WO2019245000A1 - Matériau composite à base d'aluminium - Google Patents

Matériau composite à base d'aluminium Download PDF

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Publication number
WO2019245000A1
WO2019245000A1 PCT/JP2019/024598 JP2019024598W WO2019245000A1 WO 2019245000 A1 WO2019245000 A1 WO 2019245000A1 JP 2019024598 W JP2019024598 W JP 2019024598W WO 2019245000 A1 WO2019245000 A1 WO 2019245000A1
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Prior art keywords
aluminum
based composite
carbon fiber
mass
composite material
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PCT/JP2019/024598
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English (en)
Japanese (ja)
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謙一郎 関口
慶之 大窪
今村　寿之
尚也 床尾
一寿 杉江
佐伯　智則
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日立金属株式会社
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Priority to JP2020525806A priority Critical patent/JPWO2019245000A1/ja
Publication of WO2019245000A1 publication Critical patent/WO2019245000A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent

Definitions

  • the present invention relates to an aluminum-based composite material containing carbon fibers as a reinforcing material in a base structure, and more particularly, to an aluminum-based composite material in which carbon fibers are dispersed in a base structure formed by solid bonding of aluminum particles. It is about union.
  • Patent Documents 1 to 3 an aluminum-based composite material reinforced with carbon nanotubes has been proposed (for example, Patent Documents 1 to 3).
  • the present inventors have been unable to obtain an aluminum-based composite material having excellent mechanical properties in which all of tensile strength, elongation and Young's modulus show values equal to or higher than a certain value by the conventional method. I knew it was necessary.
  • the present invention has been made in view of such a problem, and an object of the present invention is to provide an aluminum-based composite material having excellent mechanical properties in which all of tensile strength, elongation, and Young's modulus show values equal to or more than a certain value. Aim.
  • the present invention provides an aluminum-based composite material containing carbon fibers as a reinforcing material in a matrix, wherein the matrix has 1 to 5% by mass of the carbon fibers, 0.5 to 7% by mass of Mg, the balance being Al and unavoidable impurities, and composed of columnar metal crystal grains oriented in substantially the same direction, and the major axis length of the columnar metal crystal grains along the orientation direction of the columnar metal crystal grains
  • the average value of the length L1 is 5.0 ⁇ m or less
  • the average value of the maximum length L2 of the short axis is 2.0 ⁇ m or less
  • the area ratio of the columnar metal crystal grains having L1 / L2 of 4 or more is 25% or less.
  • This is an aluminum-based composite material.
  • the carbon fibers are carbon nanofibers or carbon nanotubes.
  • the area ratio of aluminum carbide particles having an equivalent circle diameter of 500 nm or less existing in the matrix is 0.5 to 5%.
  • the base structure includes, in addition to Mg, any one element selected from the group consisting of Mn, Cr, Fe, Zr, Ti, and B in a total amount of 2.2 mass% or less, and the base structure precipitates in the base structure. It is desirable that the area ratio of the compound of the element is 4% or less.
  • the carbon fiber is a carbon nanotube or a carbon nanofiber
  • the carbon fiber is dispersed in the matrix, and the matrix can be efficiently reinforced.
  • the area ratio of aluminum carbide particles having an equivalent circle diameter of 500 nm or less is set to 0.5 to 5%, more preferably, the area of precipitates of compounds such as Mn, Cr, Fe, Zr, Ti, and B.
  • the rate is 4% or less, the columnar metal crystal grains can be efficiently refined, and higher mechanical properties can be obtained.
  • an aluminum-based composite material having sufficient mechanical properties can be provided.
  • the aluminum-based composite material according to the present embodiment is an aluminum-based composite material containing a carbon fiber as a reinforcing material in a base tissue, having 1 to 5% by mass of the carbon fiber, 0.5 to 7% by mass of Mg, the balance being Al and unavoidable impurities, columnar metal crystal grains oriented in substantially the same direction, and the long axis of the columnar metal crystal grains along the orientation direction of the columnar metal crystal grains.
  • the average value of the length L1 is 5.0 ⁇ m or less, the average value of the maximum length L2 of the short axis is 2.0 ⁇ m or less, and the area ratio of the columnar metal crystal grains having L1 / L2 of 4 or more is 25% or less.
  • the carbon fiber is preferably carbon nanofiber (CNF) or carbon nanotube (CNT).
  • the aluminum alloy constituting the base structure is composed of 0.5 to 7% by mass of Mg, the balance being Al and unavoidable impurities.
  • Mg Metal-Mg-based 5000-based alloy
  • A5083 specified in JIS (Japanese Industrial Standards) H4000.
  • An aluminum alloy (hereinafter, also referred to as JIS A5083 alloy or the like) may be used. If there is too much Mg, workability and elongation will fall, and if there is too little Mg which solid-solution strengthens a structure
  • the base structure may contain, in addition to Mg, any one element selected from the group consisting of Mn, Cr, Fe, Zr, Ti, and B in a total amount of 2.2% by mass or less.
  • the carbon fiber contained in a dispersed state in the base tissue has a mass ratio of 1 to 5% by mass with respect to the aluminum-based composite material.
  • the mechanical properties of the aluminum-based composite material are basically controlled by the proportion of carbon fibers contained as a reinforcing material, and are based on the mechanical properties of each of the aluminum alloy and carbon fibers constituting the matrix and the proportion of carbon fibers. It can be set according to the general rule. That is, if the carbon fiber content is less than 1% by mass, the ability of the carbon fiber to strengthen the base structure cannot be exhibited, and if the carbon fiber content exceeds 5% by mass, the processability is deteriorated and the elongation is reduced.
  • the content of the carbon fiber is determined by the infrared absorption method (integration method) specified in JIS Z2615. Can be measured in accordance with
  • FIG. 1A is a diagram showing an electron backscatter diffraction (EBSD) image of a base tissue in a plane parallel to the extrusion molding direction of the aluminum-based composite of Example 1 described later, and FIG. It is a figure which shows the EBSD image of the base structure
  • EBSD electron backscatter diffraction
  • the matrix structure in the aluminum-based composite material according to the present invention is composed of columnar metal crystal grains oriented in substantially the same direction as a processing (extrusion) direction such as extrusion.
  • the mechanical properties improve as the columnar metal crystal grains become finer. For this reason, it is desired to make the columnar metal crystal grains after processing as fine as possible.
  • the heating temperature of the sintered body, the extrusion ratio and Aluminum with excellent mechanical properties exceeding a certain level in all of tensile strength, elongation and Young's modulus by appropriately controlling the extrusion speed and controlling the size of the columnar metal crystal grains constituting the matrix structure.
  • the inventors of the present invention extrude a sintered body (workpiece) in a relatively low strain state, and perform recovery of a work-hardened base structure during processing in a mode mainly involving dynamic recovery.
  • the average value of the length L1 of the major axis along the orientation direction of the columnar metal crystal grains of the aluminum-based composite material according to the present invention obtained by controlling the processing conditions particularly in the extrusion molding step is 5. 0 ⁇ m or less, the average value of the maximum length L2 of the minor axis is 2.0 ⁇ m or less, and L1 / L2 is 4 or more columnar metal crystal grains (hereinafter, L1 / L2 is 4 or more columnar metal crystal grains is referred to as long drawn metal). Area ratio) is 25% or less.
  • the average value of each of the long axis length L1 and the short axis maximum length L2 of the columnar metal crystal grains is in the above range, and the long drawn metal crystal Since the area ratio of the grains is as low as 25% or less, the matrix structure is such that finely divided columnar metal crystals are uniformly distributed and has low anisotropy. As a result, excellent tensile strength and elongation are both achieved. Can be. It is difficult to make the average value of the length L1 of the major axis and the average value of the maximum length L2 of the minor axis along the orientation direction of the columnar metal crystal grains less than 0.4 ⁇ m in manufacturing.
  • the average value of the length L1 of the major axis and the average value of the maximum length L2 of the minor axis along the orientation direction of the columnar metal crystal grains are each 0.4 ⁇ m or more. Further, in order to obtain an aluminum-based composite material having both excellent Young's modulus and tensile strength, it is preferable that the lower limit of the length of the major axis L1 is 1.2 ⁇ m and the upper limit is 3.7 ⁇ m. It is desirable that the lower limit of the area ratio of the elongated metal crystal grains be 8% and the upper limit be 19%.
  • the length L1 of the major axis of the columnar metal crystal grain is a length of a line connecting two points where the length is the longest in the columnar metal crystal grain along the orientation direction of the columnar metal crystal grain.
  • the maximum length L2 of the short axis is a length of a line connecting two points having the longest length in the columnar metal crystal grains in a direction orthogonal to the long axis set as described above. Refers to.
  • the length L1 of the long axis and the maximum length L2 of the short axis can be confirmed, for example, as follows.
  • a structure photograph of a 24 ⁇ 24 ⁇ m field of view at an arbitrary cross section parallel to the extrusion direction of the aluminum-based composite material is taken, the structure photograph is image-analyzed, and the length of the long axis of all the crystal grains contained in the field of view (hereinafter referred to as “length”) L1 and the maximum length of the minor axis (hereinafter sometimes referred to as the maximum minor axis length) L2, and the major axis lengths L1 and L1 of the measured crystal grains are measured.
  • the maximum short axis length L2 is averaged.
  • L1 / L2 is calculated for each crystal grain in the visual field obtained by the above-described method, and L1 / L2 is selected to be 4 or more long elongated metal crystal grains, and the total length of the long elongated metal crystal grains in the visual field is selected.
  • the area ratio it is possible to calculate the area ratio of the elongated metal crystal grains having L1 / L2 of 4 or more. (Details will be described later.)
  • FIG. 2 is a scanning electron microscope (SEM) photograph of the matrix structure of the aluminum-based composite material. Fine aluminum carbide (Al 4 C 3 ) particles were confirmed in the matrix.
  • the carbon source of the aluminum carbide particles is considered to be carbon fibers.
  • the present inventors have found that aluminum carbide particles that affect the crystal grain size are not formed at the interface between the carbon fiber and the base structure, but are formed at a position away from the carbon fiber.
  • the present inventors presumed that the carbon source of the aluminum carbide particles was carbon pieces dropped or separated from carbon fibers in the production process. That is, in the carbon fiber acid treatment step described in detail below, by giving a predetermined damage to the carbon fiber, the carbon pieces are separated (separated) from the carbon fiber, and thereby the aluminum carbide is located at a position different from the boundary with the carbon fiber. It was estimated that particles would be produced. Therefore, it was presumed that the production amount of the aluminum carbide particles could be adjusted by adjusting the acid treatment conditions of the carbon fibers. It is considered that when such fine aluminum carbide particles are properly generated, the fine aluminum carbide particles exert a pinning effect of suppressing crystal grain growth, and the crystal grains are refined.
  • the area ratio of aluminum carbide particles having a circle equivalent diameter of 500 nm or less (hereinafter, sometimes referred to as fine aluminum carbide particles) existing in the matrix is 0.5 to 0.5%. Desirably, it is 5%.
  • the size and area ratio of the fine aluminum carbide particles can be adjusted by appropriately setting the production conditions described below.
  • the area ratio of the fine aluminum carbide particles is calculated, for example, as follows. First, in an arbitrary cross section of the aluminum-based composite material, in an arbitrarily selected field of 2.0 ⁇ 2.6 ⁇ m, Al mapping was performed by element mapping using energy dispersive X-ray spectrometry (EDX).
  • EDX energy dispersive X-ray spectrometry
  • the base structure may contain, in addition to Mg, any one of elements selected from the group consisting of Mn, Cr, Fe, Zr, Ti, and B in a total amount of 2.2% by mass or less. It is desirable that the area ratio of the compound of the element precipitated therein is 4% or less.
  • the lower limit of the total content of Mn, Cr, Fe, Zr, Ti, and B is 0.002% by mass, which is the level of unavoidable impurities. In this case, the area ratio of the compound (precipitate) is The lower limit is 0.01%.
  • the components of the above-mentioned elements can be measured by inductively coupled plasma (ICP) emission spectrometry.
  • the area ratio of the compound (precipitate) composed of each element such as Mg and Mn can be basically confirmed in the same manner as the area ratio of the aluminum carbide particles. That is, in an arbitrary cross section of the aluminum-based composite material, in a 2.0 ⁇ 2.6 ⁇ m arbitrarily selected visual field, the distribution of each element is obtained by element mapping using EDX, and a region where each element is present Is regarded as a region where precipitates are present.
  • a structure photograph including the precipitate is captured by TEM observation of the region where the precipitate is present, and the region where the precipitate is present is binarized by image analysis software based on the structure photograph, and the area of the precipitate is calculated.
  • the area ratio can be calculated by dividing the area of the precipitate in the visual field by the entire area. (Details will be described later.)
  • the size (L1, L2, L1 / L2) of the columnar metal crystal grains constituting the matrix can be realized by appropriately controlling the size (L1, L2, L1 / L2) of the columnar metal crystal grains constituting the matrix to a predetermined range.
  • the Young's modulus is 80 GPa or more
  • the tensile strength is 350 MPa or more
  • the elongation is 5% or more.
  • an aluminum-based composite having excellent mechanical properties.
  • the production method of the present embodiment is a carbon fiber acid treatment step of acid-treating the carbon fiber to form a functional group on the surface of the carbon fiber;
  • the carbon fiber slurry obtained in the carbon fiber slurry forming step and the metal powder slurry obtained in the metal powder slurry forming step are mixed so that the carbon fiber content becomes 1 to 5% by mass with respect to the metal powder.
  • the metal powder used in the metal powder slurry forming step is composed of 0.5 to 7% by mass of Mg, the balance being Al and unavoidable impurities,
  • the sintered body obtained in the sintering step is extruded at a heating temperature of 350 to 500 ° C., an extrusion ratio of 20 to 30, and an extrusion speed of 0.5 to 1
  • a carbon fiber to be used is prepared (step 100).
  • the type and fiber diameter of the carbon fiber used as the raw material are not particularly limited, but it is preferable to use carbon nanofiber (CNF), carbon nanotube (CNT), or the like.
  • the preferred purity of the carbon nanofiber or carbon nanotube (carbon fiber) is 90% or more, the preferred average diameter is 200 nm or less, and the preferred average length is 0.5 ⁇ m or more. If the purity is lower than 90%, the properties of the carbon fiber itself are deteriorated. If the average diameter is larger than 200 nm and the average length is shorter than 0.5 ⁇ m, the aspect ratio becomes small, and the effect as a fiber reinforcing material is reduced.
  • the lower limit value of the average diameter and the upper limit value of the average length of the carbon fiber are not particularly limited. However, in order to obtain a carbon fiber having an appropriate cost for industrial production, it is required to be 0.5 nm or more and 1000 ⁇ m or less, respectively. Is desirable.
  • Carbon fiber acid treatment step Step 101
  • the carbon fiber is subjected to an acid treatment (step 101).
  • a functional group is formed on the surface of the carbon fiber so that the carbon fiber is adsorbed on the surface of the metal powder.
  • the carbon fiber having the functional group formed in this way has improved affinity with a solution such as water or an organic solvent, and also has improved dispersibility in the solution.
  • the acid treatment step is performed by adding carbon fibers to the acid solution and then stirring the acid solution containing the carbon fibers. At this time, it is desirable to keep the carbon fibers in an acid solution at a temperature of 50 to 90 ° C. for 10 to 90 minutes.
  • the temperature of the acid solution is low or the holding time in the acid solution is short, the formation of the functional group becomes insufficient, and the amount of carbon pieces released from the carbon fiber decreases, and the columnar metal constituting the base structure is reduced.
  • the number of carbon sources for producing fine aluminum carbide particles having a crystal grain refining effect is reduced, and the mechanical properties of the obtained aluminum-based composite material are reduced.
  • the temperature of the acid solution is high or the holding time in the acid solution is long, excessive defects are formed on the surface of the carbon fiber or the carbon fiber becomes thin, so that the resulting aluminum-based composite material can Characteristic deteriorates.
  • the surface state (defect formation state) of the carbon fiber after the acid treatment can be evaluated by the ratio Id / Ig ratio of the intensity Id of the D band and the intensity Ig of the G band (graphite structure) measured by Raman spectroscopy. That is, the Id / Ig ratio increases as the number of carbon fiber defects increases due to the acid treatment.
  • the Id / Ig ratio after the acid treatment is desirably 0.1 to 0.7. If the temperature of the acid solution in the acid treatment step is low or the holding time in the acid solution is short, the Id / Ig ratio becomes smaller than 0.1, and the formation of the functional group becomes insufficient due to insufficient acid treatment.
  • the amount of carbon pieces released (separated) from the carbon fiber is reduced, and the carbon source for generating fine aluminum carbide particles having an effect of refining the columnar metal crystal grains constituting the matrix structure is undesirably reduced.
  • the temperature of the acid solution in the acid treatment step is high or when the holding time in the acid solution is long, the Id / Ig ratio becomes larger than 0.7, and excessive acid treatment causes excessive defects in carbon fibers. As a result, the strength of the carbon fiber decreases. Therefore, in any case, the mechanical properties of the aluminum-based composite material deteriorate.
  • the acid treatment of the carbon fiber under appropriate conditions, the carbon fiber is appropriately damaged, and a carbon piece serving as an oxygen source of the aluminum carbide particles is formed.
  • Step 102 A carbon fiber slurry is formed using the carbon fiber that has been subjected to the acid treatment in step 101 (step 102).
  • the acid-treated carbon fiber obtained in step 101 is added to the aqueous solution containing 0.5 to 1.5% by mass of the dispersing agent in an amount of 0.5 to 1.5% by mass to perform the dispersion treatment.
  • the dispersion medium solvent
  • alcohols such as ethanol can be used in addition to water.
  • sodium lauryl sulfate sodium dodecyl sulfate
  • sodium dodecylbenzenesulfonate alkylbenzenesulfonic acid, or the like
  • an ultrasonic processor a wet bead mill, a wet jet mill, or the like can be used. . By performing this treatment, even the carbon fibers entangled in a bundle can be loosened to obtain a slurry in which the carbon fibers are dispersed.
  • Preferred particle size of the carbon fiber at this time is 0.15 ⁇ 8 [mu] m at D 90.
  • Metal powder preparation step Step 103
  • a metal powder is prepared in parallel with or before or after preparing the carbon fiber (step 103).
  • the component, shape, and average particle size of the metal powder as a raw material are not particularly limited.
  • the preferable range of the composition of the metal powder is Mg: 0.5 to 7% by mass, with the balance being Al and unavoidable impurities.
  • any one of the elements selected from the group consisting of Mn, Cr, Fe, Zr, Ti, and B may be added in a total amount of 2.2% by mass or less.
  • Mg increases the strength of the matrix, and other elements form a compound with Al and the like to precipitate in the matrix and suppress the growth of crystal grains during recrystallization, thereby increasing the strength of the aluminum-based composite. There is.
  • Metal powder flake forming step Step 104
  • the metal powder is subjected to a scaly treatment (step 104).
  • a scalying step substantially spherical metal particles are crushed and flattened, and the metal powder is scaly.
  • the scaly treatment can increase the specific surface area of the metal particles and increase the amount of carbon fibers adsorbed on the metal powder.
  • the preferred specific surface area of the metal powder after the scaly treatment (hereinafter sometimes referred to as scaly powder) is 1.0 to 10 m 2 / g.
  • the preferred thickness of the scale powder is about 0.1 to 10 ⁇ m.
  • Various ball mills such as an attritor, a planetary ball mill, and a vibrating ball mill that can crush the metal powder by the impact of a ball can be used for the flakes of the metal powder.
  • a solvent for example, an organic solvent such as ethanol
  • the resulting oxide (hereinafter, may be referred to as an Al oxide) is generated.
  • the temperature in the chamber is desirably 20 ° C. or lower.
  • the oxygen concentration of the scaly powder increases, and Al oxide may be generated on the scaly powder surface.
  • the metal powder is excessively pulverized, the smaller the diameter of the generated flake powder, the larger the specific surface area. Therefore, the smaller the flake powder, the larger the ratio of the Al oxide per volume. For this reason, it is preferable to add a grinding aid to a solvent such as ethanol used for the purpose of lubrication (that is, prevention of excessive grinding) and prevention of oxidation.
  • the grinding aid binds to the surface of the metal powder to form a protective layer in the process of scaling, preventing further reaction, thereby preventing oxidation of the scale powder, and also reducing the scale powder to other scale powder or scale.
  • an impact medium such as a ball used for forming.
  • stearic acid or oleic acid as an organic acid dodecylbenzenesulfonic acid or sodium lauryl sulfate as a surfactant can be used, and among them, titanate (organic titanate) is excellent.
  • Titanate is a compound in which four OH groups of titanic acid (Ti (OH) 4 ) react with an organic acid, an organic phosphoric acid, an organic sulfonic acid, or the like to form an ester bond.
  • Ti (OH) 4 titanic acid
  • This compound comes into contact with the surface of the Al oxide or the new surface generated by the scaling process, two of the four esters are decomposed to form two Al—O—Ti bonds. That is, titanate is bonded to Al by two bonds, and the remaining two bonds are bonded to an organic acid, an organic phosphoric acid, an organic sulfonic acid, or the like by an ester bond.
  • An organic acid, an organic phosphoric acid, or an organic sulfonic acid which forms an ester bond with the above two bonds can be used as a grinding aid, but the use of titanate provides a stronger bond between Al—O—Ti. As a result, it is stably present on the scale powder surface and has excellent antioxidant and lubricating functions.
  • titanate When titanate is used as a grinding aid as a grinding aid, lubrication and oxidation prevention of the scale powder in the scale formation step, and titanate in the carbon fiber-adsorbed metal powder washing step and the heat treatment step described below performed after the scale formation step This is preferable in that both removal can be achieved. Further, when titanate is used as a grinding aid, it is preferable to add the titanate to the solvent in an amount of 0.1 to 5.0 parts by mass with respect to 100 parts by mass of the metal powder as a raw material of the flake powder. If the added amount of titanate is less than 0.1 part by mass, the lubrication and oxidation prevention of the flake powder cannot be sufficiently performed.
  • the solvent used in the ball mill examples include, in addition to ethanol, alcohols such as methanol, polyhydric alcohols such as ethylene glycol and glycerin, ketones such as acetone and methyl ethyl ketone, hydrocarbons such as hexane and heptane, and minerals.
  • a petroleum-based mixed solvent such as spirit can be used.
  • the scale powder is dried, it is desirable to use a non-oxidizing atmosphere having a low oxygen concentration in the atmosphere, such as a vacuum or Ar atmosphere. It is desirable that the scale powder after drying is stored in a vacuum to prevent oxidation. Oxidation of the scale powder is suppressed by the antioxidant measures in the scale formation step, and Al oxide generated on the scale powder surface is reduced.
  • the scalying step is not necessarily an essential step, and the scalying step may not be performed as long as the carbon fibers can be sufficiently adsorbed in the next step.
  • Metal powder slurry forming step Step 105
  • the metal powder in the case of passing through the above-mentioned scalying step, the metal powder can be read as the scaly powder.
  • the functionalities formed in step 101 carbon fiber acid treatment step
  • a slurry of metal powder is formed so that carbon fibers having a group on the surface can be easily adsorbed (step 105).
  • step 105 5 to 15% by mass of a metal powder is added to an aqueous solution in which the resin is dissolved, and the resultant is immersed and coated with the resin to obtain a slurry of the metal powder having a hydroxyl group formed on the surface.
  • polyvinyl alcohol PVA
  • polyvinyl pyrrolidone PVP
  • polyethylene glycol PEG
  • polyethylene oxide / propylene oxide copolymer EOPO
  • Carbon fiber adsorption step Step 106
  • the carbon fiber slurry obtained in step 102 (carbon fiber slurry forming step) and the metal powder slurry obtained in step 105 (metal powder slurry forming step) are mixed to adsorb the carbon fibers on the metal powder (step 106).
  • a metal powder having carbon fibers adsorbed thereon such that the content of carbon fibers is 1 to 5% by mass with respect to the composite material (hereinafter sometimes referred to as carbon fiber adsorbed metal powder) can be obtained.
  • the mixing ratio of the carbon fiber slurry and the metal powder slurry is selected according to the carbon fiber content of the aluminum-based composite material to be obtained.
  • a stirrer or a stirring blade can be used for mixing and adsorption.
  • the rotation speed of stirring is 500 to 800 rpm, and the time is about 30 minutes.
  • step 107 Carbon fiber-adsorbed metal powder cleaning step: Step 107
  • the carbon fiber-adsorbed metal powder is washed (step 107).
  • step 108 heat treatment step described later, the resin remaining on the carbon fiber-adsorbed metal powder is removed by heat treatment. However, if a portion of the resin is removed by washing before the heat treatment, the heat treatment time can be reduced. Can be shortened.
  • the carbon fiber-adsorbed metal powder washing step (hereinafter sometimes referred to as a powder washing step) is a step of washing the carbon fiber-adsorbed metal powder with suction filtration using pure water or an organic solvent.
  • suction filtration with the cleaning liquid may be performed a plurality of times.
  • the cleaning liquid used in the powder cleaning step is preferably an organic solvent from the viewpoint of suppressing oxidation of the carbon fiber-adsorbed metal powder and reducing Al oxide generated in the metal powder.
  • the first cleaning may be performed with pure water and the last cleaning may be performed with the organic solvent.
  • suction filtration when washing is performed a plurality of times, since the carbon fiber-adsorbed metal powder may come into contact with the atmosphere and be oxidized between washings, it is preferable to perform suction filtration while continuously supplying the washing liquid. At this time, for example, at the start of cleaning, suction filtration may be performed while supplying pure water, and after a predetermined time, suction filtration may be performed by switching from pure water to supplying an organic solvent. By doing so, it is possible to suppress the amount of the organic solvent used and to suppress oxidation during cleaning.
  • Organic solvents used for washing include alcohols such as ethanol and methanol, polyhydric alcohols such as ethylene glycol and glycerin, ketones such as acetone and methyl ethyl ketone, hydrocarbons such as hexane and heptane, and petroleum oils such as mineral spirits. Can be used. Note that the powder washing step is not always an essential step.
  • Step 108 Excess resin contained in the carbon fiber-adsorbed metal powder obtained in step 106 (107) is removed by heat treatment (step 108).
  • the initial furnace oxygen concentration is 1000 ppm or less
  • the final furnace oxygen concentration is 0 so that the metal powder is not oxidized and an oxide containing Mg (hereinafter sometimes referred to as Mg oxide) is not generated in the metal powder.
  • the resin contained in the carbon fiber-adsorbed metal powder is removed in an inert gas atmosphere having a low oxygen concentration of less than 0.1 ppb.
  • the heat treatment is preferably performed at a heating temperature of 350 to 500 ° C. and a holding time of 1 to 24 hours.
  • the heating temperature is lower than 350 ° C. or when the holding time is shorter than 1 hour, the resin is not sufficiently removed.
  • the heating temperature is higher than 500 ° C. or when the holding time is longer than 24 hours, reduction of the Al oxide by Mg contained in the metal powder (scale powder) proceeds, and as a result, excessive Mg oxide is contained in the metal powder. Is generated.
  • the amount of residual resin contained in the carbon fiber-adsorbed metal powder after the heat treatment step can be measured by thermogravimetric analysis (for example, TG-DTA2000SA manufactured by Bruker). Further, the amount of oxygen contained in the carbon fiber-adsorbed metal powder after the heat treatment step can be measured by an inert gas melting method, and a preferable range of the amount of oxygen is 4% by mass or less.
  • a green compact of carbon fiber-adsorbed metal powder is formed (step 109).
  • the green compact forming step is a step in which the carbon fiber-adsorbed metal powder obtained in step 108 (heat treatment step) is pressed at a low temperature using a press or the like to obtain a green compact.
  • Preferred conditions at this time are a temperature of 300 ° C. or less and a pressure of 200 to 800 MPa. Since the relative density of the green compact is increased by this molding process, the sintering time in the next step can be shortened. Note that the green compact forming step is not necessarily an essential step.
  • Step 110 A sintering process is performed to make the carbon fiber-adsorbed metal powder from which the resin has been removed or the green compact obtained in the green compact forming step into a bulk (step 110). Sintering is performed at 570 to 620 ° C. for 2 to 10 hours by heating in an inert gas atmosphere having an initial furnace oxygen concentration of 1000 ppm or less and a final furnace oxygen concentration of less than 0.1 ppb. In this sintering process, solid-phase joining of metal powders proceeds. At this time, Al oxide such as Al 2 O 3 covering the surface of the metal powder is reduced and removed by Mg dissolved in the metal powder, and a new metal surface where Al is exposed appears. Is promoted.
  • hot press or spark plasma sintering which performs sintering while applying pressure, may be used.
  • spark plasma sintering which performs sintering while applying pressure.
  • the carbon pieces released (separated) from the carbon fibers in the acid treatment step and contained in the green compact formed in the green compact forming step react with aluminum to form fine aluminum carbide. Particles are formed.
  • Extrusion molding process Step 111
  • the obtained sintered body is processed by extrusion (step 111).
  • Extrusion can improve the density of the aluminum-based composite, refine the base structure, and impart shape.
  • the method for processing the sintered body is not limited to extrusion, and plastic working methods such as forging and pressing can be applied. Are suitable.
  • Preferable conditions for the extrusion molding are a heating temperature of the sintered body to be processed of 350 to 500 ° C., an extrusion ratio of 20 to 30, and an extrusion speed of 0.5 to 10.0 mm / s. When the heating temperature is lower than 350 ° C., the composition fluidity is low. When the heating temperature is higher than 500 ° C., dynamic recrystallization proceeds, crystal grains grow, and strength decreases.
  • the extrusion ratio can be calculated by the following equation.
  • R A0 / A here, R: Extrusion ratio A0: Cross-sectional area in the direction perpendicular to the extrusion direction of the workpiece (sintered body) before extrusion A: Cross-sectional area in the direction perpendicular to the extrusion direction of the workpiece after extrusion
  • the aluminum-based composite material according to the present invention is capable of forming a sintered body (workpiece) by appropriately controlling the heating temperature, the extrusion ratio, and the extrusion speed of the sintered body in the extrusion molding process during the manufacturing process. Since it is formed by extrusion molding in a low strain state, the columnar metal crystal grains constituting the matrix structure are refined, and an aluminum-based composite material having both excellent tensile strength and elongation can be realized. Furthermore, in the carbon fiber acid treatment step, the amount of the functional group attached to the carbon fiber and the damage to the carbon fiber are controlled by acid-treating the carbon fiber under appropriate conditions, and fine aluminum carbide particles are formed. The amount of carbon pieces released (separated) from the carbon fiber, which is the carbon source for the application, is also controlled, so that the fine aluminum carbide particles produced are pinned to further refine the columnar metal crystal grains constituting the matrix. Can be achieved.
  • Example 1 In Example 1, 4.52% by mass of Mg-0.66% by mass of Mn-0.21% by mass of Fe-an aluminum-based composite material in which carbon fibers are dispersed in a base structure formed using a metal powder composed of Al and unavoidable impurities was prepared as follows.
  • Carbon nanofibers (VGCF (registered trademark) manufactured by Showa Denko KK, average outer diameter 150 nm, average length 6 ⁇ m, purity 99% or more) were used as carbon fibers.
  • the carbon fiber was analyzed with a Raman spectrometer (InVia Quontor manufactured by Renishaw), and the ratio (Id / peak) of the peak intensity Id called the D band near 1350 cm ⁇ 1 and the peak called the G band near 1570 cm ⁇ 1 (Id / Ig) was confirmed to be 0.03.
  • Id / Ig of the carbon fiber described below was confirmed by the same method.
  • Carbon fiber acid treatment step Next, in order to carry out the acid treatment of the carbon fiber, 150 g of sulfuric acid and 50 g of nitric acid were mixed to prepare an acid solution, and 2 g of the carbon fiber was added thereto, and a water bath stirrer heated to 70 ° C. (EWS100RD manufactured by AS ONE) ) And stirred at 100 rpm for 60 minutes.
  • the carbon fiber was washed with pure water and ethanol, filtered by suction, and dried at 80 ° C. to obtain a carbon fiber having a carboxyl group formed on the surface.
  • Id / Ig of the carbon fiber after the acid treatment was confirmed, it was 0.47.
  • Metal powder preparation process As the metal powder, atomized powder composed of 4.52% by mass of Mg, 0.66% by mass of Mn, 0.21% by mass of Fe, the balance of Al and inevitable impurities and having a particle size (D 50 ) of about 10 ⁇ m was used. The components of the atomized powder were confirmed by ICP emission spectrometry (ICPS-8100, manufactured by Shimadzu Corporation). In this example, as described later, the metal powder is flaked to form flake powder, so that the metal powder (atomized powder) prepared in this step is a raw material for flake powder (described below). The same applies to other examples and comparative examples.
  • a substantially spherical metal powder is flattened into a flat crushed shape.
  • the temperature in the chamber at the time of the scale formation treatment was 15 ° C.
  • the room temperature of the chamber atmosphere was 20 ° C.
  • the humidity was 50%
  • the dew point temperature was 9.3 ° C. That is, the flakes were formed in the chamber at a temperature not lower than the dew point and not higher than 20 ° C.
  • the suspension was taken out, dried in the air at 85 ° C. for 2 hours, and had a thickness of about 1 to 4 ⁇ m, an average diameter (D 50 in number frequency) of 24 ⁇ m, and a specific surface area of about 4.5 m 2. / G, and a scale powder having an oxygen concentration of 1.7% by mass.
  • the specific surface area of the scale powder was measured with a specific surface area meter (Tristar II3020 manufactured by Shimadzu Corporation).
  • the oxygen concentration of the scale powder was measured with an oxygen nitrogen (ON) analyzer (ON836 manufactured by LECO).
  • the oxygen concentration of the scale powder (metal powder) described below was also confirmed by the same method.
  • Metal powder slurry forming step Next, a metal powder slurry was formed. Pure water and polyvinyl alcohol (Poval (registered trademark) manufactured by Denka) were prepared. A container filled with 1000 ml of pure water was heated in a water bath stirrer (EWS100RD manufactured by AS ONE) heated to 95 ° C., and 30 g of polyvinyl alcohol was added with stirring, followed by stirring at 450 rpm for 1 hour.
  • EWS100RD water bath stirrer
  • Carbon fiber adsorption process Next, the carbon fibers were adsorbed on the scale powder (metal powder). A metal powder slurry containing 100 g of flake powder to which PVA was attached was added to 1200 ml of pure water, and a carbon fiber slurry containing 2 g of the above-described carbon fiber was added while stirring at 750 rpm using a stirrer (F-205D manufactured by Tokyo Glass Instruments). 200 ml was added, and the carbon fiber was adsorbed on the scale powder to obtain a scale powder on which the carbon fiber was adsorbed.
  • a stirrer F-205D manufactured by Tokyo Glass Instruments
  • the scale powder after the powder washing step is heat-treated at 450 ° C. for 2 hours in an atmosphere of a heat treatment furnace in an argon atmosphere (initial furnace oxygen concentration: 312 ppm, final furnace oxygen concentration: 0.1 ppb or less).
  • the polyvinyl alcohol was removed from the powder.
  • the oxygen content of the scale powder after the heat treatment was 2.6%.
  • the carbon content of the scale powder was measured with a carbon sulfur (CS) analyzer (CS844 manufactured by LECO) in accordance with the infrared absorption method (integration method) of JIS Z2615.
  • the carbon content of the scale powder was 1.9% by mass.
  • the carbon content of the scale powder described below was confirmed by the same method.
  • extrusion molding was performed using a 2000 kN press machine (EFP-200 manufactured by Asai Sangyo) and an extrusion die 10 shown in FIG.
  • the inside diameter (A in the figure) of the extrusion die 10 is 40.5 mm
  • the inside diameter (B in the figure) on the exit side is 8.0 mm
  • the die angle (C in the figure) is 45 °.
  • a sintered body having a diameter of 40 mm and a height of 22 mm was preheated at 450 ° C., it was inserted into an extrusion die 10 heated to 450 ° C., and extruded at an extrusion ratio of 25 and an extrusion speed of 5 mm / s.
  • Example 1 With respect to the base structure of the aluminum-based composite material having a diameter of 8.0 mm of Example 1 obtained by extrusion molding, its components were confirmed by the above-described ICP emission spectrometry.
  • the components of the matrix structure of the aluminum-based composite material of Example 1 were 4.50% by mass of Mg, 0.64% by mass of Mn, 0.20% by mass of Fe, the balance being Al and inevitable impurities. That is, the total amount of (Mn, Cr, Fe, Zr, Ti, B) was 0.84% by mass.
  • the carbon content of the aluminum-based composite material was measured by the above-mentioned CS analyzer in accordance with the infrared absorption method (integration method) of JIS Z2615.
  • the carbon content of the aluminum-based composite material of Example 1 was 1.9% by mass.
  • a part of the carbon fibers adsorbed on the flake powder is combined with aluminum in the sintering process to become aluminum carbide, but the amount of the generated carbon is small with respect to the amount of the added carbon fibers, and is measured as described above.
  • the carbon content may be regarded as the content of the carbon fiber contained in the aluminum-based composite material. (The same applies to examples and comparative examples described below.)
  • EBSD Electron Diffraction
  • the average of the major axis length L1 and the maximum minor axis length L2 of each of the obtained crystal grains in the three visual fields was defined as the average value of the major axis length L1 and the average value of the maximum minor axis length L2 of the columnar metal crystal grains. .
  • L1 / L2 (aspect ratio) of each crystal grain is calculated based on the long axis length L1 and the maximum short axis length L2 of the crystal grains in each visual field obtained as described above, and L1 / L2 in 3 visual fields is 4
  • the area of the long elongated metal crystal grains was determined, and the area was divided by the area of all three visual fields to calculate the area ratio.
  • the major axis length L1, the maximum minor axis length L2, and L1 / L2 of the crystal grains were confirmed by the same method.
  • the average value of the long axis length L1 of Example 1 was 3.5 ⁇ m
  • the average value of the maximum short axis length L2 was 1.2 ⁇ m
  • the mechanical properties of the aluminum-based composite material of Example 1 were evaluated.
  • the mechanical properties were set so that the crosshead speed was 1 mm / min in accordance with JIS Z2241 using a test piece 11 having the following dimensions shown in FIG. 5 prepared by processing from an aluminum-based composite material after extrusion molding. It was determined by performing a tensile test with a universal testing machine (Instron 5982). The central axis of the test piece and the extrusion direction of the extrusion were made to coincide.
  • the mechanical properties of the aluminum-based composite were confirmed by the same method.
  • Example 1 As shown in Table 2, the mechanical properties of Example 1 were a Young's modulus of 92 GPa, a tensile strength of 386 MPa, and an elongation of 8.3%.
  • the area ratio of the fine aluminum carbide particles having an equivalent circle diameter of 500 nm or less was determined as follows. Any three visual fields of the above-mentioned arbitrary cross section are imaged by a scanning transmission electron microscope (STEM, Hitachi HD-2100) with a visual field of 2.0 ⁇ 2.6 ⁇ m, and EDX mapping is performed for each of the three visual fields. The distributions of Al and C were obtained by. For each visual field, the distribution of Al and C was converted to monochrome by the image analysis software “AT-image”, the brightness was inverted, and the coexisting region of Al and C was regarded as the region where aluminum carbide particles exist.
  • STEM scanning transmission electron microscope
  • a tissue photograph containing the aluminum carbide particles is captured as a dark-field image by TEM observation of the region where the aluminum carbide particles are present, and the structure photograph is automatically binarized by the particle analysis mode of the image analysis software “A image kun”.
  • a image kun the image analysis software “A image kun”.
  • the outer edge of the specified aluminum carbide particles is separated, the equivalent circle diameter and the area of the aluminum carbide particles are calculated, and the area of the minute aluminum carbide particles having an equivalent circle diameter of 500 nm or less in each field is divided by the area of the entire field of view.
  • the area ratio of the fine aluminum carbide particles was calculated, and the average value of the three visual fields was defined as the area ratio of the fine aluminum carbide particles.
  • the area ratio of the fine aluminum carbide particles of Example 1 was 1.6%.
  • the area ratio of the fine aluminum carbide particles in the aluminum-based composite material was confirmed by the same method.
  • the area ratio of compounds (precipitates) of elements such as Mn and Cr was determined as follows. Any three visual fields of the above-mentioned arbitrary cross section were imaged with the above-mentioned STEM at a visual field of 2.0 ⁇ 2.6 ⁇ m, and the distribution of each element was obtained by EDX mapping for each of the three visual fields. For each field of view, the distribution of each element was converted to monochrome by the image analysis software “AT-image”, the luminance was inverted, and the area where each element was present was regarded as the area where the precipitate was present.
  • a structure photograph including the precipitate is captured as a dark-field image by TEM observation of the region where the precipitate exists, and the structure photograph is automatically binarized by the particle analysis mode of the image analysis software “A image-kun” to precipitate. Identified things. Thereafter, the outer edge of the specified precipitate is separated, the area of the precipitate is calculated, the area ratio by dividing the area in each visual field by the area of the entire visual field is calculated, and the average value of the three visual fields is calculated as the area of the precipitate. Rate. As shown in Table 2, the area ratio of the precipitate of Example 1 was 1.3%. In Examples and Comparative Examples described below, the area ratio of the precipitate of the aluminum-based composite material was confirmed by the same method.
  • Example 2 The same metal powder and carbon fiber as in Example 1 were used, but the sintering conditions and extrusion molding conditions were changed. Under the same conditions as in Example 1, the carbon fiber and the metal powder were treated, the carbon fiber was adsorbed on the flake powder, and then heat treatment was performed. The carbon content of the scale powder to which the carbon fibers had been adsorbed after the heat treatment was 2.0% by mass. Thereafter, the compact obtained by compacting was held at 620 ° C. for 12 hours in the same argon atmosphere as in Example 1 and sintered to obtain a sintered body.
  • extrusion molding was performed using the same press machine as in Example 1.
  • the extrusion die used in Example 2 had an inlet inner diameter (A in FIG. 4) of 40.5 mm, an outlet inner diameter (B in FIG. 4) of 7.3 mm, and a die angle (C in FIG. 4). ) Is 45 °.
  • a sintered body having a diameter of 40 mm and a height of 22 mm was preheated at 350 ° C., it was inserted into an extrusion mold heated to 350 ° C. and extruded at an extrusion ratio of 30 and an extrusion speed of 0.5 mm / s. .
  • Example 2 With respect to the aluminum-based composite material having a diameter of 7.3 mm of Example 2 obtained by the extrusion molding, the components of the base structure and the amount of carbon were measured in the same manner as in Example 1.
  • the components of the matrix structure of the aluminum-based composite material of Example 2 were Mg 4.49% by mass, Mn 0.65% by mass, Fe 0.20% by mass, the balance Al and unavoidable impurities, and the carbon content of the aluminum-based composite material was 2%. 0.0% by mass. That is, the total amount of (Mn, Cr, Fe, Zr, Ti, B) was 0.85% by mass.
  • Example 2 When the structure of the crystal grains of the aluminum-based composite material of Example 2 was observed in the same manner as in Example 1, the average value of the major axis length L1 of Example 2 was 1.2 ⁇ m, and the average of the maximum minor axis length L2. The value was 0.8 ⁇ m, and the area ratio of the elongated metal crystal grains having L1 / L2 of 4 or more was 8%.
  • Example 2 When the mechanical properties of the aluminum-based composite material of Example 2 were evaluated in the same manner as in Example 1, the mechanical properties of Example 2 were as follows: a Young's modulus of 93 GPa, a tensile strength of 398 MPa, and an elongation of 8.1%. there were.
  • the test piece 11 of Example 2 was 7.3mm gripping portion diameter d a of FIG.
  • Example 2 when the area ratio of the fine aluminum carbide particles having a circle equivalent diameter of 500 nm or less was evaluated, the area ratio of the fine aluminum carbide particles of Example 2 was 2.1%. Similarly, when the area ratio of a compound (precipitate) of an element such as Mn or Cr was evaluated, the area ratio of the precipitate of Example 2 was 2.1%.
  • Example 3 The same metal powder and carbon fiber as in Example 1 were used, but the acid treatment conditions and the extrusion molding conditions were changed.
  • an acid solution was prepared by mixing 150 g of sulfuric acid and 50 g of nitric acid, and 2 g of carbon fiber was added thereto, followed by warm bathing in a water bath stirrer (EWS100RD manufactured by AS ONE) heated to 90 ° C. The mixture was stirred at 100 rpm for 70 minutes.
  • the carbon fiber was washed and dried in the same manner as in Example 1, and the Id / Ig of the carbon fiber after the acid treatment was confirmed to be 0.67.
  • Example 2 Under the same conditions as in Example 1, the carbon fiber and the metal powder were treated, and the carbon fiber was adsorbed on the scale powder, followed by heat treatment, compacting and sintering.
  • the carbon content of the scale powder on which the carbon fibers had been adsorbed after the heat treatment was 1.5% by mass.
  • extrusion molding was performed using the same press machine as in Example 1.
  • the extrusion die used in Example 3 had an inlet inner diameter (A in FIG. 4) of 40.5 mm, an outlet inner diameter (B in FIG. 4) of 8.9 mm, and a die angle (C in FIG. 4). ) Is 45 °.
  • a sintered body having a diameter of 40 mm and a height of 22 mm was preheated at 500 ° C., it was inserted into an extrusion mold heated to 500 ° C., and extruded at an extrusion ratio of 20 and an extrusion speed of 10 mm / s.
  • Example 3 With respect to the aluminum-based composite material having a diameter of 8.9 mm of Example 3 obtained by this extrusion molding, the components of the base structure and the amount of carbon were measured in the same manner as in Example 1.
  • the components of the matrix structure of the aluminum-based composite of Example 3 were 4.52% by mass of Mg, 0.64% by mass of Mn, 0.19% by mass of Fe, the balance of Al and inevitable impurities, and the carbon content of the aluminum-based composite was 1%. It was 0.5% by mass. That is, the total amount of (Mn, Cr, Fe, Zr, Ti, B) was 0.83% by mass.
  • Example 3 When the structure of the crystal grains of the aluminum-based composite material of Example 3 was observed in the same manner as in Example 1, the average value of the major axis length L1 of Example 3 was 4.9 ⁇ m, and the average of the maximum minor axis length L2 was 4.9 ⁇ m. The value was 1.6 ⁇ m, and the area ratio of long elongated metal crystal grains having L1 / L2 of 4 or more was 23%.
  • Example 3 When the mechanical properties of the aluminum-based composite material of Example 3 were evaluated in the same manner as in Example 1, the mechanical properties of Example 3 were as follows: a Young's modulus of 83 GPa, a tensile strength of 373 MPa, and an elongation of 8.9%. there were.
  • Example 1 the area ratio of the fine aluminum carbide particles having an equivalent circle diameter of 500 nm or less was evaluated. As a result, the area ratio of the fine aluminum carbide particles in Example 3 was 2.1%. Similarly, when the area ratio of a compound (precipitate) of an element such as Mn or Cr was evaluated, the area ratio of the precipitate of Example 3 was 0.8%.
  • Example 4 The Mg content of the metal powder was changed from that of Example 1, and as the metal powder, 6.80 mass% of Mg-0.66 mass% of Mn-0.21 mass% of Fe-the particle diameter composed of the balance of Al and inevitable impurities (D 50 ) Used an atomized powder of about 10 ⁇ m.
  • the conditions for exfoliating the atomized powder, the conditions for the carbon fiber used and its acid treatment, the conditions for adsorption, the conditions for sintering and the conditions for extrusion molding were all the same as in Example 1.
  • Example 4 With respect to the obtained aluminum-based composite material of Example 4 having a diameter of 8.0 mm, the components of the base structure and the amount of carbon were measured in the same manner as in Example 1.
  • the components of the base structure of the aluminum-based composite material of Example 4 were 6.80% by mass of Mg, 0.64% by mass of Mn, 0.20% by mass of Fe, the balance of Al and inevitable impurities, and the carbon content of the aluminum-based composite material was 1%. 9.9% by mass. That is, the total amount of (Mn, Cr, Fe, Zr, Ti, B) was 0.84% by mass.
  • Example 4 When the structure of the crystal grains of the aluminum-based composite material of Example 4 was observed in the same manner as in Example 1, the average value of the major axis length L1 in Example 4 was 3.1 ⁇ m, and the average value of the maximum minor axis length L2 was 3.1 ⁇ m. The value was 1.1 ⁇ m, and the area ratio of the elongated metal crystal grains having L1 / L2 of 4 or more was 16%.
  • Example 4 When the mechanical properties of the aluminum-based composite material of Example 4 were evaluated in the same manner as in Example 1, the mechanical properties of Example 4 were as follows: a Young's modulus of 89 GPa, a tensile strength of 390 MPa, and an elongation of 7.7%. there were.
  • Example 4 when the area ratio of the fine aluminum carbide particles having a circle equivalent diameter of 500 nm or less was evaluated, the area ratio of the fine aluminum carbide particles of Example 4 was 1.5%. Similarly, when the area ratio of a compound (precipitate) of an element such as Mn or Cr was evaluated, the area ratio of the precipitate of Example 4 was 1.4%.
  • Example 5 The Mg content of the metal powder was changed from that of Example 1, and as the metal powder, the particle diameter (D 50) of Mg 2.50 mass% -Mn 0.66 mass% -Fe 0.21 mass% -remaining Al and inevitable impurities ) Used an atomized powder of about 10 ⁇ m.
  • the conditions for exfoliating the atomized powder, the conditions for the carbon fiber used and its acid treatment, the conditions for adsorption, the conditions for sintering and the conditions for extrusion molding were all the same as in Example 1.
  • the carbon fiber was washed and dried in the same manner as in Example 1, and the Id / Ig of the carbon fiber after the acid treatment was confirmed to be 0.47.
  • Example 5 With respect to the obtained aluminum-based composite material having a diameter of 8.0 mm in Example 5, the components of the base structure and the amount of carbon were measured in the same manner as in Example 1.
  • the components of the matrix structure of the aluminum-based composite of Example 5 were Mg 2.50% by mass, Mn 0.64% by mass, Fe 0.20% by mass, the balance Al and inevitable impurities, and the carbon content of the aluminum-based composite was 1%. 9.9% by mass. That is, the total amount of (Mn, Cr, Fe, Zr, Ti, B) was 0.84% by mass.
  • Example 5 When the structure of the crystal grains of Example 5 was observed in the same manner as in Example 1, the average value of the major axis length L1 of Example 5 was 3.7 ⁇ m, and the average value of the maximum minor axis length L2 was 1.4 ⁇ m. , L1 / L2 was 4 or more, and the area ratio of the elongated metal crystal grains was 19%.
  • Example 5 When the mechanical properties of the aluminum-based composite material of Example 5 were evaluated in the same manner as in Example 1, the mechanical properties of Example 5 were as follows: a Young's modulus of 91 GPa, a tensile strength of 385 MPa, and an elongation of 8.5%. there were.
  • Example 5 when the area ratio of the fine aluminum carbide particles having a circle equivalent diameter of 500 nm or less was evaluated, the area ratio of the fine aluminum carbide particles of Example 5 was 1.6%. Similarly, when the area ratio of a compound (precipitate) of an element such as Mn or Cr was evaluated, the area ratio of the precipitate of Example 5 was 1.2%.
  • Example 6 The Mg content of the metal powder was changed from that of Example 1, and as the metal powder, the particle diameter (D 50) of Mg 1.00 mass% -Mn 0.66 mass% -Fe 0.21 mass% -remaining Al and unavoidable impurities ) Used an atomized powder of about 10 ⁇ m.
  • the conditions for exfoliating the atomized powder, the conditions for the carbon fiber used and its acid treatment, the conditions for adsorption, the conditions for sintering and the conditions for extrusion molding were all the same as in Example 1.
  • the carbon fiber was washed and dried in the same manner as in Example 1, and the Id / Ig of the carbon fiber after the acid treatment was confirmed to be 0.47.
  • Example 6 With respect to the obtained aluminum-based composite material having a diameter of 8.0 mm of Example 6, the components of the base structure and the amount of carbon were measured in the same manner as in Example 1.
  • the components of the matrix structure of the aluminum-based composite material of Example 6 were Mg 1.00% by mass, Mn 0.64% by mass, Fe 0.20% by mass, the balance of Al and inevitable impurities, and the aluminum-based composite material had a carbon content of 1%. 9.9% by mass. That is, the total amount of (Mn, Cr, Fe, Zr, Ti, B) was 0.84% by mass.
  • Example 6 When the structure of the crystal grains of the aluminum-based composite material of Example 6 was observed in the same manner as in Example 1, the average value of the major axis length L1 of Example 6 was 3.9 ⁇ m, and the average value of the maximum minor axis length L2 was The value was 1.7 ⁇ m, and the area ratio of the elongated metal crystal grains having L1 / L2 of 4 or more was 22%.
  • Example 6 When the mechanical properties of the aluminum-based composite material of Example 6 were evaluated in the same manner as in Example 1, the mechanical properties of Example 6 were as follows: a Young's modulus of 84 GPa, a tensile strength of 368 MPa, and an elongation of 9.5%. there were.
  • Example 6 when the area ratio of the fine aluminum carbide particles having an equivalent circle diameter of 500 nm or less was evaluated, the area ratio of the fine aluminum carbide particles of Example 6 was 1.5%. Similarly, when the area ratio of a compound (precipitate) of an element such as Mn or Cr was evaluated, the area ratio of the precipitate of Example 6 was 1.1%.
  • Example 7 An aluminum-based composite material in which carbon fibers were dispersed was prepared under the same conditions as in Example 1 except that the amount of carbon fibers (CNF) added in the carbon fiber slurry forming step was changed.
  • CNF carbon fibers
  • Example 1 An acid treatment and a scale treatment were performed in the same procedure as in Example 1.
  • the carbon fiber was washed and dried in the same manner as in Example 1, and the Id / Ig of the carbon fiber after the acid treatment was confirmed to be 0.47.
  • Prepare sodium lauryl sulfate (manufactured by Showa Chemical Co., concentration: 99% or more), pure water and an ultrasonic treatment device (Branson ultrasonic homogenizer DCX S20: 1.25), and add 2 g of sodium lauryl sulfate to 200 ml of pure water.
  • 5.0 g of the carbon fiber after acid treatment was added, and ultrasonic treatment was performed to obtain a carbon fiber slurry.
  • carbon fibers were adsorbed to the scale powder, and then heat treatment was performed.
  • the carbon content of the scale powder to which the carbon fibers were adsorbed was 4.8% by mass.
  • Example 7 Thereafter, under the same conditions as in Example 1, green compaction, sintering, and extrusion molding were performed on the aluminum-based composite material of Example 7 having a diameter of 8.0 mm, which was obtained in the same manner as in Example 1. And the amount of carbon were measured.
  • the components of the matrix structure of the aluminum-based composite of Example 7 were 4.51% by mass of Mg, 0.64% by mass of Mn, 0.20% by mass of Fe, the balance of Al and inevitable impurities, and the carbon content of the aluminum-based composite was 4%. It was 0.8% by mass. That is, the total amount of (Mn, Cr, Fe, Zr, Ti, B) was 0.84% by mass.
  • Example 7 When the structure of the crystal grains of the aluminum-based composite material of Example 7 was observed in the same manner as in Example 1, the average value of the major axis length L1 of Example 7 was 1.7 ⁇ m, and the average value of the maximum minor axis length L2 was 1.7 ⁇ m. The value was 0.9 ⁇ m, and the area ratio of long elongated metal crystal grains having L1 / L2 of 4 or more was 12%.
  • Example 7 When the mechanical properties of the aluminum-based composite material of Example 7 were evaluated in the same manner as in Example 1, the mechanical properties of Example 7 were as follows: a Young's modulus of 109 GPa, a tensile strength of 457 MPa, and an elongation of 5.0%. there were.
  • Example 7 when the area ratio of the fine aluminum carbide particles having an equivalent circle diameter of 500 nm or less was evaluated, the area ratio of the fine aluminum carbide particles in Example 7 was 3.8%. Similarly, when the area ratio of a compound (precipitate) of an element such as Mn or Cr was evaluated, the area ratio of the precipitate of Example 7 was 2.0%.
  • Example 8 An aluminum-based composite material in which carbon fibers were dispersed was prepared under the same conditions as in Example 1 except that the amount of carbon fibers (CNF) added in the carbon fiber slurry forming step was changed.
  • CNF carbon fibers
  • Example 1 An acid treatment and a scale treatment were performed in the same procedure as in Example 1.
  • the carbon fiber was washed and dried in the same manner as in Example 1, and the Id / Ig of the carbon fiber after the acid treatment was confirmed to be 0.47.
  • Prepare sodium lauryl sulfate (manufactured by Showa Chemical Co., concentration: 99% or more), pure water and an ultrasonic treatment device (Branson ultrasonic homogenizer DCX S20: 1.25), and add 2 g of sodium lauryl sulfate to 200 ml of pure water.
  • 1.2 g of the carbon fiber after the acid treatment was added, and ultrasonic treatment was performed to obtain a carbon fiber slurry.
  • carbon fibers were adsorbed to the scale powder, and a heat treatment was performed.
  • the carbon content of the scale powder to which the carbon fibers were adsorbed was 1.2% by mass.
  • Example 8 Thereafter, under the same conditions as in Example 1, green compaction, sintering, and extrusion molding were performed, and the base structure of the aluminum-based composite having a diameter of 8.0 mm in Example 8 was obtained in the same manner as in Example 1. And the amount of carbon were measured.
  • the components of the base structure of the aluminum-based composite of Example 8 were 4.52% by mass of Mg, 0.64% by mass of Mn, 0.20% by mass of Fe, the balance of Al and inevitable impurities, and the carbon content of the aluminum-based composite was 1%. 0.2% by mass. That is, the total amount of (Mn, Cr, Fe, Zr, Ti, B) was 0.84% by mass.
  • Example 8 When the structure of the crystal grains of the aluminum-based composite material of Example 8 was observed in the same manner as in Example 1, the average value of the major axis length L1 of Example 8 was 4.0 ⁇ m, and the average of the maximum minor axis length L2 was The value was 1.8 ⁇ m, and the area ratio of the elongated metal crystal grains having L1 / L2 of 4 or more was 20%.
  • Example 8 When the mechanical properties of the aluminum-based composite material of Example 8 were evaluated in the same manner as in Example 1, the mechanical properties of Example 8 were as follows: a Young's modulus of 82 GPa, a tensile strength of 351 MPa, and an elongation of 12.6%. there were.
  • Example 1 the area ratio of the fine aluminum carbide particles having an equivalent circle diameter of 500 nm or less was evaluated. As a result, the area ratio of the fine aluminum carbide particles in Example 8 was 0.7%. Similarly, when the area ratio of a compound (precipitate) of an element such as Mn or Cr was evaluated, the area ratio of the precipitate of Example 8 was 0.9%.
  • Example 9 An aluminum-based composite material in which carbon fibers were dispersed was produced under the same conditions as in Example 1 except that the acid treatment conditions for the carbon fibers were changed.
  • Example 9 an acid solution was prepared by mixing 150 g of sulfuric acid and 50 g of nitric acid, and 2 g of carbon fiber was added thereto, followed by warm bathing in a water bath stirrer (EWS100RD manufactured by AS ONE) heated to 90 ° C. Stirred at 100 rpm for 90 minutes.
  • EWS100RD water bath stirrer
  • the carbon fiber was washed and dried in the same manner as in Example 1, and the Id / Ig of the carbon fiber after the acid treatment was confirmed to be 0.70.
  • Example 2 Under the same conditions as in Example 1, the carbon fiber and the metal powder were treated, the carbon fiber was adsorbed on the scale powder, heat treatment, green compaction and sintering were performed, and extrusion molding was performed.
  • Example 9 With respect to the obtained aluminum-based composite material having a diameter of 8.0 mm in Example 9, the components of the base structure and the amount of carbon were measured in the same manner as in Example 1.
  • the components of the matrix structure of the aluminum-based composite material of Example 9 were 4.52% by mass of Mg, 0.64% by mass of Mn, 0.20% by mass of Fe, the balance of Al and inevitable impurities, and the carbon content of the aluminum-based composite material was 1%. It was 0.5% by mass. That is, the total amount of (Mn, Cr, Fe, Zr, Ti, B) was 0.84% by mass.
  • Example 9 When the structure of the crystal grains of the aluminum-based composite material of Example 9 was observed in the same manner as in Example 1, the average value of the major axis length L1 of Example 9 was 3.1 ⁇ m, and the average of the maximum minor axis length L2 was 3.1 ⁇ m. The value was 1.0 ⁇ m, and the area ratio of the elongated metal crystal grains having L1 / L2 of 4 or more was 13%.
  • Example 9 When the mechanical properties of the aluminum-based composite material of Example 9 were evaluated in the same manner as in Example 1, the mechanical properties of Example 9 were as follows: a Young's modulus of 85 GPa, a tensile strength of 389 MPa, and an elongation of 7.6%. there were.
  • Example 1 the area ratio of the fine aluminum carbide particles having a circle equivalent diameter of 500 nm or less was evaluated. As a result, the area ratio of the fine aluminum carbide particles in Example 9 was 4.8%. Similarly, when the area ratio of a compound (precipitate) of an element such as Mn or Cr was evaluated, the area ratio of the precipitate of Example 9 was 1.5%.
  • Example 10 An aluminum-based composite material in which carbon fibers were dispersed was produced under the same conditions as in Example 1 except that the acid treatment conditions for the carbon fibers were changed.
  • Example 10 an acid solution was prepared by mixing 150 g of sulfuric acid and 50 g of nitric acid, 2 g of carbon fiber was added thereto, and the mixture was warm-bathed in a water bath stirrer (EWS100RD manufactured by AS ONE) heated to 70 ° C. Stirred at 100 rpm for 50 minutes.
  • EWS100RD water bath stirrer
  • the carbon fiber was washed and dried in the same manner as in Example 1, and the Id / Ig of the carbon fiber after the acid treatment was confirmed to be 0.44.
  • Example 2 Under the same conditions as in Example 1, the carbon fiber and the metal powder were treated, the carbon fiber was adsorbed on the flake powder, heat treatment, green compaction and sintering were performed, and extrusion molding was performed.
  • Example 10 With respect to the obtained aluminum-based composite material of Example 10 having a diameter of 8.0 mm, the components of the base structure and the amount of carbon were measured in the same manner as in Example 1.
  • the components of the base structure of the aluminum-based composite of Example 10 were 4.51% by mass of Mg, 0.64% by mass of Mn, 0.20% by mass of Fe, the balance of Al and inevitable impurities, and the carbon content of the aluminum-based composite was 2%. 0.0% by mass. That is, the total amount of (Mn, Cr, Fe, Zr, Ti, B) was 0.84% by mass.
  • Example 10 When the structure of the crystal grains of the aluminum-based composite material of Example 10 was observed in the same manner as in Example 1, the average value of the long axis length L1 of Example 10 was 3.7 ⁇ m, and the average of the maximum short axis length L2 was The value was 1.3 ⁇ m, and the area ratio of long elongated metal crystal grains having L1 / L2 of 4 or more was 18%.
  • Example 10 When the mechanical properties of the aluminum-based composite material of Example 10 were evaluated in the same manner as in Example 1, the mechanical properties of Example 10 were as follows: a Young's modulus of 91 GPa, a tensile strength of 380 MPa, and an elongation of 8.9%. there were.
  • Example 10 ⁇ Circle around (2) ⁇
  • the area ratio of the fine aluminum carbide particles in Example 10 was 1.2%.
  • the area ratio of a compound (precipitate) of an element such as Mn or Cr was evaluated, the area ratio of the precipitate of Example 10 was 1.2%.
  • Example 11 An aluminum-based composite material in which carbon fibers were dispersed was produced under the same conditions as in Example 1 except that the acid treatment conditions for the carbon fibers were changed.
  • Example 11 an acid solution was prepared by mixing 150 g of sulfuric acid and 50 g of nitric acid, and 2 g of carbon fiber was added thereto, followed by warm bathing in a water bath stirrer (EWS100RD manufactured by AS ONE) heated to 50 ° C. Stirred at 100 rpm for 20 minutes.
  • EWS100RD water bath stirrer
  • the carbon fiber was washed and dried in the same manner as in Example 1, and the Id / Ig of the raw fiber after the acid treatment was confirmed to be 0.25.
  • Example 2 Under the same conditions as in Example 1, the carbon fiber and the metal powder were treated, the carbon fiber was adsorbed on the flake powder, heat treatment, green compaction and sintering were performed, and extrusion molding was performed.
  • Example 11 With respect to the obtained aluminum-based composite material having a diameter of 8.0 mm of Example 11, the components of the base structure and the amount of carbon were measured in the same manner as in Example 1.
  • the components of the matrix structure of the aluminum-based composite of Example 11 were 4.50% by mass of Mg, 0.64% by mass of Mn, 0.20% by mass of Fe, the balance of Al and inevitable impurities, and the carbon content of the aluminum-based composite was 2%. 0.0% by mass. That is, the total amount of (Mn, Cr, Fe, Zr, Ti, B) was 0.84% by mass.
  • Example 11 When the structure of the crystal grains of the aluminum-based composite material of Example 11 was observed in the same manner as in Example 1, the average value of the long axis length L1 of Example 11 was 3.9 ⁇ m, and the average value of the maximum short axis length L2 was 3.9 ⁇ m. The value was 1.5 ⁇ m, and the area ratio of the elongated metal crystal grains having L1 / L2 of 4 or more was 20%.
  • Example 11 When the mechanical properties of the aluminum-based composite material of Example 11 were evaluated in the same manner as in Example 1, the mechanical properties of Example 11 were as follows: a Young's modulus of 92 GPa, a tensile strength of 356 MPa, and an elongation of 11.5%. there were.
  • Example 11 when the area ratio of the fine aluminum carbide particles having an equivalent circle diameter of 500 nm or less was evaluated, the area ratio of the fine aluminum carbide particles in Example 11 was 0.6%. Similarly, when the area ratio of a compound (precipitate) of an element such as Mn or Cr was evaluated, the area ratio of the precipitate of Example 11 was 1.1%.
  • Example 12 The amount of the added element of the metal powder was changed from Example 1, and as the metal powder, 4.61% by mass of Mg—0.98% by mass of Mn—0.25% by mass of Cr—0.42% by mass of Fe—0.15% by mass of Ti -An atomized powder having a particle diameter (D 50 ) of about 10 ⁇ m consisting of the balance of Al and inevitable impurities was used.
  • the conditions for exfoliating the atomized powder, the conditions for the carbon fiber used and its acid treatment, the conditions for adsorption, the conditions for sintering and the conditions for extrusion molding were all the same as in Example 1.
  • Example 12 With respect to the obtained aluminum-based composite material of Example 12 having a diameter of 8.0 mm, the components of the base structure and the amount of carbon were measured in the same manner as in Example 1.
  • the components of the base structure of the aluminum-based composite material of Example 12 were 4.61% by mass of Mg, 0.98% by mass of Mn, 0.25% by mass of Cr, 0.42% by mass of Fe, 0.15% by mass of Ti, the balance of Al and inevitable impurities.
  • the carbon content of the aluminum-based composite material was 1.9% by mass. That is, the total amount of (Mn, Cr, Fe, Zr, Ti, B) was 1.80% by mass.
  • Example 12 When the structure of the crystal grains of the aluminum-based composite material of Example 12 was observed in the same manner as in Example 1, the average value of the major axis length L1 of Example 12 was 1.4 ⁇ m, and the average of the maximum minor axis length L2 was The value was 0.9 ⁇ m, and the area ratio of long elongated metal crystal grains having L1 / L2 of 4 or more was 10%.
  • Example 12 When the mechanical properties of the aluminum-based composite material of Example 12 were evaluated in the same manner as in Example 1, the mechanical properties of Example 12 were as follows: Young's modulus: 91 GPa, tensile strength: 397 MPa, elongation: 5.2%. there were.
  • Example 12 ⁇ Circle around (2) ⁇
  • the area ratio of the fine aluminum carbide particles having an equivalent circle diameter of 500 nm or less was evaluated.
  • the area ratio of the fine aluminum carbide particles in Example 12 was 1.7%.
  • the area ratio of a compound (precipitate) of an element such as Mn or Cr was evaluated, the area ratio of the precipitate of Example 12 was 3.6%.
  • Example 13 The amount of the element added to the metal powder was changed from that of Example 1, and as a metal powder, 4.51% by mass of Mg—0.22% by mass of Mn—0.10% by mass of Cr—the particle diameter composed of the balance of Al and inevitable impurities (D 50 ) about 10 ⁇ m atomized powder was used.
  • the conditions for exfoliating the atomized powder, the conditions for the carbon fiber used and its acid treatment, the conditions for adsorption, the conditions for sintering and the conditions for extrusion molding were all the same as in Example 1.
  • Example 13 With respect to the obtained aluminum-based composite material having a diameter of 8.0 mm of Example 13, the components of the base structure and the amount of carbon were measured in the same manner as in Example 1.
  • the components of the base structure of the aluminum-based composite of Example 13 were 4.51% by mass of Mg, 0.20% by mass of Mn, 0.10% by mass of Cr, the balance being Al and unavoidable impurities, and the carbon content of the aluminum-based composite was 1%. 9.9% by mass. That is, the total amount of (Mn, Cr, Fe, Zr, Ti, B) was 0.30% by mass.
  • Example 13 When the structure of the crystal grains of the aluminum-based composite material of Example 13 was observed in the same manner as in Example 1, the average value of the major axis length L1 of Example 13 was 3.4 ⁇ m, and the average value of the maximum minor axis length L2 was The value was 1.1 ⁇ m, and the area ratio of the elongated metal crystal grains having L1 / L2 of 4 or more was 14%.
  • Example 13 When the mechanical properties of the aluminum-based composite material of Example 13 were evaluated in the same manner as in Example 1, the mechanical properties of Example 13 were as follows: a Young's modulus of 85 GPa, a tensile strength of 370 MPa, and an elongation of 13.2%. there were.
  • Example 1 the area ratio of the fine aluminum carbide particles having an equivalent circle diameter of 500 nm or less was evaluated. As a result, the area ratio of the fine aluminum carbide particles in Example 13 was 1.6%. Similarly, when the area ratio of a compound (precipitate) of an element such as Mn or Cr was evaluated, the area ratio of the precipitate of Example 13 was 0.5%.
  • Example 1 The same metal powder and carbon fiber as in Example 1 were used, but the extrusion conditions were changed. First, a sintered body was obtained under the same conditions as in Example 1.
  • extrusion molding was performed using the same press machine as in Example 1.
  • the extrusion die used in Comparative Example 1 had an inlet inner diameter (A in FIG. 4) of 40.5 mm, an outlet inner diameter (B in FIG. 4) of 13.3 mm, and a die angle (C in FIG. 4). ) Is 45 °.
  • a sintered body having a diameter of 40 mm and a height of 22 mm was preheated at 530 ° C., then inserted into an extrusion mold heated to 530 ° C., and extruded at an extrusion ratio of 9 and an extrusion speed of 25 mm / s.
  • the components of the base structure and the amount of carbon were measured in the same manner as in Example 1.
  • the components of the matrix structure of the aluminum-based composite material of Comparative Example 1 were 4.51% by mass of Mg, 0.64% by mass of Mn, 0.20% by mass of Fe, the balance of Al and inevitable impurities, and the carbon content of the aluminum-based composite material was 2%. 0.0% by mass. That is, the total amount of (Mn, Cr, Fe, Zr, Ti, B) was 0.84% by mass.
  • the mechanical properties of the aluminum-based composite material of Comparative Example 1 were evaluated in the same manner as in Example 1.
  • the mechanical properties of Comparative Example 1 were as follows: Young's modulus: 86 GPa, tensile strength: 344 MPa, and elongation: 9.8%. there were.
  • Example 2 when the area ratio of the fine aluminum carbide particles having a circle equivalent diameter of 500 nm or less was evaluated, the area ratio of the fine aluminum carbide particles of Comparative Example 1 was 1.1%. Similarly, when the area ratio of a compound (precipitate) of an element such as Mn or Cr was evaluated, the area ratio of the precipitate of Comparative Example 1 was 2.0%.
  • Example 2 With respect to Example 1, the amount of Mg in the metal powder was changed, and as a metal powder, 7.51% by mass of Mg-0.66% by mass of Mn-0.21% by mass of Fe-the particle diameter composed of the balance of Al and inevitable impurities (D 50 ) Used an atomized powder of about 10 ⁇ m.
  • the components of the base structure and the amount of carbon were measured in the same manner as in Example 1.
  • the components of the matrix structure of the aluminum-based composite of Comparative Example 2 were 7.50% by mass of Mg, 0.64% by mass of Mn, 0.20% by mass of Fe, the balance of Al and inevitable impurities, and the carbon content of the aluminum-based composite was 1%. 9.9% by mass. That is, the total amount of (Mn, Cr, Fe, Zr, Ti, B) was 0.84% by mass.
  • Example 2 when the area ratio of the fine aluminum carbide particles having an equivalent circle diameter of 500 nm or less was evaluated, the area ratio of the fine aluminum carbide particles of Comparative Example 2 was 1.5%. Similarly, when the area ratio of a compound (precipitate) of an element such as Mn or Cr was evaluated, the area ratio of the precipitate of Comparative Example 2 was 1.5%.
  • Example 3 The Mg content of the metal powder was changed from that of Example 1, and as the metal powder, a particle diameter (D 50) composed of 0.41% by mass of Mg—0.66% by mass of Mn—0.21% by mass of Fe—the balance of Al and inevitable impurities. ) Used an atomized powder of about 10 ⁇ m.
  • the conditions for exfoliating the atomized powder, the conditions for the carbon fiber used and its acid treatment, the conditions for adsorption, the conditions for sintering and the conditions for extrusion molding were all the same as in Example 1.
  • the components of the base structure and the amount of carbon were measured in the same manner as in Example 1.
  • the components of the matrix structure of the aluminum-based composite material of Comparative Example 3 were 0.40% by mass of Mg, 0.64% by mass of Mn, 0.20% by mass of Fe, the balance of Al and inevitable impurities, and the carbon content of the aluminum-based composite material was 1%. 9.9% by mass. That is, the total amount of (Mn, Cr, Fe, Zr, Ti, B) was 0.84% by mass.
  • the test piece shown in FIG. 5 was processed, and the strength was weak and the processing could not be performed. Was. For this reason, the mechanical properties could not be evaluated.
  • Example 4 An aluminum-based composite material in which carbon fibers were dispersed was prepared under the same conditions as in Example 1 except that the amount of carbon fibers (CNF) added in the carbon fiber slurry forming step was changed.
  • CNF carbon fibers
  • Example 1 An acid treatment and a scale treatment were performed in the same procedure as in Example 1.
  • a sodium lauryl sulfate (concentration of 99% or more, manufactured by Showa Chemical), pure water and an ultrasonic treatment device (Branson ultrasonic homogenizer DCX @ S20: 1.25) were prepared, and a solution obtained by adding 2 g of sodium lauryl sulfate to 200 ml of pure water was prepared.
  • 6.0 g of the acid-treated carbon fiber was added, and ultrasonic treatment was performed to obtain a carbon fiber slurry.
  • carbon fibers were adsorbed to the scale powder, and a heat treatment was performed.
  • the carbon content of the scale powder after adsorbing the carbon fibers was 5.7% by mass.
  • the aluminum-based composite material having a diameter of 8.0 mm of Comparative Example 4 obtained by performing green compacting, sintering, and extrusion was obtained in the same manner as in Example 1. And the amount of carbon were measured.
  • the components of the matrix structure of the aluminum-based composite of Comparative Example 4 were 4.52% by mass of Mg, 0.64% by mass of Mn, 0.20% by mass of Fe, the balance of Al and inevitable impurities, and the carbon content of the aluminum-based composite was 5%. 0.7% by mass. That is, the total amount of (Mn, Cr, Fe, Zr, Ti, B) was 0.84% by mass.
  • Example 1 the area ratio of the fine aluminum carbide particles having an equivalent circle diameter of 500 nm or less was evaluated. As a result, the area ratio of the fine aluminum carbide particles of Comparative Example 4 was 3.9%. Similarly, when the area ratio of a compound (precipitate) of an element such as Mn or Cr was evaluated, the area ratio of the precipitate of Comparative Example 4 was 1.3%.
  • Example 5 An aluminum-based composite material in which carbon fibers were dispersed was prepared under the same conditions as in Example 1 except that the amount of carbon fibers (CNF) added in the carbon fiber slurry forming step was changed.
  • CNF carbon fibers
  • Example 1 An acid treatment and a scale treatment were performed in the same procedure as in Example 1.
  • a sodium lauryl sulfate (concentration of 99% or more, manufactured by Showa Chemical), pure water and an ultrasonic treatment device (Branson ultrasonic homogenizer DCX @ S20: 1.25) were prepared, and a solution obtained by adding 2 g of sodium lauryl sulfate to 200 ml of pure water was prepared.
  • 0.5 g of the carbon fiber after the acid treatment was added, and ultrasonic treatment was performed to obtain a carbon fiber slurry.
  • carbon fibers were adsorbed to the scale powder, and a heat treatment was performed.
  • the carbon content of the subsequent flake powder adsorbing the carbon fibers was 0.5% by mass.
  • Example 2 Thereafter, under the same conditions as in Example 1, green compact molding, sintering and extrusion molding were performed, and the base structure of the aluminum-based composite material having a diameter of 8.0 mm of Comparative Example 5 was obtained in the same manner as in Example 1. And the amount of carbon were measured.
  • the components of the matrix structure of the aluminum-based composite of Comparative Example 5 were 4.51% by mass of Mg, 0.64% by mass of Mn, 0.20% by mass of Fe, the balance of Al and inevitable impurities, and the carbon content of the aluminum-based composite was 0%. It was 0.5% by mass. That is, the total amount of (Mn, Cr, Fe, Zr, Ti, B) was 0.84% by mass.
  • Example 1 when the area ratio of the fine aluminum carbide particles having an equivalent circle diameter of 500 nm or less was evaluated, the area ratio of the fine aluminum carbide particles of Comparative Example 5 was 0.3%. Similarly, when the area ratio of a compound (precipitate) of an element such as Mn or Cr was evaluated, the area ratio of the precipitate of Comparative Example 5 was 1.2%.
  • the average value of the major axis length L1 of the columnar metal crystal grains constituting the matrix structure of the aluminum-based composite material was adjusted to 5 by appropriately controlling the extrusion molding conditions and the like. 0.0 ⁇ m or less, the average value of the maximum minor axis length L2 was 2.0 ⁇ m or less, and the area ratio of columnar metal crystal grains having L1 / L2 of 4 or more could be 25% or less. Therefore, in each of the examples, the Young's modulus satisfied 80 GPa or more, the tensile strength 350 MPa, and the elongation satisfied 5% or more.
  • the tensile strength, elongation, and Young's modulus all show values equal to or higher than a certain value. It has been found that an aluminum-based composite having excellent mechanical properties can be realized.
  • the optimization of the size of the columnar metal crystal grains is based on the fact that the aluminum alloy constituting the matrix structure is of the above-described embodiment.
  • the present invention is not limited to the case of the elemental composition, but also works effectively when the content of Mg is 0.5 to 7 mass% and the balance is Al and unavoidable impurities.

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Abstract

Il est souhaitable que la valeur moyenne de longueurs L1 des axes plus longs de grains cristallins métalliques en colonne soit de 5,0 µm ou moins et que la valeur moyenne de longueurs maximales L2 des axes plus courts des grains cristallins métalliques en colonne soit de 2,0 µm ou moins. Il est également souhaitable que le rapport surfacique de grains cristallins métalliques en colonne ayant chacun un rapport L1/L2 de 4 ou plus soit de 25 % ou moins. Ces tailles de grains cristallins sont affectées par des particules de carbure d'aluminium. On suppose que la source de carbone des particules de carbure d'aluminium est un morceau de carbone qui est détaché ou séparé d'une fibre de carbone pendant le processus de production, et on suppose également que le morceau de carbone est sorti de la fibre de carbone par réalisation d'un endommagement spécifique sur la fibre de carbone lors du processus de production et, en conséquence, des particules de carbure d'aluminium sont produites dans des positions qui sont différentes des interfaces avec la fibre de carbone.
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CN116287884A (zh) * 2023-03-01 2023-06-23 黄冈师范学院 一种钢结构桥梁检测小车桁架结构用合金材料

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WO2009054309A1 (fr) * 2007-10-25 2009-04-30 National University Corporation Hokkaido University Matériau métallique composite et son procédé de production
JP2010159445A (ja) * 2009-01-07 2010-07-22 Shinshu Univ 金属粒子と炭素粉末の混合方法、金属・炭素複合材料の製造方法および金属・炭素複合材料
WO2015156038A1 (fr) * 2014-04-08 2015-10-15 矢崎総業株式会社 Matériau composite de nanotube de carbone et son procédé de production
CN105441706A (zh) * 2015-11-14 2016-03-30 华文蔚 一种碳纳米管金属基复合材料的制备方法
JP2017082309A (ja) * 2015-10-30 2017-05-18 矢崎総業株式会社 締結部材

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WO2009054309A1 (fr) * 2007-10-25 2009-04-30 National University Corporation Hokkaido University Matériau métallique composite et son procédé de production
JP2010159445A (ja) * 2009-01-07 2010-07-22 Shinshu Univ 金属粒子と炭素粉末の混合方法、金属・炭素複合材料の製造方法および金属・炭素複合材料
WO2015156038A1 (fr) * 2014-04-08 2015-10-15 矢崎総業株式会社 Matériau composite de nanotube de carbone et son procédé de production
JP2017082309A (ja) * 2015-10-30 2017-05-18 矢崎総業株式会社 締結部材
CN105441706A (zh) * 2015-11-14 2016-03-30 华文蔚 一种碳纳米管金属基复合材料的制备方法

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Publication number Priority date Publication date Assignee Title
CN116287884A (zh) * 2023-03-01 2023-06-23 黄冈师范学院 一种钢结构桥梁检测小车桁架结构用合金材料

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