US20110103997A1 - Attrited titanium powder - Google Patents

Attrited titanium powder Download PDF

Info

Publication number
US20110103997A1
US20110103997A1 US12/955,646 US95564610A US2011103997A1 US 20110103997 A1 US20110103997 A1 US 20110103997A1 US 95564610 A US95564610 A US 95564610A US 2011103997 A1 US2011103997 A1 US 2011103997A1
Authority
US
United States
Prior art keywords
titanium
ligmental
alloy powder
apparent density
titanium alloy
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
Application number
US12/955,646
Inventor
Dariusz Kogut
Lance Jacobsen
William Ernst
Donn Armstrong
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to US12/955,646 priority Critical patent/US20110103997A1/en
Publication of US20110103997A1 publication Critical patent/US20110103997A1/en
Abandoned legal-status Critical Current

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1263—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction
    • C22B34/1268—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams
    • C22B34/1272—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams reduction of titanium halides, e.g. Kroll process
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/044—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by jet 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps

Definitions

  • This invention relates to a process whereby titanium and titanium alloy powders produced by the Armstrong process are inertly attrited to increase the apparent density, tap density and packing fraction while maintaining the powder chemistry for further processing to obtain high quality consolidated material.
  • the powder of the invention is produced by the Armstrong Process as previously disclosed in U.S. Pat. Nos. 5,779,761, 5,958,106 and 6,409,797, the entire disclosures of which are herein incorporated by reference.
  • agglomerated ligmental powder in which the average diameter of individual particles is less than five microns with a packing fraction in the range of from about 4% to about 11%.
  • Tap density is defined as the mass of a material that, upon packing in a precisely specified manner, fills a container to a specified volume, divided by the container volume.
  • Apparent density is defined as the weight per unit volume of a metal powder, in contrast to the weight per unit volume of the individual particles.
  • Packing fraction percentage is the tap density divided by the theoretical density and multiplied by 100.
  • Powder metallurgy processes include consolidation, molding and also several direct powder to mill shape processes such as powder extrusion and powder roll compaction.
  • a principal object of the present invention is to provide a titanium or titanium alloy powder having apparent densities and packing fractions greater than powder produced by the subsurface reduction of titanium tetrachloride vapor or mixtures of halide vapors in a flowing stream of alkali or alkaline earth metal or mixtures thereof.
  • Another object of the present invention is to provide powder with increased apparent density or packing fraction without significantly increasing the oxygen concentration or other contamination above as-produced powder.
  • Yet another objection of the present invention is to provide a method of increasing the apparent density of agglomerated ligmental titanium or titanium alloy powder produced by the subsurface reduction of titanium tetrachloride vapor or a mixture of titanium tetrachloride and other halide vapors in a flowing stream of alkali or alkaline earth metal or mixtures thereof having a first apparent density after distillation, comprising introducing the agglomerated ligmental titanium or titanium alloy powder into an attriting system, attriting the agglomerated ligmental titanium or titanium alloy powder until the powder becomes more spherical than ligmental and the first apparent density is increased by a factor of from about 3 to about 8.
  • Still another object of the present invention is to provide a method of increasing the apparent density of agglomerated ligmental titanium or titanium alloy powder produced by the subsurface reduction of titanium tetrachloride vapor or a mixture of titanium tetrachloride and other halide vapors in a flowing stream of sodium or alkaline earth metal or mixtures thereof having a first apparent density after distillation, comprising introducing the agglomerated ligmental titanium or titanium alloy powder into an attriting system, attriting the agglomerated ligmental titanium or titanium alloy powder in an inert atmosphere until the powder becomes more spherical than ligmental and the first apparent density is increased by a factor of from about 3 to about 8.
  • a final object of the present invention is to provide a method of increasing the apparent density of agglomerated ligmental titanium or titanium alloy powder produced by the subsurface reduction of titanium tetrachloride vapor or a mixture of titanium tetrachloride and other chloride vapors in a flowing stream of sodium or alkaline earth metal or mixtures thereof having a first apparent density after distillation, comprising introducing the agglomerated ligmental titanium or titanium alloy powder into an attriting system including a jet mill, attriting the agglomerated ligmental titanium or titanium alloy powder in an inert atmosphere in the jet mill until the powder becomes more spherical than ligmental and the first apparent density is increased by a factor of from about 3 to about 8.
  • FIG. 1 is a schematic of an attriting system for inertly attriting titanium and/or titanium alloy powder in a jet mill for subsequent consolidation and processing;
  • FIG. 2 is another schematic of an attriting system utilizing a jet mill
  • FIG. 3 is an SEM of agglomerated ligmental titanium powder with an as produced apparent density of 0.27 g/cc;
  • FIGS. 4( a ) and 4 ( b ) are SEMs of agglomerated ligmental titanium powder after milling with an apparent density of 1.13 g/cc;
  • FIGS. 5( a ) and 5 ( b ) are SEMs of agglomerated ligmental titanium powder after milling with an apparent density of 0.82 g/cc;
  • FIG. 6 is an SEM of agglomerated ligmental titanium powder with an as produced apparent density of 0.26 g/cc;
  • FIGS. 7( a )-( b ) are SEMs of agglomerated ligmental titanium powder after milling with an apparent density of 1.12 g/cc;
  • FIG. 8( a )-( b ) are SEMs of agglomerated ligmental titanium powder after milling with an apparent density of 0.68 g/cc.
  • an attriting system for titanium or titanium alloy powder is disclosed with powder being placed in an inert feeder containing an inert gas atmosphere.
  • the powder is fed into a jet mill that uses an inert gas to provide the milling action where it is attrited by impact between powder particles.
  • Attrited powder is carried out of the mill to a classifier by an inert gas stream.
  • the classifier removes the desired, densified powder from the gas stream, and possibly, recycles the entrained fines to the jet mill.
  • the densified powder may then pass directly to another process or container without ever making contact with oxygen that could increase the oxygen content of the powder.
  • the powder could be placed into an inerted container that could either be used directly in another process such as extrusion or roll compaction or be used to transport the powder to another process.
  • a variety of different mechanisms may be used to attritte powder such as but not limited to a ball mill, a jet mill, a high pressure water mill, a mechanco-fusion mill or a hammer mill all of which are included in the invention.
  • a jet mill is illustrated in FIGS. 1 and 2 is preferred and should be inerted to prevent undesirable oxygen pick-up. Any noble gas or nitrogen may be used, with nitrogen being preferred.
  • CP grade 2) Ti and (grade 5) 6:4 alloy are the most commonly used.
  • the milling of the titanium powder was done on two different Micron-Master jet mills, which are manufactured by the Jet Pulverizer Company.
  • the powder was fed into the mill through a rotating screw conveyor. From that conveyor, the powder flowed into the mill.
  • the compressed nitrogen entered the mill through two nuzzles and the two streams met together in the main chamber of the mill, where the actual milling takes place, as seen in FIGS. 1 and 2 .
  • the attrition study concentrated on improving the apparent density of the Armstrong Process powder while minimizing the subsequent oxygen pick up resulting from the jet milling process.
  • the purpose for improving the powder density was to make Armstrong powder more amenable to standard powder metallurgy practices. Typically, densities greater than 20% are desired.
  • ITP selected an opposed jet mill as the means to accomplish the attrition. Summary of results for the attrition study is shown in Table 3.
  • Scotts biometric density meter was used to determine the attrited batch sample's apparent densities and all samples showed considerable improvement.
  • the apparent densities ranged from approximately 6% for raw powder to 25% for milled powder.
  • the particle size analysis was preformed using Coulter LS 230 and showed as expected a decrease in particle size as the apparent density increased across all samples.
  • Inert gas fusion method was used to conduct the chemical analysis for oxygen, nitrogen, and hydrogen. The results showed an increase in oxygen level with dissimilar amounts for different samples. The large increase in oxygen could have resulted from not having a closed system during the milling process. Therefore, to optimize the milling process an inert feeding chamber and completing closed mill might minimize the oxygen increase.
  • the hydrogen level was virtually unchanged during the milling process.
  • SEM Scanning Electron Microscope
  • Table 4 shows additional results using 4 and 8 inch mills such as illustrated in FIGS. 1 and 2 .
  • the results showed that apparent densities increased from about 3 to about 8 times without significantly increasing the oxygen content of the agglomerated ligmental titanium powder produced by the Armstrong Process set forth in the incorporated patents and illustrated in the SEMs of FIGS. 3 and 6 .
  • FIGS. 4( a )-( b ), 5 ( a )-( b ), 7 ( a )-( b ) and 8 ( a )-( b ) are SEMs of powder milled and reported in Tables 1-3. Table 4 reports results of powders like FIGS. 3 and 6 milled as previously described herein.

Abstract

A method of increasing the apparent density of agglomerated ligmental titanium or titanium alloy powder produced by the subsurface reduction of titanium tetrachloride vapor or a mixture of titanium tetrachloride and other halide vapors in a flowing stream of alkali or alkaline earth metal or mixtures thereof having a first apparent density after distillation is disclosed. The agglomerated ligmental titanium or titanium alloy powder is introduced into an attriting system wherein the agglomerated ligmental titanium or titanium alloy powder is attrited until the powder becomes more spherical than ligmental and the first apparent density is increased by a factor of from about 3 to about 8. Inert atmosphere may be used to prevent unwanted oxygen contamination.

Description

    RELATED APPLICATIONS
  • This application is a continuation of U.S. Ser. No. 11/820,107 filed Jun. 18, 2007, which claims priority to U.S. Provisional Application Ser. No. 60/814,362 filed Jun. 16, 2006, the entire disclosures of both applications are hereby expressly incorporated herein by reference.
    • FIELD OF THE INVENTION
  • This invention relates to a process whereby titanium and titanium alloy powders produced by the Armstrong process are inertly attrited to increase the apparent density, tap density and packing fraction while maintaining the powder chemistry for further processing to obtain high quality consolidated material.
    • BACKGROUND OF THE INVENTION
  • The powder of the invention is produced by the Armstrong Process as previously disclosed in U.S. Pat. Nos. 5,779,761, 5,958,106 and 6,409,797, the entire disclosures of which are herein incorporated by reference.
  • Production of titanium powder by the Armstrong Process inherently produces agglomerated ligmental powder in which the average diameter of individual particles is less than five microns with a packing fraction in the range of from about 4% to about 11%. Tap density is defined as the mass of a material that, upon packing in a precisely specified manner, fills a container to a specified volume, divided by the container volume. Apparent density is defined as the weight per unit volume of a metal powder, in contrast to the weight per unit volume of the individual particles. Packing fraction percentage is the tap density divided by the theoretical density and multiplied by 100.
  • Many projected powder metallurgy uses of titanium and titanium alloy powders require a apparent density or packing fraction higher than the powder typically produced by the Armstrong Process. Increasing the apparent density or packing fraction of the powders produced by the Armstrong Process without significantly increasing oxygen concentration is important to future commercial success in the powder metallurgy field. Powder metallurgy processes include consolidation, molding and also several direct powder to mill shape processes such as powder extrusion and powder roll compaction.
    • SUMMARY OF THE INVENTION
  • Accordingly, a principal object of the present invention is to provide a titanium or titanium alloy powder having apparent densities and packing fractions greater than powder produced by the subsurface reduction of titanium tetrachloride vapor or mixtures of halide vapors in a flowing stream of alkali or alkaline earth metal or mixtures thereof.
  • Another object of the present invention is to provide powder with increased apparent density or packing fraction without significantly increasing the oxygen concentration or other contamination above as-produced powder.
  • Yet another objection of the present invention is to provide a method of increasing the apparent density of agglomerated ligmental titanium or titanium alloy powder produced by the subsurface reduction of titanium tetrachloride vapor or a mixture of titanium tetrachloride and other halide vapors in a flowing stream of alkali or alkaline earth metal or mixtures thereof having a first apparent density after distillation, comprising introducing the agglomerated ligmental titanium or titanium alloy powder into an attriting system, attriting the agglomerated ligmental titanium or titanium alloy powder until the powder becomes more spherical than ligmental and the first apparent density is increased by a factor of from about 3 to about 8.
  • Still another object of the present invention is to provide a method of increasing the apparent density of agglomerated ligmental titanium or titanium alloy powder produced by the subsurface reduction of titanium tetrachloride vapor or a mixture of titanium tetrachloride and other halide vapors in a flowing stream of sodium or alkaline earth metal or mixtures thereof having a first apparent density after distillation, comprising introducing the agglomerated ligmental titanium or titanium alloy powder into an attriting system, attriting the agglomerated ligmental titanium or titanium alloy powder in an inert atmosphere until the powder becomes more spherical than ligmental and the first apparent density is increased by a factor of from about 3 to about 8.
  • A final object of the present invention is to provide a method of increasing the apparent density of agglomerated ligmental titanium or titanium alloy powder produced by the subsurface reduction of titanium tetrachloride vapor or a mixture of titanium tetrachloride and other chloride vapors in a flowing stream of sodium or alkaline earth metal or mixtures thereof having a first apparent density after distillation, comprising introducing the agglomerated ligmental titanium or titanium alloy powder into an attriting system including a jet mill, attriting the agglomerated ligmental titanium or titanium alloy powder in an inert atmosphere in the jet mill until the powder becomes more spherical than ligmental and the first apparent density is increased by a factor of from about 3 to about 8.
  • The invention consists of certain novel features and a combination of parts hereinafter fully described, illustrated in the accompanying drawings, and particularly pointed out in the appended claims, it being understood that various changes in the details may be made without departing from the spirit, or sacrificing any of the advantages of the present invention.
    • BRIEF DESCRIPTION OF THE DRAWING
  • For the purpose of facilitating an understanding of the invention, there is illustrated in the accompanying drawing a preferred embodiment thereof, from an inspection of which, when considered in connection with the following description, the invention, its construction and operation, and many of its advantages should be readily understood and appreciated.
  • FIG. 1 is a schematic of an attriting system for inertly attriting titanium and/or titanium alloy powder in a jet mill for subsequent consolidation and processing;
  • FIG. 2 is another schematic of an attriting system utilizing a jet mill;
  • FIG. 3 is an SEM of agglomerated ligmental titanium powder with an as produced apparent density of 0.27 g/cc;
  • FIGS. 4( a) and 4(b) are SEMs of agglomerated ligmental titanium powder after milling with an apparent density of 1.13 g/cc;
  • FIGS. 5( a) and 5(b) are SEMs of agglomerated ligmental titanium powder after milling with an apparent density of 0.82 g/cc;
  • FIG. 6 is an SEM of agglomerated ligmental titanium powder with an as produced apparent density of 0.26 g/cc;
  • FIGS. 7( a)-(b) are SEMs of agglomerated ligmental titanium powder after milling with an apparent density of 1.12 g/cc; and
  • FIG. 8( a)-(b) are SEMs of agglomerated ligmental titanium powder after milling with an apparent density of 0.68 g/cc.
    •  DETAILED DESCRIPTION OF THE INVENTION
  • Referring to FIGS. 1 and 2, an attriting system for titanium or titanium alloy powder is disclosed with powder being placed in an inert feeder containing an inert gas atmosphere. The powder is fed into a jet mill that uses an inert gas to provide the milling action where it is attrited by impact between powder particles. Attrited powder is carried out of the mill to a classifier by an inert gas stream. The classifier removes the desired, densified powder from the gas stream, and possibly, recycles the entrained fines to the jet mill. The densified powder may then pass directly to another process or container without ever making contact with oxygen that could increase the oxygen content of the powder. For example, the powder could be placed into an inerted container that could either be used directly in another process such as extrusion or roll compaction or be used to transport the powder to another process.
  • A variety of different mechanisms may be used to attritte powder such as but not limited to a ball mill, a jet mill, a high pressure water mill, a mechanco-fusion mill or a hammer mill all of which are included in the invention. A jet mill is illustrated in FIGS. 1 and 2 is preferred and should be inerted to prevent undesirable oxygen pick-up. Any noble gas or nitrogen may be used, with nitrogen being preferred. Although various ASTM grades of Ti or its alloys may be used in this invention, CP (grade 2) Ti and (grade 5) 6:4 alloy are the most commonly used.
  • The milling of the titanium powder was done on two different Micron-Master jet mills, which are manufactured by the Jet Pulverizer Company. The powder was fed into the mill through a rotating screw conveyor. From that conveyor, the powder flowed into the mill. The compressed nitrogen entered the mill through two nuzzles and the two streams met together in the main chamber of the mill, where the actual milling takes place, as seen in FIGS. 1 and 2.
  • Three different batches of titanium powder were used to perform the attrition study. Batch R20.13, R20.14, and R20.15 was milled on an 8 inch mill to develop the appropriate jet milling parameters for the desired apparent density. Those parameters were subsequently used to scale up to an 12″ but a 24″ jet mill or larger could be employed. Table 1 summarizes the results from an 8″ mill test. Pre-sieving of the titanium powder was necessary in order to feed the powder into an 8″ mill, which can be eliminated by using a larger mill.
  • TABLE 1
    Parameters for an 8″ mill
    8″ mill
    Sample Size Feed rate Pressure
    Sample ID lb lb/hr psi
    R20.13 5.1 50 93
    R20.14 5.2 50 70
    R20.15 4.0 50 40
  • The feed rates and pressures determined from jet milling the powder on an 8″ mill were used to directly feed batch R19.28, R19.29, R22.23, and R22.24 into a 12″ mill. The parameters used for a 12″ mill are shown in Table 2.
  • TABLE 2
    Parameters for a 12″ mill
    12″ mill
    Sample Size Feed rate Pressure
    Sample ID lb lb/hr psi
    R19.28 7.1 110 93
    R19.29 12.5 110 30
    R22.23 11.0 110 93
    R22.24 10.8 110 30
  • The attrition study concentrated on improving the apparent density of the Armstrong Process powder while minimizing the subsequent oxygen pick up resulting from the jet milling process. The purpose for improving the powder density was to make Armstrong powder more amenable to standard powder metallurgy practices. Typically, densities greater than 20% are desired. Based on previous small scale milling experience with Armstrong powder, ITP selected an opposed jet mill as the means to accomplish the attrition. Summary of results for the attrition study is shown in Table 3.
  • TABLE 3
    Results of the attrition study
    Density Particle Size Analysis Chemical Analysis
    Apparent Tap Mean d50 d90 O2 N2 H2
    Sample ID g/cc % g/cc % um um um % % %
    R20.12 0.26 5.73 0.29 6.39 Raw powder (not milled) 0.234 0.021 0.0032
    R20.13 1.05 23.13 1.39 30.53 133.5 63.43 327.1 0.297 0.039 0.0025
    R20.14 0.95 20.93 1.25 27.62 139.1 60.88 383.9 0.361 0.05 0.0029
    R20.15 0.68 14.98 0.90 19.77 222.4 162.5 525.2 0.295 0.057 0.003
    R19.27 0.27 5.95 0.29 6.39 Raw powder (not milled) 0.175 0.003 0.0032
    R19.28 1.13 24.89 1.49 32.85  91.26 46.06 176.6 0.275 0.009 0.0038
    R19.29 0.82 18.06 1.08 23.84 187.8 102 386.2 0.238 0.01 0.0032
    R22.21 0.26 5.73 0.30 6.61 Raw powder (not milled) 0.143 0.009 0.0018
    R22.23 1.12 24.67 1.48 32.56 113.5 50.58 259  0.331 0.021 0.0045
    R22.24 0.68 14.98 0.90 19.77 240.5 200.4 473.1 0.256 0.009 0.0038
  • Scotts biometric density meter was used to determine the attrited batch sample's apparent densities and all samples showed considerable improvement. The apparent densities ranged from approximately 6% for raw powder to 25% for milled powder. The particle size analysis was preformed using Coulter LS 230 and showed as expected a decrease in particle size as the apparent density increased across all samples. Inert gas fusion method was used to conduct the chemical analysis for oxygen, nitrogen, and hydrogen. The results showed an increase in oxygen level with dissimilar amounts for different samples. The large increase in oxygen could have resulted from not having a closed system during the milling process. Therefore, to optimize the milling process an inert feeding chamber and completing closed mill might minimize the oxygen increase. The hydrogen level was virtually unchanged during the milling process. Nitrogen level for the powder samples after attrition did increase to some extent, but not enough to cause any problems in further processing of the powder. Scanning Electron Microscope (SEM) was used to evaluate the influence of jet milling on titanium powder particles. SEM's of batch samples R19 and R22 are shown in FIGS. 3, 4(a)(b), 5(a)-(b), 6, 7(a)-(b) and 8(a)-(b). The SEM's showed agglomerated ligmental that as the apparent density increased, the particles became more spherical in shape, which improved the apparent and tap densities.
  • TABLE 4
    JET PULVERIZER
    ATTRITION RESULTS
    4 inch mill Feed rate (PPH) Prssure (psi) d50/d100 (MICRON) PF (%) O2 tap density (g/cc) apparent density (g/cc)
    R7U3.10A 25 65 223/2000  20 0.329 0.908 0.69008
    R7U3.10B 8 120 25/1143 37 0.516 1.6798 1.276648
    R7U3.10C 5 120 18.5/282   45 0.666 2.043 1.55268
    R7U3.10E 20 110 45/2000 0.384
    R7U3.10D STARTING POWDER 5 0.296 0.227 0.19976
    4 inch mill Feed rate (PPH) Prssure (psi) d50/d90 (MICRON) PF (%) O2 tap density (g/cc) apparent density (g/cc)
    R6U2.15B STARTING POWDER 0.2
    R6U2.15B 20 110 39/92 25 0.37 1.135 0.8626
    R12U3.3 STARTING POWDER 0.266
    R12U3.3 20 110  48/155 27 0.39 1.2258 0.931608
    R7U3.10D STARTING POWDER 0.3
    R7U3.10D  5 130 21/75 40 0.6 1.816 1.38016
    8 inch mill Feed rate (PPH) Prssure (psi) d50/d90 (MICRON) PF (%) O2 tap density (g/cc) apparent density (g/cc)
    R15U2.06, R15U2.07 STARTING POWDER 0.22
    R15U2.06, R15U2.07 8 100 17.52/28.71 42 0.487 1.9068 1.449168
    R15U3.10, R15U3.11 STARTING POWDER 0.11
    R15U3.10, R15U3.11 7 110 20.65/33.08 41 0.395 1.8614 1.414664
    R15U3.13 STARTING POWDER 0.19
    R15U3.13 8 110 17/27 45 0.496 2.043 1.55268
  • Table 4 shows additional results using 4 and 8 inch mills such as illustrated in FIGS. 1 and 2. Here, the results showed that apparent densities increased from about 3 to about 8 times without significantly increasing the oxygen content of the agglomerated ligmental titanium powder produced by the Armstrong Process set forth in the incorporated patents and illustrated in the SEMs of FIGS. 3 and 6. FIGS. 4( a)-(b), 5(a)-(b), 7(a)-(b) and 8(a)-(b) are SEMs of powder milled and reported in Tables 1-3. Table 4 reports results of powders like FIGS. 3 and 6 milled as previously described herein.
  • For certain powder metallurgy, tap densities between about 20% to about 30% are preferred, but as illustrated in Tables 1-4, packing fractions of as produced powders (inherently in the range of from about 4% to about 11%) may be increased to at least 45%, see particularly Table 4. The jet mills were operated at various feed rates in pounds per hour (lb./hr) and at various pressures in pounds per square inch (psi). Pressure as low as 30 psi (Table 1) or up to 130 psi (Table 4) have been used and feed rates from 5 to 110 lbs/hr. have been used (Tables 1 and 4). Pressures and feed rates affect the increase in apparent density, tap density and packing fraction.
  • While there has been disclosed what is considered to be the preferred embodiment of the present invention, it is understood that various changes in the details may be made without departing from the spirit, or sacrificing any of the advantages of the present invention.

Claims (20)

1. A method of increasing the apparent density of agglomerated ligmental titanium or titanium alloy powder produced by the subsurface reduction of titanium tetrachloride vapor or a mixture of titanium tetrachloride and other halide vapors in a flowing stream of alkali or alkaline earth metal or mixtures thereof having a first apparent density after distillation, comprising:
introducing the agglomerated ligmental titanium or titanium alloy powder into an attriting system,
attriting the agglomerated ligmental titanium or titanium alloy powder until the powder becomes more spherical than ligmental and the first apparent density is increased by a factor of from about 3 to about 8.
2. The method of claim 1, wherein the attriting is performed in an inert atmosphere.
3. The method of claim 2, wherein the inert atmosphere includes argon.
4. The method of claim 2, wherein the inert atmosphere includes nitrogen.
5. The method of claim 1, wherein the attriting system includes at least one of a ball mill, a jet mill, a high pressure water mill, a mechanco-fusion mill or a hammer mill.
6. The method of claim 1, wherein the titanium or titanium alloy powder having a first apparent density has a first packing fraction in the range of from about 4% to about 11% and after attrition has a packing fraction in the range of from about 20% to about 45%.
7. The method of claim 6, wherein the packing fraction after attrition is in the range of from about 20% to about 30%.
8. A titanium or titanium alloy powder made according to the method of claim 1.
9. A titanium or titanium alloy powder made according to the method of claim 7.
10. A method of increasing the apparent density of agglomerated ligmental titanium or titanium alloy powder produced by the subsurface reduction of titanium tetrachloride vapor or a mixture of titanium tetrachloride and other halide vapors in a flowing stream of sodium or alkaline earth metal or mixtures thereof having a first apparent density after distillation, comprising
introducing the agglomerated ligmental titanium or titanium alloy powder into an attriting system,
attriting the agglomerated ligmental titanium or titanium alloy powder in an inert atmosphere until the powder becomes more spherical than ligmental and the first apparent density is increased by a factor of from about 3 to about 8.
11. The method of claim 10, wherein the inert atmosphere includes a noble gas and/or nitrogen.
12. The method of claim 10, wherein the inert atmosphere is nitrogen.
13. The method of claim 10, wherein the titanium alloy is substantially 6% Al and 4% V by weight with the balance titanium.
14. The method of claim 10, wherein the attriting system includes at least one of a ball mill, a jet mill, a high pressure water mill, a mechanco-fusion mill or a hammer mill.
15. A titanium or titanium alloy powder made according to the method of claim 10.
16. A titanium or titanium alloy powder made according to the method of claim 14.
17. A titanium alloy made according to the method of claim 13.
18. A method of increasing the apparent density of agglomerated ligmental titanium or titanium alloy powder produced by the subsurface reduction of titanium tetrachloride vapor or a mixture of titanium tetrachloride and other chloride vapors in a flowing stream of sodium or alkaline earth metal or mixtures thereof having a first apparent density after distillation, comprising
introducing the agglomerated ligmental titanium or titanium alloy powder into an attriting system including a jet mill,
attriting the agglomerated ligmental titanium or titanium alloy powder in an inert atmosphere in the jet mill until the powder becomes more spherical than ligmental and the first apparent density is increased by a factor of from about 3 to about 8.
19. The method of claim 18, wherein the jet mill is operated at a pressure of at least 70 psi.
20. The method of claim 18, wherein the jet mill is operated at a pressure of at least 90 psi.
US12/955,646 2006-06-16 2010-11-29 Attrited titanium powder Abandoned US20110103997A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US12/955,646 US20110103997A1 (en) 2006-06-16 2010-11-29 Attrited titanium powder

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US81436206P 2006-06-16 2006-06-16
US11/820,107 US20080031766A1 (en) 2006-06-16 2007-06-18 Attrited titanium powder
US12/955,646 US20110103997A1 (en) 2006-06-16 2010-11-29 Attrited titanium powder

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
US11/820,107 Continuation US20080031766A1 (en) 2006-06-16 2007-06-18 Attrited titanium powder

Publications (1)

Publication Number Publication Date
US20110103997A1 true US20110103997A1 (en) 2011-05-05

Family

ID=39029353

Family Applications (2)

Application Number Title Priority Date Filing Date
US11/820,107 Abandoned US20080031766A1 (en) 2006-06-16 2007-06-18 Attrited titanium powder
US12/955,646 Abandoned US20110103997A1 (en) 2006-06-16 2010-11-29 Attrited titanium powder

Family Applications Before (1)

Application Number Title Priority Date Filing Date
US11/820,107 Abandoned US20080031766A1 (en) 2006-06-16 2007-06-18 Attrited titanium powder

Country Status (1)

Country Link
US (2) US20080031766A1 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9421612B2 (en) 2014-05-13 2016-08-23 University Of Utah Research Foundation Production of substantially spherical metal powders
US10610929B2 (en) 2014-12-02 2020-04-07 University Of Utah Research Foundation Molten salt de-oxygenation of metal powders

Families Citing this family (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU686444B2 (en) * 1994-08-01 1998-02-05 Kroftt-Brakston International, Inc. Method of making metals and other elements
WO2004033736A1 (en) * 2002-10-07 2004-04-22 International Titanium Powder, Llc. System and method of producing metals and alloys
AU2003298572A1 (en) * 2002-09-07 2004-04-19 International Titanium Powder, Llc. Filter cake treatment method
UA79310C2 (en) * 2002-09-07 2007-06-11 Int Titanium Powder Llc Methods for production of alloys or ceramics with the use of armstrong method and device for their realization
JP2005538252A (en) * 2002-09-07 2005-12-15 インターナショナル・タイテイニアム・パウダー・リミテッド・ライアビリティ・カンパニー Method for separating Ti from Ti slurry
WO2004033737A1 (en) * 2002-10-07 2004-04-22 International Titanium Powder, Llc. System and method of producing metals and alloys
US20070180951A1 (en) * 2003-09-03 2007-08-09 Armstrong Donn R Separation system, method and apparatus
US20070017319A1 (en) 2005-07-21 2007-01-25 International Titanium Powder, Llc. Titanium alloy
CA2623544A1 (en) 2005-10-06 2007-04-19 International Titanium Powder, Llc Titanium or titanium alloy with titanium boride dispersion
US20080031766A1 (en) * 2006-06-16 2008-02-07 International Titanium Powder, Llc Attrited titanium powder
US7753989B2 (en) * 2006-12-22 2010-07-13 Cristal Us, Inc. Direct passivation of metal powder
US9127333B2 (en) * 2007-04-25 2015-09-08 Lance Jacobsen Liquid injection of VCL4 into superheated TiCL4 for the production of Ti-V alloy powder
US9555473B2 (en) * 2011-10-08 2017-01-31 The Boeing Company System and method for increasing the bulk density of metal powder
ITMI20120092A1 (en) 2012-01-26 2013-07-27 Micro Macinazione S A PHARMACO-CARRIER INCLUSION COMPOSITES PREPARED WITH MECHANICAL-CHEMICAL ACTIVATION PROCESS BY HIGH-ENERGY JET FLUID MILLS
RU2641428C1 (en) * 2016-11-18 2018-01-17 Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский государственный университет" (ТГУ, НИ ТГУ) Method of producing quasispherical particles of titanium
KR102273787B1 (en) 2018-10-22 2021-07-06 원진금속(주) Complex copper alloy comprising high entropy alloy and method for manufacturing the same
US20230166326A1 (en) * 2020-05-13 2023-06-01 Osaka Titanium Technologies Co., Ltd. Active metal particle surface modification method, and titanium particles or titanium alloy particles

Citations (95)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1771928A (en) * 1927-05-02 1930-07-29 Jung Hans Filter press
US2205854A (en) * 1937-07-10 1940-06-25 Kroll Wilhelm Method for manufacturing titanium and alloys thereof
US2607675A (en) * 1948-09-06 1952-08-19 Int Alloys Ltd Distillation of metals
US2647826A (en) * 1950-02-08 1953-08-04 Jordan James Fernando Titanium smelting process
US2823991A (en) * 1954-06-23 1958-02-18 Nat Distillers Chem Corp Process for the manufacture of titanium metal
US2827371A (en) * 1951-11-01 1958-03-18 Ici Ltd Method of producing titanium in an agitated solids bed
US2835567A (en) * 1954-11-22 1958-05-20 Du Pont Method of producing granular refractory metal
US2846304A (en) * 1953-08-11 1958-08-05 Nat Res Corp Method of producing titanium
US2846303A (en) * 1953-08-11 1958-08-05 Nat Res Corp Method of producing titanium
US2882143A (en) * 1953-04-16 1959-04-14 Nat Lead Co Continuous process for the production of titanium metal
US2882144A (en) * 1955-08-22 1959-04-14 Allied Chem Method of producing titanium
US2890112A (en) * 1954-10-15 1959-06-09 Du Pont Method of producing titanium metal
US2895823A (en) * 1956-03-20 1959-07-21 Peter Spence & Sons Ltd Method of further reducing the reaction products of a titanium tetrachloride reduction reaction
US2941867A (en) * 1957-10-14 1960-06-21 Du Pont Reduction of metal halides
US2944888A (en) * 1956-01-17 1960-07-12 Ici Ltd Manufacture of titanium
US3085871A (en) * 1958-02-24 1963-04-16 Griffiths Kenneth Frank Method for producing the refractory metals hafnium, titanium, vanadium, silicon, zirconium, thorium, columbium, and chromium
US3085872A (en) * 1958-07-01 1963-04-16 Griffiths Kenneth Frank Method for producing the refractory metals hafnium, titanium, vanadium, silicon, zirconium, thorium, columbium, and chromium
US3331666A (en) * 1966-10-28 1967-07-18 William C Robinson One-step method of converting uranium hexafluoride to uranium compounds
US3519258A (en) * 1966-07-23 1970-07-07 Hiroshi Ishizuka Device for reducing chlorides
US3650681A (en) * 1968-08-08 1972-03-21 Mizusawa Industrial Chem Method of treating a titanium or zirconium salt of a phosphorus oxyacid
US3825415A (en) * 1971-07-28 1974-07-23 Electricity Council Method and apparatus for the production of liquid titanium from the reaction of vaporized titanium tetrachloride and a reducing metal
US3867515A (en) * 1971-04-01 1975-02-18 Ppg Industries Inc Treatment of titanium tetrachloride dryer residue
US3943751A (en) * 1974-05-08 1976-03-16 Doryokuro Kakunenryo Kaihatsu Jigyodan Method and apparatus for continuously measuring hydrogen concentration in argon gas
US3966460A (en) * 1974-09-06 1976-06-29 Amax Specialty Metal Corporation Reduction of metal halides
US4007055A (en) * 1975-05-09 1977-02-08 Exxon Research And Engineering Company Preparation of stoichiometric titanium disulfide
US4009007A (en) * 1975-07-14 1977-02-22 Fansteel Inc. Tantalum powder and method of making the same
US4017302A (en) * 1976-02-04 1977-04-12 Fansteel Inc. Tantalum metal powder
US4070252A (en) * 1977-04-18 1978-01-24 Scm Corporation Purification of crude titanium tetrachloride
US4141719A (en) * 1977-05-31 1979-02-27 Fansteel Inc. Tantalum metal powder
US4149876A (en) * 1978-06-06 1979-04-17 Fansteel Inc. Process for producing tantalum and columbium powder
US4190442A (en) * 1978-06-15 1980-02-26 Eutectic Corporation Flame spray powder mix
US4331477A (en) * 1978-10-04 1982-05-25 Nippon Electric Co., Ltd. Porous titanium-aluminum alloy and method for producing the same
US4379718A (en) * 1981-05-18 1983-04-12 Rockwell International Corporation Process for separating solid particulates from a melt
US4425217A (en) * 1980-08-18 1984-01-10 Diamond Shamrock Corporation Anode with lead base and method of making same
US4432813A (en) * 1982-01-11 1984-02-21 Williams Griffith E Process for producing extremely low gas and residual contents in metal powders
US4445931A (en) * 1980-10-24 1984-05-01 The United States Of America As Represented By The Secretary Of The Interior Production of metal powder
US4454169A (en) * 1982-04-05 1984-06-12 Diamond Shamrock Corporation Catalytic particles and process for their manufacture
US4518426A (en) * 1983-04-11 1985-05-21 Metals Production Research, Inc. Process for electrolytic recovery of titanium metal sponge from its ore
US4519837A (en) * 1981-10-08 1985-05-28 Westinghouse Electric Corp. Metal powders and processes for production from oxides
US4521281A (en) * 1983-10-03 1985-06-04 Olin Corporation Process and apparatus for continuously producing multivalent metals
US4725312A (en) * 1986-02-28 1988-02-16 Rhone-Poulenc Chimie Production of metals by metallothermia
US4828008A (en) * 1987-05-13 1989-05-09 Lanxide Technology Company, Lp Metal matrix composites
US4830665A (en) * 1979-07-05 1989-05-16 Cockerill S.A. Process and unit for preparing alloyed and non-alloyed reactive metals by reduction
US4839120A (en) * 1987-02-24 1989-06-13 Ngk Insulators, Ltd. Ceramic material extruding method and apparatus therefor
US4844355A (en) * 1987-11-05 1989-07-04 Gte Products Corporation Apparatus for milling metal powder to produce high bulk density fine metal powders
US4897116A (en) * 1988-05-25 1990-01-30 Teledyne Industries, Inc. High purity Zr and Hf metals and their manufacture
US4902341A (en) * 1987-08-24 1990-02-20 Toho Titanium Company, Limited Method for producing titanium alloy
US4915729A (en) * 1985-04-16 1990-04-10 Battelle Memorial Institute Method of manufacturing metal powders
US4923577A (en) * 1988-09-12 1990-05-08 Westinghouse Electric Corp. Electrochemical-metallothermic reduction of zirconium in molten salt solutions
US4940490A (en) * 1987-11-30 1990-07-10 Cabot Corporation Tantalum powder
US4941646A (en) * 1988-11-23 1990-07-17 Bethlehem Steel Corporation Air cooled gas injection lance
US4985069A (en) * 1986-09-15 1991-01-15 The United States Of America As Represented By The Secretary Of The Interior Induction slag reduction process for making titanium
US5028491A (en) * 1989-07-03 1991-07-02 General Electric Company Gamma titanium aluminum alloys modified by chromium and tantalum and method of preparation
US5032176A (en) * 1989-05-24 1991-07-16 N.K.R. Company, Ltd. Method for manufacturing titanium powder or titanium composite powder
US5082491A (en) * 1989-09-28 1992-01-21 V Tech Corporation Tantalum powder with improved capacitor anode processing characteristics
US5176741A (en) * 1990-10-11 1993-01-05 Idaho Research Foundation, Inc. Producing titanium particulates from in situ titanium-zinc intermetallic
US5314658A (en) * 1992-04-03 1994-05-24 Amax, Inc. Conditioning metal powder for injection molding
US5409518A (en) * 1990-11-09 1995-04-25 Kabushiki Kaisha Toyota Chuo Kenkyusho Sintered powdered titanium alloy and method of producing the same
US5427602A (en) * 1994-08-08 1995-06-27 Aluminum Company Of America Removal of suspended particles from molten metal
US5498446A (en) * 1994-05-25 1996-03-12 Washington University Method and apparatus for producing high purity and unagglomerated submicron particles
USH1642H (en) * 1995-03-20 1997-04-01 The United States Of America As Represented By The Secretary Of The Navy Wear and impact tolerant plow blade
US5637816A (en) * 1995-08-22 1997-06-10 Lockheed Martin Energy Systems, Inc. Metal matrix composite of an iron aluminide and ceramic particles and method thereof
US5779761A (en) * 1994-08-01 1998-07-14 Kroftt-Brakston International, Inc. Method of making metals and other elements
US5897830A (en) * 1996-12-06 1999-04-27 Dynamet Technology P/M titanium composite casting
US5914440A (en) * 1997-03-18 1999-06-22 Noranda Inc. Method and apparatus removal of solid particles from magnesium chloride electrolyte and molten magnesium by filtration
US6010661A (en) * 1999-03-11 2000-01-04 Japan As Represented By Director General Of Agency Of Industrial Science And Technology Method for producing hydrogen-containing sponge titanium, a hydrogen containing titanium-aluminum-based alloy powder and its method of production, and a titanium-aluminum-based alloy sinter and its method of production
US6027585A (en) * 1995-03-14 2000-02-22 The Regents Of The University Of California Office Of Technology Transfer Titanium-tantalum alloys
US6040975A (en) * 1997-06-30 2000-03-21 Nec Corporation Tantalum powder and solid electrolytic capacitor using the same
US6180258B1 (en) * 1997-06-04 2001-01-30 Chesapeake Composites Corporation Metal-matrix composites and method for making such composites
US6193779B1 (en) * 1997-02-19 2001-02-27 H. C. Starck Gmbh & Co. Kg Tantalum powder, method for producing same powder and sintered anodes obtained from it
US6210461B1 (en) * 1998-08-10 2001-04-03 Guy R. B. Elliott Continuous production of titanium, uranium, and other metals and growth of metallic needles
US6238456B1 (en) * 1997-02-19 2001-05-29 H. C. Starck Gmbh & Co. Kg Tantalum powder, method for producing same powder and sintered anodes obtained from it
US20020050185A1 (en) * 1999-02-03 2002-05-02 Show A Cabot Supermetals K.K. Tantalum powder for capacitors
US6409797B2 (en) * 1994-08-01 2002-06-25 International Titanium Powder Llc Method of making metals and other elements from the halide vapor of the metal
US6502623B1 (en) * 1999-09-22 2003-01-07 Electrovac, Fabrikation Elektrotechnischer Spezialartikel Gesellschaft M.B.H. Process of making a metal matrix composite (MMC) component
US20030061907A1 (en) * 1994-08-01 2003-04-03 Kroftt-Brakston International, Inc. Gel of elemental material or alloy and liquid metal and salt
US6727005B2 (en) * 1999-12-20 2004-04-27 Centro Sviluppo Materiali S.P.A. Process for the manufacture of low-density components, having a polymer or metal matrix substrate and ceramics and/or metal-ceramics coating and low density components of high surface strength thus obtained
US6745930B2 (en) * 1999-11-17 2004-06-08 Electrovac, Fabrikation Elektrotechnischer Spezialartikel Ges.M.B.H. Method of attaching a body made of metal matrix composite (MMC) material or copper to a ceramic member
US20040123700A1 (en) * 2002-12-26 2004-07-01 Ling Zhou Process for the production of elemental material and alloys
US6861038B2 (en) * 1994-08-01 2005-03-01 International Titanium Powder, Llc. Ceramics and method of producing ceramics
US20050081682A1 (en) * 2002-09-07 2005-04-21 International Titanium Powder, Llc Method and apparatus for controlling the size of powder produced by the Armstrong Process
US6884522B2 (en) * 2002-04-17 2005-04-26 Ceramics Process Systems Corp. Metal matrix composite structure and method
US6902601B2 (en) * 2002-09-12 2005-06-07 Millennium Inorganic Chemicals, Inc. Method of making elemental materials and alloys
US20050150576A1 (en) * 2004-01-08 2005-07-14 Sridhar Venigalla Passivation of tantalum and other metal powders using oxygen
US6921510B2 (en) * 2003-01-22 2005-07-26 General Electric Company Method for preparing an article having a dispersoid distributed in a metallic matrix
US20060086435A1 (en) * 2002-11-20 2006-04-27 International Titanium Powder, Llc Separation system of metal powder from slurry and process
US7041150B2 (en) * 2002-09-07 2006-05-09 The University Of Chicago Preparation of alloys by the Armstrong method
US20060102255A1 (en) * 2004-11-12 2006-05-18 General Electric Company Article having a dispersion of ultrafine titanium boride particles in a titanium-base matrix
US20060107790A1 (en) * 2002-10-07 2006-05-25 International Titanium Powder, Llc System and method of producing metals and alloys
US20060123950A1 (en) * 2002-09-07 2006-06-15 Anderson Richard P Process for separating ti from a ti slurry
US20070017319A1 (en) * 2005-07-21 2007-01-25 International Titanium Powder, Llc. Titanium alloy
US20070079908A1 (en) * 2005-10-06 2007-04-12 International Titanium Powder, Llc Titanium boride
US20080031766A1 (en) * 2006-06-16 2008-02-07 International Titanium Powder, Llc Attrited titanium powder
US7351272B2 (en) * 2002-09-07 2008-04-01 International Titanium Powder, Llc Method and apparatus for controlling the size of powder produced by the Armstrong process
US20080152533A1 (en) * 2006-12-22 2008-06-26 International Titanium Powder, Llc Direct passivation of metal powder

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2005854A (en) * 1933-10-16 1935-06-25 Parker Meyer Dennis Company Sucker machine
US5211741A (en) * 1987-11-30 1993-05-18 Cabot Corporation Flaked tantalum powder
FI87896C (en) * 1990-06-05 1993-03-10 Outokumpu Oy Process for making metal powder
US7070252B2 (en) * 2003-08-20 2006-07-04 Xerox Corporation System and method for digital watermarking in a calibrated printing path

Patent Citations (99)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1771928A (en) * 1927-05-02 1930-07-29 Jung Hans Filter press
US2205854A (en) * 1937-07-10 1940-06-25 Kroll Wilhelm Method for manufacturing titanium and alloys thereof
US2607675A (en) * 1948-09-06 1952-08-19 Int Alloys Ltd Distillation of metals
US2647826A (en) * 1950-02-08 1953-08-04 Jordan James Fernando Titanium smelting process
US2827371A (en) * 1951-11-01 1958-03-18 Ici Ltd Method of producing titanium in an agitated solids bed
US2882143A (en) * 1953-04-16 1959-04-14 Nat Lead Co Continuous process for the production of titanium metal
US2846304A (en) * 1953-08-11 1958-08-05 Nat Res Corp Method of producing titanium
US2846303A (en) * 1953-08-11 1958-08-05 Nat Res Corp Method of producing titanium
US2823991A (en) * 1954-06-23 1958-02-18 Nat Distillers Chem Corp Process for the manufacture of titanium metal
US2890112A (en) * 1954-10-15 1959-06-09 Du Pont Method of producing titanium metal
US2835567A (en) * 1954-11-22 1958-05-20 Du Pont Method of producing granular refractory metal
US2882144A (en) * 1955-08-22 1959-04-14 Allied Chem Method of producing titanium
US2944888A (en) * 1956-01-17 1960-07-12 Ici Ltd Manufacture of titanium
US2895823A (en) * 1956-03-20 1959-07-21 Peter Spence & Sons Ltd Method of further reducing the reaction products of a titanium tetrachloride reduction reaction
US2941867A (en) * 1957-10-14 1960-06-21 Du Pont Reduction of metal halides
US3085871A (en) * 1958-02-24 1963-04-16 Griffiths Kenneth Frank Method for producing the refractory metals hafnium, titanium, vanadium, silicon, zirconium, thorium, columbium, and chromium
US3085872A (en) * 1958-07-01 1963-04-16 Griffiths Kenneth Frank Method for producing the refractory metals hafnium, titanium, vanadium, silicon, zirconium, thorium, columbium, and chromium
US3519258A (en) * 1966-07-23 1970-07-07 Hiroshi Ishizuka Device for reducing chlorides
US3331666A (en) * 1966-10-28 1967-07-18 William C Robinson One-step method of converting uranium hexafluoride to uranium compounds
US3650681A (en) * 1968-08-08 1972-03-21 Mizusawa Industrial Chem Method of treating a titanium or zirconium salt of a phosphorus oxyacid
US3867515A (en) * 1971-04-01 1975-02-18 Ppg Industries Inc Treatment of titanium tetrachloride dryer residue
US3825415A (en) * 1971-07-28 1974-07-23 Electricity Council Method and apparatus for the production of liquid titanium from the reaction of vaporized titanium tetrachloride and a reducing metal
US3943751A (en) * 1974-05-08 1976-03-16 Doryokuro Kakunenryo Kaihatsu Jigyodan Method and apparatus for continuously measuring hydrogen concentration in argon gas
US3966460A (en) * 1974-09-06 1976-06-29 Amax Specialty Metal Corporation Reduction of metal halides
US4007055A (en) * 1975-05-09 1977-02-08 Exxon Research And Engineering Company Preparation of stoichiometric titanium disulfide
US4009007A (en) * 1975-07-14 1977-02-22 Fansteel Inc. Tantalum powder and method of making the same
US4017302A (en) * 1976-02-04 1977-04-12 Fansteel Inc. Tantalum metal powder
US4070252A (en) * 1977-04-18 1978-01-24 Scm Corporation Purification of crude titanium tetrachloride
US4141719A (en) * 1977-05-31 1979-02-27 Fansteel Inc. Tantalum metal powder
US4149876A (en) * 1978-06-06 1979-04-17 Fansteel Inc. Process for producing tantalum and columbium powder
US4190442A (en) * 1978-06-15 1980-02-26 Eutectic Corporation Flame spray powder mix
US4331477A (en) * 1978-10-04 1982-05-25 Nippon Electric Co., Ltd. Porous titanium-aluminum alloy and method for producing the same
US4830665A (en) * 1979-07-05 1989-05-16 Cockerill S.A. Process and unit for preparing alloyed and non-alloyed reactive metals by reduction
US4425217A (en) * 1980-08-18 1984-01-10 Diamond Shamrock Corporation Anode with lead base and method of making same
US4445931A (en) * 1980-10-24 1984-05-01 The United States Of America As Represented By The Secretary Of The Interior Production of metal powder
US4379718A (en) * 1981-05-18 1983-04-12 Rockwell International Corporation Process for separating solid particulates from a melt
US4519837A (en) * 1981-10-08 1985-05-28 Westinghouse Electric Corp. Metal powders and processes for production from oxides
US4432813A (en) * 1982-01-11 1984-02-21 Williams Griffith E Process for producing extremely low gas and residual contents in metal powders
US4454169A (en) * 1982-04-05 1984-06-12 Diamond Shamrock Corporation Catalytic particles and process for their manufacture
US4518426A (en) * 1983-04-11 1985-05-21 Metals Production Research, Inc. Process for electrolytic recovery of titanium metal sponge from its ore
US4521281A (en) * 1983-10-03 1985-06-04 Olin Corporation Process and apparatus for continuously producing multivalent metals
US4915729A (en) * 1985-04-16 1990-04-10 Battelle Memorial Institute Method of manufacturing metal powders
US4725312A (en) * 1986-02-28 1988-02-16 Rhone-Poulenc Chimie Production of metals by metallothermia
US4985069A (en) * 1986-09-15 1991-01-15 The United States Of America As Represented By The Secretary Of The Interior Induction slag reduction process for making titanium
US4839120A (en) * 1987-02-24 1989-06-13 Ngk Insulators, Ltd. Ceramic material extruding method and apparatus therefor
US4828008A (en) * 1987-05-13 1989-05-09 Lanxide Technology Company, Lp Metal matrix composites
US4902341A (en) * 1987-08-24 1990-02-20 Toho Titanium Company, Limited Method for producing titanium alloy
US4844355A (en) * 1987-11-05 1989-07-04 Gte Products Corporation Apparatus for milling metal powder to produce high bulk density fine metal powders
US4940490A (en) * 1987-11-30 1990-07-10 Cabot Corporation Tantalum powder
US4897116A (en) * 1988-05-25 1990-01-30 Teledyne Industries, Inc. High purity Zr and Hf metals and their manufacture
US4923577A (en) * 1988-09-12 1990-05-08 Westinghouse Electric Corp. Electrochemical-metallothermic reduction of zirconium in molten salt solutions
US4941646A (en) * 1988-11-23 1990-07-17 Bethlehem Steel Corporation Air cooled gas injection lance
US5032176A (en) * 1989-05-24 1991-07-16 N.K.R. Company, Ltd. Method for manufacturing titanium powder or titanium composite powder
US5028491A (en) * 1989-07-03 1991-07-02 General Electric Company Gamma titanium aluminum alloys modified by chromium and tantalum and method of preparation
US5082491A (en) * 1989-09-28 1992-01-21 V Tech Corporation Tantalum powder with improved capacitor anode processing characteristics
US5176741A (en) * 1990-10-11 1993-01-05 Idaho Research Foundation, Inc. Producing titanium particulates from in situ titanium-zinc intermetallic
US5409518A (en) * 1990-11-09 1995-04-25 Kabushiki Kaisha Toyota Chuo Kenkyusho Sintered powdered titanium alloy and method of producing the same
US5314658A (en) * 1992-04-03 1994-05-24 Amax, Inc. Conditioning metal powder for injection molding
US5498446A (en) * 1994-05-25 1996-03-12 Washington University Method and apparatus for producing high purity and unagglomerated submicron particles
US20030061907A1 (en) * 1994-08-01 2003-04-03 Kroftt-Brakston International, Inc. Gel of elemental material or alloy and liquid metal and salt
US5779761A (en) * 1994-08-01 1998-07-14 Kroftt-Brakston International, Inc. Method of making metals and other elements
US6409797B2 (en) * 1994-08-01 2002-06-25 International Titanium Powder Llc Method of making metals and other elements from the halide vapor of the metal
US6861038B2 (en) * 1994-08-01 2005-03-01 International Titanium Powder, Llc. Ceramics and method of producing ceramics
US5427602A (en) * 1994-08-08 1995-06-27 Aluminum Company Of America Removal of suspended particles from molten metal
US6027585A (en) * 1995-03-14 2000-02-22 The Regents Of The University Of California Office Of Technology Transfer Titanium-tantalum alloys
USH1642H (en) * 1995-03-20 1997-04-01 The United States Of America As Represented By The Secretary Of The Navy Wear and impact tolerant plow blade
US5637816A (en) * 1995-08-22 1997-06-10 Lockheed Martin Energy Systems, Inc. Metal matrix composite of an iron aluminide and ceramic particles and method thereof
US5897830A (en) * 1996-12-06 1999-04-27 Dynamet Technology P/M titanium composite casting
US6193779B1 (en) * 1997-02-19 2001-02-27 H. C. Starck Gmbh & Co. Kg Tantalum powder, method for producing same powder and sintered anodes obtained from it
US6238456B1 (en) * 1997-02-19 2001-05-29 H. C. Starck Gmbh & Co. Kg Tantalum powder, method for producing same powder and sintered anodes obtained from it
US5914440A (en) * 1997-03-18 1999-06-22 Noranda Inc. Method and apparatus removal of solid particles from magnesium chloride electrolyte and molten magnesium by filtration
US6180258B1 (en) * 1997-06-04 2001-01-30 Chesapeake Composites Corporation Metal-matrix composites and method for making such composites
US6040975A (en) * 1997-06-30 2000-03-21 Nec Corporation Tantalum powder and solid electrolytic capacitor using the same
US6210461B1 (en) * 1998-08-10 2001-04-03 Guy R. B. Elliott Continuous production of titanium, uranium, and other metals and growth of metallic needles
US20020050185A1 (en) * 1999-02-03 2002-05-02 Show A Cabot Supermetals K.K. Tantalum powder for capacitors
US6689187B2 (en) * 1999-02-03 2004-02-10 Cabot Supermetals K.K. Tantalum powder for capacitors
US6010661A (en) * 1999-03-11 2000-01-04 Japan As Represented By Director General Of Agency Of Industrial Science And Technology Method for producing hydrogen-containing sponge titanium, a hydrogen containing titanium-aluminum-based alloy powder and its method of production, and a titanium-aluminum-based alloy sinter and its method of production
US6502623B1 (en) * 1999-09-22 2003-01-07 Electrovac, Fabrikation Elektrotechnischer Spezialartikel Gesellschaft M.B.H. Process of making a metal matrix composite (MMC) component
US6745930B2 (en) * 1999-11-17 2004-06-08 Electrovac, Fabrikation Elektrotechnischer Spezialartikel Ges.M.B.H. Method of attaching a body made of metal matrix composite (MMC) material or copper to a ceramic member
US6727005B2 (en) * 1999-12-20 2004-04-27 Centro Sviluppo Materiali S.P.A. Process for the manufacture of low-density components, having a polymer or metal matrix substrate and ceramics and/or metal-ceramics coating and low density components of high surface strength thus obtained
US6884522B2 (en) * 2002-04-17 2005-04-26 Ceramics Process Systems Corp. Metal matrix composite structure and method
US7041150B2 (en) * 2002-09-07 2006-05-09 The University Of Chicago Preparation of alloys by the Armstrong method
US7501089B2 (en) * 2002-09-07 2009-03-10 Cristal Us, Inc. Method and apparatus for controlling the size of powder produced by the Armstrong Process
US7351272B2 (en) * 2002-09-07 2008-04-01 International Titanium Powder, Llc Method and apparatus for controlling the size of powder produced by the Armstrong process
US20050081682A1 (en) * 2002-09-07 2005-04-21 International Titanium Powder, Llc Method and apparatus for controlling the size of powder produced by the Armstrong Process
US20060150769A1 (en) * 2002-09-07 2006-07-13 International Titanium Powder, Llc Preparation of alloys by the armstrong method
US20060123950A1 (en) * 2002-09-07 2006-06-15 Anderson Richard P Process for separating ti from a ti slurry
US6902601B2 (en) * 2002-09-12 2005-06-07 Millennium Inorganic Chemicals, Inc. Method of making elemental materials and alloys
US20060107790A1 (en) * 2002-10-07 2006-05-25 International Titanium Powder, Llc System and method of producing metals and alloys
US20060086435A1 (en) * 2002-11-20 2006-04-27 International Titanium Powder, Llc Separation system of metal powder from slurry and process
US7501007B2 (en) * 2002-11-20 2009-03-10 Cristal Us, Inc. Separation system of metal powder from slurry and process
US20040123700A1 (en) * 2002-12-26 2004-07-01 Ling Zhou Process for the production of elemental material and alloys
US6921510B2 (en) * 2003-01-22 2005-07-26 General Electric Company Method for preparing an article having a dispersoid distributed in a metallic matrix
US20050150576A1 (en) * 2004-01-08 2005-07-14 Sridhar Venigalla Passivation of tantalum and other metal powders using oxygen
US20060102255A1 (en) * 2004-11-12 2006-05-18 General Electric Company Article having a dispersion of ultrafine titanium boride particles in a titanium-base matrix
US20070017319A1 (en) * 2005-07-21 2007-01-25 International Titanium Powder, Llc. Titanium alloy
US20070079908A1 (en) * 2005-10-06 2007-04-12 International Titanium Powder, Llc Titanium boride
US20080031766A1 (en) * 2006-06-16 2008-02-07 International Titanium Powder, Llc Attrited titanium powder
US20080152533A1 (en) * 2006-12-22 2008-06-26 International Titanium Powder, Llc Direct passivation of metal powder

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9421612B2 (en) 2014-05-13 2016-08-23 University Of Utah Research Foundation Production of substantially spherical metal powders
US10130994B2 (en) 2014-05-13 2018-11-20 University Of Utah Research Foundation Production of substantially spherical metal powders
US10610929B2 (en) 2014-12-02 2020-04-07 University Of Utah Research Foundation Molten salt de-oxygenation of metal powders

Also Published As

Publication number Publication date
US20080031766A1 (en) 2008-02-07

Similar Documents

Publication Publication Date Title
US20110103997A1 (en) Attrited titanium powder
CA2233137C (en) Titanium-base powders and process for the production of the same
US20080226488A1 (en) Production of high-purity niobium monoxide and capacitor production therefrom
CN1863628A (en) Method for the production of fine metal powder, alloy powder and composite powder
US20120251416A1 (en) Process for recycling of tungsten carbide alloy
CN102534277A (en) New preparation method for coarse particles and super coarse particle hard alloy
US20200391294A1 (en) Metal-ceramic composite powders
EP3095540B1 (en) Method for preparing tantalum powder for high-reliability, high specific capacity electrolytic capacitor
CN107973299B (en) Production system and production process of high-temperature-base WC powder
US5902373A (en) Sponge-iron powder
JP2782665B2 (en) Method for producing titanium or titanium alloy powder
CN111589562A (en) Preparation method of oxygen-free high-purity arsenic powder
CN107867690A (en) A kind of high temperature base WC powder and its preparation method and application
US4054443A (en) Method of preparing iron powder
JP2821662B2 (en) Titanium-based powder and method for producing the same
US11313017B2 (en) Hard sintered body
JP2921790B2 (en) Method for producing low oxygen titanium material and low oxygen titanium dissolving material
US20230241726A1 (en) Hdh (hydride-dehydride) process for fabrication of braze alloy powders
CN110846546B (en) Method for preparing high-strength and high-toughness hard alloy by using pre-alloy powder
EP0801138A2 (en) Producing titanium-molybdenum master alloys
JPH04116161A (en) Titanium target material and production thereof
JP2987603B2 (en) Method for producing titanium-based powder
WO2019124325A1 (en) Titanium powder and method for producing same
CN117161388B (en) Low-oxygen-content titanium alloy powder and preparation method thereof
NO891629L (en) PROCEDURE FOR DISINTEGRATING FERROAL ALLOYS.

Legal Events

Date Code Title Description
STCB Information on status: application discontinuation

Free format text: ABANDONED -- FAILURE TO RESPOND TO AN OFFICE ACTION