WO2012106414A1 - Procédé thermomécanique pour améliorer la qualité de réseaux de joints de grains dans des alliages métalliques - Google Patents

Procédé thermomécanique pour améliorer la qualité de réseaux de joints de grains dans des alliages métalliques Download PDF

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Publication number
WO2012106414A1
WO2012106414A1 PCT/US2012/023458 US2012023458W WO2012106414A1 WO 2012106414 A1 WO2012106414 A1 WO 2012106414A1 US 2012023458 W US2012023458 W US 2012023458W WO 2012106414 A1 WO2012106414 A1 WO 2012106414A1
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Prior art keywords
metal alloy
temperature
force
strain
period
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Kenichi Yaguchi
Christopher A. Schuh
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Mitsubishi Materials Corp
Massachusetts Institute of Technology
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Mitsubishi Materials Corp
Massachusetts Institute of Technology
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    • 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
    • C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper

Definitions

  • the present invention relates generally to methods for processing metal alloys to enhance the quality of grain boundary networks.
  • Grain boundaries are generally less energetically stable than the interior regions of crystal grains. The level of instability depends upon the crystallographic type of the grain boundary, of which many exist. Certain types of grain boundaries, referred to in the art as "special" grain boundaries, exhibit improved properties compared to "general" grain boundaries.
  • Grain Boundary Engineering refers to a family of techniques involving the processing, evaluation, and classification of grain boundaries within polycrystalline materials, which can be used to manipulate or optimize the morphology and network of grain boundaries to produce a larger fraction of special grain boundaries, and hence, desirable bulk properties.
  • a method of processing a metal alloy comprises, while maintaining the metal alloy at a temperature expressed in Kelvins of at least about 0.95 times the solvus temperature of the metal alloy expressed in Kelvins: applying a force to strain the metal alloy over a first period of time; and reducing the applied force over a second period of time subsequent to the first period of time; wherein the metal alloy is processed to have a special grain boundary fraction of at least about 55%.
  • FIG. 1 includes an exemplary image outlining grain boundaries in Sample 3 of
  • FIG. 2 is an exemplary image outlining grain boundaries in Sample 4 of
  • the grain boundary network of a metal alloy can be improved by heating and/or maintaining the alloy to a temperature close to its solvus temperature, and straining the alloy at the elevated temperature by applying a force. After the force is applied, the force can be reduced (e.g., so that the alloy is no longer strained) and remain so over a second period of time while maintaining the metal alloy close to the solvus temperature.
  • the force application and force reduction steps can be repeated for one or more cycles, in some cases. This process can produce metal alloys including a relatively large fraction of special grain boundaries, which can improve one or more physical properties of the alloy.
  • the solvus temperature of a metal alloy with a fixed composition is known to those of ordinary skill in the art, and refers to the temperature at which a metal alloy transforms between a state in which two or more phases are present and a state in which a homogeneous solid solution is present.
  • One of ordinary skill in the art would be capable of determining the solvus temperature of a metal alloy using a phase diagram, given the composition of the alloy.
  • Performing force application and force reduction steps at an elevated temperature can eliminate the need to substantially heat and cool the metal alloy between processing steps. This can result in significant energy and time savings, which can, in some embodiments, render the process industrially feasible.
  • Metal alloys with an increased fraction of special grain boundaries can be produced using the methods described herein.
  • the methods can be used to produce metal alloys with high fractions of special grain boundaries, which may dissolve uniformly in solvents.
  • Such metal alloys might find particular use as anode materials, for example, in electrodeposition systems.
  • the metal alloys treated using the methods described herein can exhibit relatively high mechanical strength and/or weldability.
  • the treated metal alloys may also exhibit high resistance to softening, hot cracking, stress-corrosion cracking, creep, electromigration, and/or corrosion.
  • the treatment process can include the step of maintaining the metal alloy at a temperature above a selected value.
  • the metal alloy can be maintained, in some instances, at a temperature of at least about 0.9 times the solvus temperature of the metal alloy (wherein the temperature and the solvus temperature, Ts, are expressed in Kelvins).
  • 0.9Ts of a metal alloy (expressed in Kelvins) is above ambient temperature.
  • the metal alloy can be maintained at a temperature above about 750 °C (1023 K), above about 800 °C (1073 K), above about 850 °C (1123 K), above about 900 °C (1173 K), or above about 950 °C (1223 K).
  • the metal alloy may be maintained at a temperature of above about 0.9 T s , above about 0.95 T s , or above about 0.98 T s (wherein the temperature and the solvus temperature, T s , are expressed in Kelvins).
  • maintaining a metal alloy at or above a given temperature may comprise applying energy (e.g., in the form of heat) to the metal alloy to ensure that it does not cool below the given temperature.
  • a substantially uniform temperature may be maintained throughout the bulk of the metal alloy.
  • the temperature of a metal alloy described herein may be maintained, for example, using a furnace, via resistive heating, induction heating, gas burners or by any other suitable method known in the art.
  • the temperature of the metal may be maintained within a range, in some instances.
  • the range may be absolute in some cases (e.g., between about 750 °C and about 1200 °C, or between about 800 °C and about 1000 °C).
  • the range may be measured as a fraction of the solvus temperature (e.g., between about between about 0.9 T s and about 1.1 T s , between about 0.95 T s and about 1.05 T s , or between about 0.98 T s and about 1.02 T s (wherein the temperature and the solvus temperature are expressed in Kelvins)).
  • the methods described herein can involve heating the metal alloy to a
  • the heating step can occur prior to the above-described step of maintaining the metal above the selected value.
  • the metal may be heated, in some cases, above about 750 °C (1023 K), above about 800 °C (1073 K), above about 850 °C (1123 K), above about 900 °C (1173 K), or above about 950 °C (1223 K). In some cases, the metal may be heated above a temperature of about 0.9 T s , about 0.95 T s , or about 0.98 Ts (wherein the temperature and the solvus temperature, Ts, are expressed in Kelvins).
  • Heating the metal alloy can also comprise heating the metal alloy to a
  • the range can be absolute in some cases (e.g., between about 750 °C and about 1200 °C, or between about 800 °C and about 1000 °C). In some instances, the range may be measured as a fraction of the solvus temperature (e.g., between about between about 0.9 T s and about 1.1 T s , between about 0.95 T s and about 1.05 T s , or between about 0.98 T s and about 1.02 T s (wherein the temperature and the solvus temperature are expressed in Kelvins)).
  • the metal alloy is heated (and, in some cases, also maintained) above a temperature suitable to anneal the metal.
  • a temperature suitable to anneal the metal may include those described above.
  • Annealing generally involves heat treating a metal to alter its micro structure, resulting, in some embodiments, in the recrystallization of at least a portion (or, in some cases, substantially all) of the annealed metal.
  • the metal alloy may be heated in any suitable atmosphere.
  • the metal alloy can be exposed to ambient air (i.e., about 80% nitrogen and about 20% oxygen) while it is annealed.
  • the metal alloy can be exposed to an inert atmosphere while being annealed (e.g., helium, argon, nitrogen, etc.).
  • an inert atmosphere e.g., helium, argon, nitrogen, etc.
  • a working gas environment or reducing atmosphere would be desirable.
  • the atmosphere may consist of nitrogen with a small amount (e.g., up to about 3%) of hydrogen, which may react with any undesired oxygen in the atmosphere.
  • Plastically straining a metal alloy can comprise any process which alters the shape of the metal alloy, i.e., plastically deforms the metal alloy.
  • straining may comprise compressing the metal alloy on one or more axes (e.g., forging the metal alloy), stretching the metal alloy, rolling the metal alloy, extruding the metal alloy, stamping the metal alloy, drawing, deep-drawing, or blanking the metal alloy, or any other method of deformation or shape forming known in the art.
  • the applied force When the applied force is along one axis, the extent of change in the dimension of the metal alloy (e.g., along the length of the metal alloy) along that axis, divided by the original dimension of the metal alloy along that axis, is referred to as the engineering strain.
  • Engineering strain is expressed as a percentage of the change in dimension along that axis as compared to the original dimension along that axis.
  • the applied force produces an engineering strain of at least about 3%, at least about 5%, at least about 10%, at least about 25%, at least about 50%, at least about 80%, at least about 95%, at least about 99%, or at least about 99.8%.
  • Applying a force to strain a metal alloy may also produce an engineering strain between about 3% and about 99.8%, or between about 50% and about 95%.
  • the strain may be expressed as a true strain.
  • True strain is also known to those of ordinary skill in the art of shape forming and deforming. When the force deforming a metal alloy is applied along one axis, the true strain refers to the extent of change in the dimension of the metal alloy, divided by the instantaneous dimension of the metal alloy along that axis. True strain can also be expressed as a percentage change in dimension as compared with the instantaneous dimension along the axis.
  • the applied force may produce a true strain of at least about 3%, at least about 4.8%, at least about 9.5%, at least about 22.3%, at least about 40%, at least about 58%, or at least about 70%. Applying a force to strain a metal alloy may also produce a true strain between about 3% and about 70%, or between about 40% and about 58%.
  • the force applied when the force applied is complex and/or multiaxial, the change in dimension along one axis may not completely describe the resulting strain.
  • the von Mises strain which is known to those of ordinary skill in the art of shape forming and deforming, may be used to quantify the strain.
  • the applied force may produce a von Mises strain of at least about 3%, at least about 5%, at least about 10%, at least about 25%, at least about 50%, or at least about 80%.
  • the applied force may produce a von Mises strain of between about 3% and between about 80%, or between about 50% and about 70%.
  • strain values described above may relate to strains produced during the application of a force in a single cycle process, or the strain produced during each application of force during a multi-cycle process.
  • the force may be applied (e.g., to plastically strain a metal alloy) over any suitable period of time.
  • the force is applied within a range of time.
  • the lower end of the range may be at least about
  • 0.01 seconds, at least about 0.1 seconds, at least about 1 second, at least about 5 seconds, at least about 10 seconds, or at least about 1 minute while the upper end of the range may be about 10 seconds, about 1 minute, about 5 minutes, or about 10 minutes. It should be understood that the range may be bound by any suitable combination of the lower limits and upper limits described above.
  • the force may be applied to achieve any suitable rate of strain.
  • the force may be applied to produce a rate of strain in the metal alloy of at least about 0.01% per second, at least about 0.1% per second, at least about 1% per second, at least about 10% per second, at least about 100% per second, at least about 1000% per second, at least about 10,000% per second, or higher.
  • the force may be applied to achieve a rate of strain in the metal alloy of between about 0.1% per second and about 10,000% per second, or between about 1% per second and about 1000% per second. While maintaining the metal alloy at an elevated temperature (e.g., above a temperature or within a temperature range), the amount of force applied to the metal alloy may be reduced, in some embodiments.
  • the reduction in the amount of force applied may be such that the metal alloy is no longer strained.
  • the metal alloy may be annealed as described above.
  • the reduction step may comprise reducing the first force by at least about 50%, at least about 75%, at least about 85%, at least about 95%, or at least about 99%.
  • the reducing step may comprise reducing the applied force to zero. In other embodiments, the reducing step may comprise reducing the applied force to a non-zero value.
  • the amount of force may remain reduced over any suitable period of time.
  • the amount of force applied to the metal alloy may remain reduced for at least about 5 seconds, at least about 30 seconds, at least about 60 seconds, at least about
  • the amount of force applied to the metal alloy may remain reduced for between about 5 and about 600 seconds or between about 10 and about 300 seconds.
  • another force may be applied after the step of reducing the applied force.
  • a second force or third force, etc.
  • the application of multiple forces to strain the metal alloy may result in a cumulative engineering strain (or a cumulative true strain, or a cumulative von Mises strain) of at least about 3%, at least about 5%, at least about 10%, at least about 25%, at least about 50%, at least about 80%, at least about 95%, at least about 99%, or at least about 99.8%.
  • the application of multiple forces to strain the metal alloy may result in a cumulative engineering strain (or a cumulative true strain, or a cumulative von Mises strain) of between about 3% and about 99.8%, or between about 50% and about 95%.
  • each step of applying a force may produce a substantially similar strain in the metal alloy.
  • each period of time over which a force is continuously applied results in an engineering strain (or a true strain, or a von Mises strain) of about 3%, about 5%, about 10%, about 25%, about 50%, about 80%, about 95%, about 99%, or about 99.8%.
  • the amount of strain produced by at least one force application step may be substantially different than the others. For example, the application of a first force may result in a first change in engineering strain, while the application of a second force may result in a substantially larger or substantially smaller engineering strain.
  • Each force application step in a multi-step process may also strain the metal alloy at a similar rate. Alternatively, in other embodiments, one or more force application steps occurs at a substantially higher or substantially lower rate of strain.
  • the amount of time over which the applied force remains reduced may be substantially similar between each force application step of a multi-cycle process. In other instances, the amount of time over which the applied force remains reduced may be substantially longer or substantially shorter between at least two force application steps. For example, in some embodiments, the amount of time over which the force remains reduced may be substantially longer between first and second force application steps than between second and third force application steps.
  • One or more force application steps in a multi-step process may occur at a substantially different temperature than one or more other force application steps in a multi-step process.
  • the first force application step may occur at a substantially higher temperature than at least one subsequent force application step.
  • the first force application step can occur at a substantially lower temperature than at least one subsequent force application step.
  • Grain boundaries may be characterized using Coincidence Site Lattice (CSL) theory.
  • CSL theory distinguishes special and general grain boundaries according to the crystallographic misorientation between the two neighboring grains.
  • sigma represents the inverse of the number density of the coincident lattice points between two misoriented crystals such as those that meet at a grain boundary.
  • a sigma value of 3 means that 1/3 of the lattice points of the two crystal grains meeting at a grain boundary coincide.
  • special boundaries are defined under CSL theory as those with sigma values from 1 up to and including 29, while general grain boundaries are defined as those with sigma values greater than 29.
  • Grain boundary analysis is customarily performed by measuring the lengths of grain boundaries within a cross-section of the metal alloy.
  • the fraction of special grain boundaries is calculated by dividing the sum of the lengths of the special grain boundaries by the sum of the lengths of all the grain boundaries in the cross-section.
  • This analysis may be achieved by using, for example, electron backscatter diffraction (EBSD).
  • EBSD electron backscatter diffraction
  • EBSD analysis methods are known to those of ordinary skill in the art, and may be used to examine the crystallographic orientation of crystals in a material, which can be used to determine texture and/or orientation of crystalline or polycrystalline materials.
  • EBSD can be conducted using a Scanning Electron Microscope (SEM) equipped with a backscatter diffraction camera.
  • the diffraction camera can include a phosphor screen and a camera to register the image on the phosphor screen.
  • a CCD detector may be used to register the image.
  • a flat, polished crystalline specimen may be placed into position in the specimen chamber, highly tilted (e.g., about 70° from horizontal) towards the diffraction camera.
  • methods may be used to produce metal alloy articles with a relatively high fraction of special grain boundaries. For example, in some embodiments, in some
  • metal alloys and articles described herein may have special grain boundary fractions of at least about 55%, at least about 60%, at least about 65%, at least about 70%, or at least about 75%. In some embodiments, metal alloys and articles described herein may have special grain boundary fractions of between about 55% and about 75%, or between about 65% and about 75%.
  • the methods described herein may be used with a wide variety of metal alloys.
  • the metal alloy can contain, in some cases, at least 3, at least 4, at least 5, or any other number of metal components. In some cases, the largest component of the metal alloy, by mass, is copper. In some embodiments, the metal alloy can contain at least about 75 wt , at least about 90 wt , at least about 95 wt , at least about 99 wt , between about 75 wt% and about 99.99 wt%, between about 90 wt% and about 99.99 wt%, between about 95 wt% and about 99.99 wt%, or between 99 wt% and about 99.99 wt% copper.
  • the metal alloy can include a variety of minority components (i.e., components other than the most abundant component, by mass, within the metal alloy). For example, the metal alloy can comprise chromium and/or zirconium as a minority component.
  • This example describes a set of experiments in which metal alloys were subject to a thermo-mechanical process to enhance the amount of special grain boundaries.
  • the processing included subjecting the samples to one or more cycles of applied force(s) to strain the samples.
  • Cu-Cr copper-chromium alloy
  • the first Cu-Cr alloy included 0.30 wt% Cr, about 99.7 wt% copper, and small amounts of impurities (Cu-0.30 wt% Cr alloy).
  • the solvus temperature of the Cu-0.30 wt% Cr alloy was 935 °C (1208 K).
  • the second Cu-Cr alloy included
  • the solvus temperature of the Cu-0.13 wt% Cr alloy was 845 °C (1118 K).
  • a copper- zirconium alloy including 0.06 wt% zirconium, 99.94 wt% copper, and small amounts of impurities (Cu-0.06 wt% Zr alloy) was also tested.
  • the solvus temperature of the Cu-0.06 wt% Zr alloy was 860 °C (1133 K).
  • 13 metal alloy samples were cut to form rectangular pieces measuring approximately 9 mm x 9 mm x 10 mm.
  • the types of materials and process parameters for each of the 13 samples are outlined in Tables 1, 2 and 3.
  • the cut samples were preheated in air at their processing temperatures (outlined in Tables 1, 2, and 3) for 30 minutes. After preheating, one or more cycles of force were applied to deform the samples at their processing temperatures. In this example the deformation was compressive, and the applied force was a uniaxial compression.
  • Tables 1, 2, and 3 include the amounts of engineering strain produced per cycle as a measure of the deformation. In addition, Tables 1, 2, and 3 include the rates of strain for each of the tested samples.
  • Sample 1 (see Table 1) was strained at a rate of 0.017 s "1 (i.e., the sample was reduced in height by 1.7%, relative to its height at the start of the cycle, each second) until the engineering strain reached 17% (about 10 s) for the cycle.
  • the force on the material was reduced to zero and the samples were maintained at the processing temperature for an "intermediate time," as indicated in Tables 1, 2, and 3.
  • the samples were annealed. In some cases, subsequent cycles of applying and reducing force were used.
  • Tables 1, 2, and 3 include lists of the number of cycles for each of the materials. For each sample tested, the sample was quenched in water after the final cycle.
  • Each strained sample was cut through its middle.
  • the cut samples were mechanically polished using emery paper.
  • Samples were subsequently polished using a diamond suspension, followed by a colloidal silica suspension polish for at least
  • Grain orientation data was acquired using electron backscatter diffraction (EBSD, TSL/EDAX Digiview) attached to a Field Emission Scanning Electron Microscope (FE- SEM) (Zeiss Supra55) using OIMTM Data Collection Version 5 (TSL/EDAX) software.
  • the scan conditions were as follows: total scan area of 750 x 750 microns, magnification of x300, and a scan step of 3 microns.
  • the edge regions of the 750 x 750 micron scans were trimmed to 740 x 740 microns by eliminating all data within 5 microns of the scan edge, as these regions frequently contained inaccurate data due to beam control issues during data acquisition.
  • the data was appropriately cleaned up using the software to eliminate inaccurate data points during data acquisition process (e.g. corresponding to a partially rough surface or contamination particles on the surface).
  • the cleaned orientation data was analyzed to determine the percentage of special grain boundaries in each sample using OEVITM Data Analysis Version 5 software.
  • Grain boundaries were defined as boundaries whose misorientation between 2 neighboring points was more than 15 degrees. Each grain boundary was classified as either "special” (sigma between 1 and 29) or "general” (sigma greater than 29). The percentages of "special” grain boundaries were calculated by dividing the total length of the special grain boundaries by the total length of all of the grain boundaries (both special and general), and multiplying by 100%.
  • FIG. 1 includes an image of Sample 3 (see Table 1) of this example, which included 71% special grain boundaries.
  • FIG. 2 includes an image of Sample 4 (see Table 1) of this example, which included 12% special grain boundaries.

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Abstract

L'invention porte sur des procédés d'amélioration de la qualité de réseaux de joints de grains. Le procédé peut conduire à la fabrication d'un métal comprenant une fraction relativement grande de joints de grains spéciaux (par exemple une fraction de joints de grains spéciaux d'au moins environ 55 %).
PCT/US2012/023458 2011-02-01 2012-02-01 Procédé thermomécanique pour améliorer la qualité de réseaux de joints de grains dans des alliages métalliques Ceased WO2012106414A1 (fr)

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Publication number Priority date Publication date Assignee Title
US8876990B2 (en) 2009-08-20 2014-11-04 Massachusetts Institute Of Technology Thermo-mechanical process to enhance the quality of grain boundary networks
WO2018198995A1 (fr) * 2017-04-26 2018-11-01 古河電気工業株式会社 Feuille d'alliage de cuivre et son procédé de fabrication

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EP2194149A1 (fr) * 2008-11-28 2010-06-09 Dowa Metaltech Co., Ltd. Plaque d'alliage en cuivre et son procédé de production
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EP2377959A1 (fr) * 2010-04-05 2011-10-19 Dowa Metaltech Co., Ltd. Feuille d'alliage en cuivre, procédé de fabrication de feuille d'alliage en cuivre et composant électrique/électronique
JP2011219833A (ja) * 2010-04-13 2011-11-04 Mitsubishi Shindoh Co Ltd プロジェクション溶接特性に優れたＣｕ−Ｎｉ−Ｓｉ系銅合金、及びその製造方法
WO2012004868A1 (fr) * 2010-07-07 2012-01-12 三菱伸銅株式会社 Plaque d'alliage de cuivre cu-ni-si avec d'excellentes caractéristiques d'emboutissage profond et son procédé de fabrication

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JP4584692B2 (ja) * 2004-11-30 2010-11-24 株式会社神戸製鋼所 曲げ加工性に優れた高強度銅合金板およびその製造方法
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US20040003878A1 (en) * 2002-06-21 2004-01-08 Nippon Mining & Metals Co., Ltd. Titanium copper alloy having excellent strength and bendability, and manufacturing method thereof
EP2194149A1 (fr) * 2008-11-28 2010-06-09 Dowa Metaltech Co., Ltd. Plaque d'alliage en cuivre et son procédé de production
US20100243112A1 (en) * 2009-03-31 2010-09-30 Questek Innovations Llc Beryllium-Free High-Strength Copper Alloys
EP2377959A1 (fr) * 2010-04-05 2011-10-19 Dowa Metaltech Co., Ltd. Feuille d'alliage en cuivre, procédé de fabrication de feuille d'alliage en cuivre et composant électrique/électronique
JP2011219833A (ja) * 2010-04-13 2011-11-04 Mitsubishi Shindoh Co Ltd プロジェクション溶接特性に優れたＣｕ−Ｎｉ−Ｓｉ系銅合金、及びその製造方法
WO2012004868A1 (fr) * 2010-07-07 2012-01-12 三菱伸銅株式会社 Plaque d'alliage de cuivre cu-ni-si avec d'excellentes caractéristiques d'emboutissage profond et son procédé de fabrication

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8876990B2 (en) 2009-08-20 2014-11-04 Massachusetts Institute Of Technology Thermo-mechanical process to enhance the quality of grain boundary networks
WO2018198995A1 (fr) * 2017-04-26 2018-11-01 古河電気工業株式会社 Feuille d'alliage de cuivre et son procédé de fabrication

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US20120192997A1 (en) 2012-08-02
US20140311207A1 (en) 2014-10-23

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