EP3719153B1 - Heissgepresste legierung auf nickelbasis, warmschmiedewerkzeug damit und herstellungsverfahren für geschmiedetes produkt - Google Patents

Heissgepresste legierung auf nickelbasis, warmschmiedewerkzeug damit und herstellungsverfahren für geschmiedetes produkt Download PDF

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EP3719153B1
EP3719153B1 EP18883639.9A EP18883639A EP3719153B1 EP 3719153 B1 EP3719153 B1 EP 3719153B1 EP 18883639 A EP18883639 A EP 18883639A EP 3719153 B1 EP3719153 B1 EP 3719153B1
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Prior art keywords
die
less
hot
based alloy
present
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French (fr)
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EP3719153A4 (de
EP3719153A1 (de
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Shogo Suzuki
Chuya Aoki
Tomonori Ueno
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Proterial Ltd
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Proterial Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J13/00—Details of machines for forging, pressing, or hammering
    • B21J13/02—Dies or mountings therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
    • C22C19/057—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being less 10%
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
    • B21J5/02—Die forging; Trimming by making use of special dies ; Punching during forging
    • B21J5/025—Closed die forging
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working

Definitions

  • the present invention relates to a Ni-based alloy for a hot die, a hot forging die made thereof, and a method for manufacturing a forged product.
  • a material for forging is heated to a predetermined temperature to reduce the deformation resistance.
  • the heat-resistant alloy has a high strength even at a high temperature and a hot forging die to be used in the forging of the heat-resistant alloy is required to have high mechanical strength at a high temperature.
  • hot forging when the temperature of a hot forging die is lower than the temperature of a material for forging, the workability of the material for forging decreases due to heat removal, and thus, products of poor workability materials such as Alloy 718 and Ti alloy are forged by heating the hot forging die with the raw material.
  • the hot forging die should have a high mechanical strength at a high temperature equal to or near the temperature to which the material for forging is heated.
  • Ni-based heat-resistant super alloys that can be used in hot forging at a die temperature of 1000°C or more in the air are proposed (for example, see Patent Documents 1 to 5).
  • WO2017/057453 discloses a Ni-based alloy for hot metal die, hot forging die using the same, and manufacturing method for forged product (paragraph 0001), wherein the Ni base alloy for hot metal die and the hot forging comprises in terms of mass%, 10.3-11.0% W, 9.0-11.0% Mo, and 5.8-6.8% Al, the reminder being Ni and unavoidable impurities O: 5 ppm, N: 2 ppm, C: 0.016 %, Si: 0.008 %, P: 0.001 %, S: ⁇ 0.001 %, Cr: 0.001 %, Mn: 0.008 %, Fe: 0.01 %, Co: 0.001 %, and Cu: ⁇ 0.001 %.
  • hot forging includes hot die forging in which the temperature of the hot forging die is close to the temperature of the material for forging and isothermal forging in which the hot forging die is heated to the same temperature as the material for forging.
  • Ni-based heat-resistant super alloys described above have an advantage of having a high-temperature compressive strength. But in terms of oxidation resistance, fine scales of nickel oxide are scattered from a die surface upon cooling after heating in the air and this may result in the deterioration in the working environment and the shape deterioration. In order to maximize the effect of being capable of using in the air, oxidation of the die surface and scattering of scales associated therewith become large problems.
  • the present inventors have studied the deterioration in the working environment and the shape deterioration caused by oxidation of the die surface and scattering of scales associated therewith, and found a composition having a high high-temperature compressive strength and a good oxidation resistance, and thereby achieved the present invention.
  • the present invention provides a Ni-based alloy for hot metal die, a hot forging die and method of manufacturing a forged product according to the appended claims.
  • the present invention can provide a Ni-based alloy for hot die having a high high-temperature compressive strength and a good oxidation resistance. This enables to suppress the deterioration in the working environment and the shape deterioration in hot forging.
  • Ni-based alloy for hot die of the present invention will be described in detail.
  • the unit for the chemical composition is mass%. Note that the Ni-based alloy for hot die becomes the base material of the hot forging die of the present invention.
  • W forms a solid solution in an austenitic matrix, and forms a solid solution also in a gamma prime phase ( ⁇ ' phase) basically composed of Ni 3 Al that is a precipitation strengthening phase to enhance the high-temperature strength of the alloy. Meanwhile, W has an effect of reducing the oxidation resistance and an effect of facilitating the precipitation of harmful phases such as the TCP (Topologically Close Packed) phase.
  • the content of W in the Ni-based alloy of the present invention is 7.0 to 15.0%.
  • the lower limit is preferably 10.0%
  • the upper limit is preferably 12.0%
  • the upper limit is further preferably 11.0%.
  • Mo forms a solid solution in an austenitic matrix and forms a solid solution also in a gamma prime phase basically composed of Ni 3 Al that is a precipitation strengthening phase to enhance the high-temperature strength of the alloy. Meanwhile, Mo has an effect of reducing the oxidation resistance. From the viewpoint of enhancing the high-temperature strength and suppressing the reduction of the oxidation resistance, the content of Mo in the Ni-based heat-resistant super alloy of the present invention is 2.5 to 11.0%.
  • the preferred lower limit of Mo is preferably set by taking into consideration the content of W, Ta, Ti, and Nb. In order to reliably achieve the effect of Mo, the lower limit is preferably 4.0%, and the lower limit is further preferably 4.5%.
  • the upper limit of Mo is preferably 10.5%, further preferably 9.0%, and more preferably 6.0%.
  • Al has effects of binding to Ni to precipitate a gamma prime phase composed of Ni 3 Al, enhancing the high-temperature strength of the alloy, producing an alumina film on the surface of the alloy, and imparting the oxidation resistance to the alloy. Meanwhile, an excess content of Al also has an effect of excessively producing eutectic gamma prime phases to reduce the high-temperature strength of the alloy.
  • the content of Al in the Ni-based alloy of the present invention is 5.0 to 7.5%.
  • the lower limit is preferably 5.2%, and further preferably 5.4%.
  • the upper limit of Al is preferably 6.7%, further preferably 6.5%, and more preferably 6.0%.
  • Cr has effects of promoting the formation of a continuous layer of alumina on the surface of or inside the alloy and increasing the oxidation resistance of the alloy. Thus, 0.5% or more of Cr is required to be contained.
  • 3.0 to 7.5% of Cr can achieve a high compressive strength at 1000°C as shown in Table 4, Fig. 5 , and the like described below.
  • a high compressive strength can be obtained not only at 1000°C, but also at a temperature of 1000°C to 1100°C.
  • the addition of Cr in a range more than 7.5% reduces the compressive strength at 1000°C or more and thus should be avoided.
  • the addition of Cr is not necessarily disadvantageous for the high-temperature strength. It was revealed by the present invention that the addition of Cr of 0.5 to 7.5% in addition to Al, W, and the like rather increases the high-temperature strength and increases the oxidation resistance while maintaining a high high-temperature strength.
  • the lower limit is preferably 1.0%, and more preferably 1.3%.
  • an excess content of Cr also has an effect of facilitating the precipitation of harmful phases such as the TCP (Topologically Close Packed) phase. Particularly when numerous elements such as W, Mo, Ta, Ti, and Nb that increase the high-temperature strength of the alloy, harmful phases are likely to be precipitated.
  • the upper limit of the content of Cr in the present invention is preferably 3.0%.
  • the upper limit is further preferably 2.0%.
  • the Ni-based heat-resistant super alloy according to the present invention may contain Ta.
  • Ta forms a solid solution by substituting into the Al site in a gamma prime phase composed of Ni 3 Al, thereby enhancing the high-temperature strength of the alloy.
  • Ta increases the adhesiveness and the oxidation resistance of an oxide film formed on the surface of the alloy, and has an effect of further increasing the oxidation resistance of the alloy particularly under heat cycle conditions of short heating and cooling cycles of a die. Meanwhile, an excess content of Ta also has an effect of facilitating precipitation of harmful phases such as the TCP phase.
  • the upper limit of Ta according to the present invention in the case of containing Ta is 7.0%.
  • the lower limit is preferably 0.5%
  • the lower limit is further preferably 2.5%, and more preferably 5.0%.
  • the upper limit of Ta is preferably 6.7%, and further preferably 6.5%.
  • the Ni-based heat-resistant super alloy according to the present invention may contain one or two or more elements selected from Zr, Hf, rare-earth elements, Y, and Mg.
  • Zr, Hf, rare-earth elements, and Y suppress the diffusion of metal ions and oxygen at the grain boundary by segregation of the oxide film into the grain boundary. This suppression of grain boundary diffusion reduces the growth rate of the oxide film and changes the growth mechanism of promoting the spallation of the oxide film, which increases the adhesion between the film and the alloy. That is, these elements have an effect of increasing the oxidation resistance of the alloy due to the reduction of the growth rate and the increase of the film adhesion described above, particularly under heat cycle conditions of short heating and cooling cycles of a die.
  • Rare-earth elements, Y, and Mg form sulfide with S (sulfur) that reduces the adhesion of the film through the segregation to the interface between the oxide film and the alloy and the inhibition of the chemical bonding between them, and they increase the adhesion by preventing segregation of S, and have an effect of increasing the oxidation resistance of the alloy particularly under heat cycle conditions of short heating and cooling cycles of a die.
  • S is an element that may be contained as impurities.
  • La is preferably used. That is because La has a large effect of increasing the oxidation resistance. La also has an effect of preventing segregation of S in addition to the effect of suppressing the diffusion described above and is excellent in these effects, and thus La may be selected among rare-earth elements.
  • the addition of Y is also preferred since Y has a similar effect of La. Two or more elements including La and Y are particularly preferably used.
  • Hf or Zr having a lower effect of reducing the toughness than rare-earth elements and Y is preferably used.
  • Hf is particularly preferably used, since Hf has a much lower effect of reducing the toughness and an effect of preventing cracks during casting can also be expected.
  • Zr and Hf have a lower effect of preventing segregation of S than rare-earth elements and Y, and thus the simultaneous addition of Mg further increases the oxidation resistance. Consequently, in order to enhance the oxidation resistance and the toughness in a balanced manner, Hf and Mg are particularly preferably simultaneously used.
  • the upper limit of each content of Zr and Hf in the present invention in the case of containing Zr and Hf is 0.5%.
  • the upper limit of each content of Zr and Hf is preferably 0.3%, and further preferably 0.2%.
  • the lower limit in the case of containing Zr and Hf may be 0.001%.
  • the lower limit at which the effect of containing Zr and Hf can be sufficiently exerted may be preferably 0.01%, further preferably 0.05%, and more preferably 0.1% or more.
  • Rare-earth elements and Y have a higher effect of reducing the toughness than Zr and Hf as described above, the upper limit of each content of these elements according to the present invention in the case of containing rare-earth elements and Y is 0.2%, and the upper limit is preferably 0.02%, and further preferably 0.005%.
  • the lower limit in the case of containing rare-earth elements and Y may be 0.001%.
  • the lower limit at which the effect of containing rare-earth elements and Y can be sufficiently exerted may be preferably 0.002%, and further preferably 0.003% or more.
  • Mg should be contained only in an amount required to form sulfide with S that is contained in the alloy as impurities.
  • the upper limit of the content in the case of containing Mg is 0.03%.
  • the lower limit in the case of containing Mg may be 0.001%.
  • the upper limit of Mg is preferably 0.025%, and more preferably 0.02%. Meanwhile, the lower limit may be 0.005% so that the effect of adding Mg can be more reliably exerted.
  • the Ni-based alloy for hot die of the present invention may contain one or two selected from Ti and Nb in a total amount within a range of 3.5% or less.
  • Ti and Nb form a solid solution like Ta by substituting into the Al site in a gamma prime phase composed of Ni 3 Al, thereby enhancing the high-temperature strength of the alloy.
  • Ti and Nb are low-cost elements as compared with Ta and advantageous in terms of die cost. Meanwhile, an excess content of Ti and Nb has, like Ta, an effect of facilitating the precipitation of harmful phases such as the TCP phase and has also an effect of excessively producing a eutectic gamma prime phase to reduce the high-temperature strength of the alloy.
  • Ti and Nb have a lower effect of increasing the high-temperature strength as compared with Ta and have no effect of increasing the oxidation resistance, unlike Ta.
  • Ta is desired to be substituted by Ti or Nb that are advantageous in terms of die cost within a range in which the high-temperature strength property and the oxidation resistance are maintained at the same level as the case containing only Ta.
  • the upper limit of the total content of Ta, Ti, and Nb is 7.0% and the upper limit of the content of one or two elements selected from Ti and Nb is 3.5%, when Ti and/or Nb are/is contained.
  • the upper limit of the total content of Ta, Ti, and Nb is preferably 6.5%, and the upper limit of the content of one or two elements selected from Ti and Nb is preferably 2.7%. From the viewpoint of reliably achieve an effect of enhancing the high-temperature strength, the lower limit of the total content of Ta, Ti, and Nb may be 1.0%, and from the viewpoint of reliably achieve an effect of reducing the die cost, the lower limit of the content of one or two elements selected from Ti and Nb may be 0.5%.
  • the lower limit of the total content of Ta, Ti, and Nb is preferably 3.0%, and the lower limit is further preferably 4.0%.
  • the lower limit of the content of one or two elements selected from Ti and Nb is preferably 1.0%.
  • Ti is preferably used from an economical viewpoint.
  • Nb is preferably used.
  • Ti and Nb are particularly preferably simultaneously used.
  • the Ni-based alloy for hot die according to the present invention may contain Co.
  • Co forms a solid solution in an austenitic matrix to enhance the high-temperature strength of the alloy. Meanwhile, an excess content of Co increases the die cost since Co is an expensive element as compared with Ni, and Co has an effect of facilitating the precipitation of harmful phases such as the TCP phase.
  • Co may be contained within a range of 15.0% or less.
  • the lower limit is preferably 0.5%, further preferably 2.5%.
  • the upper limit is preferably 13.0%, and further preferably 6.0%.
  • the Ni-based alloy for hot die of the present invention may contain one or two elements selected from 0.25% or less of C (carbon) and 0.05% or less of B (boron).
  • C and B increase the strength of grain boundaries of the alloy and enhance the high-temperature strength and the ductility. Meanwhile, an excess content of C and B causes the formation of a coarse carbide or boride and has an effect of reducing the strength of the alloy.
  • the range of the content of C is preferably 0.005 to 0.25% and the range of the content of B is 0.005 to 0.05%, when C is contained in the present invention.
  • the lower limit is preferably 0.01% and the upper limit is preferably 0.15%.
  • the lower limit is preferably 0.01% and the upper limit is preferably 0.03%, and the upper limit is more preferably 0.02%.
  • C is particularly preferably used
  • B is particularly preferably used.
  • C and B are particularly preferably simultaneously used.
  • Ni is the main element for constituting a gamma phase and constitutes also a gamma prime phase together with Al, Ta, Mo, W, and the like.
  • S is particularly preferably 0.0030% or less. More preferably, S is limited to a range of 0.0010% or less to prevent the reduction of the adhesion of the film through the segregation to the interface between the oxide film and the alloy and the inhibition of the chemical bonding between them.
  • the composition according to the present invention preferably contains W, Mo, Al, Cr, Ta, Hf, and Mg. Especially, the following range is preferred.
  • the Ni-based alloy for hot die has a composition comprising, in mass%, W: 10.0 to 12.0%, Mo: 4.0 to 6.0%, Al: 5.0 to 6.5%, Cr: 1.0 to 3.0%, Ta: 2.5 to 6.7%, Hf: 0.01 to 0.3%, Mg: 0.001 to 0.025%, and the balance of Ni with inevitable impurities.
  • the present invention it is important that 80% or more of the surface be covered with an oxide layer of aluminum, when the die is heated to 1000 to 1100°C in the air.
  • the Ni-based alloy for hot die of the present invention can be used in hot die forging and isothermal forging in the air.
  • the temperature of 1000°C is a temperature at which the hot die forging is assumed.
  • the temperature of 1100°C is a temperature at which the isothermal forging is assumed.
  • the surface refers to a die surface that is most important in the die.
  • the die surface and the side surface of the die are preferably covered with an oxide layer of aluminum, and the whole surface of the die is more preferably covered therewith.
  • non-uniform formation of aluminum oxide is preferably prevented in advance by applying a treatment that enables to mitigate segregation of components, for example, a homogenization heat treatment at 1100 to 1300°C for about 10 to 100 hours that is performed after an antioxidant is applied to the whole surface of a casting raw material in the air or under an inert atmosphere.
  • a treatment that enables to mitigate segregation of components for example, a homogenization heat treatment at 1100 to 1300°C for about 10 to 100 hours that is performed after an antioxidant is applied to the whole surface of a casting raw material in the air or under an inert atmosphere.
  • the area fraction of aluminum oxide formed on the surface of the Ni-based alloy for hot die surface is 80% or more in the present invention.
  • the area fraction is preferably 90% or more, and most preferably 100%.
  • a range of at least 25 mm 2 may be observed with an optical microscope.
  • the pre-heating a die that is machined and thereafter degreased and cleaned at a temperature of 1000°C or more in the air and covering 80% or more of the surface with an oxide layer of aluminum By pre-heating a die that is machined and thereafter degreased and cleaned at a temperature of 1000°C or more in the air and covering 80% or more of the surface with an oxide layer of aluminum, the inhibition of the formation of the oxide layer of aluminum by dirt of fats and oils and the like that are attached to the surface during the assembling operation of the die and the like, or seizing of the die and the member can be suppressed.
  • the oxide layer of aluminum formed on the die surface has an effect of increasing the wettability of a glass lubricant that is used as the lubricant.
  • the upper limit of the pre-heating temperature may be 1150°C. Although the pre-heating time depends on the size of the hot forging die, about 10 minutes to 3 hours are sufficient.
  • a hot forging die using the Ni-based alloy for hot die that has the alloy composition described above and is covered with an aluminum oxide layer within a range defined by the present invention can be constituted.
  • the hot forging die of the present invention can be obtained by the sintering of alloy powder or casting. Casting having inexpensive manufacturing costs is preferred to sintering of alloy powder. Furthermore, in order to suppress the generation of cracks in the raw material due to the stress during solidification, a sand mold or a ceramic mold is preferably used as the casting mold.
  • At least one of the die surface or the side surface of the hot forging die of the present invention can be a surface having a covering layer of an antioxidant. This more reliably prevents the oxidation of the die surface caused by the contact of oxygen in the air and the base material of the die at a high temperature and scattering of the scale associated therewith, allowing the deterioration in the working environment and the shape deterioration to be prevented.
  • the antioxidant described above is preferably an inorganic material formed by any one or more of nitride, oxide, carbide. This is for forming dense oxygen blocking films by the coating layer formed by nitride, oxide, or carbide and for preventing the oxidation of a die base material.
  • the coating layer may be a single layer of nitride, oxide, and carbide, or may be a lamination structure formed by combining any two or more of nitride, oxide, and carbide. Furthermore, a coating layer may be a mixture of any two or more of nitride, oxide, and carbide.
  • ordinary methods such as applying and spraying can be applied to form a covering layer, but the formation of the coating layer is preferred from the economic viewpoint.
  • the formation of oxygen blocking films by the application allows to easily increase the film thickness, thereby more reliably preventing contact of oxygen in the air and the base material of the die.
  • the thickness of the application layer is preferably 100 to 200 ⁇ m.
  • the antioxidant before the application is preferably a slurry that can be easily applied, and furthermore, the application method is preferably a simple application method using a brush.
  • the hot forging die using the Ni-based alloy for hot die of the present invention described above has a high high-temperature compressive strength and a good oxidation resistance and is capable of preventing oxidation of the die surface caused by the contact of oxygen in the air and base material of the die at a high temperature and scattering of scales associated therewith, and thereby more reliably suppressing the deterioration in the working environment and the shape deterioration.
  • a material for forging is heated to a predetermined forging temperature as a first step. Since the forging temperature differs depending on materials, the temperature is appropriately adjusted.
  • the hot forging die using the Ni-based alloy for hot die has a property of being capable of being used in isothermal forging and hot die forging even at a high temperature in the air atmosphere, and thus, it is suitable for the hot forging of Ni-based heat-resistant super alloy, Ti alloy, or the like that are known as poor workability materials.
  • Representative forging temperature is within a range of 1000 to 1150°C.
  • the material for forging heated in the first step is subjected to hot forging by using the hot forging die (second step).
  • the second step can be performed by heating the hot forging die to 1000°C or more before hot forging.
  • the hot forging in the second step is preferably closed die forging.
  • the Ni-based alloy for hot die of the present invention can be used in hot forging at a high temperature of 1000°C or more in the air.
  • Ingots of the Ni-based alloy for hot die shown in Table 1 were produced by vacuum melting using a ceramic mold. The unit is mass%. Each of P, N, and O contained in the ingots described below is 0.003% or less. Each of Si, Mn, and Fe is 0.03% or less.
  • No. 1 to 20 are Ni-based alloys for hot die having the composition of "the present example” and No. 21 and 22 are Ni-based alloys for hot die having the composition of "the comparative example”. Table 1 (mass%) No.
  • Cubes having a side of 10 mm were cut out from each of the ingots and their surfaces were polished by the one equivalent to #1000 to produce oxidation resistance test specimens and then the oxidation resistance was evaluated.
  • oxidation resistance test two tests, that is, a test simulating prolonged use and a test simulating repeated use of the die for hot forging in the air were performed.
  • a heating test was performed as an oxidation resistance test simulating prolonged use as follows.
  • the test specimens were loaded into a furnace heated to 1100°C in a state being placed in a ceramic crucible made of SiO 2 and Al 2 O 3 , held at 1100°C for a predetermined time, then taken out the crucible in which test specimens are placed from the furnace.
  • the crucible was covered with a lid made of identical materials to prevent spallation of scales outside the crucible and then air-cooled.
  • the heating test was performed for each of the test specimens under the conditions of holding times of 3 hours, 8 hours, or 20 hours.
  • the first heating (3 hours) corresponds to pre-heating and it is assumed that the second heating (8 hours and 20 hours) is the accumulation of the holding time at a high temperature when hot forging is repeatedly performed.
  • the surface area and the mass of the crucible in which test specimens were placed were measured before the heating test, and the mass of the crucible in which test specimens were placed was measured after the crucible was cooled to room temperature after the heating test.
  • the mass change per unit surface area of the test specimens after each test was calculated by subtracting the mass measured before the test from the mass measured after each test, and then dividing the value by the surface area measured before the test. The higher the value of mass change is, the higher the amount of scales formed per unit area is.
  • the mass change per unit surface area of the test specimens calculated in the heating test of each holding time is shown in Table 2.
  • the unit of the mass change is mg/cm 2 .
  • the relationship between the holding time at 1100°C in the air and the mass change in No. 1 to 3, 7, 13, 17, and 20 of the present examples and No. 21 and 22 of the comparative examples is shown in Fig. 1 .
  • Optical micrographs of No. 2 and 3 of the present examples and No. 21 of the comparative example that were held at 1100°C for 8 hours in the air are shown in Fig. 2 .
  • the quantitative analysis results of the oxide formed on the surface measured by an energy dispersive X-ray analyzer are shown in Fig. 2 in combination with the area fraction of aluminum oxide analyzed by distinguishing between a black oxide layer of aluminum and green oxides made of nickel and the like from optical micrograph taken at a magnification of ⁇ 100. The area measured is 100 mm 2 .
  • FE-EPMA backscattered electron images obtained by embedding specimens after the heating test at 1100°C in the air in a resin, then they were mirror polished, and then observing near the surface from the cross-sectional direction, and element maps of Al, Mo, W, and O of No. 1 and 7 of the present examples and No. 21 of the comparative example are shown in Fig. 3 .
  • the density in element map images corresponds to the concentration of the element to be measured and a whiter color indicates a higher concentration.
  • No. 1 of the present example and No. 21 of the comparative example are specimens after holding for 8 hours
  • No. 7 of the present example is a specimen after holding for 3 hours.
  • Mass change after 3 hours Mass change after 8 hours Mass change after 20 hours 1 ⁇ 0.1 0.2 - 2 0.3 0.7 - 3 ⁇ 0.1 ⁇ 0.1 - 4 0.2 0.2 - 5 0.3 0.2 - 6 0.3 0.2 - 7 0.3 0.2 - 8 0.2 0.2 - 9 0.2 0.2 - 10 0.5 0.5 - 11 0.4 - 0.4 12 0.6 - 0.7 13 0.5 - 0.4 14 0.7 - 0.9 15 0.2 - 0.3 16 0.6 - 1.0 17 0.3 - 0.5 18 0.5 - 1.2 19 0.3 - 0.3 20 0.8 - 1.6 21 3.5 4.3 - 22 3.1 5.0 -
  • a heating test was performed as an oxidation resistance test simulating repeated use, as follows.
  • the test specimens were loaded into a furnace heated to 1100°C in a state disposed on a ceramic container made of SiO 2 and Al 2 O 3 , held at 1100°C for 3 hours, then taken out from the furnace, and air-cooled.
  • the heating test was repeated 5 times by cooling and then reloading.
  • the surface area and the mass of the test specimens were measured before the first heating test, and each mass of the test specimens that were cooled to room temperature after the first to fifth heating tests and then scales on their surfaces that were removed by a blower were measured.
  • the mass change per unit surface area of the test specimens after each test was calculated by subtracting the mass measured before the first test from the mass measured after each test, and then dividing the value by the surface area measured before the first test. The higher the absolute value of the value of mass change is, the higher the scattering amount of scales per unit area is.
  • the mass change per unit surface area of the test specimens calculated after each heating test is shown in Table 3.
  • the unit of the mass change is mg/cm 2 .
  • the relationship between the number of heating tests and the mass change is shown in Fig. 4 .
  • the test temperature of 900°C and 1000°C is mainly used to verify application to "hot die forging” and the test temperature of 1100°C is mainly used to verify application to "isothermal forging".
  • the compressive strength is 300 MPa or more at the test temperature of 1100°C at which the isothermal forging is assumed, it can be said that the die has sufficient strength.
  • the compressive strength is preferably 350 MPa or more, and further preferably 380 MPa or more.
  • the compressive strength is 500 MPa or more at the test temperature of 900°C and 1000°C at which the hot die forging is assumed, it can be said that the die has sufficient strength.
  • the compressive strength is preferably 550 MPa or more, and further preferably 600 MPa or more.
  • the 0.2% compressive strength of the test specimens of No. 1 to 20 of the present examples and No. 21 and 22 of the comparative examples at each test temperature is shown in Table 4.
  • the relationship between each test temperature and 0.2% compressive strength of No. 1 to 3 of the present examples and No. 21 of the comparative example is shown in Fig. 5 .
  • the compressive strength of No. 1 to 3 at 1000°C and at a strain rate of 10 -3 /sec is 500 MPa or more.
  • No. 1 and 2 have achieved 600 MPa or more of compressive strength.
  • the compressive strength of No. 1 and 2, 4 to 20 having a preferred amount of Cr at 1100°C and at a strain rate of 10 -3 /sec is 300 MPa or more.
  • these are ones that have achieved 350 MPa or more of compressive strength, or ones that have achieved 400 MPa or more of compressive strength.
  • Fig. 5 it is revealed from Fig. 5 that the compressive strength of No.
  • Compression test value 900°C 1000°C 1100°C 1 - 684 376 2 740 614 378 3 686 503 256 4 - - 406 5 - - 332 6 - - 396 7 - - 400 8 - - 390 9 - - 406 10 - - 332 11 - - 436 12 - - 375 13 - - 374 14 - - 418 15 - - 404 16 - - 423 17 - - 449 18 - - 456 19 - - 424 20 - - 374 21 - 504 390 22 752 648 303 * The symbol "-" means not performed.
  • FIG. 6 A photograph showing the appearance of the surface of the hot forging die that was applied with an antioxidant and thereafter heated at 1000°C or more is shown in Fig. 6 . It is found from Fig. 6 that there is no exfoliation of the antioxidant applied to the surface of the hot forging die. Scattering of scales was also not seen. From this, it is found that the antioxidant prevents oxidation and scattering of scales of a die.
  • Table 5 (mass%) Mo W Al Cr Balance 9.9 10.7 6.2 1.5 Ni and inevitable impurities* * inevitable impurities (P, S: ⁇ 0.003%, C, Si, Mn, Co, Ti, Nb, Fe: ⁇ 0.03%)
  • Table 6 (mass%) SiO 2 B 2 O 3 Al 2 O 3 CaO Balance 53.0 5.6 12.7 18.0 Trace amount of oxide added* * Trace amount of oxide added (Na 2 O: 0.6%, K 2 O: 0.1%, Fe 2 O 3 : 0.2%, MgO: 0.5%, TiO 2 : 0.6%, SrO: 0.2%)
  • the Ni-based alloy for hot die of the present invention has sufficient oxidation resistance and a high compressive strength at a high temperature at the same time when used in hot forging in the air. It is found from this that the hot forging die using the Ni-based alloy for hot die of the present invention is useful in the forging (for example, hot die forging or isothermal forging) of products made of heat-resistant alloys. Since generation of scales was able to be particularly significantly suppressed, the deterioration in the working environment and the shape deterioration can be suppressed.
  • the hot forging die made of the Ni-based alloy for hot die of the present invention is suitable for hot die forging and isothermal forging in the air.

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Claims (15)

  1. Warmschmiedegesenk, umfassend eine Ni-basierte Legierung für Warmgesenke, bestehend aus, in Masse-%,
    W: 7,0 bis 15,0 %,
    Mo: 2,5 bis 11,0 %,
    Al: 5,0 bis 7,5 %,
    Cr: 0,5 bis 7,5 %,
    optional, einem oder zwei oder mehr Elementen, die ausgewählt sind aus Zr: 0,5 % oder weniger, Hf: 0,5 % oder weniger, Seltenerdelemente: 0,2 % oder weniger, Y: 0,2 % oder weniger und Mg: 0,03 % oder weniger,
    optional, Ta: 7,0 % oder weniger,
    optional, einem oder zwei Elementen, die ausgewählt sind aus Ti und Nb in einer Gesamtmenge von 3,5 % oder weniger, wobei der Gesamtgehalt an Ta, Ti und Nb 1,0 bis 7,0 % beträgt,
    optional, Co: 15,0 % oder weniger,
    optional, einem oder zwei Elementen, die ausgewählt sind aus C: 0,25 % oder weniger und B: 0,05 % oder weniger und
    dem Rest aus Ni mit unvermeidlichen Verunreinigungen,
    wobei mindestens 80 % eines Oberflächenbereichs der Ni-basierten Legierung für Warmgesenke mit einer Aluminiumoxidschicht bedeckt sind.
  2. Warmschmiedegesenk nach Anspruch 1, wobei ein oder zwei oder mehr Elemente, die ausgewählt sind aus Zr: 0,5 % oder weniger, Hf: 0,5 % oder weniger, Seltenerdelemente: 0,2 % oder weniger, Y: 0,2 % oder weniger und Mg: 0,03 % oder weniger, vorhanden sind.
  3. Warmschmiedegesenk nach Anspruch 1 oder 2, wobei Ta mit 7,0 % oder weniger vorhanden ist.
  4. Warmschmiedegesenk nach Anspruch 2 oder 3, wobei ein oder zwei Elemente, die aus Ti und Nb ausgewählt sind, in einer Gesamtmenge von 3,5 % oder weniger vorhanden sind und ein Gesamtgehalt an Ta, Ti und Nb 1,0 bis 7,0 % beträgt.
  5. Warmschmiedegesenk nach einem der Ansprüche 1 bis 4, wobei Co mit 15,0 % oder weniger vorhanden ist.
  6. Warmschmiedegesenk nach einem der Ansprüche 1 bis 5, wobei ein oder zwei Elemente, die ausgewählt sind aus C: 0,25 % oder weniger und B: 0,05 % oder weniger, vorhanden sind.
  7. Warmschmiedegesenk nach einem der Ansprüche 1 bis 6, wobei das Warmschmiedegesenk eine Deckschicht aus einem Antioxidans auf mindestens einer von einer Gesenkoberfläche oder einer Seitenoberfläche des Warmschmiedegesenks aufweist.
  8. Ni-basierte Legierung für Warmgesenke, bestehend aus, in Masse-%,
    W: 7,0 bis 15,0 %,
    Mo: 2,5 bis 11,0 %,
    Al: 5,0 bis 7,5 %,
    Cr: 0,5 bis 7,5 %,
    Ta: 0 bis 7,0 %,
    Co: 0 bis 15,0 %,
    optional, einem oder zwei oder mehr Elementen, die ausgewählt sind aus Zr: 0,5 % oder weniger, Hf: 0,5 % oder weniger, Seltenerdelemente: 0,2 % oder weniger, Y: 0,2 % oder weniger und Mg: 0,03 % oder weniger,
    optional einem oder zwei Elementen, die ausgewählt sind aus Ti und Nb, in einer Gesamtmenge von 3,5 % oder weniger, wobei ein Gesamtgehalt an Ta, Ti und Nb 1,0 bis 7,0 % beträgt, und
    dem Rest aus Ni mit unvermeidlichen Verunreinigungen.
  9. Ni-basierte Legierung für Warmgesenke, wobei die Ni-basierte Legierung für Warmgesenke nach Anspruch 8, wobei ein oder zwei oder mehr Elemente, die ausgewählt sind aus Zr: 0,5 % oder weniger, Hf: 0,5 % oder weniger, Seltenerdelemente: 0,2 % oder weniger, Y: 0,2 % oder weniger und Mg: 0,03 % oder weniger, vorhanden sind.
  10. Ni-basierte Legierung für Warmgesenke, wobei die Ni-basierte Legierung für Warmgesenke nach Anspruch 8 oder 9, wobei ein oder zwei Elemente, die ausgewählt sind aus Ti und Nb, in einer Gesamtmenge von 3,5 % oder weniger vorhanden sind, und ein Gesamtgehalt an Ta, Ti und Nb 1,0 bis 7,0 % beträgt.
  11. Ni-basierte Legierung für Warmgesenke nach einem der Ansprüche 8 bis 10, wobei die Druckfestigkeit von 0,2 % bei einer Testtemperatur von 1000 °C und einer Dehnungsrate von 10-3/s 500 MPa oder mehr beträgt, gemessen mit einem Verfahren nach der Beschreibung.
  12. Ni-basierte Legierung für Warmgesenke nach einem der Ansprüche 8 bis 10, wobei die Druckfestigkeit von 0,2 % bei einer Testtemperatur von 1100 °C und einer Dehnungsrate von 10-3/s 300 MPa oder mehr beträgt, gemessen mit einem Verfahren nach der Beschreibung.
  13. Verfahren zum Herstellen eines geschmiedeten Produkts, umfassend:
    einen ersten Schritt des Erwärmens eines Materials zum Schmieden, und
    einen zweiten Schritt des Warmschmiedens des im ersten Schritt erwärmten Materials zum Schmieden unter Verwendung des Warmschmiedegesenks nach einem der Ansprüche 1 bis 7.
  14. Verfahren zum Herstellen eines geschmiedeten Produkts nach Anspruch 13, wobei der zweite Schritt durch Erwärmen des Warmschmiedegesenks auf 1000 °C oder mehr durchgeführt wird.
  15. Verfahren zum Herstellen eines geschmiedeten Produkts nach Anspruch 14, wobei eine Ni-basierte Legierung für Warmgesenke an der Luft auf 1000 °C oder mehr vorgewärmt wird, um eine Aluminiumoxidschicht auf 80 % oder mehr eines Oberflächenbereichs der Ni-basierten Legierung für Warmgesenke zu bilden, gemessen mit einem Verfahren nach der Beschreibung, vor dem Schritt des Erwärmen des Warmschmiedegesenks auf 1000 °C oder mehr.
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Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3719152A4 (de) 2017-11-29 2021-03-31 Hitachi Metals, Ltd. Ni-basierte legierung für warmumformungsmatrize und warmschmiedegesenk mit verwendung davon
WO2020059846A1 (ja) * 2018-09-21 2020-03-26 日立金属株式会社 熱間金型用Ｎｉ基合金及びそれを用いた熱間鍛造用金型
US20230193426A1 (en) * 2020-05-26 2023-06-22 Proterial, Ltd. Ni-based alloy for hot die, and hot forging die using same
CN112410616B (zh) * 2020-11-03 2022-07-12 中国航发北京航空材料研究院 一种低成本和低宏观偏析倾向的大型等温锻模用高温合金

Family Cites Families (30)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2311998C3 (de) * 1973-03-10 1978-04-06 Thyssen Industrie Ag, 4300 Essen Verwendung einer Nickellegierung für Bauteile mit hoher Zeitstandfestigkeit
US3973952A (en) * 1973-06-11 1976-08-10 The International Nickel Company, Inc. Heat resistant alloy casting
DE3242608A1 (de) * 1981-11-27 1983-06-01 United Technologies Corp., 06101 Hartford, Conn. Superlegierung auf nickelbasis
US4481047A (en) * 1982-09-22 1984-11-06 United Technologies Corporation High modulus shafts
GB2152082A (en) * 1983-12-27 1985-07-31 United Technologies Corp Enhancement of superalloy resistance to environmental degradation
JPS60221542A (ja) 1984-04-17 1985-11-06 Hitachi Metals Ltd 大気中で使用可能な高温鍛造金型用ニツケル基鋳造合金
US4740354A (en) 1985-04-17 1988-04-26 Hitachi, Metals Ltd. Nickel-base alloys for high-temperature forging dies usable in atmosphere
JPS6250429A (ja) * 1985-08-30 1987-03-05 Hitachi Metals Ltd 高温鍛造金型用ニツケル基鋳造合金
US4802934A (en) * 1985-11-18 1989-02-07 Hitachi Metals, Ltd. Single-crystal Ni-based super-heat-resistant alloy
JP2552351B2 (ja) * 1988-05-17 1996-11-13 日立金属株式会社 単結晶Ｎｉ基超耐熱合金
JPH0441641A (ja) * 1990-06-07 1992-02-12 Kobe Steel Ltd 金型用ニッケル基超耐熱合金
JPH09324232A (ja) * 1996-06-04 1997-12-16 Mitsubishi Materials Corp 耐摩耗性および耐食性のすぐれた成形加工用Ｎｉ基合金製金型
US6007645A (en) * 1996-12-11 1999-12-28 United Technologies Corporation Advanced high strength, highly oxidation resistant single crystal superalloy compositions having low chromium content
US20030041930A1 (en) * 2001-08-30 2003-03-06 Deluca Daniel P. Modified advanced high strength single crystal superalloy composition
JP4521610B2 (ja) * 2002-03-27 2010-08-11 独立行政法人物質・材料研究機構 Ｎｉ基一方向凝固超合金およびＮｉ基単結晶超合金
US20040042927A1 (en) * 2002-08-27 2004-03-04 O'hara Kevin Swayne Reduced-tantalum superalloy composition of matter and article made therefrom, and method for selecting a reduced-tantalum superalloy
EP1815035A2 (de) * 2004-11-18 2007-08-08 Alstom Technology Ltd Nickel-basis-superlegierung
CN100396806C (zh) * 2005-07-15 2008-06-25 中国航空工业第一集团公司北京航空材料研究院 一种高温模具用镍基铸造高温合金
US20110076181A1 (en) * 2009-09-30 2011-03-31 General Electric Company Nickel-Based Superalloys and Articles
EP2631324A4 (de) * 2010-10-19 2014-04-16 Nat Inst For Materials Science Superlegierungselement auf nickelbasis mit einer darin geformten hitzebeständigen haftbeschichtung
WO2014126086A1 (ja) * 2013-02-13 2014-08-21 日立金属株式会社 金属粉末、熱間加工用工具および熱間加工用工具の製造方法
US9738953B2 (en) * 2013-07-12 2017-08-22 Daido Steel Co., Ltd. Hot-forgeable Ni-based superalloy excellent in high temperature strength
JP2016069702A (ja) 2014-09-30 2016-05-09 日立金属株式会社 ニッケル基鋳造合金の製造方法
JP6476704B2 (ja) * 2014-09-30 2019-03-06 日立金属株式会社 ニッケル基鋳造合金及び熱間鍛造金型
WO2017057453A1 (ja) * 2015-09-29 2017-04-06 日立金属株式会社 熱間鍛造用金型及びそれを用いた鍛造製品の製造方法並びに熱間鍛造用金型の製造方法
JP6566255B2 (ja) * 2015-09-29 2019-08-28 日立金属株式会社 熱間鍛造用金型
WO2017204286A1 (ja) * 2016-05-26 2017-11-30 日立金属株式会社 熱間金型用Ｎｉ基合金及びそれを用いた熱間鍛造用金型、鍛造製品の製造方法
US20200049209A1 (en) * 2016-10-10 2020-02-13 Mohamed Ahmed ELGAMIL Rigid and/or flexible mechanisms for transmitting rectilinear and/or rotary movement in a single direction
EP3560622B1 (de) * 2016-12-21 2021-11-10 Hitachi Metals, Ltd. Verfahren zur herstellung von warmgeschmiedetem material
CN107217227B (zh) * 2017-05-17 2019-06-07 昆明理工大学 一种提高镍基合金抗氧化性能的方法

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