巴西专利BR112013030609B1 THERMOMECHANICAL PROCESS OF NICKEL AND PRODUCT BASED ALLOY

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abstract "thermo-mechanical processing of nickel-based alloys" a thermo-mechanical treatment process is disclosed. A nickel-based alloy part is heated in a first heating step to a temperature higher than the nickel-based carbide solvus temperature m23c6. The nickel-based alloy part is crafted in a first working step for an area reduction of 20% to 70%. The nickel based alloy part is at a temperature higher than the M23c6 carbide solvus temperature when the first working step begins. The nickel-based alloy part is heated in a second working step to a temperature greater than 1700 ° f (926 ° c) and lower than the nickel-based carbide solvus temperature m23c6. The nickel-based alloy part is not allowed to cool to room temperature between the completion of the first working step and the beginning of the second heating step. The nickel-based alloy part is crafted for a second reduction in area from 20% to 70%. The nickel based alloy part is at a temperature greater than 1700 ° F (926 ° C) and lower than the solvus temperature of the nickel based carbide m23c6 when the second working step begins.
公开号:BR112013030609B1
申请号:R112013030609-2
申请日:2012-05-07
公开日:2019-04-16
发明作者:Robin M. Forbes Jones；Christopher A. Rock
申请人:Ati Properties Llc；
IPC主号:

专利说明:

[001] This disclosure refers to the thermo-mechanical processing of nickel-based alloys.
BACKGROUND [002] Nickel-based alloys are excellent engineering alloys in many applications because the alloys have a number of advantageous material properties. For example, nickel-based alloys comprising additions of chromium and iron have excellent resistance to corrosion in many aqueous media and high temperature atmospheres. Nickel-based alloys also maintain metallurgical stability and high strength over a wide range of elevated temperatures, and do not form embrittlement phases during prolonged exposure to elevated temperatures. The combination of good creep and break resistance, metallurgical stability and corrosion resistance at high temperatures and for long service periods allows nickel-based alloys to work in applications involving harsh environments and under severe operating conditions. For example, nickel-based alloys can find utility in engineering applications, including: mineral acid production and equipment processing; coal gasification units; petrochemical processing equipment; incinerators; steam generating tubes, deflectors, tube sheets and other equipment; and structural components in nuclear reactor power generation systems.
SUMMARY [003] In a non-limiting modality, a thermo-mechanical treatment process for nickel-based alloys comprises at least two heating stages and at least two working stages. A piece of nickel-based alloy is heated in a first heating step to a temperature higher than the solvent temperature of the M23C6 carbide of the nickel-based alloy. The heated nickel-based alloy part is worked in a first working step with an area reduction of 20% to 70% to provide a worked nickel-based alloy part. The nickel-based alloy part is at a temperature higher than the solvent temperature of the M23C6 carbide when the first work step begins. The worked nickel-based alloy part is heated in a second heating step to a temperature greater than 926 ° C (1700 ° F) and less than the solvent temperature of the M23C6 carbide of the nickel-based alloy. The worked nickel-based alloy part is kept at an elevated temperature and is not allowed to cool to room temperature between the completion of the first working stage and the beginning of the second heating stage. The heated nickel-based alloy part is worked in a second
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2/20 work to reduce the area from 20% to 70%. The nickel-based alloy part is at a temperature greater than 926 ° C (1700 ° F) and less than the solvus temperature of the M23C6 carbide of the nickel-based alloy when the second work step begins.
[004] In another non-limiting modality, a thermo-mechanical treatment process for nickel-based alloys comprises at least two heating steps and at least two forging steps. A nickel-based alloy part is heated in a first heating step to a temperature in the range 1093 ° C to 1163 ° C (2000 ° F to 2125 ° F). The heated nickel-based alloy part is rotationally forged in a first forging step to reduce the area from 30% to 70% to provide a forged nickel-based alloy part. The heated nickel-based alloy part is at a temperature in the range of 1093 ° C to 1163 ° C (2000 ° F to 2125 ° F) when the first forging step begins. The forged nickel-based alloy part is heated in a second heating step to a temperature in the range of 954 ° C to 1052 ° C (1750 ° F to 1925 ° F). The forged nickel-based alloy part is kept at an elevated temperature and is not allowed to cool to room temperature between the completion of the first forging step and the beginning of the second heating step. The heated nickel-based alloy part is rotationally forged in a second forging step to reduce the area from 20% to 70%. The heated nickel-based alloy ingot is at a temperature in the range 954 ° C to 1052 ° C (1750 ° F to 1925 ° F) when the second stage of rotary forging begins.
[005] It is understood that the invention disclosed and described in this specification is not limited to the modalities summarized in this Summary.
BRIEF DESCRIPTION OF THE FIGURES [006] Various features and characteristics of the non-limiting and non-complete modalities disclosed and described in this specification can be better understood by reference to the accompanying figures, in which:
Figures 1 A and 1 B are schematic cross-sectional diagrams of a rotary forging operation;
Figure 2A is a schematic cross-sectional diagram and Figure 2B is a schematic diagram from the perspective of a long hot forged and heat treated product, having a region in the shape of an abnormal grain growth ring; and
Figures 3A to 3D are metallographic of the transverse macrostructure of the long product regions of the 690 alloy, showing various effects of thermo-mechanical processing, according to various non-limiting modalities described in this document.
[007] The reader will appreciate the details previously, as well as the others, when considering the following detailed description of various non-limiting and non-complete modalities,
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3/20 in accordance with this disclosure.
DESCRIPTION [008] Various modalities are described and illustrated in this specification to provide a general understanding of the structure, function, operation, manufacture and use of the disclosed processes and products. It is understood that the various modalities described and illustrated in this specification are non-limiting and not complete. Thus, the invention is not limited by the description of the various non-limiting and non-complete modalities disclosed in this specification. On the contrary, the invention is defined exclusively by the claims. The features and characteristics illustrated and / or described in connection with various modalities can be combined with the features and characteristics of other modalities. Such modifications and variations are intended to be included within the scope of this specification. As such, the claims may be amended to report any features or features expressly or inherently described, or otherwise expressly or inherently supported, by that specification. In addition, the Depositor reserves the right to change the claims to affirmatively deny the features or characteristics that may be present in the state of the art. The various modalities disclosed and described in this specification may comprise, consist or consist essentially of the features and characteristics, as described in a variable manner in this document.
[009] Any patent, publication or other disclosure material identified in this document is incorporated by reference into this specification in its entirety, unless otherwise stated, but only insofar as the incorporated material does not conflict with the definitions, statements or other disclosure material expressly presented in this specification. As such, and to the extent necessary, express disclosure, as set out in this specification, supersedes any conflicting material incorporated by reference in this document. Any material, or part of it, that is said to be incorporated by reference in this specification, but which conflicts with the definitions, statements or other disclosure material contained herein, is incorporated only to the extent that there is no conflict between that material and the existing disclosure material. The depositor reserves the right to change this specification to expressly report any topic, or part of it, incorporated for reference in this document.
[010] The reference throughout this specification to various non-limiting modalities, or similar, means that a specific feature or feature can be included in a modality. Thus, the use of the phrase in various non-limiting modalities, or similar, in this specification does not necessarily refer to a common modality and may refer to
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4/20 different modalities. In addition, specific features or characteristics can be combined appropriately in one or more modalities. Thus, the specific features or characteristics illustrated or described in connection with various modalities can be combined, in whole or in part, with the features or characteristics of one or more other modalities without limitation. Such modifications and variations are intended to be included in the scope of this specification.
[011] In this specification, unless otherwise indicated, all numerical parameters must be understood as being preceded and modified in all cases by the term about, in which the numerical parameters have the inherent variability characteristic of basic measurement techniques used to determine the numerical value of the parameter. At a minimum, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical parameter described in the present description must at least be interpreted taking into account the number of significant digits reported and, applying usual rounding techniques.
[012] Also, any numerical range reported in this specification is intended to include all sub-ranges of the same numerical precision included within the reported range. For example, a range from 1.0 to 10.0 is intended to include all subintervals between (and including) the minimum reported value of 1.0 and the maximum reported value of 10.0, that is, having a value minimum equal to or greater than 1.0 and a maximum value equal to or less than 10.0, such as 2.4 to 7.6. Any maximum numerical limitations reported in this specification are intended to include all the lowest numerical limitations included in it and any minimum numerical limitations reported in this specification are intended to include all highest numerical limitations included in it. Accordingly, the Depositor reserves the right to change this specification, including the claims, to expressly report any sub-intervals included within the ranges expressly reported in this document. All of these ranges are intended to be inherently described in this specification.
[013] Grammatical articles one, one, and the, as used in this specification, are intended to include at least one or one or more, unless otherwise noted. Thus, articles are used in this specification to refer to one or more of one (that is, at least one) of the article's grammatical objects. As an example, a component means one or more components, and thus, possibly, more than one component is contemplated and can be used or used in an implementation of the described modalities. In addition, the use of a singular noun includes the plural and the use of a plural noun includes the singular, unless the context of use requires otherwise.
[014] The various modalities disclosed and described in this specification are
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5/20 directed, in part, to the thermo-mechanical processing of nickel-based alloys. The thermo-mechanical processing disclosed and described in this specification can be used to produce nickel-based alloy products, such as, for example, bars, rods, slabs, rings, strips, plates and the like. Products manufactured by the processes described in this specification can be characterized by a defined grain size and a defined precipitated carbide distribution.
[015] The intergranular stress corrosion crack (IGSCC) is a corrosion mechanism in which cracks are formed along the grain boundaries of a metallic material under tensile stress and exposed to a corrosive environment. The tensile stress that promotes IGSCC can be in the form of stresses applied externally to a metallic component in service and / or in the form of internal residual stresses in the metallic material. IGSCC is often found in applications involving aggressively corrosive environments, such as, for example, structural components in chemical processing equipment and pressurized water reactors (PWR) for nuclear power generation. Nickel-based alloys, such as, for example, Alloy 600 (UNS N06600) and Alloy 690 (UNS N06690), can be used in such applications due to the general corrosion resistance of these alloys. However, nickel-based alloys can, however, demonstrate IGSCC under high temperature and high pressure service conditions, for example, in aqueous or steam environments.
[016] Certain thermo-mechanical treatment processes can be used to reduce the susceptibility of nickel-based alloys to IGSCC in aggressive corrosive environments. Combinations of hot work and hot treatments can be used to produce nickel-based alloy products having defined grain sizes and carbide distributions that increase IGSCC resistance. For example, nickel-based alloys, including relatively high levels of chromium and iron, such as alloy 600 and alloy 690, can be thermo-mechanically processed by certain known methods to produce products having defined grain sizes defined with an intergranular distribution of precipitated M23C6 carbides and without depletion of chromium in the grains. The intergranular precipitation of M23C6 carbides between the grains in nickel-based alloys significantly reduces the sensitization of the alloys in aggressive corrosive environments, which significantly increases the resistance to IGSCC.
[017] In various non-limiting modalities, the processes described in this document can be used to thermo-mechanically treat nickel-based alloys, such as, for example, Liga 600 and Liga 690. For example, in various non-limiting modalities , alloy 690 parts treated in accordance with the modalities of the thermo-mechanical processes described in this document may have a chemical composition comprising (in
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6/20 percentage by weight / total mass of the alloy): at least 58.0% nickel; 27.0% to 31.0% chromium; 7.0% to 1.0% iron; up to 0.5% manganese; up to 0.05% carbon; up to 0.5% copper; up to 0.5% silicon; up to 0.015% sulfur; and accidental impurities. In various non-limiting embodiments, the alloy 690 parts treated accordingly may have a chemical composition comprising any elementary subintervals included within the elementary ranges described above. For example, a part of the 690 alloy treated in accordance with the modalities of the thermo-mechanical processes described in this document may comprise (in percentage by the total weight / mass of the alloy): at least 59.0% nickel; 28.0% to 30.0% chromium; 8.0% to 10.0% iron; up to 0.25% manganese; 0.010% to 0.040% carbon; up to 0.25% copper; up to 0.25% silicon; up to 0.010% sulfur; and accidental impurities. In various non-limiting embodiments, all elemental alloy constituents described in this specification as being up to a specified maximum amount also include amounts greater than zero for the specified maximum amount.
[018] In several non-limiting embodiments, nickel-based alloy ingots can be produced by vacuum induction melting raw materials (VIM) to produce an alloy comprising a chemical composition, in accordance with a predetermined composition specification . For example, raw materials can be used to produce an alloy comprising a chemical composition, in accordance with the specifications for the 690 alloy described above. The molten alloy produced by VIM, for example, can be cast into an initial ingot. In several non-limiting embodiments, the initial ingot can be used as an input electrode for one or more vacuum arc reflow (VAR) and / or electroslag reflow (ESR) operations to produce a refined ingot. In various non-limiting modalities, other initial fusion and / or remelting operations known in the art, such as, for example, argon-oxygen decarbonation (AOD) and / or vacuum degassing, alone or in combination with VAR and / or ESR , can be used to produce nickel based alloy ingots.
[019] In several non-limiting modalities, a nickel-based alloy ingot can be homogenized, using standard and / or forged heat treatment practices to produce a nickel-based alloy part. For example, a nickel-based alloy ingot (in a molten, refined or homogenized condition) can be forged by pressure to produce a part to be used as an input for subsequent thermo-mechanical processing operations. In several other non-limiting modalities, a nickel-based alloy ingot (in a molten, refined or homogenized condition) can be converted by forging into a preform part having any shape and dimensions suitable for thermo-mechanical processing operations subsequent
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7/20 [020] In several non-limiting modalities, thermomechanical processing operations can comprise at least two heating stages and at least two working stages. A first heating step may comprise heating a nickel-based alloy piece to a carbide supersolvus temperature. A first work step may include understanding the work (e.g., forging or rolling) of the nickel-based alloy part, where the nickel-based alloy part is at a carbide supersolvus temperature when the work begins. A second heating step may comprise the nickel-based alloy part at a carbide subsolvus temperature. A second work step may comprise the work (for example, forging or rolling) of the nickel-based alloy part, wherein the nickel-based alloy part is at a temperature of carbide subsolvus when the work begins.
[021] As used in this document, including in the claims, the terms first, second, before, after, and the like, when used in connection with a step or operation, do not exclude the possibility of previous steps or operations, intervention and / or subsequent For example, in various non-limiting modalities, thermo-mechanical processing methods comprising first and second heating stages and first and second working stages may further comprise heating, working and / or other additional stages before, between and / or after first and second specified heating steps and the first and second working steps.
[022] As used herein, the term carbide supersolvus temperature refers to temperatures at least as high as the solvent temperature of an alloy's M23C6 carbide. As used herein, the term carbide subsolvus temperature refers to temperatures below the solvus temperature of the M23C6 carbide of an alloy. The solvus temperature of an alloy's M23C6 carbide is the lowest temperature at which essentially all the carbon present in the alloy is in solid solution and the alloy does not comprise any metallographically observable M23C6 carbide phases or precipitates. The solvus temperature of an alloy's M23C6 carbide depends on the chemical composition of the alloy, particularly the carbon content. For example, the solvus temperature of alloy 690 M23C6 carbide can vary from approximately 1046 ° C to 1157 ° C (1915 ° F to 2115 ° F) for carbon concentrations ranging from 0.02% to 0.05%, in weight, for a nominal composition of 29.0% chromium, 9.0% iron, 0.2% copper, 0.2% silicon, 0.2% manganese, 0.01% sulfur, 0, 25% aluminum, 0.25% titanium, 0.008% nitrogen, and 60.842% to 60.872% nickel, calculated using the JMatPr software, available from Sente Software, Surrey, UK. Carbide solvus temperatures can be determined
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8/20 empirically or approximated, using phase diagram calculation software and material property simulation, such as, for example, JMatPro software, or Pandat software, available from CompuTherm LLC, Madison, Wisconsin, USA.
[023] As used in this document, heating a part to a specified temperature or temperature range indicates that the part has been heated long enough to bring the temperature of the entire part, including the internal parts of the part material, to the specified temperature or for the specified temperature range. Likewise, a condition of a part being heated to a specified temperature or temperature range indicates that the part is heated long enough to bring the temperature of the entire part, including the internal parts of the material, to the specified temperature or to the specified temperature range. The amount of time required to heat a part to a temperature or temperature range will depend on the shape and dimensions of the part and the thermal conductivity of the part material, for example.
[024] As used in this document, heating a part for a specified period of time or time interval at a specified temperature or temperature range (that is, time-in-temperature) indicates the heating of the part by time or interval of specified time measured from the point when the surface temperature of the part (measured, for example, using a thermocouple, pyrometer or similar) reaches ± 14 ° C (± 25 ° F) of the specified temperature or temperature range. As used in this document, a specified time-at-temperature does not include the preheat time to bring the surface temperature of the part within ± 14 ° C (± 25 ° F) of the specified temperature or temperature range. As used here, the term oven time indicates the amount of time that a part is kept within a temperature-controlled environment, such as, for example, an oven, and does not include the time required to bring the temperature-controlled environment into the specified temperature or temperature range.
[025] As used here, forging, work, or other mechanical processing of driving over a part at a specified temperature or temperature range indicates that the temperature of the entire part, including the internal parts of the part material, is at the temperature or range specified temperature when forging, work or other mechanical processing begins. It is contemplated that the cooling of the surface and / or the adiabatic heating of a part during forging, work, or similar operations at a specified temperature or temperature range can change the temperature of the parts of a part from that specified during the
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9/20 operation.
[026] In several non-limiting modalities, a thermo-mechanical treatment process comprises a first heating step, comprising heating a piece of nickel-based alloy to a temperature greater than the solvus temperature of the M23C6 carbide of the alloy nickel base. The heated nickel-based alloy part can be worked to reduce the area from 20% to 70% in a first working step to provide a worked nickel-based alloy part. The heated nickel-based alloy part can be at a temperature higher than the solvus temperature of the M23C6 carbide at the beginning of the first working step. The worked nickel-based alloy part can be heated in a second heating step to a temperature greater than 926 ° C (1700 ° F) and less than the solvus temperature of the nickel-based alloy M23C6 carbide. The worked nickel-based alloy part can be maintained at an elevated temperature and is not allowed to cool to room temperature between the completion of the first work step and the start of the second heating step. The nickel-based alloy part can be worked on for a second area reduction of 20% to 70% in a second work step. The nickel-based alloy part can be at a temperature greater than 926 ° C (1700 ° F) and less than the solvus temperature of the nickel-based alloy M23C6 carbide at the beginning of the second work step. The nickel-based alloy part can be cooled in air at room temperature after the second work step is completed.
[027] In several non-limiting modalities, the first heating step, in which a nickel-based alloy part is heated to a carbide supersolvus temperature, can comprise heating the nickel-based alloy part in an oven operating at 1093 ° C to 1163 ° C (2000 ° F to 2125 ° F) for at least a 6.0 hour time-at-temperature (360 minutes). A part of the nickel-based alloy can be heated to a carbide supersolvus temperature by heating in an oven operating at 1093 ° C to 1163 ° C (2000 ° F to 2125 ° F), or any sub-range included in this, such as , for example, 1093 ° C to 1149 ° C (2000 ° F to 2100 ° F), 1093 ° C to 1135 ° C (2000 ° F to 2075 ° F), 1093 ° C to 1121 ° C (2000 ° F to 2050 ° F), 1107 ° C to 1135 ° C (2025 ° F to 2075 ° F), 1121 ° C to 1163 ° C (2050 ° F to 2125 ° F), 1121 ° C to 1149 ° C (2050 ° F) at 2100 ° F), or the like.
[028] In several non-limiting modalities, the second heating step, in which a worked nickel-based alloy part is heated to a carbide subsolvus temperature, can comprise heating the nickel-based alloy part in a furnace operating at a temperature greater than 926 ° C (1700 ° F) and less than the solvus temperature of the nickel-based alloy M23C6 carbide for an oven time greater than 2.0 hours (120 minutes). A part of the nickel-based alloy can be heated to a temperature
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10/20 carbide subsolvus by heating in an oven operating at 926 ° C to 1066 ° C (1700 ° F to 1950 ° F), or any subintervals included therein, such as, for example, 954 ° C to 1052 ° C (1750 ° F to 1925 ° F), 954 ° C to 996 ° C (1750 ° F to 1825 ° F), 996 ° C to 1052 ° C (1825 ° F to 1925 ° F), 968 ° C to 1038 ° C (1775 ° F to 1900 ° F), 982 ° C to 1024 ° C (1800 ° F to 1875 ° F), 982 ° C to 1010 ° C (1800 ° F to 1850 ° F), or the like. In several embodiments, the second heating step may comprise heating a nickel-based piece in an oven operating at a temperature of carbide subsolvus for an oven time greater than 2.0 hours (120 minutes) to 10, 0 hours (600 minutes), or any subintervals included in this, such as, for example, 2.5 to 8.0 hours (150-480 minutes), 3.0 to 10.0 hours (180-600 minutes), 3 , 0 to 8.0 hours (180-480 minutes), 4.0 to 8.0 hours (240-480 minutes), 5.0 to 8.0 hours (300480 minutes), or the like.
[029] In several non-limiting modalities, a nickel-based alloy piece can be maintained at elevated temperature and not allowed to cool to room temperature between the completion of the first working stage and the beginning of the second heating stage. For example, a nickel-based alloy part can be maintained at temperatures no lower than a temperature that is 167 ° C (300 ° C) below the solvus temperature of the alloy's M23C6 carbide. In various non-limiting embodiments, a nickel-based alloy piece can be maintained at temperatures no less than a temperature that is 111 ° C (200 ° F), 83 ° C (150 ° F), or 56 ° C (100 ° F) below the solvus temperature of the alloy M23C6 carbide. In various non-limiting embodiments, a nickel-based alloy piece can be maintained at a temperature of at least 926 ° C (1700 ° F) between the completion of the first work step and the start of the second heating step. In various non-limiting embodiments, a nickel-based alloy piece can be maintained at a temperature of at least 954 ° C (1750 ° F), 982 ° C (1800 ° F), 1010 ° C (1850 ° F), 1038 ° C (1900 ° F), or 1066 ° C (1950 ° F) between the completion of the first work step and the start of the second heating step.
[030] In several non-limiting modalities, the first work step, the second work step and any subsequent work steps can together reduce the cross-sectional area of a part by 40% to 95%, in relation to the cross-sectional area of order before the first work step. The first work step, the second work step and any subsequent work steps can independently produce area reductions of 20% to 70%, or any sub-interval included in this, such as, for example, 30% to 70% , 40% to 60%, 45% to 55%, or the like. The reduction in the area produced by the first work step is calculated based on the initial cross-sectional area of the part before the first work step. The reduction in the area produced by the second stage of the work is calculated
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11/20 based on the cross-sectional area produced by the first stage of work. The reduction in area of any subsequent work step can be calculated based on the cross-sectional area produced by the previous work step.
[031] In various non-limiting modalities, the first work step, the second work step and any subsequent work steps can, independently, comprise one or more steps through the equipment used to carry out the specific work step. For example, a first work step can comprise one or more steps through a rotary forge to reduce the cross-sectional area of a part by 20% to 70%, and a second work step can comprise one or more steps through the rotary forge to reduce the cross-sectional area of the part by 20% to 70%, in relation to the cross-sectional area of the part produced by the first work step. The total reduction in the area produced by the first work step and the second work step can be 40% to 95%, in relation to the part area before the first work step. The reduction of the area produced by each individual step through the rotary forge can be, for example, from 5% to 25%, in relation to the intermediate transversal area produced by the previous step.
[032] In several non-limiting modalities, a heated nickel-based alloy part can be at a temperature higher than the solvency temperature of the M23C6 carbide at the beginning of the first working step, and a heated nickel-based alloy part it can be at a temperature greater than 926 ° C (1700 ° F) and less than the solvus temperature of the nickel-based alloy M23C6 carbide at the beginning of the second work step. In various non-limiting embodiments, a heated nickel-based alloy piece may be at a temperature higher than the solvus temperature of the M23C6 carbide during the first entire work step. In various non-limiting embodiments, a heated nickel-based alloy piece can be at a temperature greater than 926 ° C (1700 ° F) and less than the solvent temperature of the M23C6 carbide of the nickel-based alloy during the second stage entire work. For example, the prints, anvils and / or rolls used to perform a work operation can be heated to minimize or eliminate heat loss due to the conduction of the workpiece surfaces in contact with the prints, anvils and / or work rolls. In addition, the adiabatic heating of the deformation part material during the work steps can compensate, at least in part, for the heat loss of the part.
[033] In various non-limiting modalities, the first work step and the second work step can independently comprise one or more forging or rolling operations, such as, for example, flat rolling, ring rolling, profiling, forging by pressure, extrusion, rotary forging, and the like. In various modalities, the first stage of work and the second stage of work can each comprise
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12/20 one or more rotary forging steps.
[034] As used in this document, the term rotary forging refers to the work of elongated parts, such as, for example, tubes, bars and rods, using two or more anvils / patterns to compressively deform the part perpendicular to the long axis of the thus decreasing the cross-sectional area of the piece and increasing the length of the piece to produce long products. A rotary forging operation 100 is illustrated in Figures 1A and 1B, in which a cylindrical piece of the bar / rod type 102 is compressively deformed by anvils / stamps 104, thereby decreasing the cross-sectional area of the piece and increasing the length of the piece. Rotary forging produces long solid or tubular products with constant or variable cross sections along their length. Rotary forging, also known as rotary stamping or radial forging, should not be confused with orbital forging (ie, swing pattern), in which a part is pressed between a non-rotating anvil / flat pattern and a rotating pattern (swing) ) with a conical work face that makes orbital, spiral, planetary or straight movements.
[035] In various non-limiting embodiments, a thermo-mechanical treatment process may comprise a first step comprising heating a part of the 690 alloy to a temperature higher than the solvent temperature of the alloy's M23C6 carbide. For example, the first heating step may comprise heating a part of the 690 alloy to a temperature in the range of 1093 ° C to 1163 ° C (2000 ° F to 2125 ° F). In various non-limiting embodiments, the 690 alloy piece may have a chemical composition comprising, by weight, up to 0.05% carbon; 27.0% to 31.0% chromium; up to 0.5% copper; 7.0% to 11.0% iron; up to 0.5% manganese; up to 0.015% sulfur; up to 0.5% silicon; at least 58% nickel; and accidental impurities.
[036] The heated alloy 690 part can be rotated forging to an area reduction of 20% to 70% in a first forging step, comprising one or more rotary forging steps. The heated alloy 690 part can be at a temperature higher than the solvent temperature of the M23C6 carbide at the beginning of the first forging step, such as, for example, at a temperature in the range of 1093 ° C to 1163 ° C (2000 ° F to 2125 ° F) when the first forging step begins. The alloy 690 forged part can be heated in a second heating step to a temperature greater than 926 ° C (1700 ° F) and less than the solvus temperature of the nickel-based alloy M23C6 carbide. For example, the second heating step may comprise heating a piece of alloy 690 forged to a temperature in the range 954 ° C to 1052 ° C (1750 ° F to 1925 ° F). The forged 690 alloy part can be kept at a temperature of at least 926 °
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13/20
C (1700 ° F) between the completion of the first forging step and the beginning of the second heating step.
[037] The heated alloy 690 part can be rotationally forged for a second area reduction of 20% to 70% in a second forging step, comprising one or more rotary forging steps. The heated alloy 690 part can be at a temperature greater than 926 ° C (1700 ° F) and less than the solvent temperature of the M23C6 carbide at the beginning of the second forging step, such as, for example, at a temperature in the range 954 ° C to 1051 ° C (1750 ° F to 1925 ° F) when the second forging step begins. The 690 alloy part can be cooled in air at room temperature after the second forging stage is completed.
[038] In various non-limiting modalities, nickel-based alloy parts, such as alloy 690 parts, can still be heat treated after at least two heating steps and at least two working steps . For example, parts of the nickel-based alloy can be annealed at a temperature of at least 982 ° C (1800 ° F), but no higher than the solvus temperature of the M23C6 carbide of the nickel-based alloy for at least one 3.0 hour time-at-temperature. In various non-limiting embodiments, the nickel-based alloy parts can be annealed at a temperature of 982 ° C to 1093 ° C (1800 ° F to 2000 ° F), or any sub-range included in this, such as, for example, 1004 ° C to 1071 ° C (1840 ° F to 1960 ° F), 1010 ° C to 1066 ° C (1850 ° F to 1950 ° F), 1024 ° C to 1052 ° C (1875 ° F to 1925 ° F) , or the like. In various non-limiting modalities, the nickel-based alloy parts can be annealed for at least a 4.0 hour time-at-temperature. In various non-limiting modalities, the nickel-based alloy parts can be cooled in water after annealing heat treatment.
[039] In various non-limiting modalities, nickel-based alloy parts, such as, for example, alloy 690 parts, can be aged after at least two heating steps and at least two working steps. For example, nickel-based alloy parts can be aged at a temperature of 704 ° C to 760 ° C (1300 ° F to 1400 ° F) for at least a 3.0-hour time-at-temperature. In various non-limiting embodiments, nickel-based alloy parts can be aged at a temperature of 704 ° C to 760 ° C (1300 ° F to 1400 ° F), or any sub-range included in this, such as, for example, 718 ° C to 746 ° C (1325 ° F to 1375 ° F), 710 ° C to 738 ° C (1310 ° F to 1360 ° F) or similar. In various non-limiting modalities, the nickel-based alloy parts can be aged for at least a 4.0 hour time-at-temperature. In several non-limiting modalities, the nickel-based alloy parts can be cooled in the air after aging heat treatment.
Petition 870180166138, of 12/20/2018, p. 20/33
14/20 [040] In various non-limiting modalities, the nickel-based alloy parts can be annealed and aged. For example, after at least two heating steps and at least two working steps, the nickel-based alloy parts can be cooled in air at room temperature and then annealed to a temperature of at least 982 ° C ( 1800 ° F), but not higher than the solvency temperature of the nickel-based alloy M23C6 carbide for at least a 3.0 hour time-at-temperature. Nickel-based alloy parts can be cooled in water after thermal annealing treatment and then aged at a temperature of 704 ° C to 760 ° C (1300 ° F to 1400 ° F) for at least a while -in-temperature of 3.0 hours.
[041] The processes described in this document can be used, for example, to produce forged and / or laminated products. For example, in various non-limiting modalities, the two heating steps and the two working steps convert preform parts into products, including long products, such as, for example, round bar and rod, rectangular bar and rod, hexagonal rod and rod , long rectangular forged products and long rectangular laminated products. The processes disclosed in this document can be used, for example, to produce long products with constant or variable cross sections along their length. In the modalities that produce long products having variable cross sections along their length, the first work step and the second work step can together reduce the cross area of a part by 40% to 95% in one or more places when along the length of the long product. In addition, the processes disclosed herein can be used, for example, to produce rotary forged tubes.
[042] In various non-limiting modalities, the products produced by the processes described in this document can satisfy the requirements of ASTM B166-08: Standard Specification for Nickel-Chromium-Iron Alloys (UNS N06600, N06601, N06603, N06690, N06693, N06025, N06045, and N06696) and Nickel-Chromium-Cobalt-Molybdenum Alloy (UNS N06617) Rod, Bar, and Wire (2008), and ASME SB-166: Specification for Nickel-Chromium-lron Alloys (UNS N06600, N06601, N06603, N06690, N06693, N06025, N06045, and N06696) and NickelChromium-Cobalt-Molybdenum Alloy (UNS N06617) Rod, Bar, and Wire (2007), which are incorporated by reference in this specification.
[043] In several non-limiting modalities, the products produced by the processes described in this document can have a grain size of ASTM No. 3.0 to 9.0, determined according to ASTM E 112 - 10: Standard Test Methods for Determining Average Grain Size (2010), which is incorporated by reference in this specification. In several non-limiting modalities, the products produced by the processes described in this document
Petition 870180166138, of 12/20/2018, p. 21/33
15/20 can have a grain size in the range of ASTM N °. 3.0 to 9.0, or any sub-range included in this, such as, for example, ASTM No. 3.0 to 8.0, 3.5 to 7.5, 4.0 to 7.0, 4.5 to 6.5, 3.0 to 7.0, 3.0 to 6.0, or similar. In various non-limiting modalities, the products produced by the processes described in this document may comprise precipitates of intergranular M23C6 carbide uniformly distributed over the grain boundaries. In various non-limiting embodiments, the products produced by the processes described in this document may comprise minimal metallographically observable intragranular M23C6 carbide precipitates. In various non-limiting modalities, the products produced by the processes described in this document may lack metallographically observable intragranular M23C6 carbide precipitates.
[044] The microstructural carbide distribution can be determined metallographically, for example, using scanning electron microscopy (SEM) to evaluate chemically etched specimens (eg, bromine-methanol mordant solution) of the processed nickel-based alloy, according to with the various non-limiting modalities described in this document. For example, in various non-limiting modalities, products produced by the processes described in this document, when evaluated using SEM at 500x magnification, may comprise intergranular M23C6 carbide precipitates evenly distributed across all observable grain boundaries and comprise intragranular M23C6 carbide precipitates. minimal or none. In various non-limiting modalities, the products produced by the processes described in this document comprise equiaxial grains with a grain size of ASTM No. 3.0 to 9.0, a uniform grain size distribution, intergranular M23C6 carbide precipitates uniformly distributed within the metallographically observable grain boundaries, and minimal metallographically observable intragranular M23C6 carbide precipitates.
[045] The processes described in this document reduce or eliminate abnormal grain growth that creates a non-uniform grain size distribution on a macroscopic scale. To control the grain size within the specified limits, nickel-based alloy parts, such as alloy 690 parts, can be hot worked at temperatures above the recrystallization temperature and the carbide solvus temperature of the alloy, that is, working at supersolvus temperatures. However, subsequent heat treatments to produce a uniform distribution of intergranular M23C6 carbide precipitates often cause abnormal and uneven growth of the grain in the macrostructure sections of the parts. For example, hot rods and round bars worked with nickel-based alloys, such as alloy 690, tend to develop a ring-shaped region of abnormal grain growth across the section
Petition 870180166138, of 12/20/2018, p. 22/33
16/20 transversal of the product. Figures 2A and 2B schematically illustrate a long product 200, such as a nickel-based alloy rod or round bar, such as alloy 690. Long product 200 includes a ring-shaped region 205 of abnormal grain growth through the cross section of the product.
[046] While not wishing to be bound by theory, it is believed that hot work at supersolvus temperatures to control grain size produces an intrinsic internal force on parts that causes abnormal grain growth. The intrinsic internal force is believed to be caused by the differential thermal expansion of the part during hot work and cooling after hot work. The surface material of the parts cools much more quickly than the internal material, specifically the material towards the center of the part, when in contact with the work stamp / anvil and during subsequent cooling. This establishes a clear differential temperature between the cooling surface and the material close to the surface and the hottest internal material. The differential temperature results in differential thermal expansion from the high temperature in the center to the low temperature on the surface of the hot-worked product, which is believed to produce an intrinsic internal force in the material. During subsequent heat treatments to produce a uniform distribution of intergranular M23C6 carbide precipitates, the internal force is believed to drive the abnormal growth of the grain, which is located in the regions of the internal force caused by the differential thermal expansion during cooling. This is believed to result in the observed ring-shaped regions of abnormal and uneven growth of the grain in the macrostructure of the products.
[047] These deleterious regions of abnormal grain growth can be attenuated by working nickel-based alloy parts, such as alloy 690 parts, at temperatures below the alloy carbide solvus temperature, ie , at subsolvus temperatures. However, after working at subsolvus temperatures, subsequent heat treatments to produce a uniform distribution of intergranular M23C6 carbide precipitates often cause unacceptable grain growth throughout the entire part. Grain size is difficult to control and heat treatments often produce grain sizes larger than ASTM N °. 3.0 (i.e., ASTM ^Nos. Less than 3.0.). In addition, all carbides are not dissolved during work at subsolvus temperatures. As a result, the intergranular carbide distribution produced during subsequent heat treatments often includes large grain boundary carbide stringers that were present between the large grains in the preform parts and that do not dissolve before, during or after work at subsolvus temperatures.
[048] The processes described in this document reduce or eliminate growth
Petition 870180166138, of 12/20/2018, p. 23/33
Abnormal grain 17/20 that creates a non-uniform grain size distribution on a macroscopic scale, and produces products having equiaxial grains with a grain size of ASTM No. 3.0 to 9.0, a uniform grain size distribution, intergranular M23C6 carbide precipitates uniformly distributed over the grain boundaries and minimal intragranular M23C6 carbide precipitates. In the first of the two heating steps, a nickel-based alloy part is heated to a carbide supersolvus temperature, which dissolves all the M23C6 carbides present in the preform part. In the first of the two work steps, the nickel-based alloy part is worked at a carbide supersolvus temperature, for example, to reduce the area from 20% to 70%. Working at carbide supersolvus temperature prevents carbide precipitation and produces a uniform grain size distribution with grain sizes in the range of ASTM N °. 3.0 to 9.0.
[049] In the second of the two heating steps, the nickel-based alloy part is heated to a carbide subsolvus temperature. The part stabilizes at subsolvus temperatures and it is not allowed to cool to room temperature between the first working stage and the second heating stage. This minimizes any carbide precipitation, because the part material does not cool through the critical nose region of the time-temperature-transformation curve (TTT) of the material, where the carbide precipitation kinetics is the fastest. Carbide nucleation and precipitation is very slow at carbide subsolvent temperatures within approximately 167 ° C (300 ° F) of the carbide solvus temperature, for example. This prevents uncontrolled carbide precipitation. In the second of the two working steps, the nickel-based alloy part is worked at a temperature of carbide subsolvus, for example, to reduce the area from 20% to 70%. Working on the temperature of carbide subsolvus reduces the differential thermal expansion and the intrinsic internal strength in the material that is believed to cause abnormal grain growth during subsequent heat treatments.
[050] The following non-limiting and non-complete examples are intended to further describe several non-limiting and non-complete modalities, without restricting the scope of the modalities described in this specification.
EXAMPLES [051] Alloy 690 heaters were prepared, melting the raw materials using VIM. The chemical compositions of the alloy 690 heaters were in accordance with ASTM B166-08: Standard Specification for Nickel-Chromium-Iron Alloys (UNS N06600, N06601, N06603, N06690, N06693, N06025, N06045, and N06696) and NickelChromium-Cobalt -Molybdenum Alloy (UNS N06617) Rod, Bar, and Wire (2008) and ASME SBPetition 870180166138, of 12/20/2018, p. 24/33
18/20
166: Specification for Nickel-Chromium-Iron Alloys (UNS N06600, N06601, N06603, N06690, N06693, N06025, N06045, and N06696) and Nickel-Chromium-Cobalt-Molybdenum Alloy (UNS N06617) Rod, Bar, and Wire (2007 ), which are incorporated by reference in this document.
[052] VIM heaters were molded into initial ingots that were used as entry electrodes for ESR. The ESR operation produced refined cylindrical ingots with diameters of approximately 20 inches (508 millimeters). The 20-inch ESR ingots were homogenized, using standard practices and pressure forged to produce cylindrical parts with diameters of approximately 14 inches (356 millimeters).
[053] The parts were thermo-mechanically treated, according to the non-limiting modalities of the processes described in this document, comprising two heating stages and two working stages. In a first heating step, the parts were heated in an oven operating at 1093 ° C to 1121 ° C (2000 ° F to 2050 ° F) for a time-at-temperature of at least 6 hours. In a first work stage, the heated parts were forged rotating approximately 9.6 inches (243 millimeters) in diameter, which corresponds to an area reduction of approximately 53%. The first stage of work comprised four steps through the rotary forge, each step producing a reduction in area of approximately 17% to 18%. The entire part was at a temperature in the range of approximately 1093 ° C to 1121 ° C (2000 ° F to 2050 ° F) when the first work step began. During rotary forging steps, the surface temperatures for stamping and non-stamping of parts were maintained in the range of 926 ° C to 1121 ° C (1700 ° F to 2050 ° F) for all four (4) steps.
[054] After the completion of rotary forging, the surface temperatures of the parts were not allowed to cool to room temperature and the parts were immediately loaded into an oven operating at 996 ° C (1825 ° F). In a second heating step, the forged parts were heated in the oven for approximately 1.0 hour, 2.0 hours, 4.0 hours or 8.0 hours of oven time. In a second work step, the heated parts were forged rotationally a second time in approximately 7.2 inches (182 millimeters) in diameter, which corresponds to an area reduction of approximately 44%, in relation to the intermediate diameters of 9.6 inches (243 millimeters). The second stage of work comprised three steps through the rotary forge, each step producing a reduction in area from 17% to 18%. The entire part was at a temperature of approximately 996 ° C (1825 ° F) when the second work step began. During the second work step, the surface temperatures for the pattern and outside the pattern of the part were maintained in the range of 926 ° C to 1121 ° C (1700 ° F to 2050 ° F) for all three
Petition 870180166138, of 12/20/2018, p. 25/33
19/20 steps. The pieces were cooled in air at room temperature after the second stage of the work was completed. The total reduction in the area produced by the two work stages was approximately 74%.
[055] The parts heated twice and rotated forged twice were annealed at 1024 ° C (1875 ° F) for a time-at-temperature of four (4) hours followed by cooling by water to room temperature. The cooled parts were aged at 726 ° C (1340 ° F) for a time-at-temperature of four (4) hours and cooled in air at room temperature.
[056] The cross sections of the pieces were recorded, using standard practices and the macrostructure evaluated metallographically. Figure 3A is a metallographic of a cross section of a piece heated for an oven time of approximately 1 hour in an oven operating at 996 ° C (1825 ° F), between the first work stage and the second work stage. Figure 3B is a metallographic of a cross section of a piece heated for an oven time of approximately 2 hours in an oven operating at 996 ° C (1825 ° F), between the first work stage and the second work stage. Figure 3C is a metallographic of a cross section of a piece heated for an oven time of approximately 4 hours in an oven operating at 996 ° C (1825 ° F), between the first work stage and the second work stage. Figure 3D is a metallographic of a cross section of a piece heated for an oven time of approximately 8 hours in an oven operating at 996 ° C (1825 ° F), between the first work stage and the second work stage.
[057] As shown in Figures 3A and 3B, parts heated for an oven time of approximately 1 hour and 2 hours in an oven operating at 996 ° C (1825 ° F) developed an abnormal growth ring-shaped region of the grain. As shown in Figures 3C and 3D, parts heated for an oven time of approximately 4 hours and 8 hours in an oven operating at 996 ° C (1825 ° F) do not show any abnormal grain growth. The grain size of the pieces heated by an oven time of approximately 4 hours and 8 hours was in the range of ASTM N °. 3.0 to 8.0, determined in accordance with ASTM E 112-10. The pieces formed intergranular M23C6 carbide precipitates uniformly distributed over the grain boundaries and exhibited minimal intragranular M23C6 carbide precipitation.
[058] The processes described in this specification produce nickel-based alloy products having a microstructure and macrostructure that provides superior properties for critical engineering applications, such as, for example, structural components in chemical processing equipment and PWRs for generating nuclear energy. It is
Petition 870180166138, of 12/20/2018, p. 26/33
20/20 specification was written with reference to several non-limiting and not complete modalities. However, it will be recognized by persons skilled in the art that various substitutions, modifications or combinations of any of the disclosed modalities (or parts of them) can be made within the scope of this specification. Thus, it is contemplated and understood that this specification supports additional modalities not expressly presented in this document. These modalities can be obtained, for example, by combining, modifying, or reorganizing any of the stages, components, elements, resources, aspects, characteristics, limitations and similars disclosed, of the various non-limiting modalities described in this specification. Accordingly, the Depositor reserves the right to change claims during the process to add funds, as described in a variable manner in this specification.

权利要求:
Claims (16)
[1]
1. Process CHARACTERIZED by the fact that it comprises:
a first heating step, comprising heating a piece of nickel-based alloy to a temperature greater than the solvus temperature of the M23C6 carbide of the nickel-based alloy;
a first work step, comprising the work of the heated nickel-based alloy part for a reduction in the area of 20% to 70%, in which the nickel-based alloy part is at a temperature higher than the solvus temperature M23C6 carbide when the first work stage begins;
a second heating step, comprising heating the nickel-based alloy part worked at a temperature greater than 926 ° C (1700 ° F) and less than the solvent temperature of the M23C6 carbide of the nickel-based alloy, where the nickel-based alloy part worked is kept at an elevated temperature and is not allowed to cool to room temperature between the completion of the first work step and the start of the second heating step; and a second work step, comprising the work of the heated nickel-based alloy part for a second reduction in the area of 20% to 70%, in which the nickel-based alloy part is at a temperature greater than 926 ° C (1700 ° F) and less than the solvus temperature of the M23C6 carbide of the nickel-based alloy when the second work step begins.
[2]
2. Process, according to claim 1, CHARACTERIZED by the fact that the nickel-based alloy part comprises, by weight, up to 0.05% carbon; 27.0% to 31.0% chromium; up to 0.5% copper; 7.0% to 11.0% iron; up to 0.5% manganese; up to 0.015% sulfur; up to 0.5% silicon; at least 58% nickel; and accidental impurities.
[3]
3. Process, according to claim 1, CHARACTERIZED by the fact that the nickel-based alloy part comprises, by weight, up to 0.05% carbon; 28.0% to 30.0% chromium; up to 0.25% copper; 8.0% to 10.0% iron; up to 0.25% manganese; up to 0.010% sulfur; up to 0.25% silicon; at least 58% nickel; and accidental impurities.
[4]
4. Process according to claim 1, CHARACTERIZED by the fact that the first work step and the second work step independently comprise at least one operation selected from the group consisting of flat rolling, ring rolling, profiling, pressure forging , extrusion and rotary forging.
[5]
5. Process, according to claim 1, CHARACTERIZED by the fact that the first work stage and the second work stage comprise rotary forging.
Petition 870180166138, of 12/20/2018, p. 28/33
2/3
[6]
6. Process according to claim 1, CHARACTERIZED by the fact that the first heating step comprises heating the nickel-based alloy part in an oven operating at 1093 ° C to 1163 ° C (2000 ° F to 2125 ° F) for at least 3.0 hours at temperature.
[7]
7. Process according to claim 1, CHARACTERIZED by the fact that the second heating step comprises heating the nickel-based alloy part in an oven operating at 954 ° C to 1037 ° C (1750 ° F to 1900 ° F) for an oven time longer than 2.0 hours.
[8]
8. Process according to claim 1, CHARACTERIZED by the fact that the second heating step comprises heating the nickel-based alloy part in an oven operating at 954 ° C to 1037 ° C (1750 ° F to 1900 ° F) for an oven time of 3.0 hours to 10.0 hours.
[9]
9. Process according to claim 1, CHARACTERIZED by the fact that the second heating step comprises heating the nickel-based alloy part rotationally forged in an oven operating at 954 ° C to 1037 ° C (1750 ° F) at 1900 ° F) for an oven time of 4.0 hours to 8.0 hours.
[10]
10. Process, according to claim 1, CHARACTERIZED by the fact that it also comprises:
the vacuum induction melting of raw materials to form a nickel-based alloy ingot;
the remelting of the nickel-based alloy ingot to form a refined nickel-based alloy ingot, wherein the remelting comprises at least one remelting operation selected from the group consisting of vacuum refluxing and electroslag reflow; and the pressure forging of the refined nickel-based alloy ingot to form the nickel-based alloy part.
[11]
11. Process, according to claim 1, CHARACTERIZED by the fact that it also comprises, after the two heating stages and the two working stages:
heating the nickel-based alloy part to a temperature of at least 982 ° C (1800 ° F), but no higher than the solvent temperature of the nickel-based alloy M23C6 carbide for at least one time-in- temperature of 3.0 hours; and water cooling of the part.
[12]
12. Process, according to claim 1, CHARACTERIZED by the fact that it also comprises, after the two heating steps and the two forging steps:
aging the nickel-based alloy part at a temperature of 704 ° C to 760 ° C (1300 ° F to 1400 ° F) for at least a 3.0 hour time-at-temperature; and
Petition 870180166138, of 12/20/2018, p. 29/33
3/3 cooling the part in air in room temperature.
[13]
13. Product CHARACTERIZED by the fact that it is produced by the process as defined in claim 1.
[14]
14. Product, according to claim 13, CHARACTERIZED by the fact that the product comprises a long product selected from the group consisting of a rod, a round bar and a rectangular bar.
[15]
15. Product according to claim 13, CHARACTERIZED by the fact that the product comprises equiaxial grains with a grain size of ASTM No. 3.0 to 9.0, a uniform grain size distribution, M23C6 intergranular carbide precipitates uniformly distributed within the metallographically observable grain boundaries, and substantially no metallographically observable intragranular M23C6 carbide precipitate.
[16]
16. Product according to claim 13, CHARACTERIZED by the fact that the product comprises equiaxial grains with a grain size of ASTM No. 3.0 to 9.0, a uniform grain size distribution, metallographically observable intergranular M23C6 carbide precipitates, and substantially no observable metallographically intragranular M23C6 carbide precipitate.

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公开号 | 公开日

US20140116582A1|2014-05-01|

US20170349977A1|2017-12-07|

EP3045552A1|2016-07-20|

BR112013030609A2|2016-12-13|

AU2016200033B2|2018-02-22|

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US9616480B2|2017-04-11|

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MX352006B|2017-11-06|

CN103597105B|2017-08-04|

US10287655B2|2019-05-14|

PL3045552T3|2018-03-30|

UA112648C2|2016-10-10|

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CA3057342A1|2012-12-06|

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JP2014520206A|2014-08-21|

NZ618126A|2015-12-24|

PT3045552T|2018-01-22|

AU2016200033A1|2016-01-28|

CN107254606B|2019-07-23|

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CA2836842A1|2012-12-06|

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NO3045552T3|2018-03-24|

AU2018201475B2|2019-10-03|

EP2714953A2|2014-04-09|

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WO2012166295A3|2013-01-24|

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US20120308428A1|2012-12-06|

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