up and down in the opening.
  • the supplied powder material can be laid flat on the modeling stage 210 to form a recoater 222a that forms a thin layer of the powder material.
  • the upper surface of the opening of the powder material storage unit 221a is disposed on substantially the same plane as the upper surface of the opening for moving the modeling stage 210 up and down (for forming a three-dimensional modeled object).
  • the powder supply unit 221 discharges a powder material storage unit (not shown) provided vertically above the modeling stage 210 and the powder material stored in the powder material storage unit in desired amounts. It is good also as a structure provided with the nozzle (not shown) for this. In this case, a thin layer can be formed by uniformly discharging the powder material from the nozzle onto the modeling stage 210.
  • the preheating unit 230 only needs to be able to heat a region of the surface of the thin layer where the shaped article layer is to be formed and maintain the temperature.
  • the preheating unit 230 heats the first heater 231 that can heat the surface of the thin layer formed on the modeling stage 210 and the powder material before being supplied onto the modeling stage.
  • the heater 232 is provided, but only one of them may be provided.
  • region which should form the said molded article layer may be sufficient as the preheating part 230.
  • the structure which heats the whole inside apparatus previously and controls the surface of the said thin film to predetermined temperature may be sufficient.
  • the temperature measuring device 235 may be any device that can measure the surface temperature of a thin layer, particularly the surface temperature of a region where a shaped article layer is to be formed, without contact, and may be, for example, an infrared sensor or an optical pyrometer.
  • the laser irradiation unit 240 can include a laser light source 241 and a galvano mirror 242a.
  • the laser irradiation unit 240 may include a laser window 243 that transmits laser light and a lens (not shown) for adjusting the focal length of the laser light to the surface of the thin layer.
  • the laser light source 241 may be a light source that emits the laser light having the wavelength with the output. Examples of the laser light source 241 include a YAG laser light source, a fiber laser light source, and a CO 2 laser light source.
  • the galvanometer mirror 242a may include an X mirror that reflects the laser light emitted from the laser light source 241 and scans the laser light in the X direction and a Y mirror that scans in the Y direction.
  • the laser window 243 may be made of a material that transmits laser light.
  • the stage support unit 250 may be any unit that variably supports the vertical position of the modeling stage 210. That is, the modeling stage 210 is configured to be precisely movable in the vertical direction by the stage support portion 250.
  • Various configurations can be adopted as the stage support portion 250.
  • the stage support portion 250 is related to a holding member that holds the modeling stage 210, a guide member that guides the holding member in the vertical direction, and a screw hole provided in the guide member. It can be constituted by a ball screw or the like to be combined.
  • the control unit 260 includes a hardware processor such as a central processing unit, and controls the overall operation of the 3D modeling apparatus 200 during the modeling operation of the 3D model.
  • control unit 260 may be configured to convert, for example, the three-dimensional modeling data acquired by the data input unit 285 from the computer apparatus 300 into a plurality of slice data sliced in the stacking direction of the modeled object layer.
  • Slice data is modeling data of each modeled object layer for modeling a three-dimensional modeled object.
  • the thickness of the slice data that is, the thickness of the modeled object layer matches the distance (lamination pitch) corresponding to the thickness of one layer of the modeled object layer.
  • the display unit 270 can be, for example, a liquid crystal display or a monitor.
  • the operation unit 275 can include a pointing device such as a keyboard and a mouse, for example, and may include various operation keys such as a numeric keypad, an execution key, and a start key.
  • the storage unit 280 may include various storage media such as a ROM, a RAM, a magnetic disk, an HDD, and an SSD.
  • the three-dimensional modeling apparatus 200 receives the control of the control unit 260 and decompresses the inside of the apparatus.
  • the decompression unit (not shown) such as a decompression pump or the control unit 260 controls the inert gas into the apparatus. You may provide the inert gas supply part (not shown) to supply.
  • the control unit 260 converts the three-dimensional modeling data acquired from the computer apparatus 300 by the data input unit 285 into a plurality of slice data sliced thinly in the stacking direction of the modeled object layer. Thereafter, the control unit 260 controls the following operations in the three-dimensional modeling apparatus 200.
  • the powder supply unit 221 drives a motor and a drive mechanism (both not shown) according to the supply information output from the control unit 260, moves the supply piston upward (in the direction of the arrow in FIG. 2), and the modeling Extrude the powder material on the same horizontal plane as the stage.
  • the recoater driving unit 222 moves the recoater 222a in the horizontal direction (in the direction of the arrow in the figure) according to the thin film formation information output from the control unit 260, conveys the powder material to the modeling stage 210, and the thin layer The powder material is pressed so that the thickness becomes the thickness of one layer of the shaped article layer.
  • the preheating unit 230 heats the surface of the thin layer formed in accordance with the temperature information output from the control unit 260 or the entire apparatus.
  • the temperature information is stored in the control unit 260 based on, for example, data on the temperature TC ( 65 ) at which the storage elastic modulus G ′ of the material constituting the core resin, which is input from the data input unit 285, becomes 10 6.5 Pa. It can be used as information for heating the surface of the thin layer to a temperature drawn from the portion 280 so that the difference from the above temperature is 5 ° C. or more and 50 ° C. or less.
  • the preheating unit 230 may start the heating after the thin layer is formed, or the portion corresponding to the surface of the thin layer to be formed before the thin layer is formed or heating in the apparatus. May be.
  • the laser irradiation unit 240 emits laser light from the laser light source 241 in accordance with the laser irradiation information output from the control unit 260, in accordance with the area constituting the three-dimensional object in each slice data on the thin film,
  • the galvano mirror driving unit 242 drives the galvano mirror 242a to scan the laser beam.
  • the coated particles contained in the powder material are melt-bonded by the irradiation of the laser beam, and a shaped article layer is formed.
  • the stage support unit 250 drives a motor and a drive mechanism (both not shown) according to the position control information output from the control unit 260, and moves the modeling stage 210 vertically downward (in the direction of the arrow in the drawing). )
  • the display unit 270 displays various information and messages that should be recognized by the user under the control of the control unit 260 as necessary.
  • the operation unit 275 receives various input operations by the user and outputs an operation signal corresponding to the input operation to the control unit 260. For example, a virtual three-dimensional object to be formed is displayed on the display unit 270 to check whether or not a desired shape is formed. If the desired shape is not formed, the operation unit 275 may be modified. Good.
  • the control unit 260 stores data in the storage unit 280 or extracts data from the storage unit 280 as necessary.
  • control part 260 receives the information of the temperature of the area
  • the heating by the unit 230 may be controlled.
  • the modeled object layer is laminated and a three-dimensional modeled object is manufactured.
  • powder materials 2-7, 9, and 10 In the same manner as powder material 1 except that the types of resins are as shown in Table 2, powder materials 2-7, 9, and 10 was obtained. Powder materials 2 and 3 were prepared in the same manner as powder material 1 except that the spraying time of the PAR solution was 18 minutes and 164 minutes.
  • Measurement condition Measurement frequency: 6.28 radians / second.
  • Measurement strain setting The initial value was set to 0.1%, and measurement was performed in automatic measurement mode.
  • Sample extension correction Adjusted in automatic measurement mode.
  • Measurement interval Viscoelasticity data was measured every 1 ° C.
  • Thickness of layer made of shell resin The coated particles were dispersed in a photocurable resin (manufactured by JEOL Ltd., D-800) and then photocured to form a block. Using a microtome equipped with diamond teeth, a flaky sample having a thickness of 100 to 200 nm was cut out from the block and placed on a grid with a support film for transmission electron microscope observation. The grid was placed on a scanning transmission electron microscope (JSM-7401F, manufactured by JEOL Ltd.), and a bright field image was taken under the following conditions.
  • JSM-7401F scanning transmission electron microscope
  • a cross section of a large number of coated particles is imaged with a TEM, the interface between the core resin and the shell resin of 10 coated particles randomly selected from the obtained images is confirmed, and the thickness of the shell resin of each coated particle is measured. And the average of those was calculated
  • Laser output 50W
  • Laser light wavelength 10 ⁇ m
  • Beam diameter 170 ⁇ m on the surface of the thin layer
  • Vacuum mode Low vacuum mode Acceleration voltage: 5 kV Magnification: 250 times Time from the start of electron irradiation to the start of imaging: 3 minutes Sample: Sputtered Sample stage: Made of aluminum, grounded
  • the melting characteristics were evaluated according to the following criteria. ⁇ : All coated particles found in the SEM image were sintered or melt-bonded with the adjacent powder. ⁇ : 50% or more and less than 100% of the coated particles found in the SEM image were the adjacent powder. Sintered or melt bonded X: Less than 50% of the powder material in the SEM image was sintered or melt bonded to the adjacent powder
  • the absolute value ⁇ SP of the difference between the SP value of the core resin and the SP value of the shell resin is 2.5 (J / cm 3 ) 1/2 to 7.0 (J / cm 3 )
  • the aggregation generation temperature was higher than the preheating temperature, and no aggregation occurred during the preheating.
  • the melting characteristics were all good. Since the preheating temperature could be increased to 170 ° C. or higher, each powder material could be sufficiently sintered with the same amount of laser energy.
  • the present invention is considered to contribute to further spread of the powder bed fusion bonding method.

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Abstract

Le problème décrit par la présente invention est de fournir : un matériau en poudre qui n'est pas sensible à l'agrégation de particules pendant un chauffage préliminaire, et qui permet un frittage suffisant de particules revêtues avec une quantité d'énergie laser inférieure ; et un procédé de modélisation tridimensionnelle. La solution de la présente invention porte sur un matériau en poudre qui est utilisé dans un procédé de production d'un modèle tridimensionnel par stratification d'une pluralité de couches de modèle en trois dimensions, dans chacune desquelles des particules revêtues sont fondues et liées l'une aux autres, en répétant la formation d'une couche mince d'un matériau en poudre qui contient des particules revêtues, le chauffage préliminaire de la couche mince et le rayonnement de lumière laser sélective sur la couche mince est configuré de telle sorte que chacune des particules revêtues contient une résine centrale et une résine d'enveloppe qui recouvre la résine centrale. Dans ce raccordement, la valeur absolue de la différence entre la valeur SP de la résine centrale et la valeur SP de la résine d'enveloppe est définie à 2,5 (J/cm3)1/2 à 7,0 (J/cm3)1/2, tout en définissant la température TS(65) à laquelle le module d'élasticité de stockage G' de la résine d'enveloppe est de 106,5 Pa supérieur à la température TC(65) à laquelle le module d'élasticité de stockage G' de la résine centrale est de 106,5 Pa.
PCT/JP2017/008708 2016-03-23 2017-03-06 Matériau en poudre et procédé de production d'un modèle tridimensionnel Ceased WO2017163834A1 (fr)

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WO2019117016A1 (fr) * 2017-12-13 2019-06-20 コニカミノルタ株式会社 Méthode de production d'un objet moulé tridimensionnel, et matériau en poudre utilisé dans celle-ci
CN112060572A (zh) * 2019-06-11 2020-12-11 珠海赛纳三维科技有限公司 三维物体成型方法和成型装置
CN113087928A (zh) * 2020-01-08 2021-07-09 波音公司 用于改进的增材制造部件的涂覆粉末颗粒
JP2023002536A (ja) * 2017-11-22 2023-01-10 フォージ ナノ インコーポレイティド 機能化された粉末原料からナノ構造の相を有するワークピースの製造

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JP2018118413A (ja) * 2017-01-24 2018-08-02 コニカミノルタ株式会社 粉末材料、およびこれを用いた立体造形物の製造方法、ならびに立体造形装置
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JP7696877B2 (ja) 2017-11-22 2025-06-23 フォージ ナノ インコーポレイティド 機能化された粉末原料からナノ構造の相を有するワークピースの製造
CN108044930A (zh) * 2017-11-23 2018-05-18 上海汉信模具制造有限公司 一种塑胶粉末随形阶梯温度床的增材制造方法
WO2019117016A1 (fr) * 2017-12-13 2019-06-20 コニカミノルタ株式会社 Méthode de production d'un objet moulé tridimensionnel, et matériau en poudre utilisé dans celle-ci
JPWO2019117016A1 (ja) * 2017-12-13 2020-12-24 コニカミノルタ株式会社 立体造形物の製造方法、およびそれに用いる粉末材料
JP7111111B2 (ja) 2017-12-13 2022-08-02 コニカミノルタ株式会社 立体造形物の製造方法、およびそれに用いる粉末材料
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CN112060572A (zh) * 2019-06-11 2020-12-11 珠海赛纳三维科技有限公司 三维物体成型方法和成型装置
CN113087928A (zh) * 2020-01-08 2021-07-09 波音公司 用于改进的增材制造部件的涂覆粉末颗粒
JP2021109443A (ja) * 2020-01-08 2021-08-02 ザ・ボーイング・カンパニーThe Boeing Company 改善された付加製造部品のための被覆粉末
JP7680210B2 (ja) 2020-01-08 2025-05-20 ザ・ボーイング・カンパニー 改善された付加製造部品のための被覆粉末

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