EP0340957A2 - Verfahren zur Herstellung von Verbundmetall unter Beschleunigung der Infiltration des Matrix-Metalls durch feine Teilchen eines dritten Materials - Google Patents

Verfahren zur Herstellung von Verbundmetall unter Beschleunigung der Infiltration des Matrix-Metalls durch feine Teilchen eines dritten Materials Download PDF

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Publication number
EP0340957A2
EP0340957A2 EP89304076A EP89304076A EP0340957A2 EP 0340957 A2 EP0340957 A2 EP 0340957A2 EP 89304076 A EP89304076 A EP 89304076A EP 89304076 A EP89304076 A EP 89304076A EP 0340957 A2 EP0340957 A2 EP 0340957A2
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EP
European Patent Office
Prior art keywords
metal
preform
fine pieces
metals
reinforcing material
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EP89304076A
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English (en)
French (fr)
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EP0340957B1 (de
EP0340957A3 (en
Inventor
Masahiro Kubo
Tetsuya Suganuma
Takashi Morikawa
Atsuo Tanaka
Yoshiaki Kajikawa
Tetsuya Nukami
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Toyota Motor Corp
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Toyota Motor Corp
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Priority claimed from JP63108165A external-priority patent/JPH07100834B2/ja
Priority claimed from JP63108166A external-priority patent/JP2576186B2/ja
Application filed by Toyota Motor Corp filed Critical Toyota Motor Corp
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Publication of EP0340957A3 publication Critical patent/EP0340957A3/en
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    • 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
    • B22F3/24—After-treatment of workpieces or articles
    • B22F3/26—Impregnating
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0036—Matrix based on Al, Mg, Be or alloys thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/02—Pretreatment of the fibres or filaments
    • C22C47/06—Pretreatment of the fibres or filaments by forming the fibres or filaments into a preformed structure, e.g. using a temporary binder to form a mat-like element
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/08—Making alloys containing metallic or non-metallic fibres or filaments by contacting the fibres or filaments with molten metal, e.g. by infiltrating the fibres or filaments placed in a mould
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
    • C22C49/08—Iron group metals
    • 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

  • the present invention relates to a composite material, and more particularly, to a method of producing a metal base composite material comprising short fibers, whisker or particles as a reinforcing material and an aluminum alloy or the like as a matrix material.
  • melt forging method high pressure casting method
  • the melt forging method it is required that a molten mass of matrix metal is pressurized to a very high pressure, and therefore a large scale production equipment is required, resulting in a high production cost of the composite materials, and thus presenting a principal obstacle for the practical use of this method.
  • the reinforcing fibers are continuous fibers which are generally disposed in a common direction, the capillary action is available to infiltrate a molten matrix metal into the interstices among the continuous fibers, and therefore the methods proposed in the above-mentioned publications are effective.
  • the reinforcing fibers are short fibers or a whisker
  • the infiltration of the molten matrix metal by the capillary action is not available. Therefore, the infiltration of the molten matrix metal into the short fibers or the whisker is not improved by the method of increasing the affinity as applied to the continuous fibers as described in, for example, Japanese Patent Laying-open Publication 59-205464.
  • a method of producing a metal base composite material comprising a first process of producing a porous preform from a reinforcing material selected from a group consisting of short fibers, whisker, particles and mixtures thereof, and a second process of infiltrating a molten matrix metal into the interstices of said porous preform, wherein in said first process fine pieces of a third material having good affinity to the molten matrix metal are mixed in said porous preform, and in said second process at least a part of said preform is contacted with a molten mass of the matrix metal so that the molten matrix metal infiltrates into the interstices of said porous preform with no substantial pressure being applied thereto.
  • the third material for said fine pieces may be a metal or metals selected from a group consisting of Ni, Fe, Co, Cr, Mn, Cu, Ag, Si, Mg, Al, Zn, Sn, Ti and an alloy or alloys including any one of these metals as a principal component when the matrix metal is AI or an AI alloy.
  • the third material for said fine pieces may be a metal or metals selected from a group consisting of Ni, Cr, Ag, Al, Zn, Sn, Pb and an alloy or alloys including any one of these metals as a principal component when the matrix metal is Mg or a Mg alloy.
  • the matrix metal is a metal selected from a group consisting of Al, Mg, AI alloy and Mg alloy
  • the material for said fine pieces may be an oxide or oxides of a metal or metals selected from a group consisting of W, Mo, Pb, Bi, V, Cu, Ni, Co, Sn, Mn, B, Cr, Mg and AI and mixtures thereof.
  • the infiltration of the molten matrix metal into the interstices of the preform of reinforcing material is much promoted as helped by the affinity of the third material with the molten matrix metal.
  • the molten matrix metal reacts with the fine pieces of the third material and generates heat which further improves the affinity between the molten matrix metal and the reinforcing material, thereby further improving the infiltration of the molten matrix metal into the preform of reinforcing material.
  • the method of the present invention it is not necessary to pressurize the molten matrix metal or to preheat the reinforcing material, and therefore no large scale equipment for pressurizing the molten matrix metal or for preheating the reinforcing material is required. Therefore, according to the present invention it is possible to produce a composite material including a matrix material well infiltrated in a reinforcing material at high efficiency and low cost.
  • the molten matrix metal infiltrates easily into the preform according to the method of the present invention, if the preform including a reinforcing material and fine pieces of the third material is prepared to have a predetermined shape and dimensions, the whole body of the preform can be uniformly infiltrated with the molten matrix metal by a part of the preform being brought into contact with a molten mass of the matrix metal so as immediately to provide a composite material having substantially the predetermined shape and dimensions.
  • a composite material having substantially a predetermined shape and dimensions can be produced at high efficiency and low cost with very high yielding rate.
  • the infiltration of the molten matrix metal into the preform can be improved by incorporating fine pieces of a determinate metal or metals in any optional amount.
  • the matrix metal is AI or AI alloys
  • the molten matrix metal can infiltrate into the reinforcing material in good condition when the fine pieces of a determinate metal or metals are included in the reinforcing material at a ratio of more than 150% by weight relative to the amount of the reinforcing material.
  • the matrix metal is AI or an AI alloy
  • the fine pieces of a determinate metal or metals are incorporated into the preform at a ratio more than 150% by weight relative to the amount of the reinforcing fibers.
  • the infiltration of the molten matrix metal into the preform can be improved by incorporating fine pieces of a determinate metal oxide or metal oxides in any optional amount.
  • the molten matrix metal can infiltrate into the reinforcing material in good condition when the fine pieces of a determinate metal oxide or metal oxides are included in the reinforcing material at a ratio of more than 7.5% by weight, particularly more than 10% by weight, still more particularly more than 15% by weight, relative to the amount of the reinforcing material.
  • the fine pieces of a determinate metal oxide or metal oxides are incorporated into the preform at a ratio more than 7.5% by weight, particularly more than 10% by weight, still more particularly more than 1 5% by weighty, relative to the amount of the reinforcing fibers.
  • the metal to form the fine pieces of a certain determinate metal or metals is selected from a group consisting of Ni, Fe, Co, Cu, Si, Zn, Sn, Ti and an alloy including one of these metals as a principal component when the matrix metal is AI or an AI alloy.
  • the metal or metals which form said certain metal oxide or metal oxides provided in the form of fine pieces are any one of W, Mo, Pb, Bi, Cu, Ni, Co, Sn, Mn, Cr or an alloy including one of these metals as a principal component, particularly when the metal or the metals which form said certain metal oxide or metal oxides provided in the form of fine pieces are any one of W, No, Pb, Co, Mn or an alloy including one of these metals as a principal component, the molten matrix metal can infiltrate into the preform in good condition.
  • the metal or metals to form the fine pieces of a certain determinate metal oxide or metal oxides is selected from a group consisting of W, Mo, Pb, Bi, Cu, Ni, Co, Sn, Mn, Cr or an alloy including one of these metals as a principal component, particularly a group consisting of W, Mo, Pb, Co, Mn or an alloy including one of these metals as a principal component.
  • the matrix metal when the matrix metal is an AI alloy, if the AI alloy includes at least one of Mg, Zr and Ca by an amount more than 0.5%, the molten matrix metal can more readily infiltrate into the preform. This composition is more effective to improve the affinity between the reinforcing material and the matrix metal when the preform is preheated. Therefore, according to another detailed feature of the present invention, the matrix metal is an AI alloy including at least one of Mg, Zr and Ca by an amount more than 0.5%.
  • the preform includes fine pieces of the above-mentioned determinate metal or metals, the infiltration of the molten matrix metal into the preform is improved. Particularly if the preform includes fine pieces of the above-mentioned determinate metal or metals by an amount more than 130% by weight relative to the reinforcing material, the molten matrix metal can infiltrate into the preform in good condition.
  • the matrix metal is Mg or a Mg alloy
  • the fine pieces of a certain determinate metal or metals is incorporated into the preform by an amount of more than 130% by weight relative to the reinforcing material in the preform.
  • the total volumetric ratio of the reinforcing material and the fine pieces of the determinate metal or metals in the preform is set to 5-90%, desirably 7.5-85%.
  • the total volumetric ratio of the reinforcing material and the fine pieces of the determinate metal oxide or metal oxides in the preform is set to 4-85%, desirably 5-80%.
  • the volumetric ratio of the fine pieces of the determinate metal or metals in the preform is desirably set to be less than 85%.
  • the volumetric ratio of the fine pieces of the determinate metal oxide or metal oxides in the preform is set to be less than 45%, desirably less than 40%.
  • the preform has a predetermined shape and dimensions, and only a part thereof is dipped into a bath of molten matrix metal. According to this method, a composite material having a predetermined shape and dimensions can be produced at high efficiency, low cost and very high yielding rate with no need of a casting mold for pressurizing the molten matrix metal for defining the predetermined shape of the product.
  • the preform may be preheated to a temperature which is lower than the conventional preheating temperature in order to further improve the affinity of the reinforcing material to the matrix metal.
  • a lower preheating temperature is desirable in order to avoid oxidization of the fine pieces of the determinate metal or metals.
  • the fine pieces of the determinate metal or metals according to the present invention may be in an optional shape such as short fibers, whisker or powder.
  • alumina short fibers having 3 microns mean fiber diameter and 1mm mean fiber length (“Safil RG , product of ICI, 95% A1 2 0 3 , 5% Si0 2 ), silicon carbide whisker having 0.1-1.0 micron fiber diameter and 50-200 microns fiber length (product of Tokai Carbon Kabushiki Kaisha), and silicon nitride particles having 10 microns mean particle diameter (product of Kojundo Kagaku Kabushiki Kaisha) were prepared. Further, metal fibers and metal powder as shown in Table 1 were prepared.
  • Fig. 1 shows such a preform 10 in a perspective view, wherein 12 indicates the reinforcing material and 14 indicates the metal fibers.
  • Two kinds of preforms were prepared by changing the mixing ratio of the reinforcing material and the metal fibers or the metal powder so that in the first type preform the volumetric ratio of the reinforcing material is 5%, the mass ratio of the metal fibers or the metal powder relative to the reinforcing material is 600%, and the overall volumetric ratio of the preform is 13-62%, and in a second type preform the volumetric ratio of the reinforcing material is 15%, the mass ratio of the metal fibers or the metal powder relative to the reinforcing material is 200%, and the overall volumetric ratio of the preform is 23-72%.
  • each preform was preheated to 200 C and was then placed into a vessel 16 as shown in Fig. 2. Then a molten aluminum alloy was poured to form a bath thereof, and then the molten aluminum alloy was solidified with no pressurization.
  • the aluminum alloy was prepared in seven different types which were JIS AC1A including 0.1% Mg, JIS AC4C including 0.3% Mg, JIS AC4D including 0.5% Mg, JIS AC8A including 1% Mg, JIS AC7B including 10% Mg, JIS AC4C added with 0.3% Ca, and JIS AC4C added with 0.3% Zr.
  • the composite material portion 20 corresponding to the portion of the preform was cut out from the solidified body, and the reinforcing material was cut along a phantom plane 22, and the cut section was polished and investigated by the naked eye and a microscope to evaluate the quality of composite structure.
  • Tables 2-4 The results of the evaluation are shown in Tables 2-4.
  • a double circle (@) indicates that both the macroscopic composite condition and the microscopic composite condition were good
  • a single circle (O) indicates that the macroscopic composite condition was good
  • a triangle (A) indicates that only partial composite was accomplished
  • a cross (X) indicates that no composite structure was accomplished.
  • metal fibers or metal powder other than those shown in Table 1 and consisting of an alloy including the above-mentioned determinate metal as a principal component provides a good composite quality, and when the matrix metal includes more than 0.5% Ca or Zr, the composite quality is further improved.
  • alumina short fibers as used in Embodiment 1 preforms were prepared to include only the alumina short fibers at 5%, 15% and 30% by volume.
  • silicon carbide whisker as used in Embodiment 1 preforms were prepared to include only the silicon carbide whisker at 5%, 15% and 40% by volume.
  • silicon nitride particles as used in Embodiment 1 preforms were prepared to include only the silicon nitride particles at 5%, 15% and 50% by volume.
  • Alumina short fibers having 3 microns mean fiber diameter and 1 mm mean fiber length (“Safil RF, product of ICI, 96-97% A1 2 0 3 3, 3-4% Si0 2 ), silicon nitride whisker having 0.1-0.6 micron mean fiber diameter and 20-200 microns mean fiber length (product of Tateho Kagaku Kogyo Kabushiki Kaisha) and tungsten carbide particles having 10 microns mean particle diameter (product of Kojundo Kagaku Kabushiki Kaisha) were prepared. Further, the metal fibers and the metal powder shown in Table 1 were prepared as the metal fibers and the metal powder herein referred to. Then in the same manner as Embodiment 1 the above-mentioned reinforcing materials and the metal fibers or the metal powder were mixed, and preforms having 20 x 20 x 40 mm dimensions were prepared by compression forming.
  • two types of preforms were prepared so that in a first type preform the volumetric ratio of the reinforcing material is 5%, the mass ratio of the metal fibers or the metal powder relative to the reinforcing material is 500%, and the overall volumetric ratio of the preform is 12-53%, and in a second type preform the volumetric ratio of the reinforcing material is 15%, the mass ratio of the metal fibers or the metal powder relative to the reinforcing material is 150%, and the overall volumetric ratio of the preform is 21-58%.
  • the preforms including Zn fibers and Sn fibers as the metal fibers were preheated to 150 C, the preform including Pb powder as the metal powder was preheated to 100 C, and other preforms were preheated to 400 C.
  • each preheated preform was placed in a vessel, and a molten magnesium alloy at 700 ° C was poured into the vessel, and solidified with no pressurizing.
  • the magnesium alloy was prepared in three different types of MC-2, MC-7 and MC-8 according to JIS.
  • the matrix metal is a magnesium alloy
  • the preform includes the metal fibers or the metal powder made of Ni, Cr, Ag, Zn, Sn, Pb or an alloy including one of these metals as a principal component.
  • the preform includes the metal fibers or the metal powder made of other alloys including one of Ni, Cr, Ag, Zn, Sn and Pb, or Al.
  • Embodiment 2 preforms By the same aluminum short fibers as used in Embodiment 2 preforms were prepared to include only the aluminum short fibers at 5%, 15% and 40% by volume. Further, by the same silicon nitride whisker as used in Embodiment 2 preforms were prepared to include only the silicon nitride whisker at 5%, 15% and 40% by volume. Still further, by the same silicon carbide particles as used in Embodiment 2 preforms were prepared to include only the silicon carbide particles at 5%, 15% and 40% by volume. By using these preforms it was tried to produce composite materials in the same manner and under the same conditions as adopted in Embodiment 2. No good composite material was obtained from these preforms.
  • the preform includes the determinate metal fibers or powder. Therefore, investigations were conducted to determine what amount of the metal fibers or the metal powder is appropriate.
  • the reinforcing materials shown in Tables 8 and 9, and the matrix metals, the metal fibers and the metal powder shown in Table 10 and 11 were prepared. By using these materials composite materials were produced in the same manner as in Embodiments 1 and 2 with no preheating of the preforms. The composite materials thus obtained were evaluated about the composite conditions in the same manner as in Embodiments 1 and 2. The metal fibers and the metal powder were the same as those shown in Table 1. The mass ratio of the metal fibers or the metal powder relative to the reinforcing material was set to 0%, 50%, 100%, 150%, 200%, 250% and 300%. The results of evaluation are shown in Tables 10 and 11.
  • the mass ratio of the metal fibers or the metal powder relative to the reinforcing material should desirably be more than 150%, particularly more than 200%, when the matrix metal is an aluminum alloy, and more than 130%, particularly 180%. when the matrix metal is a magnesium alloy.
  • cylindrical preforms such as 24 shown in Fig. 4 having 40 mm outer diameter, 30 mm inner diameter and 50 mm length were prepared in the same manner as in Embodiment 1 so that the volumetric ratio of the reinforcing material and the mass ratio of the metal fibers or the metal powder relative to the reinforcing material are the same as in the first type preform and the second type preform in Embodiment 1.
  • 26 indicates the reinforcing material
  • 28 indicates the metal fibers.
  • the matrix metal the same seven kinds of molten aluminum alloys as those used in Embodiment 1 were prepared.
  • each preform was preheated to the same temperature as in Embodiment 1, and then each preform 24 was held at a top portion thereof by a pincette-shaped holder 30 as shown in Fig. 5, and a bottom end portion of each preform was brought into contact with a bath of the molten aluminum alloy at 700 C contained in a vessel 32. Then the molten aluminum alloy infiltrated into the whole body of each preform from the lower end to the upper end thereof in 3-10 seconds. After the molten aluminum alloy has completely infiltrated into the whole body of the preform, the preform was removed from the bath of the molten aluminum alloy as shown in Fig. 6 and was held in that condition until the molten aluminum alloy solidified. During this process the molten aluminum alloy was maintained in the preform as attached thereto under the surface tension.
  • the dimensions of the composite material cylindrical body were measured.
  • the outer diameter, the inner diameter and the length were 39-41 mm, 28-30 mm and 48-50 mm, respectively. It was confirmed that the composite material cylindrical body had substantially the same shape and dimensions as the preform.
  • Each composite material cylindrical body was cut for the inspection of the composite condition. It was confirmed that in all of the composite material cylindrical bodies the aluminum alloy has sufficiently infiltrated up to all surfaces of the preform.
  • cylindrical preforms having 80 mm outer diameter, 70 mm inner diameter and 40 mm length were prepared in the same manner as in Embodiment 2 so that the volumetric ratio of the reinforcing material and the mass ratio of the metal fibers or the metal powder relative to the reinforcing material are the same as in the first type preform and the second type preform in Embodiment 2.
  • the matrix metal the same three kinds of molten magnesium alloys as those used in Embodiment 2 were prepared.
  • each preform was preheated to the same temperature as in Embodiment 2, and then each preform 24 was brought into contact with a bath of the molten magnesium alloy at 700 °C contained in a vessel in the same manner as in Embodiment 4. Then the molten magnesium alloy infiltrated into the whole body of each preform from the lower end to the upper end thereof in 3-8 seconds. After the molten aluminum alloy has completely infiltrated into the whole body of the preform, the preform was removed from the bath of the molten aluminum alloy and was held in that condition until the molten magnesium alloy solidified. During this process the molten magnesium alloy was maintained in the preform as attached thereto under the surface tension.
  • the dimensions of the composite material cylindrical body were measured.
  • the outer diameter, the inner diameter and the length were 79.5-80.5 mm, 69-70 mm and 39-40 mm, respectively. It was confirmed that the composite material cylindrical body had substantially the same shape and dimensions as the preform.
  • Each composite material cylindrical body was cut for the inspection of the composite condition. It was confirmed that in all of the composite material cylindrical bodies the aluminum alloy has sufficiently infiltrated up to all surfaces of the preform.
  • alumina short fibers having 3 microns mean fiber diameter and 1 mm mean fiber length (“Safil RG", product of ICI, 95% AI 2 0 1 , 5% Si0 2 ), silicon carbide whisker having 0.1-1.0 micron fiber diameter and 50-200 microns fiber length (product of Tokai Carbon Kabushiki Kaisha), and silicon nitride particles having 10 microns mean particle diameter (product of Kojundo Kagaku Kabushiki Kaisha) were prepared.
  • the above-mentioned reinforcing material was mixed with a sol of oxides (A1 2 0 3 , ZrO 2 , Fe 2 0 3 , Ce0 2 , Si0 2 ) (product of Nissan Kagaku Kabushiki Kaisha) and the mixture was formed under pressure and dried, thereby producing a first type preform including the above-mentioned reinforcing material and fine pieces of the above-mentioned oxides.
  • a sol of oxides A1 2 0 3 , ZrO 2 , Fe 2 0 3 , Ce0 2 , Si0 2
  • the above-mentioned reinforcing material was mixed with a water solution or an ethanol solution of chlorides (MnCl 2 •4H 2 O. NiCl 2 •6H 2 O, TiCI 4 ., C U CI 2 , ZnC1 2 , SnCl 2 •2H 2 O) (product of Nihon Shinkinzoku Kabushiki Kaisha) and the mixture was formed under suction and heated in the atmosphere at 500 °C so that the chlorides were converted into oxides, thereby producing a second type preform including the reinforcing material and fine pieces of the oxides converted from the above-mentioned chlorides.
  • chlorides MnCl 2 •4H 2 O. NiCl 2 •6H 2 O, TiCI 4 ., C U CI 2 , ZnC1 2 , SnCl 2 •2H 2 O
  • the above-mentioned reinforcing material was mixed with Ta 2 0s powder having 1.5 micron mean particle diameter (product of Mitsui Kinzoku Kabushiki Kaisha), Nb 2 0 s powder having 5 microns mean particle diameter (product of Mitsui Kinzoku Kabushiki Kaisha), PbO powder having 1-2 microns particle diameter (product of Kojundo Kagaku Kabushiki Kaisha), V 2 O 5 powder having 5 microns mean particle diameter (product of Kojundo Kagaku Kabushiki Kaisha), Bi 2 0 3 powder having 6 microns mean particle diameter (product of Kojundo Kagaku Kabushiki Kaisha), Co3O4 powder having 74 microns mean particle diameter (product of Sumitomo Kinzoku Kozan Kabushiki Kaisha) and MgO powder having 0.05 micron mean particle diameter (product of Ube Kosan Kabushiki Kaisha) in water, respectively, and the mixture was formed under compression and dried, thereby producing a third type preform
  • the above-mentioned reinforcing material was mixed in a water solution including polyvinyl alcohol, and the well agitated mixture was formed to a body by suction and dried, and the formed body was soaked in a water solution dissolving Cr 2 0 3 (product of Nippon Denko Kabushiki Kaisha), H 3 B0 3 (product of Kenei Seiyaku Kabushiki Kaisha) and para-ammonium molybdate (product of Nihon Shinkinzoku Kabushiki Kaisha), and the water solution was heated in the atmosphere to 500 ° C for an hour, so that fine pieces of oxides of Cr, B and Mo are generated while water and polyvinyl alcohol were evaporated, thereby producing a fourth type preform including the above-mentioned reinforcing material and fine pieces of the above-mentioned oxides.
  • the above-mentioned reinforcing material' was mixed into a water solution of polyvinyl alcohol and the well agitated mixture was formed to a body by suction and dried, and the body thus formed was soaked in a methane ammonium wolframate solution (product of Nihon Shinkinzoku Kabushiki Kaisha), and then the body was heated in the atmosphere to 700° C for one hour, so that fine pieces of oxide of W are generated while water was evaporated, thereby producing a fifth type preform including the above-mentioned reinforcing material and fine pieces of the above-mentioned oxides.
  • a methane ammonium wolframate solution product of Nihon Shinkinzoku Kabushiki Kaisha
  • the preform produced in the above-mentioned manner was also as shown in Fig. 1 by 10, wherein 12 also indicates the reinforcing material and 14 indicates in this case the fine pieces of the metal oxide.
  • two kinds of preforms were prepared by changing the mixing ratio of the reinforcing material and the metal oxide powder so that in a first kind preform the volumetric ratio of the reinforcing material is 5% and the mass ratio of the metal oxide relative to the reinforcing material is 15%, and in a second kind preform the volumetric ratio of the reinforcing material is 15% and the mass ratio of the metal oxide relative to the reinforcing material is 15%.
  • Each preform has a rectangular parallelepiped shape of 20 x 20 x 40mm, and the fine pieces of the metal oxide were distributed substantially uniformly in the body of the preform.
  • the preform which includes an oxide of B as the metal oxide was preheated to 400 ° C while the other preforms were preheated to 600 C, and each said preform 10 was placed in a vessel 16 also as shown in Fig. 2, and then a molten matrix metal was poured into the vessel so as to form a bath 18 thereof, and then the molten matrix metal was solidified.
  • the matrix alloy was prepared in eight different types of aluminum alloy which were JIS AC1A including 0.1% Mg, JIS AC4C including 0.3% Mg, JIS AC4D including 0.5% Mg, JIS AC8A including 1% Mg, JIS AC7B including 10% Mg, and JIS AC4C added with 0.3% Mg, 0.3% Ca, and 0.3% Zr, respectively, and magnesium alloys prepared in three different types which were JIS FC-2, JIS MC-7 and JIS MC-8.
  • a composite material 20 was cut out from the solidified body prepared in the above-mentioned manner corresponding to the portion occupied by the preform, and then the composite material was cut also along a phantom plane 22 at a central portion thereof in Fig. 3. Then the cutout section was polished and investigated by the naked eye and a microscope for evaluation of the composite quality.
  • the aluminum alloy includes more than 0.5 Mg, Ca or Zr.
  • alumina short fibers as used in Embodiment 6 preforms were prepared to include only the alumina short fibers at 5%, 15% and 30% by volume.
  • silicon carbide whisker as used in Embodiment 6 preforms were prepared to include only the silicon carbide whisker at 5%, 15% and 40% by volume.
  • silicon nitride particles as used in Embodiment 6 preforms were prepared to include only the silicon nitride particles at 5%, 15% and 50% by volume.
  • the preform includes fine pieces of a determinate metal oxide or metal oxides. Therefore, investigations were conducted to determine what amount of the metal oxide or metal oxides is appropriate.
  • Preforms were prepared from the reinforcing material shown in Tables 18 and 19 and the fine pieces of metal oxides shown in Table 20. Then by using these preforms with the molten matrix metals shown in Table 20 it was tried to produce composite materials in the same manner as in Embodiment 6. Then the composite condition of each composite material thus obtained was evaluated in the same manner as in Embodiment 6. The mass ratio of the fine pieces of the metal oxide relative to the reinforcing material was set to 0%, 2.5%, 5%, 7.5%, 10%, 15%, 20% and 30%. The results of evaluation are shown in Table 20.
  • the mass ratio of the fine pieces of the metal oxide relative to the reinforcing material should be more than 7.5%, particularly more than 10%, and still more particularly more than 15%.
  • cylindrical preforms such as the one shown again in Fig. 4 having 40 mm outer diameter, 30 mm inner diameter and 50 mm length were prepared in the same manner as in Embodiment 6 so that the volumetric ratio of the reinforcing material and the mass ratio of the metal oxide relative to the reinforcing material are the same as in the first kind preform and the second kind preform in Embodiment 6.
  • 26 indicates the reinforcing material
  • 28 now indicates the fine pieces of the metal oxide.
  • the matrix metal the same eight kinds of molten aluminum alloys and the same three kinds of molten magnesium alloys as those used in Embodiment 6 were prepared.
  • each preform was preheated to the same temperature as in Embodiment 6, and then each preform 24 was held at a top portion thereof by a pincette-shaped holder 30 also as shown in Fig. 5, and a bottom end portion of each preform was brought into contact with a bath 34 of the molten matrix metal at 700 C contained in the vessel 32. Then the molten matrix metal infiltrated into the whole body of each preform from the lower end to the upper end thereof in 10-30 seconds. After the molten matrix metal had completely infiltrated into the whole body of the preform, the preform was removed from the bath of the molten matrix metal also as shown in Fig. 6 and was held in that condition until the molten matrix metal solidified. During this process the molten matrix metal was maintained in the preform as attached thereto under the surface tension.
  • the dimensions of the composite material cylindrical body were measured.
  • the outer diameter, the inner diameter and the length were 40-41 mm. 29-30 mm and 49-50 mm, respectively. It was confirmed that the composite material cylindrical body had substantially the same shape and dimensions as the preform.
  • Each composite material cylindrical body was cut for the inspection of the composite condition. It was confirmed that in all of the composite material cylindrical bodies the matrix metal has sufficiently infiltrated up to all surfaces of the preform.
  • the composite material can be produced in high quality in which the matrix metal is sufficiently infiltrated into the interstices of the reinforcing material at high efficiency and low cost with no need of pressurization of the molten matrix metal so that a composite material product having a predetermined shape and dimensions is directly produced at very high efficiency and yielding rate.

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EP19890304076 1988-04-30 1989-04-24 Verfahren zur Herstellung von Verbundmetall unter Beschleunigung der Infiltration des Matrix-Metalls durch feine Teilchen eines dritten Materials Expired - Lifetime EP0340957B1 (de)

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JP63108165A JPH07100834B2 (ja) 1988-04-30 1988-04-30 金属基複合材料の製造方法
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EP0340957A3 (en) 1990-06-06
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AU3339989A (en) 1989-11-02
DE68913800D1 (de) 1994-04-21
AU620862B2 (en) 1992-02-27

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