Classifications

• • 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
• • 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
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B33—ADDITIVE MANUFACTURING TECHNOLOGY
  • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
  • B33Y70/00—Materials specially adapted for additive manufacturing
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B33—ADDITIVE MANUFACTURING TECHNOLOGY
  • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
  • B33Y80/00—Products made by additive manufacturing
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C38/00—Ferrous alloys, e.g. steel alloys
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C38/00—Ferrous alloys, e.g. steel alloys
  • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
  • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
  • C22C38/48—Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum

Definitions

• the present invention relates to hot work tool steel powder for additive manufacturing and hot work tool steel additive manufactured products.
• Hot work tool steels used in hot forging dies, die casting dies, and other tools come into contact with high-temperature workpieces, and therefore require high-temperature strength, toughness, and wear resistance.
• JIS steel grade SKD61 and improved versions of SKD61 have been used for hot work tool steels.
• additive manufacturing has been attracting attention as a means of easily creating near-net-shape metal products (components) with complex shapes.
• Additive manufacturing commonly known as 3D printing, is an additive manufacturing technology.
• Types of additive manufacturing include the powder spray method, in which a heat source is applied to metal powder to melt it and then layer it on top, and the powder bed method, in which a heat source is applied to metal powder spread on a stage to melt it, then the powder is solidified and layered repeatedly.
• Additive manufacturing allows metal products with complex shapes to be produced without requiring much of the traditional machining process, making it possible to use metal materials that are difficult to process.
• difficult-to-process metal materials are primarily high-strength metal materials, it is possible to produce metal products with complex shapes and long durability.
• Patent Document 1 proposes an additively manufactured hot work tool having a component composition containing, by mass%, 0.3 to 0.5% C, 2.0% or less Si, 1.5% or less Mn, 0.05% or less P, 0.05% or less S, 3.0 to 6.0% Cr, 0.5 to 3.5% of one or two of Mo and W according to the relationship (Mo + 1/2W), 0.1 to 1.5% V, 0 to 1.0% Ni, 0 to 1.0% Co, 0 to 1.0% Nb, and the balance being Fe and impurities, and characterized in that the area ratio of defects having an area of 1 ⁇ m2 or more in a cross section parallel to the stacking direction is 0.6% or less.
• Patent Document 2 discloses a steel powder that aims to achieve both high thermal conductivity and high corrosion resistance and is characterized by a composition, in mass%, of 0.10 ⁇ C ⁇ 0.25, 0.005 ⁇ Si ⁇ 0.600, 2.00 ⁇ Cr ⁇ 6.00, -0.0125 ⁇ [Cr]+0.125 ⁇ Mn ⁇ -0.100 ⁇ [Cr]+1.800...formula (a) (wherein [Cr] in formula (a) represents the mass % Cr content), 0.01 ⁇ Mo ⁇ 1.80, -0.00447 ⁇ [Mo]+0.010 ⁇ V ⁇ -0.1117 ⁇ [Mo]+0.901...formula (b) (wherein [Mo] in formula (b) represents the mass % Mo content), 0.0002 ⁇ N ⁇ 0.3000, with the balance being Fe and unavoidable impurities.
• an object of the present invention is to provide a hot work tool steel powder for additive manufacturing that can produce hot work tool steel additive manufactured products with high softening resistance.
• the present invention has been made in view of the above-mentioned problems. That is, one embodiment of the present invention satisfies the following conditions in mass %: 0.10% ⁇ C ⁇ 0.24%, 0.01% ⁇ Si ⁇ 0.50%, 0.01% ⁇ Mn ⁇ 0.19%, 0.5% ⁇ Ni ⁇ 1.5%, 3.6% ⁇ Cr ⁇ 4.4%, one or two of Mo and W according to the relational expression (Mo+1 ⁇ 2W): 2.1% ⁇ (Mo+1 ⁇ 2W) ⁇ 3.0%, 0.20% ⁇ V ⁇
• the hot work tool steel powder for additive manufacturing comprises C+Si/30+(Mn+Cr)/20+Ni/60+(Mo+1 ⁇ 2W)/15+V/10+Nb/20 ⁇ 0.75 (each element symbol in formula (1) indicates the content (mass %) of that element).
• Another aspect of the present invention is a hot work tool steel additive manufactured product that contains, in mass%, 0.10% ⁇ C ⁇ 0.24%, 0.01% ⁇ Si ⁇ 0.50%, 0.01% ⁇ Mn ⁇ 0.19%, 0.5% ⁇ Ni ⁇ 1.5%, 3.6% ⁇ Cr ⁇ 4.4%, one or two of Mo and W according to the relationship (Mo+1/2W): 2.1% ⁇ (Mo+1/2W) ⁇ 3.0%, 0.20% ⁇ V ⁇ 1.0%, 0.1% ⁇ Nb ⁇ 1.0%, and the remainder consisting of Fe and unavoidable impurities, and satisfies formula (1): C+Si/30+(Mn+Cr)/20+Ni/60+(Mo+1/2W)/15+V/10+Nb/20 ⁇ 0.75.
• hot work tool steel powder for additive manufacturing which can be used to manufacture hot work tool steel additive manufactured products with high softening resistance.
• 1 is a graph showing the tempering temperature and hardness of hot work tool steel additive manufactured products of an example of the present invention and a comparative example.
• 1 is a graph showing the cumulative holding time at 600°C and the hardness of hot work tool steel additive manufactured products of the present invention and comparative examples.
• 1 is a graph showing the mechanical properties ((a) 0.2% proof stress, (b) tensile strength, (c) elongation, (d) reduction of area) of an example of the present invention at room temperature.
• 1 is a graph showing the mechanical properties ((a) 0.2% yield strength, (b) tensile strength, (c) elongation, (d) reduction of area) of an example of the present invention at high temperatures.
• 1 is a graph showing Charpy impact values at room temperature of examples of the present invention.
• 1 is a graph showing the thermal conductivity of an example of the present invention.
• the present invention has a chemical composition consisting of 0.10% ⁇ C ⁇ 0.24%, 0.01% ⁇ Si ⁇ 0.50%, 0.01% ⁇ Mn ⁇ 0.19%, 0.5% ⁇ Ni ⁇ 1.5%, 3.6% ⁇ Cr ⁇ 4.4%, one or two of Mo and W according to the relationship (Mo + 1 ⁇ 2W): 2.1% ⁇ (Mo + 1 ⁇ 2W) ⁇ 3.0%, 0.20% ⁇ V ⁇ 1.0%, 0.1% ⁇ Nb ⁇ 1.0%, and the balance being Fe and unavoidable impurities.
• additive manufacturing powder or metal powder the reasons for the compositional limitations of the hot work tool steel powder for additive manufacturing (hereinafter also referred to as additive manufacturing powder or metal powder) specified in the present invention will be described.
• C 0.10% ⁇ C ⁇ 0.24%
• Carbon (C) is a fundamental element of hot-work tool steels, partially dissolving in the matrix to impart strength, while partially forming carbides to enhance wear resistance and seizure resistance. Furthermore, when added together with substitutional atoms with high affinity for C, such as Cr, C dissolved as an interstitial atom is expected to contribute to the I (interstitial atom)-S (substitutional atom) effect (which acts as drag resistance for solute atoms and increases the strength of hot-work tools). It can also enhance hardenability.
• the range of C is 0.10% ⁇ C ⁇ 0.24% in order to improve crack resistance while maintaining hardness sufficient for use in dies.
• the lower limit of C is preferably 0.12%, more preferably 0.15% or more, and even more preferably 0.18% or more.
• the upper limit of C is preferably 0.23% or less.
• Si 0.01% ⁇ Si ⁇ 0.50%
• Silicon can be used as a deoxidizer when adjusting the chemical composition of molten steel. It is difficult to eliminate silicon from the steelmaking process, and the closer one tries to eliminate silicon, the higher the manufacturing cost. Therefore, the lower limit of silicon content is set to 0.01%. A preferred lower limit is 0.05%, and more preferably 0.08% or more. On the other hand, excessive silicon content can lead to the formation of ferrite in the structure after tempering, so the upper limit is set to 0.50%. A preferred upper limit is 0.25%, more preferably 0.17% or less, and even more preferably 0.15% or less, and even more preferably 0.13% or less.
• Mn 0.01% ⁇ Mn ⁇ 0.19%
• Mn has the effects of improving hardenability, suppressing the formation of ferrite in the structure after tempering, and achieving appropriate quench-and-temper hardness.
• the lower limit of Mn is set to 0.01%.
• a preferred lower limit is 0.02%, more preferably 0.03% or more, even more preferably 0.04% or more, and even more preferably 0.05% or more.
• the upper limit is set to 0.19%.
• a preferred upper limit is 0.18%, more preferably 0.17% or less, and even more preferably 0.15% or less.
• Ni 0.5% ⁇ Ni ⁇ 1.5%
• Ni is an element that suppresses the formation of ferrite in the structure after tempering. It also imparts excellent hardenability to tool materials, along with C, Cr, Mn, Mo, W, and the like, and is an effective element for preventing a decrease in toughness by forming a martensite-based structure even when the cooling rate during quenching is slow. Furthermore, Ni also improves the intrinsic toughness of the matrix, so in the present invention, the lower limit of Ni is set to 0.5%. A preferred lower limit is 0.6%, i.e., 0.7% or more. However, excessive Ni increases the viscosity of the matrix and reduces machinability. Therefore, the upper limit of Ni is set to 1.5%. A preferred upper limit is 1.2%, more preferably 1.0% or less, and even more preferably 0.9% or less.
• Cr 3.6% ⁇ Cr ⁇ 4.4%
• Cr is a basic element of hot work tool steel that improves hardenability and forms carbides, thereby strengthening the matrix and improving wear resistance and toughness.
• the Cr content is set to 3.6% ⁇ Cr ⁇ 4.4%.
• the preferred lower limit of Cr is 3.7%, and more preferably 3.8% or more.
• the preferred upper limit of Cr is 4.3%, and more preferably 4.2% or less.
• Mo and W can be added alone or in combination to impart strength by precipitating or agglomerating fine carbides during tempering, thereby improving softening resistance and high-temperature strength.
• Mo and W can be added alone or in combination to impart strength by precipitating or agglomerating fine carbides during tempering, thereby improving softening resistance and high-temperature strength.
• the C content is reduced to improve cracking resistance, a slightly higher Mo and W content can be expected to complement the strength.
• W has approximately twice the atomic weight of Mo, the Mo content can be determined together with the Mo equivalent defined by the relationship (Mo + 1/2W).
• the content should be 2.1% or more, as determined by the relationship (Mo + 1/2W).
• the preferred lower limit is 2.2%.
• Mo and W may result in reduced machinability and toughness, resulting in reduced cracking resistance.
• their high melting points make them difficult to melt, making their inclusion in large amounts undesirable from a manufacturing perspective. Therefore, the value according to the relational expression (Mo + 1/2W) is set to 3.0% or less.
• the preferred upper limit is 2.8%, more preferably 2.6% or less, and even more preferably 2.5% or less.
• W is a more expensive element than Mo, it is preferable to contain Mo alone when cost reduction is important.
• the Nb content is 0.1% ⁇ Nb ⁇ 1.0%.
• the preferred lower limit is 0.15%.
• the upper limit is preferably 0.5%, more preferably 0.40% or less, further preferably 0.35% or less, 0.30% or less, or 0.25% or less.
• the balance consists of Fe and unavoidable impurities.
• Typical examples of unavoidable impurities include elements such as P, S, Cu, Al, Ca, Mg, O (oxygen), N (nitrogen), and B (boron). The lowest possible content of these elements is preferable. However, small amounts may be included due to additional effects such as controlling the shape of inclusions, improving other mechanical properties, and improving manufacturing efficiency. In this case, the ranges of Al ⁇ 0.04%, Ca ⁇ 0.01%, Mg ⁇ 0.01%, O ⁇ 0.05%, N ⁇ 0.05%, and B ⁇ 0.05% are sufficient and are the preferred upper limits of the present invention.
• P and S can conform to the JIS steel grade SKD61, e.g., P ⁇ 0.030% and S ⁇ 0.020%.
• the overall balance within the above-mentioned component ranges is expected to improve crack resistance during molding, making it possible to obtain hot work tool steel additive manufacturing products with excellent softening resistance.
• Formula (1) C+Si/30+(Mn+Cr)/20+Ni/60+(Mo+1/2W)/15+V/10+Nb/20 ⁇ 0.75
• the left side of formula (1) is an improved version of Pcm, which is used as a cold cracking susceptibility index for welding.
• C, Si, Mn, Cr, Cu, Ni, Mo, W, and V represent the content (mass%) of each element.
• cracking is a problem in welding. Since both processes involve molten solidification structures, this index was found to be applicable to crack suppression in additive manufacturing and was applied to the present invention.
• the hot cracking index HCS Another known cracking index for welding is the hot cracking index HCS.
• HCS hot cracking index
• prior investigations revealed that the molding cracks in this composition system were largely cracked from the surface and had a different morphology from the hot cracks that tend to occur at the solidification interface, etc. Since the molding cracks in this composition system are found in areas prone to tensile stress due to thermal contraction and therefore occur at low temperatures, it was assumed that they were similar to cold cracks in welding. Therefore, the cold cracking index Pcm was applied in the present invention.
• the left side of formula (1) is more preferably 0.72 or less. It is even more preferably 0.70 or less, 0.68 or less, or 0.66 or less.
• Formula (2) 545-330C+2Al-14Cr-13Cu-23Mn-5Mo-4Nb-13Ni-7Si+3Ti+4V ⁇ 440
• the above formula (2) can be adjusted to 440 or less.
• Formula (2) is a relationship between elements excluding Co and the Ms point, as disclosed in a literature (K. Ishida, Journal of Alloys and Compounds, Volume 220, Issue 1-2, 1995, pp. 126-131).
• a high value of formula (2) is expected to increase the Ms point, which tends to transform into brittle martensite during high-temperature additive manufacturing and become susceptible to cracking due to thermal contraction when cooled to room temperature.
• formula (2) is preferably adjusted to 300 or more.
• the hot work tool steel powder for additive manufacturing of the present invention can be produced by, for example, gas atomization, water atomization, disk atomization, plasma atomization, rotating electrode atomization, and the like.
• gas atomization is a method in which a molten raw material prepared to have the desired composition is heated to above its melting point by high-frequency induction heating, melted, and then the molten metal that flows out through fine holes is finely crushed by injecting an inert gas such as argon gas or nitrogen gas onto the molten metal, which is then rapidly cooled and solidified to obtain powder.
• This gas atomization method allows scrap metal, raw metal raw materials, etc.
• the hot work tool steel powder for additive manufacturing of the present invention preferably has a 50% particle size (hereinafter referred to as "D50") of a cumulative particle size distribution on a volume basis of 10 to 250 ⁇ m.
• D50 50% particle size
• the cumulative particle size distribution of the powder for layered manufacturing of the present invention is expressed as a cumulative volumetric particle size distribution, and its D50 can be expressed as a value measured by the laser diffraction scattering method specified in JIS Z 8825.
• the D50 of the hot work tool steel powder for additive manufacturing of the present invention may be adjusted by mesh sieving or air classification, etc., depending on the method described above.
• metal powders used in the powder bed method are melted by a laser beam, which serves as the heat source, but coarse metal powder that is difficult to melt must be removed to minimize the area affected by the heat.
• highly adhesive fine metal powder must also be removed to achieve optimal fluidity for ensuring the spreadability of the metal powder.
• the preferred upper limit of D50 is 40 ⁇ m, and the preferred lower limit of D50 is 20 ⁇ m.
• the hot work tool steel additive manufactured product of the present invention is expected to exhibit excellent mechanical properties.
• the hot work tool steel additive manufactured product of the present invention preferably has a room temperature (approximately 20°C) tensile strength of 1000 to 2000 MPa when the tempered hardness is adjusted to 45 ⁇ 1 HRC.
• a more preferred lower limit is 1200 MPa, an even more preferred lower limit is 1300 MPa, and an even more preferred lower limit is 1400 MPa.
• the room temperature 0.2% yield strength when the tempered hardness is adjusted to 45 ⁇ 1 HRC is preferably 800 to 2000 MPa.
• a more preferred lower limit is 800 MPa, and an even more preferred lower limit is 1000 MPa.
• the room temperature elongation when the tempered hardness is adjusted to 45 ⁇ 1 HRC is preferably 8% or more. A more preferred lower limit is 10%, and an even more preferred lower limit is 12%.
• the room temperature drawing is preferably 30% or more. A more preferable lower limit is 40%, and an even more preferable lower limit is 50%.
• the hot work tool steel additive manufactured product of the present invention preferably has a room temperature thermal conductivity of 10 W/(m ⁇ K) or more when the tempered hardness is adjusted to 45 ⁇ 1 HRC.
• a more preferred lower limit is 15 W/(m ⁇ K)
• an even more preferred lower limit is 20 W/(m ⁇ K)
• an especially preferred lower limit is 25 W/(m ⁇ K).
• the laser output can be set to 50 to 400 W, the scanning speed to 200 to 2000 mm/sec, and the scanning pitch to 0.02 to 0.20 mm.
• the layer thickness per laser scan is too large, heat is not easily transferred to the entire spread metal powder during laser irradiation, preventing the metal powder from melting sufficiently and promoting the formation of internal defects.
• the layer thickness per scan is preferably set to 10 to 200 ⁇ m.
• a more preferable lower limit for the layer thickness is 20 ⁇ m, and a more preferable upper limit for the layer thickness is 100 ⁇ m.
• a preheating step may be carried out before the additive manufacturing process described above. However, because the metal powder of the present invention has improved crack resistance compared to conventional hot work tool steel powders, for example, if the additive manufacturing product is small and has few stress concentration areas, it is possible to omit the preheating step before additive manufacturing or to use a lower temperature.
• the tempering temperature varies depending on the target hardness, etc., but is generally around 500 to 700°C. If quenching is performed before tempering, the quenching temperature is generally around 900 to 1100°C. For example, in the case of SKD61, a typical hot work tool steel, the quenching temperature is around 1000 to 1030°C, and the tempering temperature is around 550 to 650°C.
• the tempered hardness is preferably 50 HRC (Rockwell hardness) or less or 520 HV (Vickers hardness) or less. More preferably, it is 48 HRC or less or 500 HV or less. Also, it is preferably 40 HRC or more or 380 HV or more. More preferably, it is 42 HRC or more or 400 HV or more.
• Example 1 Each metal raw material was prepared to have the composition shown in Table 1, then charged into a high-frequency induction melting furnace and melted. The molten metal was pulverized with argon gas to obtain gas-atomized powder. The resulting atomized powder was subjected to mesh sieving and airflow classification to adjust the particle size, resulting in powders for additive manufacturing (AM) of the present invention and comparative examples with a D50 of 35 ⁇ m.
• AM additive manufacturing
• Table 4 also shows the values of formula (1): C + Si/30 + (Mn + Cr)/20 + Ni/60 + (Mo + 1 ⁇ 2W)/15 + V/10 + Nb/20 for Samples No. 1 to 4, and the values of formula (2): 545-330C + 2Al-14Cr-13Cu-23Mn-5Mo-4Nb-13Ni-7Si + 3Ti + 4V.
• Example 2 Next, the softening behavior of the inventive example and comparative example when held at high temperatures was confirmed.
• Samples No. 3 and 4 of Example 1 described above were subjected to tempering heat treatment and tempered to 45 ⁇ 1 HRC. Then, the samples were held in a heat treatment furnace at 600°C for a given time, removed from the furnace, and cooled to room temperature. Their Rockwell hardness was measured based on JIS Z 2245. This procedure was repeated several times to measure the cumulative holding time at 600°C and hardness, i.e., softening resistance at 600°C.
• Figure 2 shows the relationship between the cumulative holding time at 600°C and hardness. Figure 2 confirms that the inventive example showed less decrease in hardness than the comparative example even when held at 600°C for a long time, i.e., had high softening resistance even when held in a high-temperature environment for a long time.
• the additively manufactured products of the present invention had room temperature tensile strength of 1200 MPa or more, room temperature 0.2% yield strength of 1000 MPa or more, room temperature elongation of 13% or more, and room temperature drawing of 50% or more at all tempered hardnesses. Furthermore, as can be seen from Figure 4, the additively manufactured products of the present invention had high temperature tensile strength of 800 MPa or more, high temperature 0.2% yield strength of 600 MPa or more, high temperature elongation of 13% or more, and high temperature drawing of 50% or more at all tempered hardnesses.
• the additively manufactured products of the present invention had room temperature tensile strength of 1400 MPa or more, room temperature 0.2% yield strength of 1200 MPa or more, room temperature elongation of 13% or more, and room temperature drawing of 60% or more. Furthermore, at a hardness of 45 ⁇ 1 HRC, the additively manufactured product of this invention had a high-temperature tensile strength of 900 MPa or more, a high-temperature 0.2% yield strength of 700 MPa or more, a high-temperature elongation of 16% or more, and a high-temperature reduction of 60% or more.
• the additively manufactured product of the present invention had a Charpy impact value of 60 J/ cm2 or more at all tempered hardnesses. The Charpy impact value was also good at 45 ⁇ 1 HRC hardness, at 60 J/ cm2 or more. Furthermore, it was confirmed from FIG. 6 that the additively manufactured product of the present invention had a thermal conductivity of 25 W/(m ⁇ K) or more at room temperature at 45 ⁇ 1 HRC hardness. From Figures 3 to 6, it was confirmed that the additively manufactured product of the present invention has properties at the same level as those of ingot hot work tool steel, and is suitable for use in hot work tools, for example.
• the hot work tool steel powder for additive manufacturing and the additive manufactured product of the present invention are most preferably applied to hot work tool applications such as die-casting molds, but by taking advantage of the various excellent properties of the additive manufactured product of the present invention, it can also be used to repair molds, for example, by using additive manufacturing by powder spraying.Furthermore, by taking advantage of the various excellent properties of the additive manufactured product of the present invention, it may also be applied to molds that require an internal cooling mechanism, such as plastic molds.

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