WO2021080399A1 - Composition de liant pour préparation de corps fritté et procédé de retrait de liant - Google Patents

Composition de liant pour préparation de corps fritté et procédé de retrait de liant Download PDF

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WO2021080399A1
WO2021080399A1 PCT/KR2020/014659 KR2020014659W WO2021080399A1 WO 2021080399 A1 WO2021080399 A1 WO 2021080399A1 KR 2020014659 W KR2020014659 W KR 2020014659W WO 2021080399 A1 WO2021080399 A1 WO 2021080399A1
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binder
volume
thermoplastic component
solvent
solvent extraction
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PCT/KR2020/014659
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English (en)
Korean (ko)
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윤태식
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윤태식
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1017—Multiple heating or additional steps
    • B22F3/1021—Removal of binder or filler
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/638—Removal thereof

Definitions

  • the present invention manufactures a molded body by mixing a thermoplastic binder with metal powder, ceramic powder, carbide powder, etc., and undergoes a degreasing process to remove the binder from the molded body, and finally sintering to mass-produce three-dimensional precision parts (powder injection molding).
  • PIM' a composition of a binder and a method of removing the binder.
  • it relates to a binder composition and a method of removing the binder to increase the efficiency of removing the binder in an environment-friendly manner and to minimize deformation.
  • Powder injection molding technology is a production technology capable of manufacturing precision parts having a three-dimensional shape in large quantities, and is a part manufacturing technology using powder materials such as metal, carbide, and ceramic.
  • the biggest difference between powder injection molding technology and plastic injection molding technology is that in the powder injection molding process, the final product is manufactured through the high-temperature sintering process and removing the binder after injection molding, which is not performed in plastic injection molding.
  • the general manufacturing process of powder injection molding consists of the following processes.
  • the binder used in the powder injection molding process imparts fluidity to the mixture mixed with the powder so that a desired shape can be manufactured by injection molding. However, since the binder must be removed before final sintering, the ease of removal must also be excellent.
  • the binder component most commonly used as such a binder is a thermoplastic polymer.
  • the typical composition of the binder is a polymer material that maintains its shape until the final point of removal of the binder and is the main agent of the flow, and a low molecular weight material such as wax or polyethylene glycol that promotes the reduction of the viscosity of the mixture and lubrication with the mold.
  • a plasticizer to improve the flexibility of the polymer
  • a surfactant to improve the wettability or adhesion of the powder and polymer are added.
  • Polypropylene, polystyrene, polyethylene, ethylene vinyl acetate, polyoxymethylene, and the like are mainly used as the polymer material, and the low-molecular material is wax such as carnauba wax, paraffin wax, montan wax, beeswax, etc. Oil or polyethylene glycol is used. Solutions such as DBP and DOP are mainly used as plasticizers, and stearic acid and oleic acid are used as surfactants.
  • U.S. Patent No. 4,765,950 discloses that only a low melting point (paraffin wax, oil, etc.) material is selectively extracted from the binder by a solvent, and then the remaining main binder is removed as heat.
  • a method in which solvent extraction and thermal decomposition are mixed is disclosed.
  • the degreasing process of the organic binder used for molding has a very large effect on the manufacturing process time and cost of the entire sintered body, and therefore, it must be designed in consideration of formability and degreasing efficiency. .
  • An object of the present invention is to provide a binder composition that is not harmful to the human body, is safe, and can minimize degreasing time.
  • Another object of the present invention is to provide a method for removing a binder capable of efficiently removing the binder composition.
  • a first aspect of the present invention for solving one object of the present invention includes a first thermoplastic component and a second thermoplastic component, the first thermoplastic component includes stearic acid, paraffin wax and polyethylene glycol, the The second thermoplastic component comprises at least one selected from polyethylene, polypropylene, polyoxymethylene and ethylene vinyl acetate, the first thermoplastic component contains 30 to 70% by volume, and the second thermoplastic component is 30 to 70% by volume %, and the stearic acid is to provide a binder composition for producing a sintered body containing 1% by volume or more.
  • the first thermoplastic component may contain 40 to 60% by volume
  • the second thermoplastic component may contain 40 to 60% by volume
  • a second aspect of the present invention for solving one object of the present invention includes a first thermoplastic component, a second thermoplastic component, and a third thermoplastic component, and the first thermoplastic component is stearic acid, paraffin wax, and polyethylene glycol It includes at least one selected from among, and the second thermoplastic component includes at least one selected from polyethylene, polypropylene, polyoxymethylene and ethylene vinyl acetate, and the third thermoplastic component is styrene acrylonitrile (Styrene Acrylonitrile, SAN), wherein the sum of the first thermoplastic component and the third thermoplastic component includes 30 to 95% by volume, the second thermoplastic component includes 5 to 70% by volume, and the styrene acrylonitrile is 10 to It contains 65% by volume, and the stearic acid is to provide a binder composition for producing a sintered body containing 1% by volume or more.
  • SAN styrene acrylonitrile
  • the sum of the first thermoplastic component and the third thermoplastic component may include 40 to 60% by volume, and the second thermoplastic component may include 40 to 60% by volume.
  • a third aspect of the present invention for solving the other object of the present invention is a method of removing a binder from a molded article formed by mixing powder and a binder in a predetermined ratio.
  • a part of the binder contained in the molded article is removed using a solvent.
  • the binder is removed using a thermal decomposition method, the binder includes stearic acid, paraffin wax and polyethylene glycol, and the solvent extraction method includes n-PB (n-Propyl Bromide). It is to provide a method for removing a binder by simultaneously removing at least a part of the stearic acid, raffine wax, and polyethylene glycol using a solvent.
  • the binder further includes styrene acrylonitrile (SAN), and the styrene acrylonitrile is also removed by the n-PB (n-Propyl Bromide). can do.
  • SAN styrene acrylonitrile
  • n-PB n-Propyl Bromide
  • a fourth aspect of the present invention for solving the other object of the present invention is a method of removing a binder from a molded article formed by mixing powder and a binder in a predetermined ratio. First, a part of the binder contained in the molded article is removed using a solvent.
  • the binder After performing the solvent extraction method to remove, the binder is removed using a thermal decomposition method, the binder is a binder composition according to the first aspect or the second aspect, and the solvent extraction method is n-PB (n-Propyl Bromide)
  • n-PB n-Propyl Bromide
  • the molded article may be prepared in a ratio of 40 to 70% by volume of the powder and 30 to 60% by volume of the binder.
  • the solvent may contain 90% by volume or more of n-Propyl Bromide (n-PB).
  • the overall degreasing time can be minimized by removing polymers and small molecules through a method of immersing in a solvent. Through this, it is possible to reduce energy costs, improve productivity, and improve quality by minimizing deformation of the binder due to thermal decomposition.
  • the binder removal method according to the present invention can solve the harmful problem caused by the outflow of nitric acid gas compared to the conventional method of removing the binder using nitric acid gas.
  • the method of removing the binder according to the present invention does not require the use of a highly flammable petroleum-based solvent such as n-heptane, the risk of fire in the sintered body manufacturing process can be greatly reduced.
  • the binder removal method according to the present invention can remove the binder including stearic acid, paraffin wax, and polyethylene glycol together in a single process, which could not be removed in a single process in the prior art, and thus process efficiency can be improved.
  • FIG. 1 shows an injection molded article manufactured using a binder composition according to an embodiment of the present invention and its dimensions.
  • FIG. 2 shows a solvent extraction and drying step for removing a part of the binder contained in the injection molded article manufactured according to an embodiment of the present invention.
  • Figure 4 shows the results of measuring the amount of binder removal and the amount of deformation after removal of the binder of the binder composition according to Examples 1 to 6 of the present invention and the solvent extract of the molded article using the binder composition.
  • the binder composition according to Embodiment 1 of the present invention includes a first thermoplastic component including B1 and a second thermoplastic component including B2, as shown in Table 1 below.
  • Binder component Small molecule removed by solvent (B1) Paraffin wax Stearic acid Polyethylene glycol Polymer that cannot be removed by solvent (B2) Polyethylene Polypropylene Polyoxymethylene Ethylene vinyl acetate
  • B1 styrene acrylonitrile (SAN), which is a polymer of styrene and acrylonitrile, is used, and the crystal structure of the SAN is amorphous.
  • B1 is a paraffin wax (hereinafter referred to as paraffin wax).
  • PW paraffin wax
  • PEG polyethylene glycol
  • SA stearic acid
  • the paraffin wax is soluble in aliphatic hydrocarbon solvents such as hexane and heptane, but not in water, alcohol, acetone, and the like.
  • the polyethylene glycol is a hydrophilic polymer and is soluble in solvents such as water, toluene, alcohol, and acetone, but is not soluble in aliphatic hydrocarbon-based solvents such as hexane and heptane.
  • stearic acid is soluble in alcohol, acetone, and the like.
  • the wettability and fluidity are required at least a certain level during injection molding, it is advantageous for injection molding to contain stearic acid in an amount of 1% by volume or more when applied as a binder for injection molding.
  • the second thermoplastic component is a polymer material that is removed by thermal decomposition without being removed by a solvent, and includes B2 consisting of a single component or a composite component.
  • B2 may include one or more selected from polyethylene (polyethylene, hereinafter referred to as PE), polypropylene (polypropylene, hereinafter referred to as PP), polyoxymethylene (hereinafter referred to as POM), and ethylene vinyl acetate (hereinafter referred to as EVA). .
  • PE polyethylene
  • PP polypropylene
  • POM polyoxymethylene
  • EVA ethylene vinyl acetate
  • the polyoxymethylene has the highest softening point among the B2 components, which helps to maintain the shape of the powder formed in the pyrolysis process, and the final temperature of pyrolysis is the lowest at 400°C, so it may be effective for pyrolysis.
  • the ethylene vinyl acetate is preferably 10% by volume or less of the vinyl acetate (VA) content. This is because swelling occurs during solvent extraction as the content of vinyl acetate (VA) increases, and there is a possibility that cracks may occur in the molded body during the solvent extraction process. Because it increases.
  • B1 is a component that is removed from the solvent in the solvent extraction process, which is the first step of the binder removal process, to form pores, and maintains the shape of the molded body in the final thermal decomposition process, while B2 is decomposed into preformed pores and removed. If it is contained in less than% by volume, it is not sufficient to obtain the above effect, and if it is contained in more than 70% by volume, a large amount of pores is formed and is effective for thermal decomposition, which is the final stage, but the viscosity is low, so that the powder and the binder are separated during molding, jetting ( Since it is difficult to obtain a sound injection molded body due to the occurrence of jetting), etc., it is preferable to include it in the range of 30 to 70% by volume. More preferably, the content of B1 is 40 to 60% by volume.
  • B2 is a component that maintains its shape until the final point of removal of the binder and plays a role of a polymer material that is the main body of the flow. If it is included in less than 30% by volume, it is not sufficient to obtain the above effect, and contains more than 70% by volume. If the viscosity increases, the molding is difficult, and since the pyrolysis process must be treated for a long time, it is preferable to include in the range of 30 to 70% by volume. More preferably, the content of B2 is 40 to 60% by volume.
  • the binder composition according to Embodiment 2 of the present invention comprises a first thermoplastic component including B1, a second thermoplastic component including B2, and a third thermoplastic component including B3, as shown in Table 2 below.
  • Binder component Small molecule removed by solvent (B1) Paraffin wax Stearic acid Polyethylene glycol Polymer removed by solvent (B3) Styrene acrylonitrile Polymer that cannot be removed by solvent (B2) Polyethylene Polypropylene Polyoxymethylene Ethylene vinyl acetate
  • the B1 is composed of at least one selected from three components of paraffin wax (PW), polyethylene glycol (Polyetylene Glycol, PEG), and stearic acid (SA). That is, each of B1 may be used as a single component, or three components may be used in a certain ratio.
  • the paraffin wax is soluble in aliphatic hydrocarbon-based solvents such as hexane and heptane, but not in water, alcohol, acetone, etc. Does not.
  • the polyethylene glycol is a hydrophilic polymer and is soluble in solvents such as water, toluene, alcohol, and acetone, but is not soluble in aliphatic hydrocarbon-based solvents such as hexane and heptane.
  • stearic acid is soluble in alcohol, acetone, and the like.
  • paraffin wax, polyethylene glycol, and stearic acid constituting B1 of the first thermoplastic component in the present invention since they are removed with different solvents during conventional solvent extraction, they cannot be used at the same time.
  • a solvent containing n-PB it is possible to remove PEG, PW, and SA at the same time effectively, so that the degree of freedom in designing the blending ratio according to the properties required for the binder can be greatly increased.
  • the wettability and fluidity are required at least a certain level during injection molding, it is advantageous for injection molding to contain stearic acid in an amount of 1% by volume or more when applied as a binder for injection molding.
  • thermoplastic component B3 styrene acrylonitrile (SAN), which is a polymer of styrene and acrylonitrile, is used alone, and the crystal structure of the SAN is amorphous.
  • SAN styrene acrylonitrile
  • SAN While the SAN is removed through the solvent extraction process, it can play a role similar to the second thermoplastic component that prevents the separation of powder and binder, jetting, etc. from occurring during injection molding to obtain a sound injection molded body. It is an ingredient.
  • SAN can be removed in a solvent while playing a role similar to a polymer that is not removed in a solvent, it can be removed by any method of solvent extraction (or solvent degreasing) or thermal decomposition, thereby increasing the degree of freedom in the degreasing process.
  • injection molding properties can be improved, and solvent extraction and removal are possible through n-PB, which is a useful component in that it enables solvent extraction in a single process.
  • thermoplastic component As a second thermoplastic component, it is a polymer material that is not removed by a solvent but is removed by thermal decomposition, and includes B2 consisting of a single component or a composite component.
  • B2 may include one or more selected from polyethylene (polyethylene, hereinafter referred to as PE), polypropylene (polypropylene, hereinafter referred to as PP), polyoxymethylene (hereinafter referred to as POM), and ethylene vinyl acetate (hereinafter referred to as EVA). .
  • PE polyethylene
  • PP polypropylene
  • POM polyoxymethylene
  • EVA ethylene vinyl acetate
  • the polyoxymethylene has the highest softening point among the B2 components, which helps maintain the shape of the powder formed in the pyrolysis process, and the final temperature of pyrolysis is the lowest at 400°C, so it may be effective for pyrolysis.
  • the ethylene vinyl acetate is preferably 10% by volume or less of the vinyl acetate (VA) content. This is because swelling occurs during solvent extraction as the content of vinyl acetate (VA) increases, and there is a possibility that cracks may occur in the molded body during the solvent extraction process. Because it increases.
  • B1 and B3 are components that are removed from the solvent in the solvent extraction process, which is the first step of the binder removal process, to form pores, thereby maintaining the shape of the injection molded body in the final thermal decomposition process, while B2 is decomposed into preformed pores and removed. If the content of the combined polymer of B1 and B3 is less than 30% by volume, it is not sufficient to obtain the above effect, and if it is included in more than 95% by volume, a large amount of pores is formed, which may help the pyrolysis process, but the solvent When moving after extraction, it is fragile and may be damaged during handling, so it is preferable to include it in the range of 30 to 95% by volume. More preferably, the combined content of B1 and B3 is 40 to 80% by volume.
  • B1 is a component that is removed from the solvent in the solvent extraction process, which is the first step of the binder removal process, to form pores, and maintains the shape of the molded body in the final thermal decomposition process, while B2 is decomposed and removed into previously formed pores. If it is included in less than% by volume, it is not enough to obtain the above effect, and if it is included in more than 75% by volume, the viscosity is low, so separation of powder and binder, jetting, etc. occur during molding, making it difficult to obtain a sound injection molded body. , It is preferable to include in the range of 25 to 75% by volume.
  • Styrene Acrylonitrile (SAN) constituting B3 is a component that is removed from the solvent in the solvent extraction process, which is the first step of the binder removal process, to form pores, and when it is contained in less than 5% by volume, the It is not enough to obtain one effect, and if it is included in an amount exceeding 65% by volume, the viscosity of the mixture becomes high and injection molding is difficult, so it is preferable to include it in the range of 10 to 65% by volume.
  • B2 is a component that maintains its shape until the final point of removal of the binder and plays a role of a polymer material that is the main body of the flow. If it is included in less than 5% by volume, it is not sufficient to obtain the above effect, and contains more than 70% by volume. When the viscosity is low, separation of the powder and the binder, jetting, etc. occur during injection molding, so that it is difficult to obtain a sound injection molded body, so it is preferable to include it in the range of 5 to 70% by volume.
  • the sum of the combined amounts of the polymer materials B2 and B3 is less than 30% by volume, the viscosity is low, causing separation of the powder and the binder during injection molding, and jetting, making it difficult to obtain a sound injection molded body.
  • the sum of B1 and B2 exceeds 70% by volume, the viscosity may increase and defects such as unmolding may occur during injection molding. Therefore, the sum of B2 and B3 is preferably 30 to 70% by volume.
  • Embodiment 3 of the present invention relates to a solvent extraction method of a molded article formed by mixing a powder and a binder in a predetermined ratio.
  • the molded body may be prepared as a green body by a known method for preparing a molded body after preparing a feedstock by uniformly mixing the powder and the binder at a predetermined mixing ratio.
  • the powder various types of powders such as metal, ceramic, or a mixture thereof may be used, and any powder that can be prepared by a powder metallurgy method may be used without particular limitation.
  • the process of manufacturing the molded body may be any method capable of powder molding, such as a 3D printing method including powder injection molding, extrusion, and fused filament fabrication (FFF) methods, without limitation.
  • a 3D printing method including powder injection molding, extrusion, and fused filament fabrication (FFF) methods, without limitation.
  • FFF fused filament fabrication
  • Embodiment 3 of the present invention a solvent extraction method in which a part of the binder is removed using a solvent containing n-PB (n-Propyl Bromide) is performed, and then the remaining binder is removed through thermal decomposition. It is characterized in that the binder is removed through the process.
  • n-PB n-Propyl Bromide
  • n-PB n-Propyl Bromide
  • the n-PB is a substance represented by the molecular formula C 3 H 7 Br.
  • NFPA U.S. National Fire Protection Agency
  • the subsequent thermal degreasing process may be lengthened, and if the binder is removed in excess of 95% in the solvent degreasing process, it may be difficult to maintain the molded state. It is desirable to allow about 30 to 100% by volume, preferably 35 to 95% by volume of the possible binder composition to be removed.
  • the sum of paraffin wax (PW), polyethylene glycol (PEG), and stearic acid (SA) is 30 to 70% by volume. It is advantageous, and in the case of using a conventional petroleum solvent other than n-PB, it is advantageous to include the sum of paraffin wax (PW) and stearic acid (SA) in an amount of 30 to 70% by volume.
  • the binder includes all of stearic acid, paraffin wax, and polyethylene glycol, and solvent extraction of the binder contained in the molded article uses a solvent containing n-PB (n-Propyl Bromide).
  • n-PB n-Propyl Bromide
  • styrene acrylonitrile when included in the binder, it can be removed using a solvent including n-PB (n-Propyl Bromide) together with stearic acid, paraffin wax, and polyethylene glycol.
  • n-PB n-Propyl Bromide
  • a part of the binder was removed using a solvent extraction method, and then a thermal degreasing method by thermal decomposition was used. After removing the binder, a sintered body is manufactured through a sintering process.
  • the binder composition according to Examples 1 to 6 of the present invention is the binder composition according to the first embodiment, and the mixing amount of each component is as shown in FIG. 4. Comparative Examples 1 to 2 are prepared for comparison when out of the mixing range of Examples 1 to 6.
  • the metal powder used in the example of the present invention is a stainless steel (STS) 630 powder having an average particle diameter of 7 ⁇ m, and the injection molding mixture is a temperature of 180° C. in a sigma-type mixer at a ratio of 63:37 by volume of the metal powder and the binder. The mixture was mixed for 3 hours to prepare a feedstock.
  • STS stainless steel
  • the injection molded body was immersed in a closed solvent extraction tank containing a solution containing 90% or more of n-PB, and then B1 in the added binder was removed by circulating the solvent.
  • the solvent extraction temperature is preferably less than or equal to the boiling point of n-PB (70° C.), and at the same time, less than 70° C., which is less than or equal to the melting point of paraffin wax, polyethylene glycol, and stearic acid.
  • solvent extraction was maintained at 45° C. for 8 hours, cooled to room temperature, dried in a solvent extraction tank, weighed, and converted into a volume ratio (vol%) to calculate the extraction rate.
  • the solvent-extracted injection molded body was pyrolyzed at 20 L/min with nitrogen gas in a 30 L box furnace under a nitrogen atmosphere to remove the remaining binder components.
  • the solvent extractor was placed on an alumina plate as shown in FIG. 2, and the temperature rising rate from room temperature to 500° C. was raised to 2° C./min and maintained for 60 minutes, thereby completing the binder removal process.
  • the properties of the binder were evaluated by the strain rate, and the strain was calculated by measuring the distance deformed from the height of 11 mm in FIG. 2 in the direction of gravity with a two-dimensional projector, and the amount of strain 0.1 mm or less was used as a pass criterion.
  • the temperature was raised from 500° C. to 800° C. at 3° C./min and pre-sintered for 60 minutes to have the strength of the bwown part from which the binder was removed, and the strain rate was measured.
  • the sintering of the pre-sintered body from which the binder was removed was carried out by holding a vacuum furnace at 1,350°C for 2 hours using a vacuum furnace in an argon atmosphere.
  • FIG 3 shows an injection molded body manufactured through Examples and a sintered body sintered through a pyrolysis process after extraction of a solvent.
  • a part of the binder was removed using a solvent extraction method, and then a thermal degreasing method by thermal decomposition was used. After removing the binder, a sintered body is manufactured through a sintering process.
  • the binder composition according to Examples 7 to 16 of the present invention is the binder composition according to the second embodiment, and the mixing amount of each component is as shown in FIG. 5. Comparative Examples 3 to 5 are prepared for comparison when out of the mixing range of Examples 7 to 16.
  • the metal powder used in the embodiment of the present invention is a stainless steel (SUS) 630 powder having an average particle diameter of 7 ⁇ m.
  • the injection molding mixture is a metal powder and a binder at a temperature of 180°C in a sigma-type mixer in a volume ratio of 63:37. The mixture was mixed for 3 hours to prepare a feedstock.
  • the injection molded body was immersed in a closed solvent extraction tank containing a solution containing 90% or more of n-PB, and then B1 and B3 in the added binder were removed by circulating the solvent.
  • the solvent extraction temperature is preferably less than or equal to the boiling point of n-PB (70° C.) and at the same time less than 70° C., which is less than or equal to the melting point of paraffin wax, polyethylene glycol, and stearic acid.
  • solvent extraction was maintained at 45° C. for 8 hours, cooled to room temperature, dried in a solvent extraction tank, weighed, and converted into a volume ratio (vol%) to calculate the extraction rate.
  • the solvent-extracted injection molded body was pyrolyzed at 20 L/min with nitrogen gas in a 30 L box furnace under a nitrogen atmosphere to remove the remaining binder components.
  • the solvent extractor was placed on an alumina plate as shown in FIG. 2, and the temperature rising rate from room temperature to 500° C. was raised to 2° C./min and maintained for 60 minutes, thereby completing the binder removal process.
  • the temperature was raised from 500°C to 800°C at 3°C/min and pre-sintered for 60 minutes to have the strength of the bwown part from which the binder was removed, and the strain rate was measured.
  • the properties of the binder were evaluated by the strain rate, and the strain was calculated by measuring the distance deformed from the height of 11 mm in FIG. 2 in the direction of gravity with a two-dimensional projector, and the amount of strain 0.1 mm or less was used as a pass criterion.
  • the sintering of the pre-sintered body from which the binder was removed was carried out by holding a vacuum furnace at 1,350°C for 2 hours using a vacuum furnace in an argon atmosphere.
  • the sum of B1 and B3 removed to the solvent was the largest 95% by volume, which was smaller than 0.064 mm of the example of the first embodiment, and the smallest amount of deformation was 0.036 mm.

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Abstract

La présente invention concerne une composition de liant et un procédé de retrait de liant, pour préparer un article moulé par le mélange d'une poudre métallique, d'une poudre céramique, d'une poudre de carbure et similaires avec un liant thermoplastique, et le retrait rapide du liant à partir de l'article moulé sans dommages, qui peut être utilisé pour le moulage par injection de poudre, l'extrusion et similaires, et également pour l'impression 3D, telle qu'une fabrication par filament fondu (FFF).
PCT/KR2020/014659 2019-10-25 2020-10-26 Composition de liant pour préparation de corps fritté et procédé de retrait de liant WO2021080399A1 (fr)

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