WO2018048785A2 - Aluminum-titanium-zinc based alloy materials and products made therefrom - Google Patents

Aluminum-titanium-zinc based alloy materials and products made therefrom Download PDF

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Publication number
WO2018048785A2
WO2018048785A2 PCT/US2017/050043 US2017050043W WO2018048785A2 WO 2018048785 A2 WO2018048785 A2 WO 2018048785A2 US 2017050043 W US2017050043 W US 2017050043W WO 2018048785 A2 WO2018048785 A2 WO 2018048785A2
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Prior art keywords
zinc
solid
alloy material
vacancies
pressure
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PCT/US2017/050043
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French (fr)
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WO2018048785A3 (en
Inventor
Vivek M. Sample
Men Glenn Chu
Raymond J. Kilmer
Shawn P. Sullivan
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Arconic Inc.
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Publication of WO2018048785A2 publication Critical patent/WO2018048785A2/en
Publication of WO2018048785A3 publication Critical patent/WO2018048785A3/en

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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C18/00Alloys based on zinc
    • C22C18/04Alloys based on zinc with aluminium as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/14Refining in the solid state

Definitions

  • Aluminum alloys and titanium alloys are known to those skilled in the metallurgical art. These alloys are used in various industries and in various applications.
  • a method comprises producing an initial solid alloy material comprising aluminum, titanium, and zinc.
  • the initial solid alloy material may be produced, for instance, via high pressure casting to facilitate retention of aluminum, titanium, and zinc in a molten liquid phase.
  • This molten liquid phase may be subsequently cooled to below its solidus temperature, thereby producing the initial solid alloy material comprising the aluminum, titanium, and zinc.
  • the initial solid alloy material is cooled to ambient.
  • the method may further include removing a portion of the zinc from the initial solid alloy material, thereby producing a final solid alloy material having vacancies therein, where the vacancies are associated with the removed zinc.
  • the terms "voids" and "vacancies” are used interchangeably herein.
  • the removing step comprises subjecting the initial solid alloy material to one or more elevated temperatures, thereby sublimating at least a portion of the zinc.
  • the initial solid alloy material may be heated in a furnace (or other suitable heating apparatus) to remove at least a portion of the zinc, thereby producing vacancies within the final solid alloy material.
  • the removing step comprises maintaining the initial solid material below its incipient melting point
  • controlled pressure annealing may be used to facilitate the removing of the zinc.
  • the pressure within a suitable furnace or other suitable heating apparatus may be controlled (e.g., using a pressure-controlled inert gas atmosphere) to the appropriate pressure(s) given the appropriate temperature(s) of exposure.
  • the controlled atmosphere may facilitate control of at least one of (i) a rate of sublimation of the sublimating step and (ii) an amount of solid zinc phase dissolution.
  • high pressure(s) may be used to facilitate slow rates of zinc sublimation and/or higher rates of solid state diffusion, while lower pressure(s) may facilitate higher rates of zinc sublimation and/or lower rates of solid state diffusion.
  • the low pressures may even include a vacuum relative to ambient pressure.
  • temperature controls and changes can be used in addition to, or in lieu of, the pressure controls and changes to facilitate the proper control of the rate of sublimation of the sublimating step and/or an amount of solid zinc phase dissolution.
  • multiple different pressures and/or temperatures are used during the removing step to facilitate production of a final alloy material having a preselected amount of vacancies and/or zinc therein.
  • a first pressure may be used during a first portion of the removing step
  • a second pressure may be used during a second portion of the removing step.
  • At the first pressure at least some of the zinc may sublimate and diffuse out of the solid material.
  • the second pressure may be higher than the first pressure, and, at the second pressure, sublimation may be at least partially restricted or even eliminated.
  • at the second pressure at least some of the zinc may condense to the solid phase while in the solid material and/or at least some of the zinc may be maintained in the solid phase within the solid material.
  • the second pressure may facilitate solid state diffusion of zinc within the matrix of the solid material.
  • at least some of the zinc may solid state diffuse to one or more vacancies of the solid material.
  • the solid state diffusion of the zinc may facilitate a more homogenous distribution of the zinc and/or the vacancies within the solid material (e.g., by having zinc diffuse through the cross-section of the solid material).
  • the pressure(s) used during the removing step can facilitate preselection of a desired morphology of the vacancies, and the final solid alloy material may comprise the desired morphology of the vacancies.
  • the pressure(s) utilized during the removing step may be selected to control solid state diffusion of zinc in the initial solid material while restricting sublimation of zinc.
  • the pressure during the removing step can be alternated up and down to facilitate the desired final solid alloy material, including the amount of the vacancies (e.g., the volume fraction of the vacancies) and the size of the vacancies, and the amount of zinc within the final solid alloy material.
  • the alternating may comprise using the first and second pressures described above, or any other suitable pressures, such as a third pressure, where the third pressure is one of (i) lower than the first pressure, (ii) higher than the second pressure, or (iii) between the first and the second pressures.
  • Fourth, fifth, or any number of subsequent pressures may be used to achieve the desired final solid alloy material.
  • Any suitable temperature(s) may be used with any of the pressure(s) to facilitate the final solid alloy material.
  • the removing step generally comprises sublimating at least a portion of the zinc of the initial solid alloy material.
  • the removing step may include solid state diffusion of the zinc through and out of a crystal lattice of the initial solid alloy material.
  • the initial volume of the initial solid alloy material may be retained even though its density is being reduced due to the removal of the zinc.
  • the initial solid alloy material may be produced by any methodology that facilitates retention of aluminum, titanium and zinc therein.
  • the initial solid alloy material may be an ingot, a shape casting, a wrought product, or an additively manufactured product, among others.
  • the initial solid alloy material comprises at least 1 at. % Zn.
  • the initial solid alloy material comprises at least 5 at. % Zn.
  • the initial solid alloy material comprises at least 10 at. % Zn.
  • the initial solid alloy material comprises at least 20 at. % Zn.
  • the initial solid alloy material comprises at least 30 at. % Zn.
  • the initial solid alloy material may comprise not greater than 80 at. % Zn, or not greater than 60 at. % Zn, as examples.
  • the initial solid alloy material comprises at least 10 at. % of each of titanium and aluminum.
  • any suitable amount of zinc can be removed to produce final alloy materials having vacancies therein.
  • a method may comprise preselecting a desired amount of the vacancies based on the amount of zinc in the initial solid alloy material, and completing the removing step to achieve the desired amount of vacancies by removing a preselected amount the zinc.
  • the removing step comprises heating the initial solid alloy material at one or more preselected temperatures and soaking at the one or more preselected temperatures for one or more times to achieve removal of the preselected amount of zinc.
  • the size of the vacancies may depend on the amount of zinc contained within the initial solid material.
  • the initial solid alloy material comprises a homogeneous distribution of the zinc
  • the final solid alloy material correspondingly comprises a homogeneous distribution of vacancies.
  • the average size of the vacancies is not greater than 5 microns. The size and/or distribution of the vacancies may be controlled based on the control of the astrosphere, described above and below.
  • a final solid material comprises at least 0.1 vol. % vacancies. In another embodiment, a final solid material comprises at least 0.5 vol. % vacancies. In yet another embodiment, a final solid material comprises at least 1.0 vol. % vacancies. In another embodiment, a final solid material comprises at least 1.5 vol. % vacancies. In yet another embodiment, a final solid material comprises at least 2.0 vol. % vacancies. In another embodiment, a final solid material comprises at least 2.5 vol. % vacancies. In yet another embodiment, a final solid material comprises at least 3.0 vol. % vacancies, or more.
  • a method comprises producing an initial solid alloy material comprising aluminum, titanium, and zinc, such as by ingot casting.
  • a method may further comprise homogenizing the initial solid material by using an appropriate atmosphere (e.g., by heating to an appropriate temperature and at elevated pressure), wherein the combination of the selected temperatures and pressures facilitate solid state diffusion of the materials of the initial solid material, while also suppressing, restricting and/or eliminating zinc sublimation.
  • a homogenized solid material may be produced.
  • the homogenization step may occur prior to any removing of the zinc step (e.g., may occur after casting of the initial solid material and prior to any removing of zinc contained in the initial solid material).
  • the homogenized solid product may then be either (a) processed into a shaped form (e.g., by wrought alloy processing techniques), or (b) subjected to appropriate atmosphere(s) to facilitate removal of zinc contained therein, e.g., by solid state diffusion and/or sublimation.
  • the homogenized solid product may be extruded, forged or rolled into an appropriate end product under conditions which no appreciable amount of zinc is removed from the homogenized product.
  • This wrought product may then be subjected to the appropriate temperature(s) and pressure(s) to facilitate removal of zinc therein, as previously described.
  • a method includes removing at least some zinc from a previously homogenized material (e.g., zinc located proximal an outer surface of a wrought product), and then re-homogenizing the material.
  • a previously homogenized material e.g., zinc located proximal an outer surface of a wrought product
  • the final solid materials having the vacancies therein may be used in any suitable application. For instance, due to the unique microstructure, and the presence of titanium, the amount of zinc and vacancies may be tailored for hydrogen storage purposes.
  • the hydrogen may preferentially bond with the titanium of the solid material.
  • the solid material may be useful as a hydrogen storage apparatus.
  • this hydrogen storage apparatus may be used in a fuel cell.
  • the final solid materials may also be used in aerospace or other applications where high strength and low density are useful.
  • the final solid materials may be wrought or shape-cast aerospace products used in structural applications or high temperature applications (e.g., in engines, such as turbine engines).
  • the final solid materials may also find use in electronic applications due to the ability to control vacancy size and distribution. Such electronic materials may be doped, for instance, to facilitate the appropriate electrical properties.
  • a mixture of approximately 25 at. % Al, 30 at. % Ti, and 45 at. % Zn are induction melted at about 1475-1500°C in a high pressure casting apparatus under a pressure of about 750 psig (argon gas).
  • the high pressure maintains the alloying elements in the liquid phase molten pool.
  • the molten pool is cooled to below its solidus temperature, while maintaining the pressure, thereby forming an ingot comprising the aluminum, titanium, and zinc.
  • the ingot is then cooled to ambient and removed from the high pressure casting apparatus.
  • the ingot is heated in a furnace to about 1200°C (and at ambient pressure) and held for about 2 hours at this temperature. The ingot is then removed from the furnace.
  • Weight measurements indicate that the ingot is approximately 20% lighter after the furnace treatment. Despite the loss of weight, visual inspection shows that the volume of the ingot is substantially unchanged. Microscopy reveals the presence of a large number of vacancies (voids) (approximately 15% by volume of the material). It was estimated that a substantial amount of zinc (approx. 65 wt. %) was removed due to the loss of the weight of the material. It is hypothesized that the zinc sublimated out of the crystalline ingot structure via solid state diffusion, leaving the vacancies/voids.

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Abstract

The present disclosure relates to new alloys based on the aluminum-titanium-zinc system, and products made therefrom. A method may include producing an initial solid alloy material comprising aluminum, titanium, and zinc. The method may further include removing a portion of the zinc from the initial solid alloy material, thereby producing a final solid alloy material having vacancies therein, where the vacancies are associated with the removed zinc. In one embodiment, the removing step comprises subjecting the initial solid alloy material to one or more elevated temperatures, thereby sublimating at least a portion of the zinc.

Description

ALUMINUM-TITANIUM-ZINC BASED ALLOY MATERIALS AND PRODUCTS
MADE THEREFROM
BACKGROUND
[0001] Aluminum alloys and titanium alloys are known to those skilled in the metallurgical art. These alloys are used in various industries and in various applications.
SUMMARY
[0002] The present disclosure relates to new alloys based on the aluminum-titanium-zinc system, and products made therefrom. In one aspect, a method comprises producing an initial solid alloy material comprising aluminum, titanium, and zinc. The initial solid alloy material may be produced, for instance, via high pressure casting to facilitate retention of aluminum, titanium, and zinc in a molten liquid phase. This molten liquid phase may be subsequently cooled to below its solidus temperature, thereby producing the initial solid alloy material comprising the aluminum, titanium, and zinc. In one embodiment, the initial solid alloy material is cooled to ambient.
[0003] The method may further include removing a portion of the zinc from the initial solid alloy material, thereby producing a final solid alloy material having vacancies therein, where the vacancies are associated with the removed zinc. The terms "voids" and "vacancies" are used interchangeably herein. In one embodiment, the removing step comprises subjecting the initial solid alloy material to one or more elevated temperatures, thereby sublimating at least a portion of the zinc. For instance, the initial solid alloy material may be heated in a furnace (or other suitable heating apparatus) to remove at least a portion of the zinc, thereby producing vacancies within the final solid alloy material. In one embodiment, the removing step comprises maintaining the initial solid material below its incipient melting point
[0004] As one example, controlled pressure annealing may be used to facilitate the removing of the zinc. For instance, the pressure within a suitable furnace or other suitable heating apparatus may be controlled (e.g., using a pressure-controlled inert gas atmosphere) to the appropriate pressure(s) given the appropriate temperature(s) of exposure. The controlled atmosphere may facilitate control of at least one of (i) a rate of sublimation of the sublimating step and (ii) an amount of solid zinc phase dissolution. For instance, high pressure(s) may be used to facilitate slow rates of zinc sublimation and/or higher rates of solid state diffusion, while lower pressure(s) may facilitate higher rates of zinc sublimation and/or lower rates of solid state diffusion. The low pressures may even include a vacuum relative to ambient pressure. As may be appreciated, temperature controls and changes can be used in addition to, or in lieu of, the pressure controls and changes to facilitate the proper control of the rate of sublimation of the sublimating step and/or an amount of solid zinc phase dissolution.
[0005] In one embodiment, multiple different pressures and/or temperatures are used during the removing step to facilitate production of a final alloy material having a preselected amount of vacancies and/or zinc therein. For instance, a first pressure may be used during a first portion of the removing step, and a second pressure may be used during a second portion of the removing step. At the first pressure, at least some of the zinc may sublimate and diffuse out of the solid material. The second pressure may be higher than the first pressure, and, at the second pressure, sublimation may be at least partially restricted or even eliminated. Thus, at the second pressure, at least some of the zinc may condense to the solid phase while in the solid material and/or at least some of the zinc may be maintained in the solid phase within the solid material. The second pressure may facilitate solid state diffusion of zinc within the matrix of the solid material. In some embodiments, at least some of the zinc may solid state diffuse to one or more vacancies of the solid material. The solid state diffusion of the zinc may facilitate a more homogenous distribution of the zinc and/or the vacancies within the solid material (e.g., by having zinc diffuse through the cross-section of the solid material). Thus, the pressure(s) used during the removing step can facilitate preselection of a desired morphology of the vacancies, and the final solid alloy material may comprise the desired morphology of the vacancies. Correspondingly, the pressure(s) utilized during the removing step may be selected to control solid state diffusion of zinc in the initial solid material while restricting sublimation of zinc. Further, the pressure during the removing step can be alternated up and down to facilitate the desired final solid alloy material, including the amount of the vacancies (e.g., the volume fraction of the vacancies) and the size of the vacancies, and the amount of zinc within the final solid alloy material. The alternating may comprise using the first and second pressures described above, or any other suitable pressures, such as a third pressure, where the third pressure is one of (i) lower than the first pressure, (ii) higher than the second pressure, or (iii) between the first and the second pressures. Fourth, fifth, or any number of subsequent pressures may be used to achieve the desired final solid alloy material. Any suitable temperature(s) may be used with any of the pressure(s) to facilitate the final solid alloy material. Thus, any suitable astrospheres (temperature(s), pressure(s), types of gas(es) may be used to facilitate the final solid alloy material. [0006] As disclosed above, the removing step generally comprises sublimating at least a portion of the zinc of the initial solid alloy material. In this regard, the removing step may include solid state diffusion of the zinc through and out of a crystal lattice of the initial solid alloy material. Correspondingly, the initial volume of the initial solid alloy material may be retained even though its density is being reduced due to the removal of the zinc. In one embodiment, the initial solid alloy material has an initial volume (Vi), the final solid material has a final volume (Vf), and the final volume is from 90% to 100% of the initial volume (0.9*Vi < Vf < Vi). In one embodiment, the final volume is from 95% to 100%) of the initial volume (0.95 *Vi < Vf < Vi). In one embodiment, the final volume is from 99% to 100% of the initial volume (0.99*Vi < Vf < Vi). In one embodiment, the crystal lattice of the initial solid alloy material comprises an fee structure. In one embodiment, the removing step comprises diffusing at least a portion of the zinc through and out of the fee structure (e.g., due to the sublimation of the zinc).
[0007] The initial solid alloy material may be produced by any methodology that facilitates retention of aluminum, titanium and zinc therein. For instance, the initial solid alloy material may be an ingot, a shape casting, a wrought product, or an additively manufactured product, among others. In one embodiment, the initial solid alloy material comprises at least 1 at. % Zn. In another embodiment, the initial solid alloy material comprises at least 5 at. % Zn. In yet another embodiment, the initial solid alloy material comprises at least 10 at. % Zn. In another embodiment, the initial solid alloy material comprises at least 20 at. % Zn. In another embodiment, the initial solid alloy material comprises at least 30 at. % Zn. In any of these embodiments, the initial solid alloy material may comprise not greater than 80 at. % Zn, or not greater than 60 at. % Zn, as examples. In one embodiment, the initial solid alloy material comprises at least 10 at. % of each of titanium and aluminum.
[0008] Any suitable amount of zinc can be removed to produce final alloy materials having vacancies therein. For instance, a method may comprise preselecting a desired amount of the vacancies based on the amount of zinc in the initial solid alloy material, and completing the removing step to achieve the desired amount of vacancies by removing a preselected amount the zinc. In one embodiment, the removing step comprises heating the initial solid alloy material at one or more preselected temperatures and soaking at the one or more preselected temperatures for one or more times to achieve removal of the preselected amount of zinc. The preselected time(s) and temperature(s) may be preselected based on, for instance, the initial amount of zinc within the initial solid alloy material and/or based on a preselected amount of vacancies to be included in the final solid alloy material, among other criteria. The pressure(s) may likewise be selected relative to the selected temperature(s) based on a preselected amount of vacancies to be included in the final solid alloy material.
[0009] Irrespective of whether the amount of removed zinc is preselected, the removing step may comprise removing a substantial amount of the zinc from the initial solid alloy material. In one approach, at least 1 wt. % of the Zinc is removed from the initial solid alloy material. In one embodiment, at least 5 wt. % of the zinc is removed from the initial solid alloy material. In another embodiment, at least 10 wt. % of the zinc is removed from the initial solid alloy material. In yet another embodiment, at least 25 wt. % of the zinc is removed from the initial solid alloy material. In another embodiment, at least 33 wt. % of the zinc is removed from the initial solid alloy material. In yet another embodiment, at least 50 wt. % of the zinc is removed from the initial solid alloy material. In another embodiment, at least 66 wt. % of the zinc is removed from the initial solid alloy material. In yet another embodiment, at least 75 wt. % of the zinc is removed from the initial solid alloy material. In another embodiment, at least 90 wt. % of the zinc is removed from the initial solid alloy material. In yet another embodiment, at least 95 wt. % of the zinc is removed from the initial solid alloy material. In yet another embodiment, at least 99 wt. % of the zinc is removed from the initial solid alloy material. In yet another embodiment, substantially all of the zinc is removed from the initial solid alloy material.
[0010] The size of the vacancies may depend on the amount of zinc contained within the initial solid material. In one embodiment, the initial solid alloy material comprises a homogeneous distribution of the zinc, and the final solid alloy material correspondingly comprises a homogeneous distribution of vacancies. In one embodiment, the average size of the vacancies is not greater than 5 microns. The size and/or distribution of the vacancies may be controlled based on the control of the astrosphere, described above and below.
[0011] As disclosed above, due to solid state diffusion of zinc out of the crystal lattice, the final solid alloy material may retain the same product form as the initial solid alloy material. In one embodiment, the final solid alloy material is one of an ingot, a shape casting, a wrought product, or an additively manufactured product, among others. In one embodiment, the final solid alloy material is a solid material comprising aluminum, titanium, and a predetermined amount of vacancies therein. In one embodiment, the final solid alloy material is a solid material comprising aluminum, titanium, zinc, and a predetermined amount of vacancies therein. In one embodiment, at least 90 vol. % of the vacancies are wholly contained within the solid material. As used herein, "wholly contained within the solid material" means that a vacancy is wholly encapsulated by the final solid material. [0012] The volume of vacancies within the final solid material may be substantial. In one embodiment, a final solid material comprises at least 0.1 vol. % vacancies. In another embodiment, a final solid material comprises at least 0.5 vol. % vacancies. In yet another embodiment, a final solid material comprises at least 1.0 vol. % vacancies. In another embodiment, a final solid material comprises at least 1.5 vol. % vacancies. In yet another embodiment, a final solid material comprises at least 2.0 vol. % vacancies. In another embodiment, a final solid material comprises at least 2.5 vol. % vacancies. In yet another embodiment, a final solid material comprises at least 3.0 vol. % vacancies, or more.
[0013] In one embodiment, a method comprises producing an initial solid alloy material comprising aluminum, titanium, and zinc, such as by ingot casting. A method may further comprise homogenizing the initial solid material by using an appropriate atmosphere (e.g., by heating to an appropriate temperature and at elevated pressure), wherein the combination of the selected temperatures and pressures facilitate solid state diffusion of the materials of the initial solid material, while also suppressing, restricting and/or eliminating zinc sublimation. Thus, a homogenized solid material may be produced. The homogenization step may occur prior to any removing of the zinc step (e.g., may occur after casting of the initial solid material and prior to any removing of zinc contained in the initial solid material). The homogenized solid product may then be either (a) processed into a shaped form (e.g., by wrought alloy processing techniques), or (b) subjected to appropriate atmosphere(s) to facilitate removal of zinc contained therein, e.g., by solid state diffusion and/or sublimation. For instance, the homogenized solid product may be extruded, forged or rolled into an appropriate end product under conditions which no appreciable amount of zinc is removed from the homogenized product. This wrought product may then be subjected to the appropriate temperature(s) and pressure(s) to facilitate removal of zinc therein, as previously described. Any number of pressure and/or temperature cycles may be used to produce the appropriate end product having the appropriate vacancy size and/or distribution and/or zinc content and/or distribution of zinc within the wrought product. Use of higher pressure(s) at appropriate temperature(s) may facilitate homogenizing the zinc content and/or vacancies of the materials (e.g., via solid state diffusion of zinc), while use of lower pressure(s) at appropriate temperature(s) may facilitate removal of zinc and/or tailored gradients of zinc and/or vacancies. In one approach, a method includes removing at least some zinc from a previously homogenized material (e.g., zinc located proximal an outer surface of a wrought product), and then re-homogenizing the material. Such removal and/or re-homogenization steps can be repeated as necessary / appropriate to produce a final product, wrought or otherwise. Thus, the final product may include a predetermined amount of zinc, a predetermined amount of vacancies, have a predetermined density and/or have a predetermined strength, among others. In one embodiment, the final product may include a generally homogeneous distribution of zinc and/or vacancies. In another embodiment, the final product may include predetermined zinc concentration gradients and/or predetermined vacancy distributions.
[0014] The final solid materials having the vacancies therein may be used in any suitable application. For instance, due to the unique microstructure, and the presence of titanium, the amount of zinc and vacancies may be tailored for hydrogen storage purposes. The hydrogen may preferentially bond with the titanium of the solid material. Thus, the solid material may be useful as a hydrogen storage apparatus. Correspondingly, this hydrogen storage apparatus may be used in a fuel cell. The final solid materials may also be used in aerospace or other applications where high strength and low density are useful. For instance, the final solid materials may be wrought or shape-cast aerospace products used in structural applications or high temperature applications (e.g., in engines, such as turbine engines). The final solid materials may also find use in electronic applications due to the ability to control vacancy size and distribution. Such electronic materials may be doped, for instance, to facilitate the appropriate electrical properties.
DETAILED DESCRIPTION
[0015] A mixture of approximately 25 at. % Al, 30 at. % Ti, and 45 at. % Zn are induction melted at about 1475-1500°C in a high pressure casting apparatus under a pressure of about 750 psig (argon gas). The high pressure maintains the alloying elements in the liquid phase molten pool. The molten pool is cooled to below its solidus temperature, while maintaining the pressure, thereby forming an ingot comprising the aluminum, titanium, and zinc. The ingot is then cooled to ambient and removed from the high pressure casting apparatus. Next, the ingot is heated in a furnace to about 1200°C (and at ambient pressure) and held for about 2 hours at this temperature. The ingot is then removed from the furnace. Weight measurements (before and after) indicate that the ingot is approximately 20% lighter after the furnace treatment. Despite the loss of weight, visual inspection shows that the volume of the ingot is substantially unchanged. Microscopy reveals the presence of a large number of vacancies (voids) (approximately 15% by volume of the material). It was estimated that a substantial amount of zinc (approx. 65 wt. %) was removed due to the loss of the weight of the material. It is hypothesized that the zinc sublimated out of the crystalline ingot structure via solid state diffusion, leaving the vacancies/voids.

Claims

CLAIMS What is claimed is:
1. A method comprising:
producing an initial solid alloy material comprising aluminum, titanium, and zinc; removing at least a portion of the zinc from the initial solid alloy material, thereby producing a final solid alloy material having vacancies therein, wherein the vacancies are associated with the removed zinc.
2. The method of claim 1, wherein the initial solid alloy material has an initial volume (¼), wherein the final solid material has a final volume (Vf), and wherein the final volume is from 90% to 100% of the initial volume (0.9*Vi < Vf < Vj).
3. The method of claim 1, wherein the removing step comprises:
subjecting the initial solid alloy material to one or more atmospheres, thereby sublimating at least a portion of the zinc.
4. The method of claim 3, wherein the subjecting step comprises comprising maintaining the initial solid alloy material below its incipient melting point.
5. The method of claim 3, wherein the subject step comprises:
controlling pressure and/or temperature during the subjecting step, thereby controlling at least one of (i) a rate of sublimation of the sublimating step and (ii) an amount of solid zinc phase dissolution.
6. The method of claim 5, wherein the controlling the pressure step comprises:
preselecting a desired morphology of the vacancies, and
based, on the preselecting step, completing the controlling the pressure and/or temperature step;
wherein the final solid alloy material comprises the desired morphology of the vacancies.
7. The method of claim 5, wherein the controlling the pressure and/or temperature step comprises: utilizing a first pressure during a first portion of the subjecting step; and utilizing a second pressure during a second portion of the subjecting step;
wherein the first pressure is lower than the second pressure; and wherein, during the utilizing the first pressure step, at least some of the zinc sublimates and diffuses out of the initial solid material.
8. The method of claim 6, wherein, during the second pressure step, a portion of the zinc is solid phase zinc, and where the method comprises:
diffusing at least some of the solid phase zinc into vacancies of the initial solid material.
9. The method of claim 6, comprising:
selecting the second pressure to control solid state diffusion of zinc in the initial solid material while restricting sublimation of zinc.
10. The method of claim 8, comprising:
alternating the utilizing a first pressure and the utilizing a second pressure steps, thereby controlling a volume fraction and a distribution of the vacancies of the final solid material.
11. The method of claim 10, wherein the final solid material comprises a homogenous distribution of the vacancies.
12. The method of claim 1, wherein the initial solid alloy material comprises a crystal lattice, and wherein the removing step comprises solid state diffusion of at least a portion of the zinc through and out of the crystal lattice.
13. The method of claim 12, wherein the crystal lattice comprises an fee structure.
14. The method of claim 1, comprising:
preselecting a desired amount of the vacancies based on the amount of zinc in the initial solid alloy material; and
completing the removing step to achieve the desired amount of vacancies by removing a preselected amount of the zinc.
15. The method of claim 1, wherein the initial solid alloy material is an ingot, a shape casting, a wrought product, or an additively manufactured product.
16. The method of claim 1, wherein the final solid material is an ingot, a shape casting, a wrought product, or an additively manufactured product.
17. A solid alloy material comprising Al, Ti and a predetermined amount of vacancies therein.
18. A solid alloy material comprising Al, Ti, Zn, and a predetermined amount of vacancies therein.
19. The solid alloy materials of either claim 17 or 18, wherein the vacancies are associated with removed zinc atoms.
20. The solid alloy material of claim 19, wherein the solid material comprises a homogenous distribution of the vacancies.
21. The solid alloy material of any of claims 17-20, wherein the average size of the vacancies is not greater than 5 microns.
22. The solid alloy material of any of claims 17-21, wherein at least 90 vol. % of the vacancies are wholly contained within the solid material.
23. The solid alloy material of any of claims 17-22, wherein the solid material is crystalline and comprises an fee structure.
24. A hydrogen storage apparatus comprising the solid alloy material of any of claims 17-23.
25. A fuel cell comprising the hydrogen storage apparatus of claim 24.
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