WO2019039058A1 - 積層造形用銅合金粉末、積層造形物の製造方法及び積層造形物 - Google Patents
積層造形用銅合金粉末、積層造形物の製造方法及び積層造形物 Download PDFInfo
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- WO2019039058A1 WO2019039058A1 PCT/JP2018/023020 JP2018023020W WO2019039058A1 WO 2019039058 A1 WO2019039058 A1 WO 2019039058A1 JP 2018023020 W JP2018023020 W JP 2018023020W WO 2019039058 A1 WO2019039058 A1 WO 2019039058A1
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- Prior art keywords
- copper alloy
- alloy powder
- laminate
- lamination
- copper
- Prior art date
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- 239000000843 powder Substances 0.000 title claims abstract description 68
- 229910000881 Cu alloy Inorganic materials 0.000 title claims abstract description 65
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 238000003475 lamination Methods 0.000 title abstract description 8
- 238000007493 shaping process Methods 0.000 title abstract description 4
- 239000010949 copper Substances 0.000 claims abstract description 27
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052802 copper Inorganic materials 0.000 claims abstract description 23
- 239000006104 solid solution Substances 0.000 claims abstract description 21
- 239000000654 additive Substances 0.000 claims description 27
- 230000000996 additive effect Effects 0.000 claims description 27
- 238000000465 moulding Methods 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 19
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 238000010894 electron beam technology Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 229910052721 tungsten Inorganic materials 0.000 claims description 8
- 229910052779 Neodymium Inorganic materials 0.000 claims description 6
- 229910052758 niobium Inorganic materials 0.000 claims description 6
- 229910052727 yttrium Inorganic materials 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- 229910052707 ruthenium Inorganic materials 0.000 claims description 5
- 238000000034 method Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 5
- 238000000889 atomisation Methods 0.000 description 5
- 229910052804 chromium Inorganic materials 0.000 description 5
- 239000011651 chromium Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000007088 Archimedes method Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000010030 laminating Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000010587 phase diagram Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000000470 constituent Substances 0.000 description 2
- 150000001879 copper Chemical class 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004993 emission spectroscopy Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 230000001678 irradiating effect Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
- 229910052778 Plutonium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 238000001739 density measurement Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012778 molding material Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910052713 technetium Inorganic materials 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/09—Mixtures of metallic powders
-
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
-
- 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
- B22F3/12—Both compacting and sintering
- B22F3/16—Both compacting and sintering in successive or repeated steps
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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
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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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
- B33Y10/00—Processes of additive manufacturing
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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
- B33Y50/00—Data acquisition or data processing for additive manufacturing
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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
-
- 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
- C22C1/0425—Copper-based alloys
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- 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
- C22C1/045—Alloys based on refractory metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/30—Process control
- B22F10/38—Process control to achieve specific product aspects, e.g. surface smoothness, density, porosity or hollow structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F2009/0804—Dispersion in or on liquid, other than with sieves
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
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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
- B22F2202/00—Treatment under specific physical conditions
- B22F2202/11—Use of irradiation
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/10—Copper
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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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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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
- B33Y80/00—Products made by additive manufacturing
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- 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
- C22C1/047—Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Definitions
- the present invention relates to a copper alloy powder for laminate molding, a method for producing a laminate molded article, and a laminate molded article, and in particular, a copper alloy powder for laminate molding comprising a copper alloy that can achieve both mechanical strength and electrical conductivity, a laminate molded article Manufacturing method and laminated shaped article.
- the 3D printer is also called additive manufacturing (AM), and as a method of producing a metal three-dimensional shaped object, a lamination method using an electron beam (EB) or a laser is well known.
- AM additive manufacturing
- a metal powder layer is formed on a sintering table, and a predetermined portion of the powder layer is irradiated with a beam or a laser to be sintered, and then a new powder layer is formed on the powder layer. Then, a predetermined portion is irradiated with a beam and sintered to form a sintered portion integrated with the lower-layer sintered portion.
- the laminate-molded articles to be obtained by laminate molding there are those which are required to have high electrical conductivity as well as mechanical strength.
- heat sinks, molds, welding torches, parts of power distribution equipment, etc. may be mentioned.
- the copper alloy powder is rapidly heated and cooled by rapid cooling, so that the structure of the laminated molded article is controlled.
- these elements form a solid solution, which causes the conductivity to be lowered.
- the additive element is not contained, it becomes difficult to obtain the required mechanical strength.
- Patent Document 1 is a metal powder for laminate molding and contains 0.10 mass% or more and 1.00 mass% or less of at least one of chromium and silicon, A metal powder is disclosed wherein the total amount of the chromium and the silicon is 1.00% by mass or less and the balance is copper. According to this invention, the effect that mechanical strength and conductivity can be compatible is expected.
- Patent Document 1 does not propose a specific solution regarding the problem of solid solution of the additive element.
- chromium is easily dissolved in copper, adding chromium in order to obtain mechanical strength does not solve the problem that the conductivity is lowered this time.
- the present invention has been made in view of the above problems, and provides a copper alloy powder for laminate molding comprising a copper alloy, which is compatible in mechanical strength and conductivity, a method for producing a laminate molded article, and a laminate molded article. With the goal.
- the inventors of the present invention conducted intensive studies to find that the solid solution is reduced by using an additive element having a small amount of solid solution to copper, and the tradeoff between mechanical strength and conductivity is caused. They found that they could be resolved, and further study and consideration were added to complete the present invention.
- a laminate formed from a copper alloy, The copper alloy contains an additive element having a solid solution content of less than 0.2 at%, a relative density to the theoretical density of 98% or more, a conductivity of 50% IACS or more, and a 0.2% proof stress Laminated object having a pressure of 700 MPa or more.
- a copper alloy powder for laminate molding comprising a copper alloy, a method for manufacturing a laminate molded article, and a laminate molded article, which are compatible in mechanical strength and conductivity.
- Copper alloy powder As the copper alloy powder, copper alloy powder produced by a known method can be used. If the particle size is a few ⁇ m or more, although it is general to use a copper alloy powder manufactured by a dry method typified by the atomization method which is industrially excellent in manufacturing cost, it is generally used a wet method such as a reduction method It is also possible to use a copper alloy powder produced by the method. Specifically, while dropping the molten alloy component from the bottom of the tundish, the alloy component is brought into contact with high pressure gas or high pressure water to rapidly solidify the alloy component, thereby pulverizing the alloy component. Other than this, for example, the metal powder may be manufactured by a plasma atomization method, a centrifugal force atomization method, or the like. By using the metal powder obtained by these production methods, a dense layered object tends to be obtained.
- the copper alloy powder contains an additive element in which the solid solution amount with respect to copper is less than 0.2 at%.
- the additive element By including the additive element, it is possible to obtain a laminate-shaped article having higher mechanical strength as compared with pure copper.
- the solid solution amount to copper is less than 0.2 at%, the formation of the phase in which the additive element is solid-solved in copper is suppressed even by rapid heating and cooling in shaping, so higher conductivity can be obtained. be able to.
- the solid solution amount with respect to copper is an inherent property of the additive element, and can be extracted from a diagram showing a phase relationship to temperature of two elements generally called a phase diagram.
- phase Diagrams for Binary Alloys (ISBN: 0-87170-682-2) published by ASM International. From this phase diagram, referring to the amount of solid solution on the Cu side, an element having a maximum amount of solid solution of 0.2 at% or less at the temperature below the liquid phase is the target element. More specifically, Ba, Bi, Ca, Gd, Eu, Ho, La, Lu, Mo, Nd, Nb, Os, Pb, Pm, Pu, Re, Ru, S, Se, Sr, Sm, Tb, Tc , Te, Th, Tm, U, V, W, Y, Yb, Zr. Moreover, these elements may add only 1 type, and 2 or more types may be added.
- the additional element be at least one selected from the group consisting of W, Zr, Nb, Nd, Y, Mo, Os or Ru.
- W, Zr, Nb, Nd, Y, Mo, Os or Ru are selected from the group consisting of W, Zr, Nb, Nd, Y, Mo, Os or Ru.
- These additive elements each have a solid solution amount with respect to copper of less than 0.2 at%, and are easily precipitated, so that the mechanical strength of the layered object can be significantly improved.
- the content of the additive element is preferably 0.1 to 12.0 at%. If the content of the additive element is 0.1 at% or more, the effect of improving the mechanical strength appears more, and if it is 12.0 at% or less, unnecessary decrease in the conductivity can be prevented. . When two or more additive elements are added, the total amount thereof may be 0.1 to 12.0 at%.
- the content of the additive element can be measured, for example, by ICP-OES (high frequency inductively coupled plasma emission spectrometry) of SPS3500 DD manufactured by SII.
- the average particle diameter D50 of the copper alloy powder is preferably 20 to 100 ⁇ m.
- the average particle diameter D50 refers to the particle diameter at an integrated value of 50% in the particle diameter distribution, where the diameter of a circle corresponding to the area calculated from the image of particles obtained by microscopic image analysis is the particle diameter. For example, it can be measured by a dry particle image analyzer Morphello G3 manufactured by Spectris Co., Ltd. (Malvern Division).
- the oxygen concentration in the copper alloy powder is preferably 1000 wtppm or less, more preferably 500 wtppm or less. More preferably, it is 250 wtppm or less. This is because if the amount of oxygen is small inside the copper alloy powder, the inclusion of oxygen can be avoided from becoming a shaped article, and the possibility of adversely affecting the conductivity of the shaped article can be reduced. In order to realize this oxygen concentration, the use of disk atomization is preferred. In gas atomization, there is a high possibility that oxygen contained in the gas used for spraying is contained, and the oxygen concentration often exceeds 300 wtppm.
- the oxygen concentration can be measured by an inert gas melting method with TCO600 manufactured by LECO.
- the copper alloy powder may contain unavoidable impurities other than the above-mentioned additive elements and copper, but may contain impurities as long as the properties necessary for the copper alloy powder are not affected.
- concentration of the unavoidable impurities excluding the gas component be 0.01 mass% or less from the viewpoint that the copper alloy powder can be efficiently melted and bonded.
- the specific means is not particularly limited as long as the method uses the copper alloy powder of the present invention.
- a thin layer of the copper alloy powder of the present invention is formed, and the copper alloy powder in the thin layer is solidified by sintering or fusion bonding with an electron beam or a laser beam to form a shaped object layer.
- the step of forming the thin layer by laying the copper alloy powder of the present invention on a stage for forming, and irradiating the portion to be formed with an electron beam to the thin layer dissolve the copper alloy powder.
- the laminate molded article of the present invention can be manufactured by repeatedly performing the step of solidifying by natural cooling a plurality of times.
- the step of forming the thin layer by laying the copper alloy powder of the present invention on a forming stage, and irradiating the portion to be formed with the thin layer with a laser beam to form the thin layer.
- the layered object of the present invention can be manufactured by repeating the step of dissolving the powder and then coagulating by natural cooling a plurality of times.
- the laser beam can be appropriately selected according to the facility environment, the required product performance, etc., as long as it can dissolve the copper alloy powder. For example, a fiber laser with a wavelength of about 1060 nm or a wavelength of about 1060 nm A 450 nm blue laser can be selected.
- the laminate-molded article manufactured by the manufacturing method of the present invention is excellent in mechanical strength and conductivity. Specifically, it is possible to obtain the characteristic that the relative density to the theoretical density is 98% or more, the conductivity is 50% IACS or more, and the 0.2% proof stress is 700 MPa or more. In this respect, the relative density is more preferably 99% or more, and more preferably 99.5% or more.
- the laminate of the present invention has a relative density to the theoretical density of 98% or more. If the relative density to the theoretical density is 98% or more, it is possible to use the layered object of the present invention even in a situation where the mechanical strength is highly required.
- the density of the layered object is indicated by relative density.
- the theoretical density is calculated as (density of Cu (g / cm 3 ) ⁇ 95 + W density (g / cm 3 ) ⁇ 5) / 100 (g / cm 3 ).
- the theoretical density of W is the theoretical density of 19.25 g / cm 3
- Cu is calculated as 8.94 g / cm 3
- the theoretical density is calculated to be 9.455 (g / cm 3).
- the measured density of the layered product can be measured, for example, by the Archimedes method.
- the density measurement by the Archimedes method can be performed according to "JIS Z 2501: Sintered metal material-density, oil content and open porosity test method". Water may be used as the liquid.
- the laminate of the present invention has a conductivity of 50% IACS or more. If the conductivity is 50% IACS or more, it is possible to use the layered object of the present invention even in a situation where the conductivity requirement is high. From this viewpoint, the conductivity is more preferably 70% IACS or more, and more preferably 90% IACS or more. The conductivity can be measured by a commercially available eddy current conductivity meter.
- IACS international annealed copper standard
- IACS is the conductivity of annealing standard soft copper (volume resistivity: 1.7241 ⁇ 10 -2 ⁇ m) adopted internationally as a standard of electric resistance (or electric conductivity). Is defined as 100% IACS.
- the laminate-molded article of the present invention has a 0.2% proof stress of 700 MPa or more. If the 0.2% proof stress is 700 MPa or more, it is possible to use the layered object of the present invention even in a situation where the mechanical strength is highly required. 0.2% proof stress is measured according to JIS Z2241 using a tensile tester.
- composition The composition of the elements contained in the copper alloy powder, which is a raw material of the laminate-molded article, was measured by ICP-OES (high frequency inductively coupled plasma emission spectrometry) of SPS3500 DD manufactured by SII. The balance not shown in the table is copper and unavoidable impurities.
- ICP-OES high frequency inductively coupled plasma emission spectrometry
- the layered products of Examples 1 to 45 and Comparative Examples 1 to 5 were produced using the copper alloy powder shown in Table 1, respectively. All of these copper alloy powders used the copper powder produced by the disk atomization method.
- the layered object forms a copper alloy powder in a thin layer, which is irradiated with an electron beam or a laser beam to solidify the copper alloy powder to form an object layer, and laminating the object layer.
- the shape of the modeling thing was taken as the plate-shaped test piece of W80xL100xH35.
- the apparent density was divided by the theoretical density (8.93 g / cm 3 ) and multiplied by 100 to define the relative density (%).
- [conductivity] A sample was cut out of a shaped article in a size of 20 mm, and the conductivity was evaluated with a commercially available eddy current conductivity meter. [0.2% proof stress] Each test piece is subjected to a tensile test in each direction parallel to rolling and perpendicular to rolling based on JIS Z2241 to measure 0.2% proof stress (YS: MPa), and 0.2% of them. The difference in proof stress was calculated.
- Comparative Examples 1 to 45 it is understood that the addition of an additive element having a solid solution content to copper of less than 0.2 at% can provide high conductivity while enhancing the mechanical strength of the layered object. Ru.
- Comparative Examples 1 and 2 contain chromium having a solid solution content of 0.2 at% with respect to copper, so that it was not possible to realize both mechanical strength and conductivity.
- Comparative Example 3 contains silicon having a solid solution content of 0.2 at% or more with respect to copper, and although the content is low, all forms a solid solution in copper, thus achieving both mechanical strength and conductivity. It was not.
- Comparative Example 4 contains aluminum having a solid solution content of at least 0.2 at% to copper, and although the content is low, all forms a solid solution in copper, so coexistence of mechanical strength and conductivity can be realized. It was not. Comparative Example 5 could not obtain sufficient mechanical strength because it was shaped with pure copper powder.
- a copper alloy powder for laminate molding comprising a copper alloy, a method for manufacturing a laminate molded article, and a laminate molded article, which are compatible in mechanical strength and conductivity. Therefore, when used in a 3D printer, it is possible to achieve both mechanical strength and conductivity.
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Abstract
Description
(1)銅に対する固溶量が0.2at%未満である添加元素を含有する積層造形用銅合金粉末。
(2)前記添加元素がW、Zr、Nb、Nd、Y、Mo、Os又はRuからなる群から選択される少なくとも一種である(1)に記載の積層造形用銅合金粉末。
(3)前記添加元素を0.1~12.0at%含有する(1)又は(2)に記載の積層造形用銅合金粉末。
(4)平均粒子径D50が20~100μmである(1)~(3)のいずれかに記載の積層造形用銅合金粉末。
(5)酸素濃度が1000wtppm以下である(1)~(4)のいずれかに記載の積層造形用銅合金粉末。
(6)(1)~(5)のいずれかに記載の積層造形用銅合金粉末を用いて積層造形物を製造する方法であって、
造形用のステージに前記銅合金粉末を敷き詰めて薄層を形成する工程と、
前記薄層に対し、造形すべき部分に電子ビームを照射して前記銅合金粉末を溶解させ、その後自然冷却により凝固させる工程、
を複数回繰り返して積層造形物を製造する方法。
(7)(1)~(5)のいずれかに記載の積層造形用銅合金粉末を用いて積層造形物を製造する方法であって、
造形用のステージに前記銅合金粉末を敷き詰めて薄層を形成する工程と、
前記薄層に対し、造形すべき部分にレーザービームを照射して前記銅合金粉末を溶解させ、その後自然冷却により凝固させる工程、
を複数回繰り返して積層造形物を製造する方法。
(8)銅合金から構成される積層造形物であって、
前記銅合金は、固溶量が0.2at%未満である添加元素を含有し、理論密度に対する相対密度が98%以上であり、導電率が50%IACS以上であり、0.2%耐力が700MPa以上である、積層造形物。
(9)前記添加元素がW、Zr、Nb、Nd、Y、Mo、Os又はRuからなる群から選択される少なくとも一種である(8)に記載の積層造形物。
(10)前記添加元素を0.1~12.0at%含有する(8)又は(9)に記載の積層造形物。
銅合金粉末は、公知の方法によって製造された銅合金粉末を使用することができる。粒径数μm以上のサイズであれば、工業的には製造コストに優れるアトマイズ法に代表される乾式法によって製造された銅合金粉末を使用することが一般的ではあるが、還元法などの湿式法によって製造された銅合金粉末を使用することも可能である。具体的には、タンデッシュの底部から、溶融状態の合金成分を落下させながら、高圧ガスまたは高圧水と接触させ、合金成分を急冷凝固させることにより、合金成分を粉末化する。この他、たとえばプラズマアトマイズ法、遠心力アトマイズ法などによって、金属粉末を製造してもよい。これらの製造方法で得られた金属粉末を用いることにより、緻密な積層造形物が得られる傾向にある。
銅に対する固溶量は、添加元素の固有の性質であり、一般的に相図と呼ばれる二つの元素の温度に対する相関係を示す図から抽出することができる。例えば、ASM International社発行のPhase Diagrams for Binary Alloys(ISBN:0-87170-682-2)を参考にして判断する。この相図から、Cu側の固溶量を参照し、液相以下の温度で最大の固溶量が0.2at%以下の元素が対象の元素となる。より詳細には、Ba、Bi、Ca、Gd、Eu、Ho、La、Lu、Mo、Nd、Nb、Os、Pb、Pm、Pu、Re、Ru、S、Se、Sr、Sm、Tb、Tc、Te、Th、Tm、U、V、W、Y、Yb、Zrである。
また、これらの元素は1種のみを添加してもよく、2種以上を添加してもよい。
また、添加元素を2種以上添加する場合、その合計量は0.1~12.0at%であればよい。
添加元素の含有量は、例えばSII社製SPS3500DDのICP-OES(高周波誘導結合プラズマ発光分析法)で測定することができる。
平均粒子径D50とは、顕微鏡画像解析により得られる粒子の画像から算出した面積に相当する円の直径を粒径として、当該粒度分布において、積算値50%での粒径をいう。
例えば、スペクトリス株式会社(マルバーン事業部)製の乾式粒子画像分析装置Morphologi G3により測定することができる。
酸素濃度は、LECO社製のTCH600にて、不活性ガス融解法で測定することができる。
本発明の銅合金粉末を用いる方法であれば、その具体的手段は特に制限されない。ここで、もっとも典型的な方法として、本発明の銅合金粉末の薄層を形成し、この薄層における銅合金粉末を、電子ビーム又はレーザービームで焼結又は溶融結合により固化させて造形物層を形成し、この造形物層を積層することにより積層造形物を製造することができる。
好ましくは、造形用のステージに、本発明の銅合金粉末を敷き詰めて薄層を形成する工程と、当該薄層に対し、造形すべき部分に電子ビームを照射して前記銅合金粉末を溶解させ、その後自然冷却により凝固させる工程を複数回繰り返して行うことで、本発明の積層造形物を製造することができる。
別の好ましい実施態様では、造形用のステージに、本発明の銅合金粉末を敷き詰めて薄層を形成する工程と、当該薄層に対し、造形すべき部分にレーザービームを照射して前記銅合金粉末を溶解させ、その後自然冷却により凝固させる工程を複数回繰り返して行うことで、本発明の積層造形物を製造することができる。レーザービームは、銅合金粉末を溶解させることができるものであれば、設備環境や要求される製品の性能等に応じて適宜選択することができ、例えば、波長約1060nmのファイバーレーザーや、波長約450nmの青色レーザーを選択することができる。
本発明の製造方法により製造される積層造形物は、機械強度及び導電率が優れている。具体的には、理論密度に対する相対密度が98%以上であり、導電率が50%IACS以上であり、0.2%耐力が700MPa以上という特性を得ることが可能である。この観点から、相対密度は99%以上がより好ましく、99.5%以上がより好ましい。
本発明では、積層造形物の密度は相対密度で示す。相対密度は、測定された密度及び理論密度によって、相対密度=(測定密度/理論密度)×100(%)で表される。理論密度とは、積層造形物の各構成元素において、各元素の理論密度から算出される密度の値である。例えば、W(タングステン)を5.0質量%含有するのであれば、各構成元素であるCuとWとの質量比を、Cu:W=95:5として、理論密度の算出に用いる。この場合、理論密度は、(Cuの密度(g/cm3)×95+Wの密度(g/cm3)×5)/100(g/cm3)として算出する。そして、Wの理論密度は19.25g/cm3、Cuの理論密度は8.94g/cm3として計算し、理論密度は9.455(g/cm3)と算出される。
なお、分析機器によってat%の測定結果となるが、質量%に換算することで計算できる。
一方、積層造形物の測定密度は、たとえばアルキメデス法により測定することができる。アルキメデス法による密度測定は、「JIS Z 2501:焼結金属材料-密度、含油率および開放気孔率試験方法」に準拠して行うことができる。液体には水を用いればよい。
導電率は、市販の渦流式導電率計によって測定できる。なお、IACS(international annealed copper standard)とは、電気抵抗(又は電気伝導度)の基準として、国際的に採択された焼鈍標準軟銅(体積抵抗率:1.7241×10-2μΩm)の導電率を、100%IACSとして規定されたものである。
0.2%耐力は、引張試験機を用いてJIS Z2241に準拠して測定する。
[組成]
積層造形物の原料となる銅合金粉末に含まれる元素の組成は、SII社製SPS3500DDのICP-OES(高周波誘導結合プラズマ発光分析法)で測定した。
なお、表に示されない残部は、銅及び不可避的不純物である。
[積層造形物]
実施例1~45及び比較例1~5の積層造形物は、それぞれ表1に示される銅合金粉末により作製されたものである。これらの銅合金粉末いずれもディスクアトマイズ法で作製した銅粉を用いた。
積層造形物は、銅合金粉末を薄層に形成し、これに電子ビーム又はレーザービームを照射して、銅合金粉末を固化させて造形物層を形成し、この造形物層を積層することによって作製した。また、評価を容易にするため造形物の形状は、W80×L100×H35の板状試験片とした。
[酸素濃度]
酸素濃度は、LECO社製のTCH600にて、不活性ガス融解法で測定した
[平均粒子径D50]
平均粒子径D50(体積基準)は、以下の装置及び条件で測定した。
メーカー:スペクトリス株式会社(マルバーン事業部)
装置名 :乾式粒子画像分析装置 Morphologi G3
測定条件:
粒子導入量:11mm3
射出圧:0.8bar
測定粒径範囲:3.5-210μm
測定粒子数:20000個
[相対密度]
造形物からサンプルを20mm四方で切り出し、アルキメデス法にて測定密度を算出する。そして見かけ密度を理論密度(8.93g/cm3)で除して100倍したものを相対密度(%)と定義した。
[導電率]
造形物からサンプルを20mm四方で切り出し、市販の渦流式導電率計にて導電率を評価した。
[0.2%耐力]
各試験片に対し、JIS Z2241に基いて圧延平行方向及び圧延直角方向の各方向の引張り試験を行って、0.2%耐力(YS:MPa)を測定し、また、それらの0.2%耐力の差を算出した。
一方、比較例1及び2は銅に対する固溶量が0.2at%であるクロムを含有するため、機械強度と導電率の両立を実現できなかった。
比較例3は、銅に対する固溶量が0.2at%以上あるシリコンを含有するため、含有量が低いものの、すべて銅中に固溶してしまうため、機械強度と導電率とも両立が実現できなかった。
比較例4は、銅に対する固溶量が0.2at%以上あるアルミニウムを含有するため、含有量が低いものの、すべて銅中に固溶してしまうため、機械強度と導電率の両立が実現できなかった。
比較例5は、純銅粉での造形であったため、十分な機械強度を得ることができなかった。
Claims (10)
- 銅に対する固溶量が0.2at%未満である添加元素を含有する積層造形用銅合金粉末。
- 前記添加元素がW、Zr、Nb、Nd、Y、Mo、Os又はRuからなる群から選択される少なくとも一種である請求項1に記載の積層造形用銅合金粉末。
- 前記添加元素を0.1~12.0at%含有する請求項1又は2に記載の積層造形用銅合金粉末。
- 平均粒子径D50が20~100μmである請求項1~3のいずれかに記載の積層造形用銅合金粉末。
- 酸素濃度が1000wtppm以下である請求項1~4のいずれかに記載の積層造形用銅合金粉末。
- 請求項1~5のいずれかに記載の積層造形用銅合金粉末を用いて積層造形物を製造する方法であって、
造形用のステージに前記銅合金粉末を敷き詰めて薄層を形成する工程と、
前記薄層に対し、造形すべき部分に電子ビームを照射して前記銅合金粉末を溶解させ、その後自然冷却により凝固させる工程、
を複数回繰り返して積層造形物を製造する方法。 - 請求項1~5のいずれかに記載の積層造形用銅合金粉末を用いて積層造形物を製造する方法であって、
造形用のステージに前記銅合金粉末を敷き詰めて薄層を形成する工程と、
前記薄層に対し、造形すべき部分にレーザービームを照射して前記銅合金粉末を溶解させ、その後自然冷却により凝固させる工程、
を複数回繰り返して積層造形物を製造する方法。 - 銅合金から構成される積層造形物であって、
前記銅合金は、固溶量が0.2at%未満である添加元素を含有し、理論密度に対する相対密度が98%以上であり、導電率が50%IACS以上であり、0.2%耐力が700MPa以上である、積層造形物。 - 前記添加元素がW、Zr、Nb、Nd、Y、Mo、Os又はRuからなる群から選択される少なくとも一種である請求項8に記載の積層造形物。
- 前記添加元素を0.1~12.0at%含有する請求項8又は9に記載の積層造形物。
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TWI770220B (zh) | 2022-07-11 |
EP3674016A4 (en) | 2020-12-16 |
EP3674016A1 (en) | 2020-07-01 |
CA3057056C (en) | 2022-12-06 |
TW201912421A (zh) | 2019-04-01 |
CN110366459A (zh) | 2019-10-22 |
JP2021059789A (ja) | 2021-04-15 |
KR102639553B1 (ko) | 2024-02-23 |
KR20190110117A (ko) | 2019-09-27 |
JP7008076B2 (ja) | 2022-02-10 |
US20200122229A1 (en) | 2020-04-23 |
JPWO2019039058A1 (ja) | 2019-12-19 |
CN110366459B (zh) | 2022-09-23 |
KR20220000912A (ko) | 2022-01-04 |
JP7419227B2 (ja) | 2024-01-22 |
CA3057056A1 (en) | 2019-02-28 |
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