WO2023203892A1 - Procédé de fabrication de comprimé de titane et procédé de fabrication de corps fritté de titane - Google Patents

Procédé de fabrication de comprimé de titane et procédé de fabrication de corps fritté de titane Download PDF

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Publication number
WO2023203892A1
WO2023203892A1 PCT/JP2023/007918 JP2023007918W WO2023203892A1 WO 2023203892 A1 WO2023203892 A1 WO 2023203892A1 JP 2023007918 W JP2023007918 W JP 2023007918W WO 2023203892 A1 WO2023203892 A1 WO 2023203892A1
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Prior art keywords
titanium
mold
core material
powder
compact
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PCT/JP2023/007918
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English (en)
Japanese (ja)
Inventor
昌志 早川
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東邦チタニウム株式会社
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Publication of WO2023203892A1 publication Critical patent/WO2023203892A1/fr

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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
    • B22F3/02—Compacting 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
    • B22F3/02—Compacting only
    • B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
    • 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
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/10—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of articles with cavities or holes, not otherwise provided for in the preceding subgroups
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy

Definitions

  • the present invention relates to a method for producing a titanium-based green compact and a method for producing a titanium-based sintered body.
  • titanium and titanium alloys are being considered for use in various parts because of certain excellent properties such as fatigue resistance, corrosion resistance, light weight, and high specific strength.
  • manufacturing parts made of titanium or titanium alloys generally involves a number of steps such as melting by electron beam melting or vacuum arc melting, casting, and in some cases further hot rolling, heat treatment and machining, and welding. This increases manufacturing costs. Due to such high costs, it cannot be said that the scope of application of titanium and titanium alloys has been sufficiently expanded.
  • some parts made of titanium or titanium alloy have an internal space or a recessed part including an opening to the outside.
  • a core material is placed in a position corresponding to the internal space of the mold, and the mold, whose forming space is filled with raw material powder, is cooled. Apply isostatic pressure for a while.
  • Patent Document 1 states, ⁇ Production of a hollow structure obtained by immersing a sintered body having a base material and a core made of an iron-based material in an acid solution to dissolve and remove the core.
  • the base material is made of a material nobler than the iron-based material constituting the core, and the base material is formed with a non-conductive coating on at least a part of the surface of the base material.
  • a method for manufacturing a hollow structure comprising a film forming step that reduces the surface that comes into contact with an acid solution has been proposed.
  • An example of the "hollow structure” is an "impeller (pump impeller)."
  • Patent Document 2 describes a method for manufacturing a metal green compact having a recess, in which a resin mold having a shape corresponding to the recess is placed in a position corresponding to the recess of a resin mold.
  • a method for producing a green compact comprising the step of applying cold isostatic pressure to the raw material powder filled in the mold with the core material positioned in the mold. According to the method described in Patent Document 2, "it is possible to suppress the occurrence of bulges on the surface of the green compact near the core material.”
  • Patent Document 3 states, ⁇ When performing cold isostatic pressure molding by enclosing powder in a mold, storing it in a pressure vessel, and applying isostatic pressure using a liquid such as water as a pressure medium, A method for cold isostatic pressure molding of powder, characterized in that a mold made of a viscoplastic material is used as the mold.
  • Patent Document 4 states, ⁇ In a method of manufacturing a green compact by molding raw powder, a cavity of a desired shape is provided in a mold made of a semi-solid material with a consistency of 15 to 300, and a cavity of a desired shape is formed in the cavity. "A method for producing a green compact, which comprises filling the powder raw material with pressure, and then pressurizing the powder raw material using the mold as a pressure medium.”
  • the core material When using a highly rigid core material such as the "core made of iron-based material” described in Patent Document 1, the core material hardly undergoes elastic deformation during cold isostatic pressurization. Differences may occur in the transmission of pressurizing force in the raw material powder, which may result in insufficient compaction. As a result, in the case of a highly rigid core material, the surface near the core material may bulge, and as a result, it may not be possible to satisfactorily produce a titanium-based green compact having a predetermined shape.
  • Patent Document 1 requires "immersing a sintered body having a base material and a core made of an iron-based material in an acid solution to dissolve and remove the core.”
  • parts made of titanium or titanium alloy have a more complicated shape, such as a closed impeller, in which a plate part such as a blade part is provided upright on the inner surface facing the internal space including the opening to the outside.
  • a titanium-based green compact having a plate portion provided in the internal space may not be manufactured even if a resin core material is placed in a mold for cold isostatic pressing.
  • Patent Documents 3 and 4 do not consider producing a titanium-based compact having a plate portion in the internal space as described above.
  • An object of the present invention is to provide a method for manufacturing a titanium-based green compact that can relatively easily produce a titanium-based green compact having a predetermined complicated shape, and a method for producing a titanium-based sintered body. There is a particular thing.
  • the inventor found that if a core component material with a consistency of 50 or higher is used as the core material placed in a resin mold, titanium-based powder compacts with a plate section erected in the internal space can be obtained. It has been found that it can be produced satisfactorily. For materials with a consistency of less than 50 and poor fluidity, springback of the core material when the load is unloaded by cold isostatic pressing may cause the plate part, which is thin to some extent, of titanium-based powder compacts to It is assumed that it will be easily damaged. By using a core constituent material having a consistency of 50 or more, damage to the plate portion is suppressed, and it becomes possible to manufacture a titanium-based green compact having the plate portion. Moreover, the core material constituent material having a consistency of 50 or more can be easily taken out from the titanium-based green compact after cold isostatic pressing.
  • the method for producing a titanium-based green compact according to the present invention is such that the titanium-based powder green body has a hollow main body portion forming an internal space including an opening to the outside, and a hollow main body portion having an internal space including an opening to the outside.
  • the manufacturing method includes a step of arranging a core material forming the inner space in a core material arrangement space of a resin mold; filling the molding space of the mold with raw material powder, and applying a pressure of 300 MPa or more to the mold with the molding space filled with the raw material powder with the core material arranged in the core material arrangement space;
  • the method includes a step of performing cold isostatic pressurization in a step, and a core material constituting material having a consistency of 50 or more is used as the core material.
  • the core constituent material has a consistency of 60 or more and 240 or less.
  • the core constituent material contains a polybutene resin or clay.
  • the hollow main body portions are spaced apart from each other.
  • a casing portion including a pair of disk-shaped portions arranged to provide the internal space therebetween, and the plate portion is oriented radially outward from the center of the disk-shaped portion between the disk-shaped portions.
  • the blade portion may extend straight or include curved and/or bent portions.
  • the titanium-based green compact has a cross section perpendicular to the central axis including the plate portion of the titanium-based green compact,
  • the ratio of the length corresponding to the thickness of the plate portion to the total length of each space portion located on both sides of the plate portion in the circumferential direction on a perpendicular line perpendicular to the extending direction of the plate portion is 0.05.
  • the mold is made of a thermoplastic resin having a Shore D hardness within the range of 30 to 120. It is preferable to use a mold consisting of: (7) In the method for producing a titanium green compact described in (6) above, it is preferable to use a mold made of a thermoplastic resin having a Shore D hardness in the range of 30 to 85. (8) In the method for producing a titanium green compact according to any one of (1) to (7) above, the thickness of the mold is preferably 0.5 mm to 2.0 mm.
  • the mold may be a mold produced using a three-dimensional modeling device.
  • the method for producing a titanium-based sintered body of the present invention is a method for producing a titanium-based powder compact produced by the method for producing a titanium-based powder compact according to any one of (1) to (9) above. This includes a sintering step of heating and sintering.
  • a titanium-based powder compact having a predetermined complicated shape can be produced relatively easily.
  • FIG. 1 is a perspective view showing an example of a titanium-based powder compact that can be manufactured by a manufacturing method according to an embodiment of the present invention.
  • 2(a) is a plan view of the titanium-based compact shown in FIG. 1
  • FIG. 2(b) is a cross-sectional view taken along line bb in FIG. 2(a).
  • FIG. 3(a) is a side view of the titanium-based compact shown in FIG. 1
  • FIG. 3(b) is a cross-sectional view taken along line bb in FIG. 3(a).
  • FIG. 4(a) is a sectional view taken along the central axis line, showing a mold and core material that can be used for manufacturing the titanium-based compact shown in FIG.
  • FIG. 3 is a cross-sectional view taken along line bb.
  • FIG. 5 is a cross-sectional view taken along the central axis line, schematically showing a state in which cold isostatic pressing is performed using the mold and core material of FIG. 4 .
  • FIG. 3 is a perspective view showing another example of a titanium-based powder compact that can be manufactured by the manufacturing method according to one embodiment of the present invention.
  • 7(a) is a plan view of the titanium-based powder compact of FIG. 6, and
  • FIG. 7(b) is a sectional view taken along line bb of FIG. 7(a).
  • FIG. 8(a) is a side view of the titanium-based powder compact of FIG. 6, and
  • FIG. 8(b) is a sectional view taken along line bb of FIG.
  • FIG. 8(a) It is a perspective view showing still another example of the titanium-based green compact which can be manufactured by the manufacturing method concerning one embodiment of this invention.
  • 10(a) is a plan view of the titanium-based compact shown in FIG. 9, and FIG. 10(b) is a sectional view taken along line bb in FIG. 10(a).
  • 11(a) is a side view of the titanium-based green compact shown in FIG. 9, and FIG. 11(b) is a sectional view taken along line bb in FIG. 11(a).
  • 13(a) is a plan view of the titanium-based powder compact of FIG. 12, and FIG.
  • FIG. 13(b) is a sectional view taken along line bb of FIG. 13(a).
  • 14(a) is a side view of the titanium-based powder compact of FIG. 12, and FIG. 14(b) is a sectional view taken along the line bb of FIG. 14(a).
  • 16(a) is a plan view of the titanium-based compact shown in FIG. 15, and FIG. 16(b) is a cross-sectional view taken along line bb in FIG. 16(a).
  • 16 is a side view of the titanium-based powder compact of FIG. 15.
  • a titanium-based powder compact 1 is provided with a plate portion 3 in an internal space 2b including an opening 2a, as illustrated in FIGS. 1 to 3. etc.
  • titanium-based herein includes not only pure titanium but also titanium alloys.
  • the core material placement space of the resin mold is When arranging the core material forming the internal space, a material constituting the core material having a consistency of 50 or more is used as the core material.
  • a core made of core material with a consistency of 50 or higher has a relatively low viscosity and high fluidity, so when the load is removed after cold isostatic pressing, it will not have much springback. It is presumed that this prevents damage to the plate portion of the titanium-based green compact from occurring. Moreover, since the core material of the core material having a consistency of 50 or more has fluidity, it can be easily taken out from the titanium compact after cold isostatic pressing. As a result, a titanium-based green compact having a predetermined complicated shape can be produced relatively easily.
  • This titanium-based powder compact 1 is provided upright on a hollow main body part 2 forming an internal space 2b including an opening 2a to the outside, and an inner surface 2c facing the inner space 2b of the hollow main body part 2, and the inner surface 2c It has a plate portion 3 extending above.
  • the hollow main body part 2 includes a pair of disc-shaped parts 4a and 4b arranged parallel to each other at intervals, and a disc-shaped part 4a extending parallel to the central axis between the disc-shaped parts 4a and 4b. , 4b are included (see FIGS. 2 and 3).
  • the internal space 2b is defined on the outer peripheral side of the connecting portion 5 between the disc-shaped portions 4a and 4b, and is recessed from the outer surface of the hollow main body portion 2 and exists at a position deeper than the outer surface.
  • This internal space 2b has an opening 2a to the outside between the outer peripheral surfaces of the disk-shaped portions 4a and 4b of the outer surface of the hollow main body portion 2.
  • the boundary between the outer end surface facing the outside of each disk-shaped part 4a, 4b, and an outer peripheral surface can form the chamfered part 4c of the curved surface shape over the entire circumference as needed.
  • the plate portion 3 has an inner surface 2c facing the inner space 2b of the disc-shaped parts 4a, 4b and facing the inner space 2b (more specifically, an inner end face of the disc-shaped parts 4a, 4b facing the inner space 2b). It is set in.
  • the number of plate portions 3 can be one or more, and in the illustrated example, there are six.
  • Each plate portion 3 is formed integrally with the inner surface 2c (the inner end surface of each disc-shaped portion 4a, 4b), and extends on the inner surface 2c in an upright position from the inner surface 2c.
  • the plurality of plate parts 3 are connected to a connecting part 5 at the center of the disc-shaped parts 4a and 4b, and have a shape that extends straight radially outward from the connecting part 5.
  • the internal space 2b is divided into a corresponding number of space parts by a plurality of plate parts 3, and a plurality of openings are provided at the outermost radial direction of each space part. 2a exists.
  • the mold 51 for molding the titanium-based green compact 1 is provided with a molding space 52 having a shape corresponding to the shape of the titanium-based green compact 1, as shown in FIGS. 4(a) and (b). More specifically, this mold 51 includes a pair of hollow disc-shaped walls 53a, 53b arranged at intervals, and a wall extending parallel to the central axis at the center between the disc-shaped walls 53a, 53b. A hollow cylindrical wall 54 connected to the disc-shaped walls 53a, 53b, and a hollow columnar wall 54 connected to each of the disc-shaped walls 53a, 53b and the cylindrical wall 54 between the disc-shaped walls 53a, 53b. It has a plurality of hollow plate-like wall portions 55 extending radially.
  • a molding space 52 is defined inside the hollow disc-shaped walls 53a, 53b, the cylindrical wall 54, and the plate-shaped wall 55.
  • the disk-shaped parts 4a and 4b of the titanium-based powder compact 1 are connected on the forming surfaces inside the disk-like walls 53a and 53b, and the titanium-based powder compact 1 is connected on the forming surface inside the columnar wall 54.
  • the plate portion 3 of the titanium-based powder compact 1 is formed at the portion 5 and the molding surface inside the plate-like wall portion 55, respectively.
  • a through hole 53c used for supplying the raw material powder 71 to the molding space 52 is provided in the center portion of the outside of one disk-shaped wall portion 53a, but the through hole is not provided in the other part of the mold. It may be provided in some parts. Further, the number of through holes 53c is not limited to one, but may be plural.
  • the mold 51 is made of resin, preferably thermoplastic resin, and is particularly preferably made of acrylic resin, elastomer-containing acrylic resin, polylactic acid (PLA) resin, or the like.
  • the resin mold 51 is preferably made of a thermoplastic resin with a Shore D hardness within the range of 30 to 120 in order to ensure the required strength and maintain its shape even when filling the raw material powder 71. It may also be a thermoplastic resin having a molecular weight within the range of 30 to 85. Shore D hardness can be measured by a test method based on JIS K7215 (1986). From the same viewpoint, the thickness of the resin mold 51 is preferably 0.5 mm to 2.0 mm.
  • the resin mold 51 can be produced by various methods, it is preferably produced using a three-dimensional modeling device (so-called 3D printer). Thereby, molds 51 of various shapes can be easily produced.
  • the modeling method of the three-dimensional printer is not particularly limited, and may be any one of, for example, a stereolithography method, an inkjet method, an inkjet powder layering method, a powder sintering layered manufacturing method, a hot melt layering method, or a powder fixation method.
  • the raw material powder 71 to be filled into the molding space 52 of the mold 51 various powders such as titanium powder, alloying element powder, mother alloy powder, etc. can be used in combination as necessary.
  • This titanium powder includes pure titanium powder consisting essentially only of titanium, titanium hydride powder mainly containing titanium, and containing hydrogen in an amount of 5% by mass or less.
  • the pure titanium powder may be, for example, a hydride-dehydrogenated powder obtained by dehydrogenating titanium hydride powder.
  • the above-mentioned alloying element powder means a powder containing a single alloying element of a titanium alloy
  • the mother alloy powder means a powder containing a plurality of elements.
  • the raw material powder 71 may be, for example, only titanium powder, or may include titanium powder, an alloying element powder selected from the group consisting of iron, aluminum, vanadium, zirconium, tin, molybdenum, copper, and nickel, and/or powder. Alternatively, a mixture of two or more types of master alloy powders may be used. Alternatively, it is also possible to use only a powder containing titanium and an alloying element as the raw material powder 71.
  • pure titanium means titanium having a titanium content of 99% by mass or more.
  • the mass ratio of the alloying element to titanium in the raw material powder 71 may be in the range of 0 to 0.33, for example, 0 to 0.11, where titanium is 1.
  • the average particle size of the raw material powder 71 is preferably 10 ⁇ m to 150 ⁇ m. By using such relatively fine particles, it is possible to improve the compressed density of the titanium-based green compact after cold isostatic pressing and furthermore of the titanium-based sintered body after heating.
  • the average particle diameter means the particle diameter D50 (median diameter) of the particle size distribution (volume basis) obtained by a laser diffraction scattering method.
  • known powders such as crushed powder and atomized powder can be used as the raw material powder 71.
  • a core material 61 is placed in the core arrangement space of the mold 51 to form the internal space 2b of the titanium-based powder compact 1. Place. As shown in FIG. 4, between the pair of disc-shaped walls 53a and 53b in the mold 51, a core material is formed in the space between the circumferentially adjacent plate-shaped walls 55 on the outer peripheral side of the columnar wall 54. 61 is arranged, and this space corresponds to the core material arrangement space.
  • the core material having flowability can be filled by pouring into the core material arrangement space from the opening to the outside around the core material arrangement space, whereby the core material 61 is arranged in the core material arrangement space. be done. After arranging the core material 61, the opening of the core material arrangement space can be closed with a sealing member 56, such as a plate, to seal the core material arrangement space (see FIG. 5).
  • the raw material powder 71 is filled into the molding space 52 of the mold 51 through the through hole 53c.
  • a plate-shaped lid member 57 made of, for example, substantially the same material as the mold 51 is provided in the through hole 53c, thereby sealing the molding space 52. (See Figure 5).
  • the process of arranging the core material 61 in the core material arrangement space and the process of filling the molding space 52 of the mold 51 with the raw material powder 71 may be performed in any order, and either process may be performed first.
  • the entire mold may be covered with a bag-like covering member, although not shown. . In this case, if necessary, the interior of the covering member surrounding the mold may be depressurized before the cold isostatic press described below.
  • the mold 51 with the raw material powder 71 filled in the molding space 52 is subjected to cold isostatic pressure in a cold isostatic pressure device. CIP).
  • CIP cold isostatic pressure device
  • the mold 51 is pressurized from the outside.
  • the sealing member 56 and the lid member 57 constitute a part of the mold 51, and pressure is applied to the sealing member 56 and the lid member 57 from the outside.
  • the raw material powder 71 in the molding space 52 of the mold 51 is compressed and compacted, and becomes the titanium-based compact 1 .
  • the mold 51 In cold isostatic pressurization, the mold 51 is pressurized with isostatic pressure (hydrostatic pressure, etc.) by the surrounding fluid, regardless of its shape. Therefore, by cold isostatic pressing, the titanium-based powder compact 1 can be manufactured using molds 51 of various shapes.
  • the pressure applied to the mold 51 by cold isostatic pressing is 300 MPa or more, preferably 400 MPa or more. If the pressing force is less than 300 MPa, the raw material powder 71 will not be sufficiently compressed, and the shape accuracy of the titanium-based compact 1 will become insufficient.
  • the pressing force may be, for example, 750 MPa or less, or 600 MPa or less, and typically 500 MPa or less. Further, the holding time under such pressure may be, for example, 0.5 minutes to 30 minutes.
  • the titanium-based powder compact 1 is taken out together with the mold 51 and the core material 61 from the cold isostatic pressing device. Thereafter, the mold 51 and the core material 61 are removed from the titanium-based compact 1. At this time, since the core material 61 has fluidity, it can be easily removed. Depending on the type of core material forming the core material 61, the core material 61 may be taken out together with a part of the mold 51. Note that the mold 51 may be heated to about 100° C. in the atmosphere to soften it before removal, if necessary. Thereby, the titanium-based green compact 1 can be manufactured.
  • a step of heating the titanium-based compact 1 is performed after the cold isostatic pressing step.
  • the particles constituting it are sintered to become a titanium-based sintered body.
  • the manufactured titanium-based green compact and titanium-based sintered body can be subjected to further processing such as cutting and polishing.
  • the titanium-based powder compact 1 can be heated without pressure at a temperature of, for example, 1200° C. to 1300° C. for 1 hour to 3 hours.
  • hot isostatic pressing HIP
  • argon gas An isostatic pressure of about 100 MPa to 200 MPa may be applied for 30 minutes to 180 minutes using a pressure medium such as gas.
  • a titanium-based sintered body can be produced by pressureless heating and/or hot isostatic pressing.
  • pressureless heating and hot isostatic pressing are performed, the order is not particularly limited, but for example, hot isostatic pressing can be performed after pressureless heating.
  • the core material 61 arranged in the core material arrangement space of the mold 51 is made of a core material constituting material having a consistency of 50 or more.
  • the core material 61 exhibits a certain degree of low viscosity and high fluidity. 51.
  • the titanium-based powder compact 1 tends to be less likely to be damaged after cold isostatic pressing. This is because the consistency of the core material constituent material is 50 or more, so that the core material 61, which has appropriate viscosity and fluidity, does not recover so much when the load of cold isostatic pressing is removed. It is assumed that this is due to the following. If a core material 61 made of a core material having a consistency of less than 50 is used, a large springback of the core material 61 may occur when the load of cold isostatic pressing is removed. As a result, the relatively thin plate portion 3 of the titanium-based powder compact 1 that is adjacent to the core material 61 with the plate-like wall portion 55 interposed therebetween is likely to be damaged.
  • the core material 61 whose core material constituting material has a consistency of 50 or more can be filled and arranged in core material arrangement spaces of various shapes because of its fluidity. Therefore, by using such a core material 61, titanium-based powder compacts 1 having internal spaces 2b of various shapes can be manufactured.
  • a material constituting the core material whose consistency does not change is used; however, in the case of a material constituting the core material whose consistency can change due to hardening due to heat, etc., immediately before filling the core material arrangement space of the mold 51. , and the consistency of the core constituent material immediately after being taken out from the titanium-based powder compact 1 may all be 50 or more. Even if the consistency of the core component material before filling into the core material placement space is 50 or more, if the consistency becomes less than 50 due to hardening after filling, cold isostatic pressure is applied. Springback of the core material may occur when unloading.
  • the consistency of the core constituent material is preferably 60 or more and 240 or less.
  • the consistency is 60 or more, damage to the titanium-based powder compact 1 as described above can be suppressed even more effectively.
  • the consistency is set to 240 or less, contamination of the titanium-based powder compact 1 due to adhesion of the core material 61 or penetration into the interior when the core material 61 is removed from the titanium-based powder compact 1 can be suppressed.
  • the core material constituent material adheres to or permeates into the titanium-based green compact 1, the concentration of oxygen, carbon, nitrogen, etc. increases locally during subsequent sintering, and the mechanical properties of the titanium-based sintered body deteriorate. There are concerns about this.
  • the consistency is appropriate, it becomes easy to fill the core material into the core material arrangement space and to take it out from there.
  • the consistency of the core material is measured using a standard cone in accordance with JIS K2220:2013.
  • core material constituent materials include polybutene resin, clay, and the like.
  • Clay is an aggregate of artificial or natural soil or particles containing soil, sand, oil, pulp, etc. and having a predetermined adhesive property, such as oil clay.
  • titanium-based green compact According to the manufacturing method of the embodiment described above, the titanium-based powder compact 1 shown in FIGS. 1 to 3 can be manufactured.
  • the specific structure of this titanium-based powder compact 1 is as described above, and its explanation will be omitted.
  • the titanium-based powder compact 1 is made of titanium made of pure titanium, or made of Ti-5Al-1Fe, Ti-5Al-2Fe, Ti-6Al-4V, Ti-6Al-6V-2Sn, Ti-6Al-2Sn-4Zr. It may be made of a titanium alloy such as -2Mo, Ti-6Al-2Sn-4Zr-6Mo, or Ti-10V-2Fe-3Al. In addition, in the components of the titanium alloy listed here, the number attached before each alloy element symbol means the content (mass %). For example, "Ti-6Al-4V" represents a titanium alloy containing 6% by mass of Al and 4% by mass of V.
  • What can be manufactured is not limited to the titanium-based compact 1 shown in FIGS. 1 to 3.
  • the titanium-based powder compact 11 shown in FIGS. 6 to 8 does not have a portion corresponding to the connecting portion 5 of the titanium-based powder compact 1 shown in FIGS. It has almost the same structure as the titanium-based powder compact 1, except that it is ring-shaped with a through hole 15 connected to the gap between the titanium-based powder compact 1 and the disc-shaped part 14b.
  • the through hole portion 15 constitutes a part of the internal space 12b, and an opening portion 15a to the outside is also present on the outer end surface side of the disk-shaped portion 14a (see FIGS. 6 and 7). Note that the pair of disk-shaped portions 14a and 14b are connected to each other by a plate portion 13 between them.
  • the titanium-based powder compact 21 shown in FIGS. 9 to 11 has a connecting portion 25 having a larger diameter than the connecting portion 5 of the titanium-based powder compact 1 in FIGS. 1 to 3, and each plate portion 23 is , extends radially outward from the center of the disc-shaped portions 24a, 24b, including a curved portion that protrudes toward one side in the circumferential direction (counterclockwise in FIG. 11(b)). Except for this, it has almost the same configuration as the titanium-based powder compact 1.
  • the entire plate portion 23 is a curved portion.
  • the plate portion may partially include at least one curved portion instead of the entire plate portion.
  • the titanium-based powder compact 31 shown in FIGS. 12 to 14 has a connecting portion 35 having a larger diameter than the connecting portion 5 of the titanium-based powder compact 1 in FIGS. 1 to 3, and each plate portion 33 has a , has almost the same structure as the titanium-based powder compact 1, except that it extends radially outward from the center of the disc-shaped portions 34a and 34b, including at least one bent point.
  • each plate portion 33 has a plurality of bending points, and as shown in FIG. It has a zigzag shape with alternate locations and bent locations protruding to the other side. Note that a corner portion 33 a is formed on the outer surface of the columnar connecting portion 35 by connecting with an end portion of the zigzag plate portion 33 .
  • the curved portions included in the plate portion 23 of the titanium-based powder compact 21 shown in FIGS. 9 to 11 and the plate portion 33 of the titanium-based powder compact 31 shown in FIGS. 12 to 14 It is also possible to have a plate portion that has both such bending points.
  • the titanium-based powder compacts 1, 11, 21, and 31 shown in FIGS. 1 to 14 can be used as an impeller such as a closed impeller.
  • the pair of disc-shaped parts 4a, 4b, 14a, 14b, 24a, 24b, 34a, 34b and the connecting parts 5, 25, 35 are the casing part of the impeller.
  • the casing portion includes a pair of disk-shaped portions 4a, 4b, 14a, 14b, 24a, 24b, 34a, and 34b.
  • the plate portions 3, 13, 23, and 33 of the titanium-based powder compacts 1, 11, 21, and 31 correspond to the blade portions of the impeller.
  • the plate portions 3, 13, 23, and 33 which are blade portions existing in the internal spaces 2b, 12b, 22b, and 32b, are relatively thick. May be thin.
  • the thickness of the plate portion 3 occupies a small proportion or area in the internal space 2b. More specifically, in the above-mentioned cross section, the titanium-based powder compact 1 has a plate portion in the circumferential direction on a perpendicular line PL (indicated by a broken line in FIG. 3(b)) perpendicular to the direction in which the plate portion 3 extends.
  • the ratio (Lt/Ls) of the length Lt corresponding to the thickness of the plate portion 3 to the total length (Ls) of the lengths (Ls/2) in each space portion located on both sides of the plate portion 3 is, for example, 0.05 or more and There may be locations where the value is 0.25 or less. It is not necessary that the entire plate portion of the titanium-based powder compact has the above ratio (Lt/Ls). If there is a portion where the above ratio (Lt/Ls) is 0.05 or more and 0.25 or less in at least a part of the plate part, the titanium-based compacted powder has a portion where the ratio (Lt/Ls) is Applies to the body.
  • each space portion on both sides in the circumferential direction of the plate portion 3 is as shown in FIG. means the length in the direction along the perpendicular line PL from the side surface of the plate section 3 to the side surface of another plate section.
  • the length in the perpendicular direction from the side of the plate to the inner surface is corresponds to the length of each spatial portion on both sides of .
  • the ratio (Lt/Ls) between the length Lt corresponding to the thickness of the plate portion 3 and the total length (Ls) of the space portions on both sides in the circumferential direction is 0.05 or more and 0.25
  • a titanium-based powder compact 1 having the following locations tends to be easily damaged due to the springback of the core material 61 mentioned above during its manufacture.
  • by using a predetermined core constituent material even such a titanium-based powder compact 1 can be manufactured satisfactorily while suppressing damage to the plate portion 3. be able to.
  • the titanium-based powder compact 41 shown in FIGS. 15 to 17 is provided upright on a hollow main body 42 forming an internal space 42b including an opening 42a to the outside, and on an inner surface 42c of the hollow main body 42 facing the internal space 42b. , and three plate portions 43 extending on the inner surface 42c.
  • the hollow main body 42 has a pair of disc-shaped parts 44a and 44b arranged at intervals, which are connected to each other by a cylindrical connecting part 45 extending along the central axis. .
  • the internal space 42b is recessed from the outer surface of the hollow main body portion 42 and is defined by the pair of disc-shaped portions 44a, 44b and the inner surface of the connecting portion 45 on the inner space 42b side.
  • each plate portion 43 provided around the cylindrical connecting portion 45 extends in the circumferential direction on the inner surface 42c facing the internal space 42b side of the connecting portion 45, and has a radial radius. It has a circular plate shape whose thickness gradually decreases toward the outside. Note that the number of plate portions 43 can be changed as appropriate, and may be one, two, or four or more.
  • the titanium-based green compact 41 shown in FIGS. 15 to 17 is not intended for use in an impeller, it can be manufactured using this embodiment in order to be molded without causing damage to the plate portion 43 provided in the internal space 42b. can.
  • the titanium-based powder compact A has a length in each space portion located on both sides of the plate portion in the circumferential direction on a perpendicular line perpendicular to the extending direction of the plate portion in a cross section including the plate portion and perpendicular to the central axis.
  • the minimum value of the ratio (Lt/Ls) of the length Lt corresponding to the thickness of the plate portion to the total length Ls is 0.05.
  • the minimum value of the similar ratio (Lt/Ls) in the titanium-based green compact B is 0.09.
  • Example 1 to 8 and Comparative Examples 1 to 3 titanium compacts were produced.
  • Hydrodehydrogenation powder (HDH powder) was used as the raw material powder in Examples 1 to 7 and Comparative Examples 1 to 3.
  • a mixture of HDH powder and titanium hydride powder at a mass ratio of 1:1 was used.
  • the above HDH powder had a titanium content of 99% by mass or more and an average particle size of 66 ⁇ m.
  • the titanium hydride powder had a titanium content of 95% by mass or more, a hydrogen content of 5% by mass or less, and an average particle size of 66 ⁇ m.
  • Example 9 a powder compact made of titanium alloy was produced, and a mixture of the above HDH powder and 60Al40V powder at a mass ratio of 9:1 was used as the raw material powder.
  • the above 60Al40V powder was produced by crushing an ingot, contained 60% by mass of aluminum and 40% by mass of vanadium, and had an average particle size of 35 ⁇ m.
  • the mold used for manufacturing was modeled using a 3D printer.
  • the resin material constituting the mold was polylactic acid (PLA), and had a Shore D hardness of 83.
  • the thickness of the mold was 1.0 mm.
  • Each core material constituent material shown in Table 1 was used for the core material arranged in the core material arrangement space of the mold.
  • "putty for air conditioner piping” is made of polybutene resin.
  • the consistency of the core constituent material was measured in accordance with JIS K2220:2013, as described above. However, since the silicone sealant of Comparative Example 1 hardens over time, and the carbon steel of Comparative Example 2 and the thermosetting resin of Comparative Example 3 do not have fluidity at room temperature, the consistency was could not be measured. From this, it can be considered that Comparative Examples 1 to 3 are hard materials and have a consistency of clearly less than 50.
  • the entire mold After placing the core material in the above mold and filling it with raw material powder, the entire mold is wrapped in a plastic bag, the inside of the mold is depressurized, and then hydrostatic pressure is applied in a cold isostatic pressurizer.
  • Cold isostatic pressing CIP
  • CIP Cold isostatic pressing
  • a pressing force of 490 MPa was applied to the mold filled with the raw material powder for 1 minute.
  • the mold was taken out of the plastic bag, and most of the core material was removed manually. The mold was then heated to about 100° C. in air to soften it. Thereafter, the mold was removed from the titanium compact inside using a tool such as pliers.
  • the titanium-based green compact produced in this way was visually observed to check for damage, adhesion of the core material, and penetration into the interior. The results are shown in Table 1.

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  • Materials Engineering (AREA)
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Abstract

Dans un procédé de fabrication d'un comprimé de titane (1) selon la présente invention, le comprimé de titane (1) a une partie de corps creux (2) dans laquelle est formé un espace interne (2b) qui comprend une partie d'ouverture (2a) s'ouvrant vers l'extérieur, et des parties de plaque (3) qui sont disposées de façon à reposer sur une surface interne (2c) de la partie de corps creux (2) faisant face à l'espace interne (2b) et qui s'étendent sur la surface interne (2c). Le procédé de fabrication comprend : une étape consistant à placer un matériau de noyau (61), pour former l'espace interne (2b), dans un espace de placement de matériau de noyau dans un moule (51) constitué d'une résine ; une étape consistant à remplir un espace de moulage (52) du moule (51) avec une poudre de matière première (71) ; et une étape consistant à effectuer un pressage isostatique à froid, à une force de pression de 300 MPa ou plus, sur le moule (51) dans lequel l'espace de moulage (52) est rempli avec la poudre de matériau (71), dans un état dans lequel le matériau de noyau (61) est placé dans l'espace de placement de matériau de noyau. Un matériau constituant un matériau de noyau ayant une consistance de (50) ou plus est utilisé en tant que matériau de noyau (61).
PCT/JP2023/007918 2022-04-21 2023-03-02 Procédé de fabrication de comprimé de titane et procédé de fabrication de corps fritté de titane WO2023203892A1 (fr)

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JP2022070294A JP2023160150A (ja) 2022-04-21 2022-04-21 チタン系圧粉体の製造方法及び、チタン系焼結体の製造方法

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003154494A (ja) * 2001-11-21 2003-05-27 Osaka Prefecture 圧粉体製造方法
JP2007162090A (ja) * 2005-12-15 2007-06-28 Nissan Motor Co Ltd 成形金型
JP2017522488A (ja) * 2014-07-04 2017-08-10 ヌオーヴォ ピニォーネ ソチエタ レスポンサビリタ リミタータＮｕｏｖｏ Ｐｉｇｎｏｎｅ Ｓ．Ｒ．Ｌ． 複数の管状部品を組み立てることによるターボ機械羽根車の製造
WO2021060363A1 (fr) * 2019-09-27 2021-04-01 東邦チタニウム株式会社 Procédé de production de comprimé cru et procédé de production de corps fritté

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003154494A (ja) * 2001-11-21 2003-05-27 Osaka Prefecture 圧粉体製造方法
JP2007162090A (ja) * 2005-12-15 2007-06-28 Nissan Motor Co Ltd 成形金型
JP2017522488A (ja) * 2014-07-04 2017-08-10 ヌオーヴォ ピニォーネ ソチエタ レスポンサビリタ リミタータＮｕｏｖｏ Ｐｉｇｎｏｎｅ Ｓ．Ｒ．Ｌ． 複数の管状部品を組み立てることによるターボ機械羽根車の製造
WO2021060363A1 (fr) * 2019-09-27 2021-04-01 東邦チタニウム株式会社 Procédé de production de comprimé cru et procédé de production de corps fritté

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