WO2012148471A1 - Procédés de métallurgie des poudres pour la production de titane à grains fins et ultrafins et alliages de titane associés - Google Patents

Procédés de métallurgie des poudres pour la production de titane à grains fins et ultrafins et alliages de titane associés Download PDF

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Publication number
WO2012148471A1
WO2012148471A1 PCT/US2011/061685 US2011061685W WO2012148471A1 WO 2012148471 A1 WO2012148471 A1 WO 2012148471A1 US 2011061685 W US2011061685 W US 2011061685W WO 2012148471 A1 WO2012148471 A1 WO 2012148471A1
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Prior art keywords
titanium metal
titanium
sintering
sintered
metal alloy
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PCT/US2011/061685
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English (en)
Inventor
Zhigang Zak Fang
Hongtao Wang
Pei Sun
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The University Of Utah
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Publication of WO2012148471A1 publication Critical patent/WO2012148471A1/fr
Priority to US14/152,787 priority Critical patent/US9816157B2/en

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • 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
    • C22C1/045—Alloys based on refractory metals
    • C22C1/0458—Alloys based on titanium, zirconium or hafnium
    • 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

Definitions

  • the technology is generally related to the production of titanium metal and titanium metal alloys.
  • Powder metallurgy has been regarded as a viable and promising approach for reducing the cost of Ti fabrication because of its near-net-shape capability and potentially melt- less nature of the process.
  • powder metallurgy approaches for making PM titanium products There are generally two kinds of powder metallurgy approaches for making PM titanium products: blended elemental (BE) method and pre-alloyed (PA) method.
  • BE method in general refers to the pressing and sintering of blended elemental powders. Sintering is generally carried out under vacuum.
  • the PA method refers to sintering pre-alloyed powders, typically produced using gas atomization or plasma rotating electrode techniques. Since pre-alloyed powders have high hardness, and, therefore, poor press-ability if compacted using conventional uni-axial cold pressing methods, pre-alloyed powders are usually
  • the as-sintered microstructure for Ti-6A1-4V consists of coarse Widmanstatten lamellar alpha plate colony structures which have a coarse microstructure that is not optimum with respect to tensile or fatigue strength.
  • the as-sintered coarse microstructures can be refined only by post-sintering thermal mechanical working and heat treatments, which, once again, increase the cost of PM Ti parts, reducing the economic benefits of PM Ti.
  • a microstructure engineering approach is provided to produce PM titanium alloys with a fine grain microstructure, and other desired microstructure features. Such features lead to improved mechanical properties, without having to rely on subsequent processing steps, such as thermal mechanical working, after sintering
  • a process includes sintering TiH 2 or Ti metal powders in a controlled atmosphere, and at elevated temperature, to form a sintered titanium material containing hydrogen; cooling the sintered titanium material; holding the sintered titanium material at a hold temperature and a hold time sufficient for eutectoid decomposition of the sintered titanium material; and heating the sintered titanium material under vacuum at a temperature which is less than that of the sintering temperature; where the controlled atmosphere includes a mixture of hydrogen and an inert gas.
  • the sintering also includes sintering the TiH 2 in the presence of an alloying additive.
  • the inert gas includes helium, argon, or xenon.
  • the sintered titanium material may include titanium solid solutions phases: ⁇ , ⁇ and ⁇ phases.
  • the titanium metal or the titanium metal alloy obtained from the process may have a grain size of less than 10 ⁇ .
  • the titanium metal or the titanium metal alloy obtained from the process has a grain size of from about 10 nm to about 10 ⁇ .
  • the titanium metal or the titanium metal alloy obtained from the process has a grain size of from about 10 ⁇ to about 100 ⁇ .
  • the titanium metal or the titanium metal alloy may have a density greater than 95%. In some such
  • the titanium metal or the titanium metal alloy has a density of greater than 98%.
  • the titanium metal or the titanium metal alloy may have an oxygen content of less than 0.5 wt%.
  • the titanium metal or the titanium metal alloy has an oxygen content of from about 0.001 wt% to about 0.3 wt%.
  • the TiH 2 or Ti metal may be provided as a powder. In some such embodiments, the powder has an initial size from about 20 mesh to about 600 mesh.
  • the elevated temperature is from about 1000°C to about 1500°C.
  • the sintering is conducted from about 1 hour to about 240 hours.
  • the re-heating for eutectic decomposition is conducted from about 200°C to about 900°C, below ⁇ -phase transition temperature which is a function of alloy compositions.
  • the re-heating for eutectic decomposition is conducted from about 1 hour to about 24 hours.
  • the hydrogen to inert gas ratio in the controlled atmosphere is from 1 : 100 to 1 : 1.
  • the hold temperature for dehydrogenation in vacuum is from about 300°C to about 800 °C below the ⁇ -phase transition temperature. In any of the above embodiments, the hold time is conducted from about 2 hours to about 100 hours depending on the size of the components.
  • the process may be void of mechanical processing steps after sintering. As used herein, the term "mechanical processing steps" refers to forging, rolling, extrusion, drawing, swaging, and the like as known in the art.
  • the process may also include powder milling of the TiH 2 or Ti and the alloying additive, if present. In any of the above embodiments, the process also includes blending of the TiH 2 and/or Ti and the alloying additive, if present.
  • a material that includes any of the titanium metal or titanium metal alloys produced by any of the above processes.
  • the material may be a commercially pure titanium (CP-Ti).
  • CP-Ti is a term that is widely used in the art. CP-Ti is classified on scale of Grade 1 to 5, each level of the scale being based upon the oxygen content and/or alloying according to industry standards.
  • the material may be a commercial alloy of Ti. In one embodiment, the material is Ti-6A1-4V.
  • FIG. 1 is a graphical representation of an illustrative temperature vs. time cycle for titanium production, according to one embodiment.
  • FIG. 2 is an SEM micrograph illustrating the ultrafme microstructure of a Ti-6A1-
  • FIG. 3 illustrates a shrinkage curve of controlled hydrogen sintering of TiH 2 -AlV, according to the examples.
  • FIG. 4 is a group of SEM and TEM micrographs showing the microstructures produced by vacuum sintering of TiH 2 (FIG. 4A: SEM image), hydrogen sintering of TiH 2 (FIG. 4B: SEM image; FIG. 4C: TEM image), typical wrought processes (FIG. 4D: SEM image) and vacuum sintering of Ti metal powder (FIG. 4E: SEM image), according to the examples.
  • a process is provided for producing Ti and Ti alloys with near- full density, and fine or ultrafme grain sizes in an as-sintered state without, or with only minimal, post-sintering processing.
  • the ultrafme grain and near-porosity-free microstructure of the resulting material allows for flexibility in custom engineering of the microstructure of Ti materials.
  • the near porosity-free ultrafme microstructure is achieved by sintering under atmospheres with a controlled partial pressure of H 2 at high temperatures, followed by subjecting the material to eutectoid transformation and dehydrogenation at moderate temperatures.
  • the thermal cycle is designed such that the phase transformations during the eutectoid reaction and dehydrogenation are controlled so that they lead to ultrafme microstructure features without significant grain growth.
  • the process provides for powder compacts of titanium with alloying elements
  • H 2 is controlled during sintering.
  • the present process controls the partial pressure of H 2 in the atmosphere, and hydrogen content in the powder throughout the sintering process.
  • the process includes three primary steps: (1) ⁇ - ⁇ ( ⁇ ) densification, (2) eutectoid decomposition, and (3) dehydrogenation in vacuum.
  • FIG. 1 illustrates the process in a graph of temperature v. time.
  • FIG. 1 illustrates that ramping up and down of the temperature in each of the steps and the hold periods that may be used. Note that the steps may be completely separated as separate processes conducted in different runs, or as a single integrated continuous run.
  • the process maintains sintering in ⁇ -Ti phase region.
  • Self-diffusion of the titanium in the ⁇ -Ti phase is significantly faster than in the a-Ti phase, and a solid solution of hydrogen atoms in titanium can reduce the activation energy of Ti self-diffusion due to the decrease of Ti-Ti bonding strength. It is believed that each of these effects help to achieve full densification during ⁇ - ⁇ ( ⁇ ) sintering.
  • the densified samples are cooled in a controlled H 2 atmosphere to temperatures below the eutectoid reaction, and holding the samples at this temperature for a period of time to complete the eutectoid reaction.
  • the term "eutectoid reaction” refers to the formation of new phases (a-Ti(H) + 5-TiH x ) that precipitate in the interior of the ⁇ - ⁇ ( ⁇ ) grains.
  • the coarse ⁇ - ⁇ ( ⁇ ) grains break into finely dispersed (a-Ti(H) + ⁇ - ⁇ ( ⁇ )+ ⁇ - ⁇ ⁇ ) grains, thereby refining the microstructure.
  • the hydrogen atoms in the titanium are removed by vacuum annealing.
  • the phase transformations during dehydrogenation further refine and modify the microstructure.
  • the hydrogen can be removed to a level much lower than allowable levels according to ASTM standards (150 ppm).
  • ASTM standards 150 ppm
  • the residual hydrogen content after vacuum sintering of TiH 2 or thermohydrogen processing (THP) can be as low as 10 ppm, which is not detrimental to the mechanical properties of titanium materials.
  • a process of powder metallurgy technology includes producing titanium metal and titanium metal alloys.
  • the process may be used to produce low-cost Ti alloys that are nearly fully dense (>99%CP-Ti, >98%Ti-6Al-4V) Ti materials and which have a fine, and/or ultrafme, grain size
  • the processes also provide for sintering titanium metal in hydrogen to produce near full dense titanium materials.
  • ultrafme grain sizes on the microscopic scale provide for high strength and ductility in the macroscale materials.
  • the process employs a microstructure engineering approach of controlling densification and phase transformation processes during sintering of titanium hydride (TiH 2 ) and/or Ti metal and alloying powders to form a sintered titanium material.
  • the process includes sintering blended powder of TiH 2 and/or Ti metal and alloying powders in a controlled atmosphere with a partial pressure of hydrogen (H 2 ) gas, to form a sintered titanium material containing hydrogen.
  • the controlled atmosphere may also contain an inert gas such as helium, argon, or xenon.
  • blended powder under the partial hydrogen pressure, blended powder sinters to near full density with a microstructure having one, two, or three phases including alpha (a), delta ( ⁇ ) and beta ( ⁇ ) phases after cooling to room temperature. After cooling, the sintered titanium material is then re-heated under vacuum to dehydrogenate.
  • the material is then re-cooled to form a titanium metal alloy with a microstructure having alpha (a) and beta ( ⁇ ) phases.
  • the sintering in the controlled atmosphere, eutectoid decomposition, and the dehydrogenation under vacuum, can be three separate processes, or they can be integrated in a single process.
  • the first and second step may be processed in sequence with the third step following later, or the first step may be completed with the second and third steps being processed together later.
  • the single, integrated process of all three steps includes sintering blended powders of TiH 2 and alloying powders in a controlled atmosphere with a partial pressure of hydrogen (H 2 ) gas, cooling and holding for euctectoid decomposition, and then switching the atmosphere condition to vacuum, or very low pressure, conditions at certain temperatures during the cooling step of the sintering process.
  • H 2 hydrogen
  • near full density refers to a minimization of porosity in the material, such that if full density were achieved, the density of the bulk material would be equal to that of the theoretical density of the material.
  • near full density refers to the material having a relative density of greater than 98%.
  • full density refers to the material having a relative density of greater than 99%.
  • the titanium metal or the titanium metal alloy has a relative density greater than 97%. In other embodiments, the titanium metal or the titanium metal alloy has a near full density. In other embodiments, the titanium metal or the titanium metal alloy has a full density.
  • a-phase refers to a hexagonal close-packed (HCP) solid solution of Ti with alloying elements.
  • the a-phase may or may not contain some hydrogen.
  • ⁇ - phase refers to a face-centered cubic (FCC) titanium hydride, TiH x , where x varies from 1.5 to 2, at room temperature.
  • FCC face-centered cubic
  • BCC body-centered cubic
  • the definitions of the phases are further illustrated by the phase diagrams of Ti-H, and Ti-6A1-4V-H (ASM Handbook, Vol 3, p238, 1992). It should be noted that the phase diagrams of a titanium alloy with hydrogen vary considerably with the exact composition of the alloy. Therefore, the exact temperatures and time of sintering, isothermal holding for eutectoid transformation, and dehydrogenation will all vary accordingly.
  • the sintering is conducted at a temperature from about 1100°C to about 1500°C to form a ⁇ - ⁇ ( ⁇ ) densified material.
  • the sintering is also conducted for a time period sufficient to gain near full density.
  • the sintering time may vary from about 30 minutes to about 30 hours.
  • the sintering is performed from about 1 hour to 24 hours.
  • the sintering may be conducted in any chamber in which the temperature and atmosphere may be controlled.
  • the sintering may be conducted in a furnace which is capable of attaining a working temperature of up to 1500°C or even higher, is capable of being used under vacuum, and is capable of using gases such as hydrogen, argon, nitrogen, and the like, or a mixture of any two or more such gases.
  • the heating elements of the furnace may be made of those as are known in the art, including, but not limited to, tungsten or molybdenum mesh, silicon carbide, or M0S1 2 .
  • the ⁇ - ⁇ ( ⁇ ) densified material is held at a temperature sufficient for the above-described decomposition to take place and form a eutectoid decomposed material.
  • the temperature may range from about 200°C to about 800°C depending on exact alloy compositions. In some embodiments, the temperature ranges from about 500°C to about 700°C for Ti-6A1-4V alloy and 150°C to about 300°C for CP- Ti.
  • the time period for eutectoid decomposition is sufficient for the process to proceed sufficiently toward completion.
  • the temperature may be held constant, or nearly constant, from about 10 minutes to about 12 hours. In some embodiments, the temperature may be held constant, or nearly constant, from about 30 minutes to about 6 hours.
  • the material is re -heated to a temperature from about 500°C to about 900°C under a vacuum. At this temperature, the sintered material releases the hydrogen by a process called dehydrogenation, and the material may then form the fine grain microstructure.
  • the material is a Ti-6A1-4V alloy
  • such fine grain microstructure includes both a-phases and ⁇ -phases.
  • the re-heating of the material may be conducted for a time period sufficient to reduce hydrogen content in materials to less than 150 ppm.
  • the reheating- dehydrogenation process is believed to decompose the ⁇ - phase and release the hydrogen in the material. During the reheating process, the ⁇ - phase transforms to a ⁇ + ⁇ phase mixture.
  • Hydrogen then diffuses through the material to the surface, where it escapes as hydrogen gas.
  • the time of the reheating process may vary depending on the size of the specimen, or the components used.
  • the reheating process may be conducted for from 1 hour to about 100 hours, at the temperature.
  • the actual time required is governed by the law of diffusion.
  • the re -heating is performed from about 10 to 24 hours.
  • dehydrogenation may be conducted in the same chamber as the initial sintering, or in a separate furnace chamber in which the temperature and atmospheric pressure may be controlled.
  • the TiH 2 is provided as a powder for the sintering step.
  • the powder may have a size from about 20 mesh to about 600 mesh. In one embodiment, the powder has a size of from about 100 mesh to about 400 mesh. In one embodiment, the powder has a size of about -200 to +325 mesh. In another embodiment, the powder has a size of about 40 mesh.
  • the coarser the initial powder the lower the final oxygen content of the material.
  • coarse powders are very difficult to consolidate, and also lead to coarse final microstructure. In contrast, fine Ti metal powders are prone to oxygen contamination.
  • the present technology allows for use of a coarse TiH 2 powder as the starting raw material, thereby making it easier to control oxygen content in the subsequent powder pressing, forming, sintering, and dehydrogenation steps, while coarse TiH 2 powder poses few difficulties in densification to near full density provided that proper powder processing and compaction techniques are used.
  • the use of coarse powders does not lead to coarse final grain microstructure because of the controlled stages of densification and phase transformation.
  • the grain sizes of the final material do not depend as much on the initial particle size of the powder as does the titanium metal powder, but rather the grain size is primarily a function of the kinetics and temperature versus time profiles of both the densification and the dehydrogenation steps.
  • the materials prepared by the above processes are achieved at lower cost because of the high yield of the processes, fewer processing steps, and lower energy consumption, compared to materials produced by traditional wrought alloy methods.
  • the traditional wrought alloy methods refers to the manufacturing process by melting, casting, hot working, cold working and machining.
  • the materials prepared by the presently described processes have fine grain sizes, and thus exhibit equivalent or superior mechanical properties to traditionally wrought alloys.
  • the instant materials have lower oxygen content than equivalent titanium materials prepared using traditional powder metallurgy approaches, and are substantially free of impurities.
  • the titanium metal or titanium metal alloy prepared using the above process has a grain size of less than 100 ⁇ .
  • the titanium metal or titanium metal alloy prepared using the above process has a grain size of less than 5 ⁇ . In other embodiments, the titanium metal or the titanium metal alloy has a grain size of from about 10 nm to about 10 ⁇ . In other embodiments, the titanium metal or the titanium metal alloy has a grain size of from about 10 ⁇ to about 100 ⁇ .
  • the titanium metal or titanium metal alloy has an oxygen content of less than 0.5 wt%. In other embodiments, the titanium metal or titanium metal alloy has an oxygen content of less than 0.2 wt%. In other embodiments, the titanium metal or titanium metal alloy has an oxygen content of from about 0.001 wt% to about 0.3 wt%.
  • mechanical process steps are those steps where the material is deliberately deformed plastically at either elevated (thermal mechanical or hot working) or room temperatures (cold working). After the plastic deformation of cold working, or during hot working the microstructure of the material is transformed at elevated temperatures via recrystallization to achieve desired microstructure. The desired fine grain microstructure is formed in situ during the integrated densification- dehydrogenation process. In some cases, thermal mechanical working may be done to further enhance the properties.
  • a titanium metal or titanium metal alloy produced by any of the above processes is provided.
  • the titanium metal or titanium metal alloy may have a relative density of 98 % or greater.
  • the titanium metal or titanium metal alloy has a relative density of 99 % or greater.
  • the titanium metal or titanium metal alloy has a relative density of from about 99 % to about 99.9%.
  • the titanium metal or titanium metal alloy produced by any of the above processes may have a grain size of less than 100 ⁇ . In some embodiments, the titanium metal or titanium metal alloy produced by any of the above processes has a grain size of less than 5 ⁇ .
  • the titanium metal or the titanium metal alloy produced by any of the above processes has a grain size of from about 10 nm to about 10 ⁇ . In other embodiments, the titanium metal or the titanium metal alloy produced by any of the above processes has a grain size of from about 10 ⁇ to about 100 ⁇ .
  • the titanium metal or titanium metal alloy produced by the any of the above processes may have an oxygen content of less than 0.5 wt%. In other embodiments, the titanium metal or titanium metal alloy has an oxygen content of less than 0.2 wt%. In other embodiments, the titanium metal or titanium metal alloy has an oxygen content of from about 0.001 wt% to about 0.3 wt%.
  • the titanium metal or titanium metal alloy materials above may find utility in any of a number of applications where titanium and its alloys are currently used, or will be used.
  • the materials may be used in, but not limited to, automobile parts, biomedical implants, medical surgical tools, aircraft equipment, diving equipment, oil field equipment, sports equipment, chemical equipment, food processing equipment, among others.
  • Example 1 Commercial TiH 2 powder (46.8750 g) and 60A1-40V alloy powder
  • a molybdenum crucible was used as the sample holder during sintering process.
  • the entire sintering process was conducted in a stream of high purity argon (purity> 99.999%, 0 2 % ⁇ 1 ppm, H 2 0 ⁇ 1 ppm) and hydrogen (purity> 99.999%, 0 2 % ⁇ 1 ppm, H 2 0 ⁇ 2 ppm) with a slightly positive pressure.
  • the flow rates of the argon and hydrogen were 1.8 L/min and 320 mL/min, respectively.
  • FIG. 2 is a photograph of the fine grain material produced.
  • the mean grain size of the ⁇ phases is about 0.5 ⁇ (bright spots), and the mean grain size of a phases is about 1-4 ⁇ (dark color) in as-dehydrogenated article.
  • the relative density of the material was 98.5%.
  • Example 2 Production of Ti-6A1-4V alloy.
  • Ti metal, TiH 2 , and Al-V master alloy powders were supplied by Reading Alloys. The powders were mixed according to compositions of Ti-6A1-4V alloy. Cylindrical powder compacts were made in a cold iso-static press (CIP) using 350 MPa pressure. Dimensions of the green compacts were approximately ⁇ 15 x L60 mm. The compacts were then subjected to sintering in either vacuum or partial hydrogen atmosphere. In the case of vacuum sintering, vacuum level was 10 "5 torr. In the case of atmospheric sintering, mixtures of H 2 with Ar were used. The atmosphere is slightly positive, meaning slightly higher than 1 atm.
  • FIG. 4 shows SEM (scanning electron microscope) micrographs of the as-sintered microstructures of both vacuum sintered (FIG. 4A) and those sintered in partial hydrogen (FIG. 4B).
  • the SEM micrographs show that the microstructures produced by these two processes are drastically different.
  • the specimen produced by vacuum sintering show typical coarse ( ⁇ + ⁇ ) lamellar microstructure (FIG. 4A: a in dark and ⁇ in bright contrast; ⁇ phase distributed at inter-granular a phases), which is the typical as-sintered microstructure of Ti-6A1-4V alloy by BE processes using Ti metal powder.
  • the specimen of sintered in hydrogen shows a clearly different microstructure.
  • the microstructure produced by the hydrogen sintering process consists of ultrafme broken-up ⁇ phases (bright) in the matrix of refined a phases (dark contrast) as shown in FIG. 4B.
  • the refined microstructure is further examined using a transmission electron microscope (TEM; FIG. 4C). Based on the SEM and TEM images, the mean grain size of ⁇ phases is about 0.5 ⁇ and the mean grain size of a phase is about 1 ⁇ .
  • hydrogen sintering refers to sintering in pure hydrogen gas or in a gas mixture that contains hydrogen.
  • FIG. 4 also compares the microstructure of hydrogen sintered Ti to typically annealed, wrought Ti-6A1-4V (FIG. 4D), and typical vacuum sintered Ti metallic powder (FIG. 4E).
  • the vacuum sintered TiH 2 powder is almost identical to that of vacuum sintered Ti metallic powder as it should be, albeit that the density of sintered TiH 2 is usually higher than that of sintered Ti under similar conditions.
  • the hydrogen-sintered Ti microstructure is finer. It should be noted that the microstructure of wrought materials can vary significantly depending on exact thermomechanical processing history.
  • microstructure produced by the above methods have many advantages over coarse lamellar structure of conventional sintered Ti materials, particularly with respect to mechanical properties.
  • the microstructure of materials produced and described above show that such refined microstructure leads to improved tensile and fatigue properties as compared to the coarse lamellar microstructure.
  • Evaluations of basic tensile mechanical properties were carried out and are present in Table 1.
  • Table 1 compares the tensile mechanical properties of the as-sintered, microstructured specimens produced herein (hydrogen-sintered) with ASTM standards as well as vacuum sintered Ti-6A1-4V.
  • Table 1 also shows the chemical analysis of the as-sintered specimen. It illustrates that the oxygen content of these specimens is higher than that of ASTM standard for wrought material. The oxygen content can be further reduced by controlling powder material handling procedures. The hydrogen content in the finished specimen is sufficiently low to meet ASTM standards. Carbon and nitrogen content of the material also meet the ASTM standards.

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Abstract

L'invention concerne un procédé consistant à fritter TiH2 et/ou un métal de Ti dans une atmosphère contrôlée, à une température élevée, pour former un matériau de titane fritté ; à refroidir le matériau de titane fritté ; et à chauffer ledit matériau sous vide pour former un métal de titane ou un alliage de métaux de titane présentant des tailles de grain fines ou ultrafines ; l'atmosphère contrôlée contenant un mélange d'hydrogène et d'un gaz inerte.
PCT/US2011/061685 2011-04-26 2011-11-21 Procédés de métallurgie des poudres pour la production de titane à grains fins et ultrafins et alliages de titane associés WO2012148471A1 (fr)

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CN104388720A (zh) * 2014-10-30 2015-03-04 太仓市锦立得粉末冶金有限公司 一种粉末冶金产品含镍元素原材料的烧结工艺
CN104690272A (zh) * 2013-10-22 2015-06-10 波音公司 由至少一种元素金属粉末制造零件的方法
WO2015175726A1 (fr) * 2014-05-13 2015-11-19 University Of Utah Research Foundation Production de poudres métalliques sensiblement sphériques
FR3028784A1 (fr) * 2014-11-25 2016-05-27 Snecma Procede de fabrication de pieces tridimensionnelles en alliage d'aluminium et de titane, et aube de turbomachine obtenue par un tel procede
EP3103568A1 (fr) * 2015-06-08 2016-12-14 The Boeing Company Procédés de fabrication additive
EP3231536A1 (fr) * 2016-04-14 2017-10-18 Element 22 GmbH Procede de production metallurgie pulverulente de composants en titane ou en alliage de titane
WO2017202726A1 (fr) * 2016-05-24 2017-11-30 Arcam Ab Procédé de fabrication additive introduisant de l'hydrogène dans une chambre de construction
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