US20110103997A1 - Attrited titanium powder - Google Patents
Attrited titanium powder Download PDFInfo
- 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
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.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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
- 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.
- 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.
- 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.
- 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.
- 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. - 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 ofFIGS. 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 likeFIGS. 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.
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)
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)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP3391461B2 (en) * | 1994-08-01 | 2003-03-31 | 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 | Manufacturing method of elemental materials |
US7621977B2 (en) * | 2001-10-09 | 2009-11-24 | Cristal Us, Inc. | System and method of producing metals and alloys |
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 |
US20050284824A1 (en) * | 2002-09-07 | 2005-12-29 | International Titanium Powder, Llc | Filter cake treatment apparatus and method |
AU2003273279B2 (en) * | 2002-09-07 | 2007-05-03 | Cristal Us, Inc. | Process for separating ti from a ti slurry |
AU2003270305A1 (en) * | 2002-10-07 | 2004-05-04 | 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)
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 |
US2882144A (en) * | 1955-08-22 | 1959-04-14 | Allied Chem | Method of producing titanium |
US2882143A (en) * | 1953-04-16 | 1959-04-14 | Nat Lead Co | Continuous process for the production of titanium metal |
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 |
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 |
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 |
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)
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 |
-
2007
- 2007-06-18 US US11/820,107 patent/US20080031766A1/en not_active Abandoned
-
2010
- 2010-11-29 US US12/955,646 patent/US20110103997A1/en not_active Abandoned
Patent Citations (99)
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)
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 | |
US7585486B2 (en) | Production of high-purity niobium monoxide and capacitor production therefrom | |
CA2233137C (en) | Titanium-base powders and process for the production of the same | |
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 | |
JP2006291306A (en) | Hopper for compounding titanium sponge and compounding method using the same | |
KR101917512B1 (en) | The method and apparatus for the fine powder | |
CN117161388B (en) | Low-oxygen-content titanium alloy powder and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
STCB | Information on status: application discontinuation |
Free format text: ABANDONED -- FAILURE TO RESPOND TO AN OFFICE ACTION |