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WO1997031738A1 - Materiaux poreux et procede de production associe - Google Patents

Materiaux poreux et procede de production associe Download PDF

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Publication number
WO1997031738A1
WO1997031738A1 PCT/US1997/002561 US9702561W WO9731738A1 WO 1997031738 A1 WO1997031738 A1 WO 1997031738A1 US 9702561 W US9702561 W US 9702561W WO 9731738 A1 WO9731738 A1 WO 9731738A1
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WO
WIPO (PCT)
Prior art keywords
organic
binder
degrees
slurry
impregnated
Prior art date
Application number
PCT/US1997/002561
Other languages
English (en)
Inventor
Robert D. Burns
Michael D. Mitchel
Sokhorn Eam
Original Assignee
Astro Met, Inc.
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 Astro Met, Inc. filed Critical Astro Met, Inc.
Priority to AU21901/97A priority Critical patent/AU2190197A/en
Publication of WO1997031738A1 publication Critical patent/WO1997031738A1/fr

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
    • F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
    • F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
    • F01N3/28—Construction of catalytic reactors
    • F01N3/2882—Catalytic reactors combined or associated with other devices, e.g. exhaust silencers or other exhaust purification devices
    • F01N3/2885—Catalytic reactors combined or associated with other devices, e.g. exhaust silencers or other exhaust purification devices with exhaust silencers in a single housing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/11—Making porous workpieces or articles
    • B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
    • B22F3/1137—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers by coating porous removable preforms
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N13/00—Exhaust or silencing apparatus characterised by constructional features ; Exhaust or silencing apparatus, or parts thereof, having pertinent characteristics not provided for in, or of interest apart from, groups F01N1/00 - F01N5/00, F01N9/00, F01N11/00
    • F01N13/009—Exhaust or silencing apparatus characterised by constructional features ; Exhaust or silencing apparatus, or parts thereof, having pertinent characteristics not provided for in, or of interest apart from, groups F01N1/00 - F01N5/00, F01N9/00, F01N11/00 having two or more separate purifying devices arranged in series
    • F01N13/0097—Exhaust or silencing apparatus characterised by constructional features ; Exhaust or silencing apparatus, or parts thereof, having pertinent characteristics not provided for in, or of interest apart from, groups F01N1/00 - F01N5/00, F01N9/00, F01N11/00 having two or more separate purifying devices arranged in series the purifying devices are arranged in a single housing
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
    • F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
    • F01N3/18—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control
    • F01N3/20—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control specially adapted for catalytic conversion ; Methods of operation or control of catalytic converters
    • F01N3/2006—Periodically heating or cooling catalytic reactors, e.g. at cold starting or overheating
    • F01N3/2013—Periodically heating or cooling catalytic reactors, e.g. at cold starting or overheating using electric or magnetic heating means
    • F01N3/2026—Periodically heating or cooling catalytic reactors, e.g. at cold starting or overheating using electric or magnetic heating means directly electrifying the catalyst substrate, i.e. heating the electrically conductive catalyst substrate by joule effect
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N2490/00—Structure, disposition or shape of gas-chambers
    • F01N2490/02—Two or more expansion chambers in series connected by means of tubes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T10/00—Road transport of goods or passengers
    • Y02T10/10—Internal combustion engine [ICE] based vehicles
    • Y02T10/12—Improving ICE efficiencies

Definitions

  • This invention relates to a method of producing porous materials and structures therefrom. More particularly, this invention relates to improvements in the production of porous materials, said improvement providing porous materials previously unavailable in the art and providing porous materials previously available in the art, but having improved quality and properties.
  • porous materials also know as foam materials
  • the porous materials produced in the art are in the family of ceramics, porous metals and porous metal compounds.
  • the porous or foam materials hereinafter referred to as porous materials, comprise an aggregation of closed cells resulting in a density of the porous material being less than that of the solid material.
  • the porous materials best developed are generally free of directionality and have significant structural strength.
  • the prior art teaches the use of various methods for the production of porous materials.
  • Porous metals having a plurality of randomly disbursed closed cells throughout a metal matrix are generally prepared by using a heat decomposable firming agent to generate the gas to form the cells.
  • the prior art teaches the use of various methods for the production of both ceramic and metallic porous materials.
  • Ball - U.S. Patent No. 3,111,396 teaches the method of making a porous material comprising the steps of impregnating a porous organic structure with a suspension of a powered material in a fluid, slowing drying the impregnated organic structure, heating the impregnated organic structure to decompose the organic structure and the fluid while closely retaining the shape and size of the original organic structure, and then heating the impregnated carbon-powered material structure to further join the powder into a continuous form.
  • Ball teaches the use of an inert atmosphere for refractory metals to complete the required heating steps and a reducing atmosphere in most other cases.
  • Patent No. 5,281,251 provides a method for producing metal foam by discharging gas bubbles into a molten metal composite to form a foam.
  • Baumeister, et al. - U.S. Patent No. 5,151,246 discloses a method for producing a foam metal body utilizing a gas-splitting propellant powder.
  • Ginn, et al - U.S. Patent No. 4,973,385 describes a method for producing foam metal through the introduction of gaseous bubbles within a mass of molten metal during foaming.
  • a second patent by Ginn, et al - U.S. Patent No. 5,112,697 further describes a method for producing foam metal in which gaseous bubbles are retained within a mass of molten metal during foaming. Additional methods disclosing the formation of foamed metal products are shown by Akiyama, et al - U.S. Patent No. 4,713, 277 and U.S. Patent No. 4,099,961 and Niebylski, et al - U.S. Patent No. 3,794,481 and Rock - U.S. Patent No. 3,782,919 and Rock - U.S. Patent
  • the prior art provides for the method of producing ceramic composite foams such as, Park, et al. - U.S. Patent No. 5,296,416, Park, et al - U.S. Patent No. 5,185,297, Kaettlitz, et al - U.S. Patent No. 5,169,542, Narumiya - U.S. Patent No. 4,302,502, Dore, et al - U.S. Patent No. 4,024,212, Kesten, et al - U.S. Patent No.
  • a primary objective of the present invention is to provide a new and novel method for producing porous metals.
  • a second object of the present invention is to provide porous metals, previously unavailable, having a high level and repeatability of quality.
  • Another object of the present invention is to provide a method for producing porous metals in a reduced number of steps as required by the prior art.
  • Yet another object of the present invention is to provide a method for producing porous metals with controlled pore size.
  • a further object of the present invention is to provide a method for producing porous metals using binders with little or no carbon residue.
  • Another object of the present invention is to provide a method of dry powder application to an organic precursor material that does not require the use of a binder-powder slurry.
  • a still further object of the present invention is to provide a method for producing porous metals utilizing vacuum techniques.
  • the prior art teaches the development of porous metal structures utilizing binders having a high carbon content, drying the sample slowly, heating the sample to a temperature capable of volatilizing the binder and foam but not destroying the structure, heating the structure to a second temperature to weakly bond the carbon-metal powder structure and heating the sample to a third temperature to sinter.
  • the prior art teaches the use of steam to be added to Hydrogen to reduce the amount of carbon present to give a strong final product.
  • the prior art work utilizes heating in a retort.
  • Ball teaches that the mechanical step of sintering the metal or further joining of other powders to produce a foamed product may not be effectively utilized in the production of certain porous materials such as columbium because of their affinity for carbon presenting the possibility of forming carbides which can be undesirable.
  • the present invention provides a method of producing a wide range of porous materials, particularly metals and metal compounds capable of producing porous metals with properties equal to the base or elemental metal.
  • the present invention provides a method of producing porous materials which eliminates the preparation and use of a binder-metal powder slurry required by the practice of the prior art.
  • one form of the present invention provides a method for producing a porous material including the steps of preparing a slurry comprising a binder and metal powder, impregnating a foam structure or organic material, curing the impregnated slurry with the foam structure, burning off the foam structure, decarburizing the resulting structure and sintering the resulting porous material product in vacuum.
  • the improved method of the present invention offers uses not previously available in the art.
  • Fig. 1 is a flow chart of the method of making porous material, utilized in the present invention.
  • Fig. 2 is a flow chart of an alternate method of making porous material, utilized in the present invention.
  • Fig. 3 is a sectional view of a porous material structure developed by application of the present invention.
  • the present invention overcomes the deficiencies previously discussed in the prior art and provides a method for producing porous metals which are fully sintered open cell reticulated foam-like structures.
  • a typical resulting open cell porous metal developed by the method of the present invention is shown in Fig. 3.
  • the present invention starts with a reticulated interconnected web precursor to which a slurry of binder and metal coating is applied or to which metal powder is applied by other means.
  • a thermal cycle or cycles is applied during which the precursor is removed and the coating sintered leaving a rigid structure. Part or all of the thermal cycles are to be conducted in a vacuum to overcome the prior art limitations.
  • the porous metal foam thus produced is 2% to 20% dense (98% to 80% porous) and is extremely lightweight.
  • the resultant porous metal product has a very high surface area when compared to that of a same sized, non porous shape. Approximately a 1500 times or greater surface area is provided.
  • the following examples are given as illustrative of the method of the present invention for preparing porous materials and are exemplary of the wide variety of modifications and variations of which the invention is capable. The examples are meant to be illustrations of, rather than limitations, on the scope of the present invention which is defined in the appended claims.
  • Copper porous material is produced using the general steps shown in Fig. 1.
  • Initial steps include preparing a slurry of binder and elemental powder mixed in a 2-4 parts binder to 6-8 parts copper oxide or copper powder mixture.
  • Current binder systems for copper porous materials include a phenolic binder from Borden and a PVA (poly vinyl acetate) binder from H.B. Fuller. It is to be understood by one skilled in the art that other binder systems are capable of use if the proper curing cycles are used. Mixing of the slurry may be done by hand, electric mixing device or a ball mill may be used.
  • the slurry is next impregnated into the pores of a selected reticulated foam material with an interconnecting web of structural material and void spaces.
  • the pore size of the selected foam material is selected based upon the desired pore size of the final porous material product.
  • the slurry is introduced into the pores of the selected foam material and the excess is removed by hand, rollers or other method until only the webbing of the foam material is coated.
  • the foam material can also be impregnated without the use of a slurry mixture by coating the foam with binder and sprinkling or spraying the copper powder on the webs or by application using a fluidized bed. This process is repeated to achieve the web thickness or density desired.
  • the foam material can also be impregnated with a mixture of binder and powder using an air brush or paint gun apparatus. This slurry requires more binder than the hand impregnation slurry when this procedure is used.
  • the impregnated foam structure is cured in air to set the binders (either phenolic or PVA) at 250 to 350 Degrees F for 0.5 to 3 hours.
  • the foam structure is heated from room temperature to 1200 -
  • the foam structure can alternatively be burned off by heating in an air furnace at 1700 Degrees F to 1900 Degrees F.
  • the parts are then decarburized by processing water through a retort at 0.5 to 1.0 gallons/hr. at 1200 - 1600 Degrees F. The time that the water is running depends on the amount of material present. Five (5) hours will decarburize approximately six (6) sheets of copper 12x12x0.5 inches.
  • the porous metal parts can alternatively be decarburized by heating them in an air furnace from 1100 to 1900 Degrees F for 1 to 3 hours.
  • Nickel porous material is produced using the general steps shown in Fig. 1. Initial steps include preparing a slurry of binder and elemental powder mixed in a 2-4 parts binder to 6-8 parts nickel oxide or nickel powder mixture.
  • Current binder systems for nickel porous materials include a phenolic binder from Border) and a PVA (poly vinyl acetate) binder from H.B. Fuller. It is to be understood by one skilled in the art that other binder systems are capable of use if the proper curing cycles are used.
  • Mixing of the slurry may be done by hand, electric mixing device or a ball mill may be used.
  • the slurry is next impregnated into the pores of a selected reticulated foam material with an interconnecting web of structural material and void spaces.
  • the pore size of the selected foam material is selected based upon the desired pore size of the final porous material product.
  • the slurry is introduced into the pores of the selected foam material and the excess is removed by hand, rollers or other method until only the webbing of the foam material is coated.
  • the foam material can also be impregnated without the use of a slurry mixture by coating the foam with binder and sprinkling or spraying the nickel powder on the webs or by application using a fluidized bed. This process is repeated to achieve the web thickness or density desired.
  • the foam material can also be impregnated with a mixture of binder and powder using an air brush or paint gun apparatus. This slurry requires more binder than the hand impregnation slurry when this procedure is used.
  • the impregnated foam structure is cured in air to set the binders (either phenolic or PVA) at 250 to 350 Degrees F for 0.5 to 3 hours.
  • binders either phenolic or PVA
  • the foam structure is heated from room temperature to 1200 - 1600 Degrees F in 2 - 3 hours in 20 -30 scfh of any inert or reducing atmosphere to burn off the reticulated foam material.
  • the foam structure can alternatively be burned off by heating in an air furnace at 1700 Degrees F to 1900 Degrees F.
  • the parts are then decarburized by processing water through a retort at 0.5 to 1.0 gallons/hr. at 1200 - 1600 Degrees F.
  • the time that the water is running depends on the amount of material present. Five (5) hours will decarburize approximately six (6) sheets of nickel 12x12x0.5 inches.
  • the porous metal parts can alternatively be decarburized by heating them in an air furnace from 1100 to 2800 Degrees F for 1 to 3 hours.
  • the porous metal parts are then sintered at 1800 to 2300 Degrees F for 0.5 to 1.0 hrs. in Hydrogen.
  • porous metallic material from the group of nickel, cobalt and iron may be formed using the method of Example 2.
  • High chromium containing nickel, nickel alloys and iron alloy porous material is produced using the general steps shown in Fig. 2.
  • Initial steps include preparing a slurry of binder and elemental powder mixed in a 2-4 parts binder to 6-8 parts nickel oxide or nickel powder mixture.
  • Current binder systems for most stainless steel porous materials include PVA (poly vinyl acetate) binder from H.B. Fuller. It is to be understood by one skilled in the art that other binder systems such as low carbon acrylics are capable of use if the proper curing cycles are used, as well as higher carbon binders such as phenolics, depending on the porous metal alloy to be produced. Mixing of the slurry may be done by hand, electric mixing device or a ball mill may be used.
  • the slurry is next impregnated into the pores of a selected reticulated foam material with an interconnecting web of structural material and void spaces.
  • the pore size of the selected foam material is selected based upon the desired pore size of the final porous material product.
  • the slurry is introduced into the pores of the selected foam material and the excess is removed by hand, rollers or other method until only the webbing of the foam material is coated.
  • the foam material can also be impregnated without the use of a slurry mixture by coating the foam with binder and sprinkling or spraying the iron or nickel based powder on the webs or by application using a fluidized bed. This process is repeated to achieve the web thickness or density desired.
  • the foam material can also be impregnated with a mixture of binder and powder using an air brush or paint gun apparatus. This slurry requires more binder than the hand impregnation slurry when this procedure is used.
  • the impregnated foam structure is cured in air to set the binders (either phenolic or PVA) at 250 to 350 Degrees F for 0.5 to 3 hours.
  • binders either phenolic or PVA
  • the foam structure of the current example is easily oxidized at elevated temperatures if heated in air or reducing atmospheres at the temperatures required to burn off the organic foam precursor material.
  • the cured foam structure is then heated to 1600 Degrees F to 2000 Degrees F in vacuum, nitrogen or an inert gas. If vacuum is used it should be a partial pressure of argon of 2500 to 3500 microns.
  • the heating cycle discussed herein can alternatively be performed in a retort furnace at a gas level of 20 to 30 scfh of nitrogen or argon.
  • the preferred method will utilize vacuum heating. Previous consideration of the industry shunned this step for fear of significantly reducing the life of the vacuum diffusion pump. It is to be understood that hydrogen atmospheres are not to be used for this example.
  • the parts are then decarburized by heating in vacuum at 900 - 1200
  • the resultant product will have extremely low carbon content (less than 0.1 %) and will result in significant high temperature corrosion resistance of this class of alloys.
  • porous metal parts are then sintered at 2200 to 2500 Degrees F for 0.5 to 1.0 hrs. in vacuum with partial pressure of Argon as previously discussed.
  • Alpha 4 ® (Registered Trademark of Alleghny Ludlum) porous metal, with a nominal chemistry of .015 C, .34 Mn, .014 P, .0001 S, 20.9 Cr., .15 Ni, 5.03 Al, .003 Cb, .0065 Ti, .014 N, .004 Mg, .014 Ce, and .006 La, is produced using the general steps shown in Fig. 2. Initial steps include preparing a slurry of binder and elemental powder mixed in a 2-4 parts binder to 6-8 parts Alpha 4 ® powder mixture. Current binder systems for most Alpha 4 ® porous materials include PVA (poly vinyl acetate) binder from H.B. Fuller. It is to be understood by one skilled in the art that other binder systems such as low carbon acrylics are capable of use if the proper curing cycles are used. Mixing of the slurry may be done by hand, electric mixing device or a ball mill may be used.
  • the Alpha 4 ® slurry is next impregnated into the pores of a selected reticulated foam material with an interconnecting web of structural material and void spaces.
  • the pore size of the selected foam material is selected based upon the desired pore size of the final porous material product.
  • the slurry is introduced into the pores of the selected foam material and the excess is removed by hand, rollers or other method until only the webbing of the foam material is coated.
  • the foam material can also be impregnated without the use of a slurry mixture by coating the foam with binder and sprinkling or spraying the Alpha 4 ® powder on the webs or by application using a fluidized bed. This process is repeated to achieve the web thickness or density desired.
  • the foam material can also be impregnated with a mixture of binder and powder using an air brush or paint gun apparatus.
  • This slurry requires more binder than the hand impregnation slurry when this procedure is used. This process is best accomplished on pore sizes generating 50 ppi (pores per linear inch) or larger.
  • the impregnated foam structure is cured in air to set the binder
  • the Alpha 4 ® material of the current example contains elements that form stable oxides which cannot be reduced by hydrogen at any temperature. In order to sinter these materials elements such as chromium and aluminum must remain metallic. A vacuum furnace allows heating of these materials without formation of such oxides. The vacuum furnace further results in a quick and repeatable operation.
  • the cured foam structure is placed in a vacuum furnace, the chamber evacuated and the structure heated in vacuum to 2300 Degrees F to 2450 Degrees F for 0.5 to 2.0 hrs.
  • This operation is performed in a partial pressure of approximately 2500 to 3500 microns of Nitrogen or Argon to prevent vaporization of certain volatile elements such as chromium and the like and to further reduce wear of the vacuum diffusion pump. Previous consideration of the industry shunned this step for fear of significantly reducing the life of the vacuum diffusion pump. It is to be understood that hydrogen atmospheres are not to be used for this example.
  • porous metallic materials from the group comprising aluminum in solution, chromium, columbium, iron aluminides, nickel aluminides, materials containing rare earths in solution, and titanium aluminides may be produced using the method of Example 4.
  • EXAMPLE 5 Titanium and Titanium alloy porous material is produced using the general steps shown in Fig. 2. Initial steps include preparing a slurry of binder and elemental powder mixed in a 5-8 parts binder to 7-10 parts Titanium powder mixture. Current binder systems for most Titanium alloy materials include PVA (poly vinyl acetate) binder from H.B. Fuller.
  • binder systems such as low carbon acrylics are capable of use if the proper curing cycles are used.
  • Mixing of the slurry may be done by hand, electric mixing device or a ball mill may be used.
  • the slurry is next impregnated into the pores of a selected reticulated foam material with an interconnecting web of structural material and void spaces.
  • the pore size of the selected foam material is selected based upon the desired pore size of the final porous material product.
  • the slurry is introduced into the pores of the selected foam material and the excess is removed by hand, rollers or other method until only the webbing of the foam material is coated.
  • the foam material can also be impregnated without the use of a slurry mixture by coating the foam with binder and sprinkling or spraying the Titanium powder on the webs or by application using a fluidized bed. This process is repeated to achieve the web thickness or density desired. This is best accomplished on pore sizes of 50 ppi (pores per linear inch) or larger.
  • the foam material can also be impregnated with a mixture of binder and powder using an air brush or paint gun apparatus. This slurry requires more binder than the hand impregnation slurry when this procedure is used.
  • the impregnated foam structure is cured in air to set the binders at 250 to 350 Degrees F for 0.5 to 3 hours.
  • the foam structure of the current example is highly reactive at elevated temperatures if heated in air or reducing atmospheres at the temperatures required to burn off the organic foam structure.
  • the cured foam structure is placed in a vacuum furnace, the chamber evacuated and the structure heated in vacuum. This operation is performed in a partial pressure of approximately 2500 - 3500 microns of Argon to prevent vaporization of certain volatile elements such as aluminum and the like and to further reduce wear of the vacuum diffusion pump. It is to be understood that Nitrogen and Hydrogen atmospheres are not to be used with Titanium products as same will adversely react with the Titanium products resulting in undesirable properties.
  • porous metal parts are then sintered at 2200 to 2700 Degrees F for 0.5 to 1.0 hrs. in vacuum or partial pressure.
  • the sintered Titanium porous metal product can be decarburized by heating in air at 900 - 1100 Degrees F for 3 - 12 hours depending on the amount of material to be decarburized.
  • An oxide layer will be formed on the porous metal which can be removed by treating in a dilute mixture of HF and HNO3.
  • a layer of clean Titanium powder is placed on the porous metal product by the sprinkling technique or by spraying binder and powder to the structure and resintered in vacuum or partial pressure at a temperature of 2200 - 2700
  • Platinum porous material is produced using the general steps shown in Fig. 1. Initial steps include preparing a slurry of binder and elemental powder mixed in a 2-4 parts binder to 6-8 parts platinum powder mixture.
  • Current binder systems for Platinum porous materials include PVA (poly vinyl acetate) binder from H.B. Fuller. It is to be understood by one skilled in the art that other binder systems such as low carbon acrylics are capable of use if the proper curing cycles are used.
  • the slurry is next impregnated into the pores of a selected reticulated foam material with an interconnecting web of structural material and void spaces.
  • the pore size of the selected foam material is selected based upon the desired pore size of the final porous material product.
  • the slurry is introduced into the pores of the selected foam material and the excess is removed by hand, rollers or other method until only the webbing of the foam material is coated.
  • the foam material can also be impregnated without the use of a slurry mixture by coating the foam with binder and sprinkling or spraying the Platinum powder on the webs or by application using a fluidized bed. This process is repeated to achieve the web thickness or density desired. This is best accomplished on pore sizes of 50 ppi (pores per linear inch) or larger.
  • the foam material can also be impregnated with a mixture of binder and powder using an air brush or paint gun apparatus. This slurry requires more binder than the hand impregnation slurry when this procedure is used.
  • the impregnated foam structure is sintered in air at 2700 Degrees F to 3000 Degrees F for 0.5 to 2 hours. It is to be understood that unlike the previous examples, the precious metals will be treated in a single sintering cycle after the reticulated precursor foam is impregnated with the binder and metal powder using either the slurry or the dry powder method of powder application.
  • the variation to the general steps shown in Fig. 1 relates to the single sintering step described herein.
  • Metals and alloys comprising the group of molybdenum, tantalum, columbium and tungsten metals may be produced as follows. Molybdenum porous material is produced using a combination of the general steps shown in Figs. 1 and 2.
  • Initial steps include preparing a slurry of binder and elemental powder mixed in a 2-4 parts binder to 6-8 parts molybdenum powder mixture.
  • Current binder systems for molybdenum porous materials include a phenolic binder from Borden and a PVA (poly vinyl acetate) binder from H.B. Fuller. It is to be understood by one skilled in the art that other binder systems such as low carbon acrylics are capable of use if the proper curing cycles are used.
  • Mixing of the slurry may be done by hand, electric mixing device or a ball mill may be used.
  • the slurry is next impregnated into the pores of a selected reticulated foam material with an interconnecting web of structural material and void spaces.
  • the pore size of the selected foam material is selected based upon the desired pore size of the final porous material product.
  • the slurry is introduced into the pores of the selected foam material and the excess is removed by hand, rollers or other method until only the webbing of the foam material is coated.
  • the foam material can also be impregnated without the use of a slurry mixture by coating the foam with binder and sprinkling or spraying the molybdenum powder on the webs or by application using a fluidized bed. This process is repeated to achieve the web thickness or density desired.
  • the foam material can also be impregnated with a mixture of binder and powder using an air brush or paint gun apparatus. This slurry requires more binder than the hand impregnation slurry when this procedure is used.
  • the impregnated foam structure is heated to 1600 Degrees F to
  • the material is next decarburized by holding at 1600 Degrees F to 2000 Degrees F in an atmosphere of 20 to
  • metals and alloys comprising the group tungsten, tantalum, molybdenum or other refractory alloys may be produced using the method of Example 7.
  • the present invention has application to the following pure metals and/or alloys containing these metals in the production of porous metal products therefrom: Chromium, Cobalt, Columbium, Copper, Iron
  • porous metal products produced by the methods of the current invention will find a wide variety of commercial application and in particular will find application in air and gas filters, catalyst supports, catalytic converters, flame arrestors, electro-chemical cathodes, biomaterial applications, lightweight structures, sound dampeners and diesel particulate traps, as well as waste water particulate filters and/or traps.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Combustion & Propulsion (AREA)
  • General Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)

Abstract

On décrit un procédé amélioré de production de matériaux poreux, lequel comprend les étapes consistant à préparer une boue comprenant un liant et une poudre métallique, à imprégner à l'aide de celle-ci une structure alvéolaire réalisée en une matière organique, à durcir la boue imprégnée dans la structure alvéolaire, à brûler la structure, puis à décarburer celle-ci et enfin à fritter sous vide le produit en matériau poreux résultant. On peut effectuer les étapes de frittage et de décarburation dans une atmosphère sous pression partielle de gaz réactifs ne devant pas réagir défavorablement avec le produit métallique poreux.
PCT/US1997/002561 1996-02-27 1997-02-25 Materiaux poreux et procede de production associe WO1997031738A1 (fr)

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AU21901/97A AU2190197A (en) 1996-02-27 1997-02-25 Porous materials and method for producing

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US60776896A 1996-02-27 1996-02-27
US08/607,768 1996-02-27

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WO1997031738A1 true WO1997031738A1 (fr) 1997-09-04

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US5857328A (en) * 1997-11-24 1999-01-12 General Motors Corporation Exhaust manifold catalytic converter
US5857326A (en) * 1997-11-24 1999-01-12 General Motors Corporation Exhaust poison trap
US6062020A (en) * 1997-11-12 2000-05-16 General Motors Corporation Exhaust manifold converter apparatus
US6358345B1 (en) * 1999-11-16 2002-03-19 Shao-Chien Tseng Method for producing porous sponge like metal of which density of pores is controllable
WO2002066693A1 (fr) * 2001-02-19 2002-08-29 Isotis N.V. Metaux poreux et revetements metalliques pour implants
WO2003033192A2 (fr) * 2001-10-11 2003-04-24 Inco Limited Procede de production de corps poreux frittes
WO2003099235A1 (fr) * 2002-05-23 2003-12-04 Ast Acquisition, L.L.C. Implants metalliques a haute porosite
US6733692B2 (en) 2000-04-20 2004-05-11 Conocophillips Company Rhodium foam catalyst for the partial oxidation of hydrocarbons
US6746658B2 (en) 2000-04-20 2004-06-08 Conocophillips Company Rhodium cloth catalyst for partial oxidation of hydrocarbons
US6911161B2 (en) 2002-07-02 2005-06-28 Conocophillips Company Stabilized nickel-containing catalysts and process for production of syngas
EP1688600A2 (fr) * 2005-02-02 2006-08-09 Pankl Emission Control Systems GmbH Dispositif pour purifier les gaz d'échappement d'un véhicule
EP1731247A1 (fr) * 2005-06-07 2006-12-13 Vlaamse Instelling Voor Technologisch Onderzoek (Vito) Matériaux poreux de titane, alliages de titane ou NiTi avec une ductilité élevée
GR1006099B (el) * 2007-08-02 2008-10-09 Παρασκευη τρισδιαστατων μεταλλικων σπογγων ανοικτου κελιου με την μεθοδο εμποτισμου αφρου πολυουρεθανης και αντιστοιχων συγγενικων υλικων σε παχυρευστο μειγμα κονεως μεταλλου και αλατων
DE102009015176A1 (de) * 2009-03-20 2011-07-14 Alantum Corporation, Kyonggi Offenporiger Metallschaumkörper und Verfahren zu seiner Herstellung
CN102451911A (zh) * 2010-10-19 2012-05-16 重庆润泽医疗器械有限公司 一种医用金属植入材料多孔钽的制备方法
CN102462862A (zh) * 2010-11-17 2012-05-23 重庆润泽医疗器械有限公司 一种医用金属植入材料多孔钽的制备方法
CN102462861A (zh) * 2010-11-17 2012-05-23 重庆润泽医疗器械有限公司 一种医用金属植入材料多孔钽的制备方法
CN102475903A (zh) * 2010-11-29 2012-05-30 重庆润泽医疗器械有限公司 医用金属植入材料多孔铌的制备方法
CN102475905A (zh) * 2010-11-29 2012-05-30 重庆润泽医疗器械有限公司 一种医用金属植入材料多孔铌的制备方法
CN102475904A (zh) * 2010-11-29 2012-05-30 重庆润泽医疗器械有限公司 医用金属植入多孔材料的制备方法
CN102793945A (zh) * 2011-09-29 2012-11-28 重庆润泽医药有限公司 一种替代牙骨的医用多孔钽材料及其制备方法
CN103463674A (zh) * 2010-11-17 2013-12-25 重庆润泽医药有限公司 一种医用植入材料多孔钽的制备方法
CN103463673A (zh) * 2010-11-29 2013-12-25 重庆润泽医药有限公司 医用金属植入材料多孔铌的制备方法
CN104225673A (zh) * 2011-09-29 2014-12-24 重庆润泽医药有限公司 一种替代牙骨的医用多孔金属材料及其制备方法
US9039939B2 (en) * 2007-03-29 2015-05-26 Tdk Corporation Production method of active material, and active material
US9246193B2 (en) 2007-03-29 2016-01-26 Tdk Corporation All-solid-state lithium-ion secondary battery and production method thereof
EP2966184A4 (fr) * 2013-03-05 2016-12-21 Taisei Kogyo Co Ltd Matière frittée poreuse et procédé de fabrication d'une matière frittée poreuse
US20200376547A1 (en) * 2019-05-28 2020-12-03 Desktop Metal, Inc. Furnace for sintering printed objects
CN113584402A (zh) * 2021-08-03 2021-11-02 西部宝德科技股份有限公司 一种铁铝铬过滤材料制备方法
RU2759860C1 (ru) * 2020-12-30 2021-11-18 Государственное Научное Учреждение Институт Порошковой Металлургии Имени Академика О.В. Романа Способ получения высокопористого ячеистого материала
CN114619031A (zh) * 2022-03-14 2022-06-14 北京理工大学 一种微米孔径泡沫铜的制备方法

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US3163528A (en) * 1963-02-01 1964-12-29 Gen Electric Method for producing copper articles
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EP0099337A2 (fr) * 1982-07-09 1984-01-25 Eltech Systems Limited Structures réticulées au titane et à l'hydrure de titane et procédé de fabrication
WO1995026844A1 (fr) * 1994-03-31 1995-10-12 Hitachi Chemical Company, Ltd. Procede de production de corps poreux

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Publication number Priority date Publication date Assignee Title
GB963885A (en) * 1959-09-14 1964-07-15 Gen Electric Sintered porous metallic material and method of making it
US3163528A (en) * 1963-02-01 1964-12-29 Gen Electric Method for producing copper articles
US3313621A (en) * 1965-06-15 1967-04-11 Mott Metallurg Corp Method for forming porous seamless tubing
EP0099337A2 (fr) * 1982-07-09 1984-01-25 Eltech Systems Limited Structures réticulées au titane et à l'hydrure de titane et procédé de fabrication
WO1995026844A1 (fr) * 1994-03-31 1995-10-12 Hitachi Chemical Company, Ltd. Procede de production de corps poreux

Cited By (43)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6062020A (en) * 1997-11-12 2000-05-16 General Motors Corporation Exhaust manifold converter apparatus
US5857328A (en) * 1997-11-24 1999-01-12 General Motors Corporation Exhaust manifold catalytic converter
US5857326A (en) * 1997-11-24 1999-01-12 General Motors Corporation Exhaust poison trap
US6358345B1 (en) * 1999-11-16 2002-03-19 Shao-Chien Tseng Method for producing porous sponge like metal of which density of pores is controllable
US6733692B2 (en) 2000-04-20 2004-05-11 Conocophillips Company Rhodium foam catalyst for the partial oxidation of hydrocarbons
US6746658B2 (en) 2000-04-20 2004-06-08 Conocophillips Company Rhodium cloth catalyst for partial oxidation of hydrocarbons
WO2002066693A1 (fr) * 2001-02-19 2002-08-29 Isotis N.V. Metaux poreux et revetements metalliques pour implants
WO2003033192A2 (fr) * 2001-10-11 2003-04-24 Inco Limited Procede de production de corps poreux frittes
WO2003033192A3 (fr) * 2001-10-11 2003-09-04 Inco Ltd Procede de production de corps poreux frittes
WO2003099235A1 (fr) * 2002-05-23 2003-12-04 Ast Acquisition, L.L.C. Implants metalliques a haute porosite
US6911161B2 (en) 2002-07-02 2005-06-28 Conocophillips Company Stabilized nickel-containing catalysts and process for production of syngas
EP1688600A2 (fr) * 2005-02-02 2006-08-09 Pankl Emission Control Systems GmbH Dispositif pour purifier les gaz d'échappement d'un véhicule
EP1688600A3 (fr) * 2005-02-02 2008-05-14 Pankl Emission Control Systems GmbH Dispositif pour purifier les gaz d'échappement d'un véhicule
EP1731247A1 (fr) * 2005-06-07 2006-12-13 Vlaamse Instelling Voor Technologisch Onderzoek (Vito) Matériaux poreux de titane, alliages de titane ou NiTi avec une ductilité élevée
US9039939B2 (en) * 2007-03-29 2015-05-26 Tdk Corporation Production method of active material, and active material
US9419308B2 (en) 2007-03-29 2016-08-16 Tdk Corporation All-solid-state lithium-ion secondary battery and production method thereof
US9246193B2 (en) 2007-03-29 2016-01-26 Tdk Corporation All-solid-state lithium-ion secondary battery and production method thereof
GR1006099B (el) * 2007-08-02 2008-10-09 Παρασκευη τρισδιαστατων μεταλλικων σπογγων ανοικτου κελιου με την μεθοδο εμποτισμου αφρου πολυουρεθανης και αντιστοιχων συγγενικων υλικων σε παχυρευστο μειγμα κονεως μεταλλου και αλατων
EP2045029A1 (fr) 2007-08-02 2009-04-08 Aristotle University Thessaloniki Production d'aluminium mousse par l'impregnation de mousse de polyurethane avec boue comprenant aluminium et sel
DE102009015176A1 (de) * 2009-03-20 2011-07-14 Alantum Corporation, Kyonggi Offenporiger Metallschaumkörper und Verfahren zu seiner Herstellung
DE102009015176A8 (de) * 2009-03-20 2011-11-10 Alantum Corporation Offenporiger Metallschaumkörper und Verfahren zu seiner Herstellung
DE102009015176B4 (de) * 2009-03-20 2017-02-09 Alantum Corporation Verfahren zu Herstellung offenporiger Metallschaumkörper
CN102451911A (zh) * 2010-10-19 2012-05-16 重庆润泽医疗器械有限公司 一种医用金属植入材料多孔钽的制备方法
CN102462861A (zh) * 2010-11-17 2012-05-23 重庆润泽医疗器械有限公司 一种医用金属植入材料多孔钽的制备方法
CN103463674B (zh) * 2010-11-17 2015-05-20 重庆润泽医药有限公司 一种医用植入材料多孔钽的制备方法
CN102462862A (zh) * 2010-11-17 2012-05-23 重庆润泽医疗器械有限公司 一种医用金属植入材料多孔钽的制备方法
CN102462862B (zh) * 2010-11-17 2013-10-09 重庆润泽医药有限公司 一种医用金属植入材料多孔钽的制备方法
CN103463674A (zh) * 2010-11-17 2013-12-25 重庆润泽医药有限公司 一种医用植入材料多孔钽的制备方法
CN102475904A (zh) * 2010-11-29 2012-05-30 重庆润泽医疗器械有限公司 医用金属植入多孔材料的制备方法
CN102475903B (zh) * 2010-11-29 2013-09-18 重庆润泽医药有限公司 医用金属植入材料多孔铌的制备方法
CN103463673B (zh) * 2010-11-29 2015-02-11 重庆润泽医药有限公司 医用金属植入材料多孔铌的制备方法
CN103463673A (zh) * 2010-11-29 2013-12-25 重庆润泽医药有限公司 医用金属植入材料多孔铌的制备方法
CN102475903A (zh) * 2010-11-29 2012-05-30 重庆润泽医疗器械有限公司 医用金属植入材料多孔铌的制备方法
CN102475905A (zh) * 2010-11-29 2012-05-30 重庆润泽医疗器械有限公司 一种医用金属植入材料多孔铌的制备方法
CN104225673B (zh) * 2011-09-29 2016-01-13 温州智创科技有限公司 一种替代牙骨的医用多孔金属材料及其制备方法
CN102793945B (zh) * 2011-09-29 2015-08-19 朱启东 一种替代牙骨的医用多孔钽材料及其制备方法
CN102793945A (zh) * 2011-09-29 2012-11-28 重庆润泽医药有限公司 一种替代牙骨的医用多孔钽材料及其制备方法
CN104225673A (zh) * 2011-09-29 2014-12-24 重庆润泽医药有限公司 一种替代牙骨的医用多孔金属材料及其制备方法
EP2966184A4 (fr) * 2013-03-05 2016-12-21 Taisei Kogyo Co Ltd Matière frittée poreuse et procédé de fabrication d'une matière frittée poreuse
US20200376547A1 (en) * 2019-05-28 2020-12-03 Desktop Metal, Inc. Furnace for sintering printed objects
RU2759860C1 (ru) * 2020-12-30 2021-11-18 Государственное Научное Учреждение Институт Порошковой Металлургии Имени Академика О.В. Романа Способ получения высокопористого ячеистого материала
CN113584402A (zh) * 2021-08-03 2021-11-02 西部宝德科技股份有限公司 一种铁铝铬过滤材料制备方法
CN114619031A (zh) * 2022-03-14 2022-06-14 北京理工大学 一种微米孔径泡沫铜的制备方法

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