JPH03111526A - Manufacture of fiber reinforced metal matrix composite - Google Patents
Manufacture of fiber reinforced metal matrix compositeInfo
- Publication number
- JPH03111526A JPH03111526A JP24795489A JP24795489A JPH03111526A JP H03111526 A JPH03111526 A JP H03111526A JP 24795489 A JP24795489 A JP 24795489A JP 24795489 A JP24795489 A JP 24795489A JP H03111526 A JPH03111526 A JP H03111526A
- Authority
- JP
- Japan
- Prior art keywords
- fibers
- prepreg sheet
- prepreg
- metal
- formwork
- 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.)
- Pending
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 239000011156 metal matrix composite Substances 0.000 title claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 47
- 239000002184 metal Substances 0.000 claims abstract description 47
- 239000011888 foil Substances 0.000 claims abstract description 23
- 239000011159 matrix material Substances 0.000 claims abstract description 16
- 239000012784 inorganic fiber Substances 0.000 claims abstract description 15
- 238000009792 diffusion process Methods 0.000 claims abstract description 14
- 239000007791 liquid phase Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 11
- 238000005507 spraying Methods 0.000 claims description 5
- 238000010030 laminating Methods 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 abstract description 5
- 239000000956 alloy Substances 0.000 abstract description 5
- 229910052719 titanium Inorganic materials 0.000 abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 abstract description 2
- 229910052802 copper Inorganic materials 0.000 abstract description 2
- 238000007789 sealing Methods 0.000 abstract description 2
- 150000002739 metals Chemical class 0.000 abstract 3
- 238000007731 hot pressing Methods 0.000 abstract 1
- 229910052759 nickel Inorganic materials 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 238000009415 formwork Methods 0.000 description 28
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- -1 polycyclic aromatic compound Chemical class 0.000 description 8
- 229920000642 polymer Polymers 0.000 description 8
- 238000002844 melting Methods 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 230000008018 melting Effects 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000003780 insertion Methods 0.000 description 4
- 230000037431 insertion Effects 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000009987 spinning Methods 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 238000003466 welding Methods 0.000 description 4
- 241000234282 Allium Species 0.000 description 3
- 235000002732 Allium cepa var. cepa Nutrition 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000011300 coal pitch Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 239000011301 petroleum pitch Substances 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 239000011295 pitch Substances 0.000 description 2
- 238000007750 plasma spraying Methods 0.000 description 2
- 229920005604 random copolymer Polymers 0.000 description 2
- 125000003808 silyl group Chemical group [H][Si]([H])([H])[*] 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000007751 thermal spraying Methods 0.000 description 2
- 239000011882 ultra-fine particle Substances 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- 208000031872 Body Remains Diseases 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005058 metal casting Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 229920001558 organosilicon polymer Polymers 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Landscapes
- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、耐熱性に優れ、軽量で強度が大きく、宇宙・
航空機材料及び自動車材料としての用途に適した繊維強
化金属基複合材料（以下ＦＲＭということがある。）の
製造方法に関する。[Detailed Description of the Invention] (Industrial Field of Application) The present invention has excellent heat resistance, is lightweight, has high strength, and is suitable for space applications.
The present invention relates to a method for manufacturing a fiber reinforced metal matrix composite material (hereinafter sometimes referred to as FRM) suitable for use as an aircraft material and an automobile material.
（従来の技術及びその問題点）
ＦＲＭの製造方法の一つとして、無機繊維束を引揃え、
プラズマスプレーによってマトリックス金属を溶射して
プリプレグシートを作り、その後、それを所要枚数積層
し液相拡散接合することよりなる製造方法が知られてい
る。(Prior art and its problems) One of the methods for manufacturing FRM is to align inorganic fiber bundles,
A manufacturing method is known in which prepreg sheets are made by spraying a matrix metal using plasma spray, and then a required number of sheets are laminated and liquid-phase diffusion bonded.
しかし、この方法では、マトリックス金属が活性である
場合、大気中で上記接合を実施すると、プリプレグシー
トの表面が酸化され、酸化物が生成するため良好な接合
ができない。そのため、活性な金属をマトリックスとす
るプリプレグシートの接合においては、加熱、加圧を減
圧雰囲気、あるいは不活性ガス雰囲気中で行わなくては
ならず、真空チャンバーを備えたプレス装置が必要であ
り、経済的、効率的にＦＲＭを製造することができない
一方、上記問題点を解決する簡便な方法として、用村広
人らは、三菱重工技報＋Ｖｏｌ、１３＋Ｎｏ−３＋ ｐ
−１〜ｐ、１０において、厚さ５００μｍのステンレス
鋼薄板製の容器にプリプレグシートの積層体を挿入し、
真空排気状態（１〜５×１ｏ弓ｍｍ Ｈｇ ）で液相拡
散接合によりＦＲＭを製造する方法を記載している。However, in this method, when the matrix metal is active and the above bonding is performed in the atmosphere, the surface of the prepreg sheet is oxidized and oxides are generated, so that good bonding cannot be achieved. Therefore, when bonding prepreg sheets with active metal as a matrix, heating and pressurization must be performed in a reduced pressure atmosphere or an inert gas atmosphere, and a press device equipped with a vacuum chamber is required. While it is not possible to manufacture FRM economically and efficiently, as a simple method to solve the above problems, Hiroto Yomura et al.
-1 to p, 10, inserting a laminate of prepreg sheets into a container made of thin stainless steel plate with a thickness of 500 μm,
A method is described for manufacturing FRMs by liquid phase diffusion bonding under evacuated conditions (1-5×10 mm Hg).
しかし、この方法では、容器が上記のステンレス！ｉｉ
ｌ薄板製であるため、真空排気に際し、容器形状は変化
せず、容器の形状またはプリプレグシートの積層体の挿
入状態によっては、減圧下のプリプレグシートを封入し
た容器中には、プリプレグシートの積層体では置換でき
ない未充填の空間が残り、上記封入容器に液相拡散接合
法を適用した場合、未充填空間部に溶融金属が流出する
ため繊維体積率（Ｖ、）の制御が困難であると共に、Ｆ
ＲＭの形状を一定にしにくいという問題点がある。However, with this method, the container is made of stainless steel! ii
Since it is made of a thin plate, the shape of the container does not change during vacuum evacuation. An unfilled space that cannot be replaced by the body remains, and when liquid phase diffusion bonding is applied to the above-mentioned sealed container, the molten metal flows into the unfilled space, making it difficult to control the fiber volume fraction (V,). ,F
There is a problem that it is difficult to keep the shape of the RM constant.
（問題点を解決するための手段）
本発明は上記問題点を解消したＦＲＭの製造法を提供す
る。(Means for Solving the Problems) The present invention provides a method for manufacturing an FRM that eliminates the above problems.
本発明によれば、
連続無機繊維束を開繊し、次いで一方向に引き揃えた繊
維にマトリックス金属を溶射してプリプレグシートを製
造する第１工程、
上記プリプレグシートを所要枚数積層して、型枠中にセ
ットし、この型枠を金属箔製袋中に減圧下に封入後、該
金属箔製袋中のプリプレグシートを液相拡散接合する第
２工程
よりなる繊維強化金属基複合材料の製造方法が提供され
る。According to the present invention, a first step of manufacturing a prepreg sheet by opening a continuous inorganic fiber bundle and then thermally spraying a matrix metal onto the fibers aligned in one direction; laminating a required number of the above prepreg sheets; Production of a fiber-reinforced metal matrix composite material, which comprises a second step of setting the form in a frame, enclosing the form under reduced pressure in a metal foil bag, and then liquid-phase diffusion bonding the prepreg sheet in the metal foil bag. A method is provided.
連続無機繊維束を構成する繊維としては、例えば炭化ケ
イ素繊維、窒化ケイ素繊維、窒化硼素繊維、窒化アルミ
ニウム繊維、シリカ繊維、ボロン繊維、アルミナ繊維、
炭素繊維、ポリメタロカルボシランを焼成して得られる
５ｉ−Ｔｉ又はＺｒ−Ｃ−０系の無機繊維（宇部興産■
製、チラノ繊維：登録商標）、これらの繊維は単独又は
組み合わせて用いることが出来る。Examples of the fibers constituting the continuous inorganic fiber bundle include silicon carbide fibers, silicon nitride fibers, boron nitride fibers, aluminum nitride fibers, silica fibers, boron fibers, alumina fibers,
5i-Ti or Zr-C-0 based inorganic fiber obtained by firing carbon fiber, polymetallocarbosilane (Ube Industries)
(Tyranno Fiber: Registered Trademark), these fibers can be used alone or in combination.
さらに、本発明における連続無機繊維束として、本願出
願人の平成１年８月１１日付は出願（２）及び平成１年
９月１日付は出願（１１）に添付された明細書の特許請
求の範囲に記載の無機繊維も好適に使用することができ
る。Furthermore, as the continuous inorganic fiber bundle in the present invention, the patent claims of the applicant of the present invention are filed in Application (2) dated August 11, 1999 and Application (11) dated September 1, 1999. The inorganic fibers described in the above range can also be suitably used.
上記出願（２）の明細書に記載された無機繊維は、ｊ）
該重合体を構成するメソフェーズ状態にある多環状芳香
族化合物から導かれるラジアル構造、オニオン構造、ラ
ンダム構造、コアラシアル構造、スキンオニオン構造及
びモザイク構造からなる群から選ばれる少なくとも一種
の結晶配列状態を示す炭素質、
ｉｉ）該重合体を構成する有機溶媒不溶分を含む光学的
等方性の多環状芳香族化合物から導かれる、無配向状態
の結晶質炭素及び／又は非晶質炭素、及び
１ｉｉ）Ｓｉ、Ｃ及びＯから実質的になる非晶質相及び
／又は粒径が５００Å以下の実質的にβＳｉＣからなる
結晶質超微粒子と非晶質のＳ ｉ Ｏｘ （０＜ ｘ
≦２）からなる集合体であり、
構成元素の割合が、Ｓ １ ｉ ３０〜７０重量％、Ｃ
；２０〜６０重景％及重量 ；０．５〜１０重量％であ
る５ｉ−Ｃ−０物質
であることを特徴とする高強度・高弾性率無機繊維であ
る。The inorganic fibers described in the specification of application (2) above are j)
At least one type of crystal orientation state selected from the group consisting of a radial structure, an onion structure, a random structure, a co-radial structure, a skin-onion structure, and a mosaic structure derived from a polycyclic aromatic compound in a mesophase state constituting the polymer. carbonaceous, ii) unoriented crystalline carbon and/or amorphous carbon derived from an optically isotropic polycyclic aromatic compound containing an organic solvent insoluble component constituting the polymer, and 1ii) An amorphous phase consisting essentially of Si, C and O and/or crystalline ultrafine particles consisting essentially of βSiC with a particle size of 500 Å or less and amorphous SiOx (0< x
≦2), and the proportions of the constituent elements are S 1 i 30 to 70% by weight, C
It is a high-strength, high-modulus inorganic fiber characterized by being a 5i-C-0 material having a weight ratio of 20 to 60% and a weight of 0.5 to 10%.
上記繊維は、
ｉ）結合単位（Ｓ ｉ −ＣＨ，） 、または結合単位
（Ｓｉ ＧＨｚ）と結合単位（Ｓｔ−３ｔ）から主と
してなり、珪素原子の側鎖に水素原子、低級アルキル基
、フェニル基及びシリル基からなる群から選ばれる側鎖
基を有し、結合単位（Ｓｉ ＣＨ２）の全数対結合単
位（Ｓｉ−３ｉ）の全数の比が１：０〜２０の範囲にあ
る有機珪素重合体の珪素原子の少なくとも一部が、石油
系又は石炭系のピッチあるいはその熱処理物の芳香族環
と珪素−炭素連結基を介して結合したランダム共重合体
１００重量部、及びｉｉ）石油系又は石炭系ピッチを熱
処理して得られるメソフェーズ状態又はメソフェーズと
光学的等吉相との両相からなる多環状芳香族化合物５〜
５００００重量部を、
２００〜５００°Ｃの範囲の温度で加熱反応及び／又は
加熱溶融して、珪素含有多環状芳香族重合体を得る第１
工程、
上記珪素含有多環状芳香族重合体の紡糸原液を調製して
紡糸する第２工程、
該紡糸原糸を張力下あるいは無張力下で不融化する第３
工程、及び
不融化した前記紡糸繊維を真空中あるいは不活性ガス雰
囲気中で８００〜３０００°Ｃの範囲の温度で焼成する
第４工程
からなることを特徴とする繊維の製造方法により得られ
る。The above-mentioned fiber mainly consists of i) a bonding unit (S i -CH,) or a bonding unit (Si GHz) and a bonding unit (St-3t), and has a hydrogen atom, a lower alkyl group, or a phenyl group in the side chain of a silicon atom. and a silyl group, and the ratio of the total number of bonding units (Si CH2) to the total number of bonding units (Si-3i) is in the range of 1:0 to 20. 100 parts by weight of a random copolymer in which at least a portion of the silicon atoms are bonded to an aromatic ring of petroleum-based or coal-based pitch or a heat-treated product thereof via a silicon-carbon linking group; and ii) petroleum-based or coal-based pitch. Polycyclic aromatic compound consisting of mesophase state obtained by heat treating system pitch or both phases of mesophase and optically isotonic phase 5 ~
A first step of obtaining a silicon-containing polycyclic aromatic polymer by heat-reacting and/or heat-melting 50,000 parts by weight at a temperature in the range of 200 to 500°C.
a second step of preparing a spinning dope of the silicon-containing polycyclic aromatic polymer and spinning it; a third step of infusibleizing the spun yarn under tension or without tension;
and a fourth step of firing the infusible spun fibers at a temperature in the range of 800 to 3000°C in vacuum or in an inert gas atmosphere.
また、前記出願（ＩＱに添付された明細書に記載の無機
繊維は、
ａ）該重合体を構成するメソフェーズ状態にある多環状
芳香族化合物から導かれるラジアル構造、オニオン構造
、ランダム構造、コアラシアル構造、スキンオニオン構
造及びモザイク構造からなる群から選ばれる少なくとも
一種の結晶配列状態を示す炭素質、
ｂ）該重合体を構成する有機溶媒不溶分を含む光学的等
方性の多環状芳香族化合物から導かれる、無配向状態の
結晶質炭素及び／又は非晶質炭素、及び
Ｃ）■Ｓｉ、Ｍ、Ｃ及びＯから実質的になる非晶質物質
、及び／又は
■実質的にβ−３ｉＣ，、ＭＣ，β−３ｉＣとＭＣの固
溶体及びＭＣ，、からなる粒径が５００Å以下の結晶超
微粒子と、非晶質の５ｔＯｙ及びＭＯ，との集合体であ
り
構成元素の割合がＳｉ；５〜７０重量％、Ｍ；０．５〜
４５重量％、Ｃ；２０〜４０重量％及びＯ；０．０１〜
３０重量％である、Ｓｉ−Ｍ−Ｃ−０物質（上記式中、
ＭはＴｉ、Ｚｒ及びＨ「から選択される少なくとも一種
の元素であり、Ｏ＜ｘ＜１．０〈ｙ≦２、Ｏ＜ｚ≦２で
ある。）
であることを特徴とする高強度・高弾性率無機繊維であ
る。In addition, the inorganic fibers described in the specification attached to the above application (IQ) have: a) a radial structure, an onion structure, a random structure, or a core radial structure derived from a polycyclic aromatic compound in a mesophase state constituting the polymer; , a carbonaceous material exhibiting at least one type of crystal orientation selected from the group consisting of a skin onion structure and a mosaic structure, b) an optically isotropic polycyclic aromatic compound containing an organic solvent insoluble component constituting the polymer; C) an amorphous substance consisting essentially of Si, M, C and O, and/or ■ substantially β-3iC, , MC, a solid solution of β-3iC and MC, and MC, an aggregate of crystalline ultrafine particles with a particle size of 500 Å or less, and amorphous 5tOy and MO, and the proportion of the constituent elements is Si; 70% by weight, M; 0.5~
45% by weight, C: 20-40% by weight and O: 0.01-
30% by weight of Si-M-C-0 material (in the above formula:
M is at least one element selected from Ti, Zr, and H, and O<x<1.0<y≦2, O<z≦2. High elastic modulus inorganic fiber.
上記繊維は、
１）結合単位（Ｓ １−ＣＨ２） 、又は結合単位（Ｓ
ｉ −ＣＨ，）と結合単位（Ｓｉ−３ｔ）から主とし
てなり、珪素原子の側鎖に水素原子、低級アルキル基、
フェニル基あるいはシリル基を有し、上記結合単位から
なる主骨格の珪素原子に、Ｍ （Ｍはチタン、ジルコニ
ウム及びハフニウムからなる群から選ばれる少なくとも
一種類の元素である。）が、直接又は酸素原子を介して
、珪素原子の少なくとも一部と結合している遷移金属含
有有機珪素重合体の珪素原子の少なくとも一部が、石油
系又は石炭系のピッチあるいはその熱処理物であって、
有機溶媒不溶分を含むピッチより得られた多環状芳香族
化合物の芳香族環の炭素と結合したランダム共重合体及
び、
２）石油系又は石炭系のピッチから得られる、メソフェ
ーズ又はメソフェーズと光学的等吉相との両相からなる
多環状芳香族化合物とを、２００〜５００°Ｃの範囲の
温度で加熱反応及び／又は加熱溶融して、上記Ｍ及び珪
素を含有する多環状芳香族重合体を得る第１工程、
上記金属含有多環状芳香族重合体の紡糸原液を調製して
紡糸する第２工程、
該紡糸原糸を張力下あるいは無張力下で不融化する第３
工程、及び
不融化した前記紡糸繊維を真空中あるいは不活性ガス雰
囲気中で８００〜３０００°Ｃの範囲の温度で焼成する
第４工程
からなることを特徴とする繊維の製造方法により得られ
る。The above fiber has 1) a bonding unit (S 1-CH2) or a bonding unit (S
i -CH,) and a bonding unit (Si-3t), with hydrogen atoms, lower alkyl groups,
M (M is at least one element selected from the group consisting of titanium, zirconium, and hafnium) is directly attached to the silicon atom of the main skeleton consisting of the above-mentioned bonding units, which has a phenyl group or a silyl group, or is attached to oxygen. At least some of the silicon atoms of the transition metal-containing organosilicon polymer bonded to at least some of the silicon atoms via atoms are petroleum-based or coal-based pitch or a heat-treated product thereof,
2) A random copolymer bonded to the carbon of the aromatic ring of a polycyclic aromatic compound obtained from pitch containing organic solvent-insoluble matter; The polycyclic aromatic compound consisting of both the Tokichi phase and the polycyclic aromatic compound consisting of both phases is heated and reacted and/or heated and melted at a temperature in the range of 200 to 500 ° C to obtain the polycyclic aromatic polymer containing the above M and silicon. a second step of preparing a spinning dope of the metal-containing polycyclic aromatic polymer and spinning it; a third step of infusibleizing the spun yarn under tension or without tension;
and a fourth step of firing the infusible spun fibers at a temperature in the range of 800 to 3000°C in vacuum or in an inert gas atmosphere.
なお、前述した本願出願人の平成１年８月１１日付は出
願（２）及び平成１年９月１日付は出願（ＩＩ）に添付
された明細書の記載は、本明細書の一部として援用され
る。In addition, the description of the above-mentioned specification attached to the application (2) dated August 11, 1999 and the application (II) dated September 1, 1999 by the applicant of the present application is included as a part of the present specification. It will be used.
本発明で使用される連続無機繊維束は開繊操作により薄
く展開された後に張力をかけながら一方向に引揃えられ
る。The continuous inorganic fiber bundle used in the present invention is spread thinly by a fiber opening operation, and then pulled in one direction while applying tension.
マトリックス金属としては、通常、Ａｆ、Ｔｉ、Ｃｕ、
Ｎｉ、これらの合金及びＦｅｇ耐熱合金などが用いられ
る。The matrix metal is usually Af, Ti, Cu,
Ni, alloys thereof, Feg heat-resistant alloys, and the like are used.
溶射方法としては、通常、ガス溶射法、アーク溶射法、
プラズマ溶射法などが用いられる。Thermal spraying methods usually include gas spraying, arc spraying,
Plasma spraying method etc. are used.
一方向に引揃えられた繊維に、溶射操作により、瞬間的
に溶融されたマトリックス金属を吹きつける。これより
シート状の中間素材であるプリブレグシートが得られる
。プリプレグシートは成形可能な程度の厚さを有したも
のであればよく、通常、１００〜２００μｍ程度の厚さ
を有している。The fibers aligned in one direction are instantly sprayed with molten matrix metal using a thermal spraying operation. From this, a prepreg sheet, which is a sheet-like intermediate material, is obtained. The prepreg sheet may have a thickness that can be molded, and usually has a thickness of about 100 to 200 μm.
上記プリプレグシートを所要枚数積層して得られるプリ
プレグシート積層体をセットする型枠は、通常、マトリ
ックス金属より高融点を有し、塑性変形し易い金属ある
いは合金の型枠を使用することが、得られるＦＲＭの繊
維体積率を一定とし、またＦＲＭの形状を一定とするた
めに好ましい。It is usually advantageous to use a formwork made of a metal or alloy that has a higher melting point than the matrix metal and is easily plastically deformed as the formwork in which the prepreg sheet laminate obtained by laminating the required number of prepreg sheets is set. This is preferable in order to keep the fiber volume fraction of the FRM constant and the shape of the FRM constant.
−例を挙げれば、Ａｌがマトリックス金属の場合、Ｃｕ
でできた型枠が好適に使用される。- For example, if Al is the matrix metal, Cu
Formwork made of is preferably used.
上記型枠の形状の一例としては、第１図に示した型枠１
が好適に用いられる。As an example of the shape of the above-mentioned formwork, formwork 1 shown in FIG.
is preferably used.
型枠の内側の形状とセ・ントされるプリプレグシートの
形状は同一であることが好ましく、型枠ｌの内側の寸法
（Ｍ、横の長さ）は、セ・ントされるプリプレグシート
の寸法（縦、横の長さ）より太き（、セットされるプリ
プレグシートの寸法（縦、横の長さ）の１．０１倍以下
であることが好ましい。It is preferable that the shape of the inside of the formwork and the shape of the prepreg sheet to be set are the same, and the inside dimension of the formwork l (M, horizontal length) is the dimension of the prepreg sheet to be set. It is preferable that the thickness is 1.01 times or less the dimensions (length and width) of the prepreg sheet to be set.
セットされるプリプレグシートの寸法（縦、横の長さ）
に対し型枠１の内側の寸法（縦、横の長さ）が過度に大
きいと型枠１にプリプレグシートの積層体２をセットし
ても、型枠１と積層体間に空隙が残り、液相拡散接合す
る際その空隙部に溶融マトリックス金属が流出するため
ＦＲＭの繊維体積率を一定にすることができない。Dimensions of the prepreg sheet to be set (length and width)
On the other hand, if the inside dimensions (length and width) of the formwork 1 are excessively large, even if the prepreg sheet laminate 2 is set in the formwork 1, a gap will remain between the formwork 1 and the laminate. During liquid phase diffusion bonding, the molten matrix metal flows into the voids, making it impossible to keep the fiber volume fraction of the FRM constant.
また、型枠１の上下面は、通常の金属鋳造法で得られる
程度の平面性が確保されていれば充分である。該型枠１
の下面が過度に凸凹であると、液相拡散接合する際、金
属箔と型枠の下面との間に間隙が残り、この間隙部から
溶融マトリックス金属が型枠外に流出するためＦＲＭの
繊維体積率を一定にすることができない。Further, it is sufficient that the upper and lower surfaces of the mold 1 have a level of flatness that can be obtained by a normal metal casting method. The formwork 1
If the bottom surface is excessively uneven, a gap will remain between the metal foil and the bottom surface of the formwork during liquid phase diffusion bonding, and the molten matrix metal will flow out of the formwork from this gap, resulting in a decrease in the fiber volume of the FRM. It is not possible to keep the rate constant.
第１図に、型枠工にプリプレグシートの積層体２をセッ
トした状態の好適な一例を示す。FIG. 1 shows a preferred example of a prepreg sheet laminate 2 set in a formwork.
プリプレグシートの積層体をセットした型枠を封入する
金属箔製袋の素材金属は、７１−リックス金属より高い
融点を有することが好ましい。上記金属箔製袋の素材金
属の融点がマトリックス金属の融点以下では、液相拡散
接合の際、融解等のため上記金属箔製袋が破損し、減圧
状態を保持できず好ましくない。−例を挙げれば、ＡＰ
がマトリックス金属の場合、ステンレス鋼が前記金属箔
製袋の素材金属として好適に使用される。Preferably, the material metal of the metal foil bag that encloses the formwork in which the prepreg sheet laminate is set has a melting point higher than that of 71-Rix metal. If the melting point of the material metal of the metal foil bag is lower than the melting point of the matrix metal, the metal foil bag will be damaged due to melting during liquid phase diffusion bonding, and a reduced pressure state cannot be maintained, which is not preferable. -For example, AP
When the matrix metal is stainless steel, stainless steel is suitably used as the material metal for the metal foil bag.
金属箔製袋は、その厚さが１０〜１００μｍであるのが
好ましい。上記より薄いと、プリプレグシートの積層体
をセットした型枠を封入する際、袋が破壊したり、また
、熱を加え封じる場合、その熱により袋全体が溶解した
りして好ましくない。It is preferable that the metal foil bag has a thickness of 10 to 100 μm. If it is thinner than the above, the bag may be destroyed when enclosing the formwork in which the laminate of prepreg sheets is set, or the entire bag may melt due to the heat when it is sealed with heat, which is undesirable.
上記より厚いと製造・加工がしにくくなり、かつ金属箔
製袋を真空排気する際、袋そのものの変形がおこりにく
く、型枠上下面と袋の間に隙間が住じ、液相拡散接合の
際、その隙間より溶融金属が型枠外の空隙部に流失し、
本発明の目的を達成することができない。If it is thicker than the above, it will be difficult to manufacture and process, and when the metal foil bag is evacuated, the bag itself will be less likely to deform, and a gap will exist between the top and bottom of the formwork and the bag, making it difficult for liquid phase diffusion bonding to occur. At this time, molten metal flows from the gap into the void outside the formwork,
The purpose of the present invention cannot be achieved.
金属箔製袋の大きさは、プリプレグシート積層体をセッ
トした型枠が入る大きさであればよいが、型枠の大きさ
と同程度であることが好ましい。型枠の大きさに比べ、
大き過ぎてもそれによる効果はなく経済的でない。The size of the metal foil bag may be large enough to accommodate the mold in which the prepreg sheet laminate is set, but it is preferably about the same size as the mold. Compared to the size of the formwork,
If it is too large, there will be no effect and it will not be economical.
プリプレグシート積層体がセットされた型枠を金属箔製
袋に封入する好適な方法としては、型枠挿入端部及び真
空排気用端部を備えた金属箔製袋に前記挿入端部より型
枠を挿入後、その挿入端部を封じ、次いで真空排気用端
部より真空排気を行い、減圧下に排気用端部も封じる方
法を挙げることができる。A preferred method for enclosing a formwork in which a prepreg sheet laminate is set in a metal foil bag is to insert the formwork from the insertion end into a metal foil bag equipped with a formwork insertion end and a vacuum evacuation end. After insertion, the insertion end is sealed, and then the evacuation end is evacuated from the evacuation end, and the evacuation end is also sealed under reduced pressure.
金属箔製袋の上記端部を封じる手段として、レーザー溶
接法、電子ビーム溶接法及びティグ溶接法を用いること
が、良好な溶接部を得るために好ましい。レーザー溶接
法は取扱が簡便であり、特に好ましい。It is preferable to use laser welding, electron beam welding, or TIG welding as a means for sealing the ends of the metal foil bag in order to obtain a good welded area. Laser welding is easy to handle and is particularly preferred.
本発明によれば、型枠の上下面を金属箔で密閉した状態
とすることができるため、液相拡散接合する際、型枠か
ら溶融金属が漏れることがなく、従ってＦＲＭの繊維体
積率や形状を一定に保持することができる。According to the present invention, since the upper and lower surfaces of the formwork can be sealed with metal foil, molten metal does not leak from the formwork during liquid phase diffusion bonding. The shape can be kept constant.
上記の減圧状態で封じられた金属箔製袋は、通常のホッ
トプレス装置により、液相拡散接合処理を施す。The metal foil bag sealed under reduced pressure is subjected to liquid phase diffusion bonding using a normal hot press device.
液相拡散接合条件はＦＲＭのマトリックス金属によって
異なるが、例えば、マトリックス金属がＡｌの場合、加
熱温度が６６０〜７００°Ｃ１圧力が１０ゞ５００ ｋ
ｇ／ｅｔａ、ホットプレス時間が３０〜３００秒の範囲
であるのが好ましい。Liquid phase diffusion bonding conditions vary depending on the matrix metal of the FRM, but for example, if the matrix metal is Al, the heating temperature is 660 to 700°C, the pressure is 10° to 500°C.
g/eta and hot press time are preferably in the range of 30 to 300 seconds.
（発明の効果） 本発明によれば以下のような優れた効果が奏される。(Effect of the invention) According to the present invention, the following excellent effects are achieved.
（１）プリプレグシート積層体がセットされた型枠を収
納する金属箔製袋は、金属薄板製容器に比べ、薄いため
、製造・加工し易い。(1) The metal foil bag that houses the formwork in which the prepreg sheet laminate is set is thinner than the thin metal plate container, so it is easier to manufacture and process.
（２）プリプレグシートの積層体を型枠内にセットし、
その型枠を上記袋中に真空封入しているため繊維体積率
（■ｆ）、形状が一定のＦＲＭを製造することができる
。(2) Set the prepreg sheet laminate in the formwork,
Since the mold is vacuum sealed in the bag, it is possible to produce an FRM with a constant fiber volume fraction (■f) and a constant shape.
（実施例） 以下に実施例を示す。(Example) Examples are shown below.
実施例１
直径１０μｍの５ｉ−Ｔｉ−Ｃ−０繊維（宇部興産■製
チラノ繊維：登録商標）４００本よりなる繊維束を均一
に開繊し張力をかけながら一方向に引揃えた。このよう
にして引揃えた繊維にプラズマ溶射により溶融したアル
ミニウムをプラズマスプレー、プリプレグシートを作成
した。その際、プラズマスプレー装置のノズルは繊維面
より１４０ ｍｍ離れていた。Example 1 A fiber bundle consisting of 400 5i-Ti-C-0 fibers (Tyranno Fiber manufactured by Ube Industries, Ltd.: registered trademark) having a diameter of 10 μm was uniformly opened and pulled in one direction while applying tension. The thus arranged fibers were plasma sprayed with molten aluminum by plasma spraying to create a prepreg sheet. At that time, the nozzle of the plasma spray device was 140 mm away from the fiber surface.
このようにして作成したプリプレグシートの厚さは１３
０〜１５０μｍであった。このプリプレグシートより、
繊維方向に９０ｍｍ、繊維と垂直方向に６０胴のシート
を切り出し、そのシートを５０枚積層して一方向積層体
とし、これを型枠内にセットした。この積層体を型枠と
共にステンレス箔（厚さ＝６０μｍ）製袋に挿入し、挿
入端部をレーザービームにて溶接した。その後、他端部
より、内部がＩ Ｘ １０−２ｍｎ＋Ｈｇになるまで真
空吸弓を行った後、この部分をレーザービームにて溶接
した。The thickness of the prepreg sheet created in this way was 13
It was 0 to 150 μm. From this prepreg sheet,
A sheet of 90 mm in the fiber direction and 60 cylinders in the direction perpendicular to the fiber was cut out, and 50 of the sheets were laminated to form a unidirectional laminate, which was set in a mold. This laminate was inserted into a stainless steel foil (thickness = 60 μm) bag together with a mold, and the inserted end was welded with a laser beam. Thereafter, vacuum suction was performed from the other end until the inside became I x 10-2 mn+Hg, and then this part was welded with a laser beam.
上記減圧状態で両端を封じた金属箔製袋は、ホットプレ
ス装置内に入れ、６６０°Ｃに加熱後、油圧プレスにて
金型を１００ ｋｇ／ｃ＋１１の圧力で１分間プレスし
てＦＲＭを得た。得られたＦＲＭは繊維分布が均一であ
り、八！のみの部分は存在せず、繊維体積率を一定に保
つことができた。The metal foil bag sealed at both ends in the reduced pressure state was placed in a hot press device and heated to 660°C, then the mold was pressed with a hydraulic press at a pressure of 100 kg/c + 11 for 1 minute to obtain an FRM. Ta. The obtained FRM had a uniform fiber distribution and an 8! There were no cracked parts, and the fiber volume fraction could be kept constant.
また、型枠に沿った一定の形状を保持していた。Moreover, it maintained a certain shape along the formwork.
第１図は、プリプレグシートの積層体がセットされた型
枠を示す斜視図である。FIG. 1 is a perspective view showing a formwork in which a laminate of prepreg sheets is set.
Claims (1)
維にマトリックス金属を溶射してプリプレグシートを製
造する第１工程、 上記プリプレグシートを所要枚数積層して、型枠中にセ
ットし、この型枠を金属箔製袋中に減圧下に封入した後
、該金属箔製袋中のプリプレグシートを液相拡散接合す
る第２工程よりなることを特徴とする繊維強化金属基複
合材料の製造方法。[Claims] A first step of manufacturing a prepreg sheet by opening a continuous inorganic fiber bundle and then thermally spraying a matrix metal onto the fibers aligned in one direction; laminating a required number of the above prepreg sheets; A second step of setting a prepreg sheet in a frame, enclosing the form under reduced pressure in a metal foil bag, and liquid-phase diffusion bonding the prepreg sheet in the metal foil bag. A method for manufacturing a metal matrix composite material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24795489A JPH03111526A (en) | 1989-09-26 | 1989-09-26 | Manufacture of fiber reinforced metal matrix composite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24795489A JPH03111526A (en) | 1989-09-26 | 1989-09-26 | Manufacture of fiber reinforced metal matrix composite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03111526A true JPH03111526A (en) | 1991-05-13 |
Family
ID=17171023
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24795489A Pending JPH03111526A (en) | 1989-09-26 | 1989-09-26 | Manufacture of fiber reinforced metal matrix composite |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03111526A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7726942B2 (en) * | 2004-01-23 | 2010-06-01 | Lm Glasfiber A/S | Connector box partly embedded in a fibre-reinforced part for protecting and connecting purposes |
| KR20160047715A (en) * | 2014-10-23 | 2016-05-03 | 한국에너지기술연구원 | Mixed flow impeller having hollow airfoil blades |
-
1989
- 1989-09-26 JP JP24795489A patent/JPH03111526A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7726942B2 (en) * | 2004-01-23 | 2010-06-01 | Lm Glasfiber A/S | Connector box partly embedded in a fibre-reinforced part for protecting and connecting purposes |
| KR20160047715A (en) * | 2014-10-23 | 2016-05-03 | 한국에너지기술연구원 | Mixed flow impeller having hollow airfoil blades |
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