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• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
  • B22F1/05—Metallic powder characterised by the size or surface area of the particles
  • B22F1/054—Nanosized particles
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C1/00—Making non-ferrous alloys
  • C22C1/10—Alloys containing non-metals
  • C22C1/1084—Alloys containing non-metals by mechanical alloying (blending, milling)
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
  • B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C1/00—Making non-ferrous alloys
  • C22C1/04—Making non-ferrous alloys by powder metallurgy
  • C22C1/0433—Nickel- or cobalt-based alloys
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C1/00—Making non-ferrous alloys
  • C22C1/10—Alloys containing non-metals
  • C22C1/1094—Alloys containing non-metals comprising an after-treatment
• • 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
  • C22C—ALLOYS
  • C22C30/00—Alloys containing less than 50% by weight of each constituent
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C30/00—Alloys containing less than 50% by weight of each constituent
  • C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
  • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
  • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
  • C22C32/0026—Matrix based on Ni, Co, Cr or alloys thereof
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C33/00—Making ferrous alloys
  • C22C33/02—Making ferrous alloys by powder metallurgy
  • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
  • C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
• • 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
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
  • B22F2998/10—Processes characterised by the sequence of their steps
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
  • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
  • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents

Definitions

• Sintered nanocrystalline materials are often subjected to pressure or other postsintering processing techniques to achieve higher density materials.
• the metal alloy can be a nano-phase separating powder.
• the second metal can include chromium, cobalt, vanadium, silver, molybdenum, tungsten, or iron.
• the metal alloy powder can include manganese.
• the metal alloy powder can include molybdenum.
• the metal alloy powder can include zirconium.
• the first metal can have a concentration of about 25 at% to about 95 at% of the alloy.
• a method of nano-phase separation sintering of a powder can include providing a fine grained powder including a first metal element and a second metal forming a metal alloy and a third metal having a miscibility gap with the metal alloy, and sintering the fine grained powder to form a sintered product.
• a metal alloy powder for sintering can include a mechanically alloyed powder including a first metal element and a second metal forming a metal alloy and a third metal having a miscibility gap with the metal alloy.
• the sintered product achieves at least 90% density at low temperatures without the need for an applied pressure during the sintering.
• the metal alloy powder can include: NiCu having 5 at% to 20 at% Cr; NiCu having 5 at% to 45 at% Fe; NiCu having 5 at% to 45 at% Co; NiFeCu having 5at% or 8at% Mn; NiCu having 5 at% to 15 at% V; or NiCu having 5at% to 45 at% Co.
• FIG. IB depicts a phase diagram
• FIG. 2B is a graph illustrating a behavior of the system.
• FIG. 4A is a graph showing densification rate.
• FIG. 4B is a graph showing change in relative density.
• FIG. 6B depicts a Ni-Cu phase diagram at 10 at% Cr.
• FIG. 6C depicts a Ni-Cu phase diagram at 15 at% Cr.
• FIG. 12E is a table showing the stable phases at 1150°C.
• FIG. 12F is a graph showing the temperature dependence of the densification rate for 10 at 5°C/min to 1200°C and 40°C/min cooling.
• FIG. 13 is a chart showing the diffusion rates and temperature range for metals described herein.
• Rapid densification can be achieved through nano-phase separation and the design of ternary Ni systems, quaternary Ni systems, or higher order Ni systems.
• the Ni-Cu phase diagram exhibits a miscibility gap having a Ni- and a Cu-rich phase at low temperatures and a single phase at temperatures above 400 °C over the entire compositional range.
• the phase separating element is Cu to form interparticle necks between the powders.
• Thermo-Calc Software can be used to assess the equilibrium bulk phase diagrams of the ternary, or higher order, nano-phase separating Ni alloys with all of the following described characteristics and properties, such as volume fraction and chemical composition of the involved phases. Calculations, for example, Thermo-Calc, can be used as design tool to identify and predict potential alloy candidates for nano-phase separating ternary, or higher order, Ni systems.
• a method of designing a metal alloy powder having a miscibility gap at low temperature can include identifying a first metal element and a second metal to form a metal alloy, selecting a third metal having a miscibility gap with the metal alloy, and mechanically alloying the third metal and the metal alloy to form a metal alloy powder having a nanoscale grain size.
• the alloy can include an oxygen scavenging metal.
• the oxygen scavenging metal can be at a low concentration of the alloy, for example, 5 at%, 4 at%, 3 at%, 2 at%, 1 at%, or lower.
• the oxygen scavenging metal can be manganese or zirconium.
• the oxygen scavenging metal can be added to a ternary alloy to for a quaternary alloy.
• the mechanical alloying (e.g., ball milling) may be conducted for a time of greater than or equal to 6 hours (e.g., greater than or equal to 8 hours, greater than or equal to 10 hours, greater than or equal to 12 hours, or greater than or equal to 15 hours). In certain embodiments, the mechanical alloying (e.g., ball milling) may be conducted for a time of less than or equal to 18 hours. In some embodiments, the mechanical alloying (e g., ball milling) may be conducted for a time of 6 hour to 18 hours.
• the mechanical alloying e.g., ball milling
• an inert atmosphere for example, an argon atmosphere.
• the grain size may be between 1000 nm and about 2 nm — e.g., about 500 nm and about 2 nm, about 200 nm and about 2 nm, about 100 nm and about 2 nm, about 50 nm and about 2 nm, about 30 nm and about 2 nm, about 20 and about 2 nm, about 10 nm and about 2 nm.
• the size may refer to the largest dimension of the grain.
• the size of the grains referred herein may be determined as an “average” and may be measured by any suitable techniques.
• the dimensions may refer the diameter, length, width, height, depending on the geometry of the grain.
• a stable nanocrystalline material may also refer to a material comprising an amorphous phase.
• the alloy can be composed of three, four or more metals. Each metal can have a concentration of about 25 at% (atomic percent) to about 95 at% of the alloy. When two metal components of a ternary alloy each has a concentration of about 25 at% to about 95 at% of the alloy, the third metal component can have a concentration of about 5 at% to about 50 at% of the alloy.
• a method of nano-phase separation sintering of a powder can include providing a fine grained powder including a first metal element and a second metal forming a metal alloy and a third metal having a miscibility gap with the metal alloy, and sintering the fine grained powder to form a sintered product.
• sintering the plurality of particles involves heating the particles to a sintering temperature of less than or equal to 2200° C., less than or equal to 2000° C., less than or equal to 1900° C., less than or equal to 1800° C., less than or equal to 1700° C., less than or equal to 1600° C , less than or equal to 1500° C , less than or equal to 1400° C , less than or equal to 1300° C., less than or equal to 1200° C., less than or equal to 1100° C., less than or equal to 1000° C., less than or equal to 900° C., less than or equal to 850° C., less than or equal to 800° C., or less than or equal to 750° C.
• sintering the plurality of particles involves heating the particles to a sintering temperature of greater than or equal to 750° C., greater than or equal to 850° C., greater than or equal to 1000° C., greater than or equal to 1200° C., greater than or equal to 1450° C., or greater than or equal to 1600° C. Combinations of these ranges are also possible.
• sintering the plurality of particles involves heating the particles to a sintering temperature that is greater than or equal to 750° C. and less than or equal to 2200° C.
• the temperature of the sintered material is within these ranges for at least 10%, at least 25%, at least 50%, at least 75%, at least 90%, or at least 99% of the sintering time.
• the Co content can be 1 at%, 2 at%, 3 at%, 4 at%, 5 at%, 6 at%, 7 at%, 8 at%, 9 at%, 10 at%, 11 at%, 13 at%, 14 at%, 15 at%, 20 at%, 30 at%, 35 at%, 40 at%, 45 at%, 50 at%, 55 at%, 60 at%, 65 at%, 70 at%, 75at%, 80 at%, 85 at%, 90 at%, or 95 at% of the composition.
• the V content can be 1 at%, 2 at%, 3 at%, 4 at%, 5 at%, 6 at%, 7 at%, 8 at%, 9 at%, 10 at%, 11 at%, 13 at%, 14 at%, 15 at%, 20 at%, 30 at%, 35 at%, 40 at%, 45 at%, 50 at%, 55 at%, 60 at%, 65 at%, 70 at%, 75at%, 80 at%, 85 at%, 90 at%, or 95 at% of the composition.
• the Mo content can be 1 at%, 2 at%, 3 at%, 4 at%, 5 at%, 6 at%, 7 at%, 8 at%, 9 at%, 10 at%, 11 at%, 13 at%, 14 at%, 15 at%, 20 at%, 30 at%, 35 at%, 40 at%, 45 at%, 50 at%, 55 at%, 60 at%, 65 at%, 70 at%, 75at%, 80 at%, 85 at%, 90 at%, or 95 at% of the composition.
• the W content can be 1 at%, 2 at%, 3 at%, 4 at%, 5 at%, 6 at%, 7 at%, 8 at%, 9 at%, 10 at%, 11 at%, 13 at%, 14 at%, 15 at%, 20 at%, 30 at%, 35 at%, 40 at%, 45 at%, 50 at%, 55 at%, 60 at%, 65 at%, 70 at%, 75at%, 80 at%, 85 at%, 90 at%, or 95 at% of the composition.
• NiCu can have 5 at% to 20 at% Cr; NiCu can have 5 at% to 45 at% Fe; NiCu can have 5 at% to 45 at% Co; NiFeCu can have 5at% or 8at% Mn; NiCu can have 5 at% to 15 at% V; or NiCu can have 5at% to 45 at% Co.
• the metal alloy powder can include: NiCu having 5at%, 10at% 1 lat%, 12at%, 13at%, 14at%, 15at%, 16at%, 17at%, 18at%, or 19at% Cr; NiCu having 5 at%, 10at% 12at%, 14at%, 16at%, 18at%, 20at%, 22at%, 24at%, 26at%, 28at%, 30at%, 32at%, 34at%, 36at%, 38at%, 40at%, or 42at% Fe; NiCu having 5at%, 10at% 12at%, 14at%, 16at%, 18at%, 20at%, 22at%, 24at%, 26at%, 28at%, 30at%, 32at%, 34at%, 36at%, 38at%, 40at%, 42at%, or 44at% Co; NiFeCu having 5at% or 8at% Mn; NiCu having 6at%, 7at%, 8at%, 9at%, 10at%, 1 lat%
• the mechanically powder is a quaternary nano-phase separating powder.
• the metal alloy powder can include NiCu having 5at%, 10at% 12at%, 14at%, 16at%, 18at%, 20at%, 22at%, 24at%, 26at%, 28at%, 30at%, 32at%, 34at%, 36at%, 38at%, 40at%, 42at%, or 44at% Co and up to 5at% Mn.
• phase diagram suggests the interplay between concentration, tempature, phase separation, reduced surface energy and high solubility that least to the phase seperation enhanced sintering described herein.
• FIG. 1C illustrates an example of the general process example with Fe.
• FIG. 6D An alloy of 60 at% Ni, 25 at% Cu and 15 at% Cr was studied.
• a phase diagram of 60 at% Ni and 15% Cr is shown in FIG. 6D.
• FIG. 6E is a table showing the compositions of stable phases at 550°C.
• FIG. 6F shows the temperature dependence of densification at 5°C/min to 1200°C and 40°C/min cooling.
• FIG. 7A is a Ni-Fe phase diagram.
• FIG. 7B is a Cu-Fe phase diagram.
• Other phase diagrams at other Fe concentrations can be found at FIGS. 8A-8C.
• FIG. 8A is a Ni-Cu phase diagram at 5 at% Fe.
• FIG. 8B is a Ni-Cu phase diagram at 20 at% Fe.
• FIG. 8C is a Ni-Cu phase diagram at 42 at% Fe.
• FIG. 8D is a Ni-Cu phase diagram at 42at% Fe.
• FIG. 8E is a table showing the compositions of stable phases at 550°C. One set of experiments were conducted at 15 at% Cu.
• FIG. 8F shows the temperature dependence of densification at 5°C/min to 945°C and 40°C/min cooling.
• FIG. 8G shows the change in relative density over time at 5°C/min heating.
• FIG. 8H shows the temperature dependence of densification at 10°C/min to 1000°C and 40°C/min cooling.
• FIG. 81 shows the change in relative density over time at 5°C/min heating to a final relative density of 0.5864%.
• FIG. 8J shows the temperature dependence of densification at 15°C/min to 1000°C and 40°C/min cooling.
• FIG. 8K shows the change in relative density over time at 15°C/min heating to a final relative density of 0.5477%.
• FIG. 8L shows the temperature dependence of densification at 20°C/min to 1000°C and 40°C/min cooling.
• FIG. 8M shows the change in relative density over time at 20°C/min heating to a final relative density of 0. 4276%.
• FIG. 8N shows the temperature dependence of densification at 5°C/min to 1100°C and 40°C/min cooling.
• FIG. 80 shows the change in relative density over temperature at 5°C/min heating.
• FIG. 8P shows the change in relative density over time at 5°C/min heating.
• FIG. 8Q shows the temperature dependence of densification at 10°C/min to 1100°C and 40°C/min cooling.
• FIG. 8R shows the change in relative density over temperature at 10°C/min heating.
• FIG. 8S shows the change in relative density overtime at 15°C/min.
• FIG. 8T shows the temperature dependence of densification at 20°C/min to 1100°C and 40°C/min cooling.
• FIG. 8U shows the temperature dependence of densification at 20°C/min to 1100°C and 40°C/min cooling.
• FIG. 8V shows the change in relative density over time at 20°C/min.
• FIG. 9A is a Ni-Co phase diagram.
• FIG. 9B is a Cu-Co phase diagram.
• Other phase diagrams at other Co concentrations can be found at FIGS. 10A-10C.
• FIG. 10A is a Ni-Cu phase diagram at 5 at% Co.
• FIG. 10B is a Ni-Cu phase diagram at 20 at% Co.
• FIG. 10C is a Ni-Cu phase diagram at 44 at% Co.
• a V alloy was studied.
• FIG. 11 A is a Ni-V phase diagram.
• FIG. 1 IB is a Cu-V phase diagram.
• Other phase diagrams at other V concentrations can be found at FIGS. 12A-12C.
• FIG. 12A is a Ni-Cu phase diagram at 6 at% V.
• FIG. 12A is a Ni-Cu phase diagram at 6 at% V.
• FIG. 12B is a Ni-Cu phase diagram at 10 at% V.
• FIG. 12C is a Ni-Cu phase diagram at 13 at% V.
• FIG. 12D is a Ni-Cu phase diagram and 13 at% V.
• FIG. 12E shows the stable phases at 1150°C.
• FIG. 12F shows the temperature dependence of the densifi cation rate for 10 at 5°C/min to 1200°C and 40°C/min cooling.
• FIG. 12G shows the temperature dependences of the change in relative density.
• FIG. 13 is a chart showing the diffusion rates and temperature range for metals described herein.
• FIG. 14A is a phase diagram for Fe-Cu with 40 at% Ni from an Fe database.
• FIG. 14B is a phase diagram for Fe-Cu with 40 at% Ni from a Ni database.
• FIG. 14C is a phase diagram for Fe-Cu with 40 at% Ni from a Cu database.
• FIG. 14D is a phase diagram for Fe-Cu with 40 at% Ni from a high entropy alloy database.
• Pretreatment of an alloy in a reducing atmosphere can improve the sintering performance of the alloy.
• pretreatment with hydrogen gas at 300°C for 24 hours can reduce swelling.
• FIGS. 18A, 18B and 18C show densification after pretreatment with hydrogen at different heating rates.
• oxygen scavenger can be included in an alloy.
• FIG. 19 shows the impact on density of 5 at% and 8 at% Mn to a Ni-Fe-Cu composition.

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