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WO1992008560A1 - Procede de fabrication d'un produit moule par pression a partir d'une poudre d'aluminium - Google Patents

Procede de fabrication d'un produit moule par pression a partir d'une poudre d'aluminium Download PDF

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Publication number
WO1992008560A1
WO1992008560A1 PCT/JP1991/001599 JP9101599W WO9208560A1 WO 1992008560 A1 WO1992008560 A1 WO 1992008560A1 JP 9101599 W JP9101599 W JP 9101599W WO 9208560 A1 WO9208560 A1 WO 9208560A1
Authority
WO
WIPO (PCT)
Prior art keywords
aluminum powder
powder
gas
film
aluminum
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP1991/001599
Other languages
English (en)
Japanese (ja)
Inventor
Akira Yoshino
Haruo Senbokuya
Masaaki Tahara
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Daido Sanso Co Ltd
Original Assignee
Daido Sanso Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Daido Sanso Co Ltd filed Critical Daido Sanso Co Ltd
Publication of WO1992008560A1 publication Critical patent/WO1992008560A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
    • C01B21/0722—Preparation by direct nitridation of aluminium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/145—Chemical treatment, e.g. passivation or decarburisation
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0068—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only nitrides

Definitions

  • the present invention relates to a method for producing an aluminum powder press molded article.
  • a thin metal container 26 having a desired shape for example, a shape of a chassis of an automobile part or the like
  • Aluminum powder 11 containing titanium powder, magnesium powder and the like is vacuum-sealed in the metal container 26.
  • an inert gas such as an argon gas is injected into the above-mentioned metal container 26 by pressing the inert gas such as argon gas at a temperature of 100 or more by the heater 25 to apply a pressure of 10 O MPa or more.
  • the internal aluminum powder 11 is pressed into the same shape as the metal container 26 to obtain an aluminum alloy product.
  • 2 2 is the upper side, and 2 3 is the lower lid.
  • the present invention has been made in consideration of the problem that aluminum alloy products are inferior in strength, toughness, etc., and is an aluminum powder press-formed product capable of obtaining an aluminum alloy product having excellent strength and toughness. Its purpose is to provide a manufacturing method.
  • a method of manufacturing an aluminum powder press-molded product of the present invention comprises contacting aluminum powder with a fluorine-based gas in a heated state, and then contacting the aluminum powder with a nitriding gas in a heated state. Then, hard nitrided ⁇ is formed on the surface layer of the aluminum powder, and the aluminum powder on which the nitrided layer is formed is directly pressed and formed into a pressed product.
  • the method for producing an aluminum powder press-molded article of the present invention comprises: before press-forming the aluminum powder, contacting the aluminum powder with a fluorine-based gas in a heated state to form fluoride on the surface thereof.
  • the upper sa-fluoride film is removed by being brought into contact with a nitriding gas in a heated state, and at the same time, the removal layer (the surface layer of the aluminum powder) is formed into a hard nitride).
  • the surface of the aluminum powder is purified and activated by performing fluoridation prior to nitriding, so that the nitriding layer can be formed evenly and deeply. This makes it possible to make the thickness of the hard honey layer rich in properties uniform and thick. In this way, since no oxide film is formed on the surface of the aluminum powder at the time of E-forming and a hard nitrided layer is formed, the obtained press-formed product has excellent toughness, particularly excellent strength. It will be worthwhile.
  • the fluorinated gas used for the fluorination treatment of the present invention is NF 3 , B F,, CF 4 , HF, SF,, Fi At least one fluorine source component selected from inert gas such as N 2 . Among these fluorine ⁇ content, reactivity, surface in NF S such as handling properties is practical and best.
  • the manufacturing method of the present invention comprises, as described above, aluminum powder (a mixture of aluminum alone or other metal powder such as titanium powder and magnesium powder) with the above-mentioned fluorine-based gas, for example, NF
  • the surface of the aluminum powder is fluorinated by contacting at a temperature of 250 to 400, and then nitriding (or nitriding) is performed using a known nitriding gas such as ammonia.
  • the concentration of a fluorine source component such as NF in such a fluorine-based gas is, for example, from 1,000 to 10,000 ppm, preferably from 20,000 to 70,000 ppm, and more preferably from 30,000 to 50,000 ppm.
  • the time of contact with such a fluorine-based gas may be selected from an appropriate time according to the type of aluminum powder, the type of powder mixed with the aluminum powder, the heating temperature, etc., and is usually several minutes. .
  • aluminum powder is introduced into, for example, a gas treatment chamber 9 provided in the heat treatment furnace 1 shown in FIG. 1 and brought into contact with a fluorine-based gas.
  • the above furnace 1 is a bit furnace in which an inner vessel 4 is placed inside a heater 3 provided in an outer shell 2, and an exhaust pipe 6 is inserted into the inner vessel 4 from outside the furnace 1, and a gas inlet pipe 5 is provided.
  • the powder outlet pipe 8 is inserted into the room from the upper side of the gas processing chamber 9 through the inner container 4, passing through the inner container 4 from the lower side of the gas processing chamber 9. Gas is supplied to the gas introduction pipe 5 from the cylinders 15 and 16 via the flowmeter 17 and the valve 18.
  • reference numeral 13 denotes a vacuum bomb and reference numeral 14 denotes an abatement system S.
  • the gas processing chamber 9 ⁇ is heated to a predetermined reaction temperature. Then, a fluorine-based gas, for example, a mixed gas of NF, and N 2 gas is blown up from the gas outlet 5a opened at the top of the gas introduction pipe 50.
  • the on-off valve (not shown) provided in the powder storage tank 7 is opened to supply the aluminum powder 11 in the powder storage tank 7 to the powder outlet pipe 8, and the powder outlet 8a at the lower end thereof is provided.
  • I5NF generates fluorine as an active group at a temperature of 250-400, and removes organic and inorganic contamination on the surface of aluminum powder 11 by collision with aluminum powder. Reacts with oxides such as Ajg 2 Oa, A £ (OH), etc. on the surface of powder 11 as shown in the following formula to form ultra-thin fluoride AjgF, on the surface of aluminum powder 11 I do.
  • the oxide film on the surface of the aluminum powder 11 is converted into a fluoride film, and the 0, adsorbed on the surface is also removed.
  • the fluorinated aluminum in the absence of 0 3 ⁇ 4 , ⁇ ,, ⁇ , 0, the fluorinated aluminum is stable at the following temperature at 600, and the aluminum powder before the subsequent nitriding treatment is 1 1 to prevent the adsorption of formation and 0 2 of the oxide film to the fabric.
  • a fluoride film is formed on the surface of the furnace material in the first stage, and the film is used to form a fluorine-based gas on the surface of the furnace material thereafter. Damage will be prevented.
  • These fluorinated aluminum powders 11 are stored in a powder storage box 10 arranged at the bottom of the gas processing chamber 9.
  • the aluminum powder 11 stored in the powder storage box 10 is nitrided using the same heat treatment furnace as the heat treatment furnace 1. Ie, heating the gas treatment chamber provided in the heat treatment furnace to nitrided temperature at 450 to 550, have a Nyuita 3 or NH S and a carbon source, in this state A mixed gas with the gas to be blown (eg, RX gas) is blown up from the gas outlet at the end of the gas inlet tube, and the aluminum powder 11 is dropped from the powder outlet tube to bring them into contact.
  • the above-mentioned fluoride film is reduced or destroyed by H or a trace amount of water, for example, as shown in the following formula, whereby the active aluminum powder 11 is exposed and formed.
  • the active aluminum powder 11 is formed into the dough, and at the same time, the active N atoms penetrate and diffuse into the aluminum powder 11 and, as a result, contain AN on the surface of the dough.
  • a compound layer (nitriding) is formed.
  • the formation of such a nitrided layer is the same in the conventional nitridation method, but in the conventional method, the oxide film formed on the surface rising from the room temperature to the honey temperature, Since the activity of the surface is reduced by the amount, the degree of surface adsorption of N atoms is low and non-uniform. Such non-uniformity is also magnified by the fact that it is practically difficult to keep the degree of decomposition of NH, uniformly in the reactor. According to the production method of the present invention, the adsorption of N atoms on the surface of the aluminum powder 11 is performed uniformly and quickly, so that the above-mentioned problem does not occur. As shown in FIG. 2, the aluminum powder 11 thus obtained has a surface layer formed of hard and uniform hard nitride A, as shown in FIG. Thereafter, the aluminum powder 11 is press-formed into an aluminum alloy product having a desired shape using a known HIP device 20.
  • the oxide film on the surface of the aluminum powder 11 is removed before being applied to the HIP device 20, it is necessary to heat the aluminum powder 11 mixed with various powders. Powder with low melting temperature as powder to be mixed with aluminum powder 1 Even when ⁇ is used, the resulting molded product has excellent mechanical properties such as strength and toughness. Moreover, since the surface calendar of the aluminum powder 11 is formed of hard nitrided shoes, it is particularly excellent in strength.
  • fluorination is performed prior to nitriding.
  • an erroneous film such as an oxide film on the surface of the aluminum powder is changed to a fluoride film, and the surface of the aluminum powder is protected. Therefore, even if there is a time passage between the formation of the fluoride film and the nitriding treatment, the fluoride film formed on the surface of the aluminum powder can protect the surface of the aluminum powder in good condition. As a result, the formation of the oxide film again on the surface of the aluminum powder is prevented. This fluoride film is decomposed and removed during the subsequent nitriding treatment, thereby exposing the surface of the aluminum powder.
  • the ⁇ atom in the nitriding treatment spreads in the surface layer of the aluminum powder, and the ⁇ atom diffuses deeply and uniformly. Thereby, the surface layer of the aluminum powder is formed into a thick and uniform hard nitrided layer. Therefore, the resulting molded product has excellent mechanical properties such as strength and toughness.
  • FIG. 1 is a cross-sectional view of a heat treatment furnace used in one embodiment of the present invention
  • FIG. 2 is a cross-sectional view showing a state of a nitride layer of aluminum powder
  • FIG. 3 is a conceptual diagram of a ⁇ . ⁇ . ⁇ . .
  • the NF 3 in the heat treatment furnace 1 as shown in FIG. 1 5 0 0 O ppm content to N 2 gas Kiri ⁇ Contact at 300 ° C for several minutes.
  • nitriding treatment was performed in the above heat treatment furnace 1 at 530 with a mixed gas of 50% NK15QHNi for several minutes, and then, the mixture was air-cooled and taken out.
  • the obtained aluminum powder had a nitride thickness of 5 to 10 m and a surface hardness of 190 to 210 OHv. This surface hardness is much higher than that obtained by nitriding by a conventionally known method.
  • an aluminum alloy product having a desired shape was obtained by using the HI device as described above. This aluminum alloy product had much higher strength and toughness than the conventional aluminum alloy product.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Powder Metallurgy (AREA)

Abstract

Procédé de fabrication d'un produit moulé par pression à partir d'une poudre d'aluminium, consistant à effectuer un processus de fluoration avant le processus de nitruration. De la sorte, un film passif tel qu'un film d'oxyde à la surface de la poudre d'aluminium se transforme en un film fluoré qui protège la surface de la poudre. Par conséquent, même après l'étape de nitruration, le film fluoré formé à la surface de la poudre d'aluminium protège ladite surface et empêche qu'un film d'oxyde ne s'y forme à nouveau. Etant donné que le film fluoré est décomposé lors du processus de nitruration successif, les atomes de N actifs pendant le processus de nitruration sont dispersés uniformément et profondément dans la couche de surface de la poudre d'aluminium pour former une couche de nitrure dure et uniforme.
PCT/JP1991/001599 1990-11-20 1991-11-20 Procede de fabrication d'un produit moule par pression a partir d'une poudre d'aluminium Ceased WO1992008560A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2/316563 1990-11-20
JP2316563A JP2868889B2 (ja) 1990-11-20 1990-11-20 アルミニウム粉末加圧成形品の製法

Publications (1)

Publication Number Publication Date
WO1992008560A1 true WO1992008560A1 (fr) 1992-05-29

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PCT/JP1991/001599 Ceased WO1992008560A1 (fr) 1990-11-20 1991-11-20 Procede de fabrication d'un produit moule par pression a partir d'une poudre d'aluminium

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JP (1) JP2868889B2 (fr)
WO (1) WO1992008560A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0577436A1 (fr) * 1992-07-02 1994-01-05 Sumitomo Electric Industries, Limited Alliages d'aluminium frittés et comprimés en azote et procédé de fabrication
EP2905096B1 (fr) * 2014-04-07 2018-11-28 Thierry Präzisionslackiertechnik GmbH Procédé de fabrication des particules modifiées d'énergie de surface, et dispositif á cet effet

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB0413135D0 (en) * 2004-06-12 2004-07-14 Rolls Royce Plc A method of manufacturing a component by consolidating a metal powder
KR100721780B1 (ko) * 2005-05-30 2007-05-25 주식회사 다이너머트리얼스 고강도 극미세/나노구조 알루미늄/질화알루미늄 또는알루미늄합금/질화알루미늄 복합재료의 제조 방법

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5022707A (fr) * 1973-07-02 1975-03-11
JPS5773103A (en) * 1980-10-27 1982-05-07 Res Dev Corp Of Japan Production of high strength heat resistant metallic material
JPS621836A (ja) * 1985-06-28 1987-01-07 Komatsu Ltd 強靭性超硬材の製造方法
JPS6283404A (ja) * 1985-10-04 1987-04-16 Furukawa Electric Co Ltd:The 金属複合粉末の製造法
JPS62199703A (ja) * 1986-02-26 1987-09-03 Sumitomo Light Metal Ind Ltd Ａ１−Ｓｉ系粉末合金の熱間静水圧圧縮成形法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5022707A (fr) * 1973-07-02 1975-03-11
JPS5773103A (en) * 1980-10-27 1982-05-07 Res Dev Corp Of Japan Production of high strength heat resistant metallic material
JPS621836A (ja) * 1985-06-28 1987-01-07 Komatsu Ltd 強靭性超硬材の製造方法
JPS6283404A (ja) * 1985-10-04 1987-04-16 Furukawa Electric Co Ltd:The 金属複合粉末の製造法
JPS62199703A (ja) * 1986-02-26 1987-09-03 Sumitomo Light Metal Ind Ltd Ａ１−Ｓｉ系粉末合金の熱間静水圧圧縮成形法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0577436A1 (fr) * 1992-07-02 1994-01-05 Sumitomo Electric Industries, Limited Alliages d'aluminium frittés et comprimés en azote et procédé de fabrication
US5460775A (en) * 1992-07-02 1995-10-24 Sumitomo Electric Industries, Ltd. Nitrogen-combined aluminum sintered alloys and method of producing the same
EP2905096B1 (fr) * 2014-04-07 2018-11-28 Thierry Präzisionslackiertechnik GmbH Procédé de fabrication des particules modifiées d'énergie de surface, et dispositif á cet effet

Also Published As

Publication number Publication date
JP2868889B2 (ja) 1999-03-10
JPH04187704A (ja) 1992-07-06

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