JPH0920570A - Production of composite material of three-dimensionally woven fiber - Google Patents
Production of composite material of three-dimensionally woven fiberInfo
- Publication number
- JPH0920570A JPH0920570A JP7170899A JP17089995A JPH0920570A JP H0920570 A JPH0920570 A JP H0920570A JP 7170899 A JP7170899 A JP 7170899A JP 17089995 A JP17089995 A JP 17089995A JP H0920570 A JPH0920570 A JP H0920570A
- Authority
- JP
- Japan
- Prior art keywords
- slurry
- mold
- woven fiber
- dimensional woven
- pouring
- 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 11
- 239000002131 composite material Substances 0.000 title claims description 11
- 239000002002 slurry Substances 0.000 claims abstract description 34
- 239000011159 matrix material Substances 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract 4
- 229910018404 Al2 O3 Inorganic materials 0.000 abstract 2
- 229910052681 coesite Inorganic materials 0.000 abstract 2
- 229910052906 cristobalite Inorganic materials 0.000 abstract 2
- 239000000377 silicon dioxide Substances 0.000 abstract 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract 2
- 229910052682 stishovite Inorganic materials 0.000 abstract 2
- 229910052905 tridymite Inorganic materials 0.000 abstract 2
- 229910007277 Si3 N4 Inorganic materials 0.000 abstract 1
- 229910003465 moissanite Inorganic materials 0.000 abstract 1
- 229910010271 silicon carbide Inorganic materials 0.000 abstract 1
- 239000000919 ceramic Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 6
- 238000002347 injection Methods 0.000 description 6
- 239000007924 injection Substances 0.000 description 6
- 239000012752 auxiliary agent Substances 0.000 description 5
- 238000010304 firing Methods 0.000 description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011226 reinforced ceramic Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 229910003077 Ti−O Inorganic materials 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は３次元織繊維複合体
の製造方法に関し、特にガスタービンの燃焼環（燃焼器
内筒）、静翼、動翼等として有利に適用できる同複合体
の製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a three-dimensional woven fiber composite, and particularly to the production of the composite which can be advantageously applied as a combustion ring (combustor inner cylinder) of a gas turbine, a stationary blade, a moving blade or the like. Regarding the method.
【０００２】[0002]
【従来の技術】３次元織繊維複合体の製造方法として
は、３次元織繊維構造体にガス前駆体を用いて化学反応
によりマトリックスを形成する化学蒸着法や、３次元織
繊維構造体に粘度の高いスラリを圧力をかけて注入する
手法などがある。前者の方法では目的のマトリックスを
作るためのガスが必要で、これによって作られるマトリ
ックスが制限される。後者の方法は高圧によって３次元
織繊維構造体が変形したり、乾燥に時間がかゝるという
問題がある。2. Description of the Related Art As a method for producing a three-dimensional woven fiber composite, a chemical vapor deposition method in which a gas precursor is used in a three-dimensional woven fiber structure to form a matrix by a chemical reaction, and a three-dimensional woven fiber structure having a viscosity There is a method of injecting a high slurry under pressure. The former method requires a gas to produce the desired matrix, which limits the matrix produced. The latter method has the problems that the three-dimensional woven fiber structure is deformed by high pressure and it takes a long time to dry.
【０００３】さらに、この種の繊維複合体の製法とし
て、繊維状セラミックスを均一に分散させたセラミック
ス泥漿を所定形状の型によって成形して脱水乾燥させる
方法（特公平５−４５５５６号公報）があるが不連続繊
維を用いているため製造されたセラミックスには高靱性
が望めない。また、接触部を接合した繊維の間隙にセラ
ミックスを含む泥漿物を充填して乾燥焼結して良好な靱
性、耐熱衝撃性および耐熱性を有する繊維強化セラミッ
クスを製造する方法（特公昭５８−５１９１３号公報）
があるが、泥漿物を充填する際に圧力をかけていないた
め、密に織られた繊維構造物に泥漿物を注入することが
困難であるばかりでなく、固化に時間がかゝるという問
題があった。さらに、またセラミックス粉末スラリを含
浸させた繊維のみの成形体を焼成することにより高強
度、高靱性の繊維強化セラミックスの製造方法（特開昭
６３−２４８７７７号公報）もあるが、不連続繊維を用
いているため、製造されたセラミックスの高靱性は不十
分であった。Further, as a method for producing this kind of fiber composite, there is a method (Japanese Patent Publication No. 5-45556) in which a ceramic slurry in which fibrous ceramics are uniformly dispersed is molded by a mold having a predetermined shape and dehydrated and dried. However, high toughness cannot be expected in the produced ceramics because of the use of discontinuous fibers. Further, a method of manufacturing a fiber reinforced ceramic having good toughness, thermal shock resistance and heat resistance by filling a slurry containing ceramics in the gap between the fibers bonded to the contact portions and drying and sintering (Japanese Patent Publication No. 58-51913). Issue)
However, since pressure is not applied when filling the sludge, not only is it difficult to inject the sludge into the densely woven fiber structure, but it also takes time to solidify. was there. Furthermore, there is also a method for producing a fiber-reinforced ceramic having high strength and high toughness by firing a molded body of only fibers impregnated with a ceramic powder slurry (Japanese Patent Laid-Open No. 63-248777). Since it is used, the high toughness of the manufactured ceramic was insufficient.
【０００４】[0004]
【発明が解決しようとする課題】本発明は上記技術水準
に鑑み、従来のスラリ注入法における欠点、例えば乾燥
時に収縮が大きいこと、密な３次元織繊維構造体中への
セラミックススラリの注入が困難なことなどの欠点を解
消しうる３次元織繊維複合体の製造方法を提供しようと
するものである。SUMMARY OF THE INVENTION In view of the above-mentioned state of the art, the present invention has drawbacks in the conventional slurry injection method, such as large shrinkage during drying and injection of ceramics slurry into a dense three-dimensional woven fiber structure. It is an object of the present invention to provide a method for producing a three-dimensional woven fiber composite, which can solve the drawbacks such as difficulty.
【０００５】[0005]
【課題を解決するための手段】本発明は分割可能な多孔
質鋳型中に３次元織繊維構造体をセットし、マトリック
ス前駆体となる低粘度スラリを気体圧力によって該３次
元織繊維構造体に注入充填したのち、前記鋳型から取出
して乾燥、焼成することを特徴とする３次元織繊維複合
体の製造方法である。According to the present invention, a three-dimensional woven fiber structure is set in a dividable porous mold, and a low viscosity slurry serving as a matrix precursor is applied to the three-dimensional woven fiber structure by gas pressure. A method for producing a three-dimensional woven fiber composite, which comprises injecting and filling, taking out from the mold, drying and firing.
【０００６】[0006]
【発明の実施の形態】本発明にいう３次元織繊維構造体
とはそのものばかりでなく、二次元織繊維構造体の積層
体をステッチ糸で固定したものをも含まれる。この３次
元織繊維構造体の繊維としてはＡｌ2 Ｏ3 ，ＳｉＣ，チ
ラノ（宇部興産製繊維で、Ｓｉ−Ｃ−Ｔｉ−Ｏ系のも
の），Ｃ，ＺｒＯ2 ，ＳｉＯ2 などの材質の繊維が使用
される。また、マトリックス前駆体となる低粘度スラリ
（以下、これを”原料スラリ”という）の材料としては
Ａｌ2 Ｏ3 ，ＳｉＣ，Ｓｉ3 Ｎ4 ，ＺｒＯ2 ，ＳｉＯ2
などが用いられ、これら原料スラリに対して種々の助剤
を添加したものも用いられる。例えばＡｌ2 Ｏ3 スラリ
に対しては助剤としてＭｇＯを、Ｓｉ3 Ｎ4 スラリに対
しては助剤としてＡｌ2 Ｏ3 ，Ｙ2 Ｏ3 を、ＺｒＯ2 ス
ラリに対しては助剤としてＹ2 Ｏ3 ，ＣｅＯ，ＣａＯ，
ＭｇＯを添加したものなどがあげられる。さらに原料ス
ラリを安定化するために界面活性剤を分散剤として添加
してもよい。原料スラリの粘度は１００〜４００ｃｐ
ｓ、特に好ましくは２００〜３０ｃｐｓの範囲である。
１００ｃｐｓ未満では３次元織繊維構造体への着床に時
間がかゝりやすく、４００ｃｐｓを越えると該構造体中
への注入がし難いからである。BEST MODE FOR CARRYING OUT THE INVENTION Not only the three-dimensional woven fiber structure referred to in the present invention but also a two-dimensional woven fiber structure in which a laminate is fixed with a stitch thread. As the fibers of this three-dimensional woven fiber structure, fibers of materials such as Al 2 O 3 , SiC, Tyranno (fibers manufactured by Ube Industries, Si-C-Ti-O type), C, ZrO 2 , SiO 2 and the like. Is used. The low viscosity slurry (hereinafter referred to as "raw material slurry") as a matrix precursor Al 2 O 3 as a material for, SiC, Si 3 N 4, ZrO 2, SiO 2
Etc. are used, and those obtained by adding various auxiliary agents to these raw material slurries are also used. For example, MgO as an auxiliary agent for Al 2 O 3 slurry, Al 2 O 3 , Y 2 O 3 as an auxiliary agent for Si 3 N 4 slurry, and Y as an auxiliary agent for ZrO 2 slurry. 2 O 3 , CeO, CaO,
Examples include those to which MgO is added. Further, a surfactant may be added as a dispersant to stabilize the raw material slurry. The viscosity of the raw material slurry is 100-400 cp
s, particularly preferably in the range of 200 to 30 cps.
When it is less than 100 cps, it takes a long time to land on the three-dimensional woven fiber structure, and when it exceeds 400 cps, it is difficult to inject it into the structure.
【０００７】原料スラリは任意の気体、一般的には空
気、によって３次元織繊維構造体中に注入される。注入
圧力は限定的なものではないが、一般的に３０Ｋｇｆ／
ｃｍ2以下でよく、１〜５Ｋｇｆ／ｃｍ2 の範囲が好ま
しい。注入後、乾燥するが、乾燥はなるべくゆっくりな
条件が好ましく、一般的には湿度：８０〜９０％，室温
下で乾燥することが好ましい。乾燥後の焼成温度は各セ
ラミックスによって異なり一概に限定できないが、焼結
反応が生じ、かつ粒の粗大化、溶融が生じない条件にす
べきであり、概略的にいえば１５００〜２０００℃で１
〜１０時間の条件である。なお、焼成前に、セラミック
ススラリに有機バインダが添加されている場合には４０
０〜７００℃，１〜６時間の条件で脱脂することが望ま
しい。The raw slurry is injected into the three-dimensional woven fiber structure by any gas, generally air. The injection pressure is not limited, but is generally 30 Kgf /
cm 2 or less is preferable, and a range of 1 to 5 Kgf / cm 2 is preferable. After the injection, it is dried, but it is preferable that the drying is performed as slowly as possible, and in general, it is preferable to dry at a humidity of 80 to 90% at room temperature. The firing temperature after drying varies depending on each ceramic and cannot be unconditionally limited. However, the conditions should be such that a sintering reaction occurs, grain coarsening, and melting do not occur.
It is a condition of 10 hours. If an organic binder is added to the ceramics slurry before firing, it will be 40
It is desirable to degrease under conditions of 0 to 700 ° C. and 1 to 6 hours.
【０００８】[0008]
【実施例】以下、図１を参照しながら、本発明の一実施
例を説明する。アルミナの長繊維を用いてあらかじめ製
織した３次元織繊維構造体２を石膏製の鋳型１（１ａ：
上型，１ｂ：下型）にセットする。スラリタンク５の中
に、アルミナ粉末：３０００ｇに対して助剤のマグネシ
ア粉末：３ｇを混合したものに対してｎ−ブチルアルコ
ール：９００ｇと分散剤：３０ｇを入れてボールミルに
て混合して調合したスラリ７を入れる。コンプレッサ６
によって圧力：３Ｋｇｆ／ｃｍ2 で結合管４、導管３を
介してスラリ７を３次元織繊維構造中に注入し約１時間
後に注入を終了する。マトリックスとなるスラリ７を注
入した３次元織繊維構造体２を、鋳型１を分割して取出
し、湿度：８５％，温度：３０℃で４８時間乾燥させ
る。これを６００℃で３時間かけて大気中で脱脂後、１
６００℃で２時間大気中で焼成し３次元織繊維複合体を
得た。得られた複合体は本発明が狙いとする曲げ強度：
６０Ｋｇｆ／ｍｍ2 以上、破壊靱性値：１５Ｋｇｆ／ｍ
ｍ3/2 以上の物性を有していた。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be described below with reference to FIG. A three-dimensional woven fiber structure 2 previously woven using long filaments of alumina is cast in a plaster mold 1 (1a:
Upper mold, 1b: lower mold). In a slurry tank 5, n-butyl alcohol (900 g) and dispersant (30 g) were added to a mixture of alumina powder (3000 g) and auxiliary agent magnesia powder (3 g). Add Slurry 7. Compressor 6
Then, the slurry 7 is injected into the three-dimensional woven fiber structure through the connecting pipe 4 and the conduit 3 at a pressure of 3 Kgf / cm 2 and the injection is finished after about 1 hour. The three-dimensional woven fiber structure 2 in which the slurry 7 serving as a matrix is injected is taken out by dividing the mold 1 and dried at a humidity of 85% and a temperature of 30 ° C. for 48 hours. After degreasing this in air at 600 ° C for 3 hours, 1
A three-dimensional woven fiber composite was obtained by firing in air at 600 ° C. for 2 hours. The resulting composite has a bending strength targeted by the present invention:
60 kgf / mm 2 or more, fracture toughness value: 15 kgf / m
It had physical properties of m 3/2 or more.
【０００９】[0009]
【発明の効果】本発明によれば、粘度の低い液状のスラ
リを用いるので３次元織繊維構造体への注入が容易とな
りかつ注入できるスラリの種類も増える。同時に小規模
の装置で実施できるため、コスト低減が図れる。処理時
間に関しても化学蒸着法と較べて短時間となる。さら
に、多孔質鋳型、特に石膏型を用いてスラリ中の水分を
吸収させるため、スラリの乾燥に必要な時間を短縮する
ことができる。According to the present invention, since a liquid slurry having a low viscosity is used, the injection into the three-dimensional woven fiber structure is facilitated and the types of slurries that can be injected are increased. At the same time, the cost can be reduced because it can be performed by a small-scale device. The processing time is also shorter than that of the chemical vapor deposition method. Furthermore, since the water content in the slurry is absorbed by using a porous mold, particularly a gypsum mold, the time required for drying the slurry can be shortened.
【図１】本発明の一実施例の説明図。FIG. 1 is an explanatory diagram of an embodiment of the present invention.
Claims (1)
構造体をセットし、マトリックス前駆体となる低粘度ス
ラリを気体圧力によって該３次元織繊維構造体に注入充
填したのち、前記鋳型から取出して乾燥、焼成すること
を特徴とする３次元織繊維複合体の製造方法。1. A three-dimensional woven fiber structure is set in a dividable porous mold, and a low-viscosity slurry that serves as a matrix precursor is injected and filled into the three-dimensional woven fiber structure by gas pressure. A method for producing a three-dimensional woven fiber composite, which is characterized in that the three-dimensional woven fiber composite is taken out from the product, dried and fired.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7170899A JPH0920570A (en) | 1995-07-06 | 1995-07-06 | Production of composite material of three-dimensionally woven fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7170899A JPH0920570A (en) | 1995-07-06 | 1995-07-06 | Production of composite material of three-dimensionally woven fiber |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0920570A true JPH0920570A (en) | 1997-01-21 |
Family
ID=15913397
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7170899A Pending JPH0920570A (en) | 1995-07-06 | 1995-07-06 | Production of composite material of three-dimensionally woven fiber |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0920570A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0426564A (en) * | 1990-05-22 | 1992-01-29 | Nippon Cement Co Ltd | Production of fiber-reinforced ceramics |
-
1995
- 1995-07-06 JP JP7170899A patent/JPH0920570A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0426564A (en) * | 1990-05-22 | 1992-01-29 | Nippon Cement Co Ltd | Production of fiber-reinforced ceramics |
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| Date | Code | Title | Description |
|---|---|---|---|
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Free format text: JAPANESE INTERMEDIATE CODE: A02 Effective date: 19970930 |