JPS63312328A - Production of polyimide polymer reinforced with sic whisker - Google Patents
Production of polyimide polymer reinforced with sic whiskerInfo
- Publication number
- JPS63312328A JPS63312328A JP14711987A JP14711987A JPS63312328A JP S63312328 A JPS63312328 A JP S63312328A JP 14711987 A JP14711987 A JP 14711987A JP 14711987 A JP14711987 A JP 14711987A JP S63312328 A JPS63312328 A JP S63312328A
- Authority
- JP
- Japan
- Prior art keywords
- polyimide resin
- whisker
- sic
- polyimide polymer
- polymer
- 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.)
- Granted
Links
- 229920001721 polyimide Polymers 0.000 title claims abstract description 55
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 229920000642 polymer Polymers 0.000 title abstract 11
- 239000004642 Polyimide Substances 0.000 title abstract 7
- 239000002612 dispersion medium Substances 0.000 claims abstract description 11
- 239000011812 mixed powder Substances 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims abstract description 7
- 239000011159 matrix material Substances 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 239000009719 polyimide resin Substances 0.000 claims description 46
- 239000002131 composite material Substances 0.000 abstract description 11
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 238000005299 abrasion Methods 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000011247 coating layer Substances 0.000 abstract 2
- 230000006835 compression Effects 0.000 abstract 1
- 238000007906 compression Methods 0.000 abstract 1
- 238000000748 compression moulding Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 101001120264 Arabidopsis thaliana Polyadenylate-binding protein 1 Proteins 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- XQUPVDVFXZDTLT-UHFFFAOYSA-N 1-[4-[[4-(2,5-dioxopyrrol-1-yl)phenyl]methyl]phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C(C=C1)=CC=C1CC1=CC=C(N2C(C=CC2=O)=O)C=C1 XQUPVDVFXZDTLT-UHFFFAOYSA-N 0.000 description 1
- 240000006439 Aspergillus oryzae Species 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000007970 homogeneous dispersion Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920003192 poly(bis maleimide) Polymers 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Landscapes
- Reinforced Plastic Materials (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、SiCウィスカーを複合強化したポリイミド
樹脂組成物の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for producing a polyimide resin composition composite-reinforced with SiC whiskers.
ポリイミド樹脂は、耐熱性に優れ、エンジニアリングプ
ラスヂックとして航空機、自動車、建設機械あるいは電
気・電子産業の分野などで有用されている。更に、ポリ
イミド樹脂にカーボン繊維、ケプラー繊維などを複合し
、高強度、高弾性の要求される機能部品としての用途開
発も試みられている。Polyimide resin has excellent heat resistance and is useful as an engineering plastic in the fields of aircraft, automobiles, construction machinery, and the electrical and electronic industries. Furthermore, attempts are being made to composite polyimide resin with carbon fibers, Kepler fibers, etc., and develop applications for functional parts that require high strength and high elasticity.
SiCウィスカーは直径0.1〜lμL長さ30〜10
0μMの針状単結晶からなる微細繊維状物質であり、結
晶内の格子欠陥が殆んと無いために極めて高度の比強度
、比弾性率を有し、更に耐熱性、耐蝕性なども優れてい
るために樹脂や金属などの補強フィラーとして有用され
ている。このSiCウィスカーを複合強化したポリイミ
ド樹脂は、軽量化および機械的強度や耐摩耗性の高度化
が要求される各種用途分野における構造部材として有用
されることが期待される。SiC whiskers have a diameter of 0.1 to 1μL and a length of 30 to 10
It is a fine fibrous material consisting of acicular single crystals with a density of 0 μM, and because there are almost no lattice defects within the crystal, it has extremely high specific strength and specific modulus, and also has excellent heat resistance and corrosion resistance. Because of this, it is useful as a reinforcing filler for resins and metals. This polyimide resin composite reinforced with SiC whiskers is expected to be useful as a structural member in various application fields where weight reduction and high mechanical strength and wear resistance are required.
しかしながら、ポリイミド樹脂とSiCウィスカーは界
面濡れ性が悪く、なじみ難いので、両者を単に均質混合
して複合化しても、ポリイミド樹脂とSiCウィスカー
の強固な接着状態が形成され難いために複合効果が充分
に発揮されず、強度特性の向上をはかることができない
。However, polyimide resin and SiC whiskers have poor interfacial wettability and are difficult to mix, so even if they are simply mixed homogeneously to form a composite, it is difficult to form a strong adhesive state between polyimide resin and SiC whiskers, so the composite effect is not sufficient. Therefore, it is not possible to improve the strength properties.
例えば、エタノールなどの有機分散媒中にポリイミド樹
脂およびSiCウィスカーを混合し、撹拌分散させた後
ろ過乾燥して均質な混合粉末を得、この混合粉末を成形
しても、充分な強度特性の複合材を得ることが困難であ
る。また、ポリイミド樹脂を95〜110℃に加熱溶融
してSiCウィスカーをローラーなどで強力に混合する
方法は、混合過程でウィスカーの折損やポリイミド樹脂
の劣化を生じ易い難点がある。For example, even if a polyimide resin and SiC whiskers are mixed in an organic dispersion medium such as ethanol, stirred and dispersed, and then overdried to obtain a homogeneous mixed powder, this mixed powder can be molded and still have sufficient strength properties. It is difficult to obtain wood. Furthermore, the method of heating and melting polyimide resin at 95 to 110° C. and vigorously mixing SiC whiskers with a roller or the like has the drawback that the whiskers are likely to break or the polyimide resin is likely to deteriorate during the mixing process.
本発明は、上記問題点を解決するために、SiCウィス
カーの表面に予めポリイミド樹脂の被膜を形成させ、次
いでマトリックスとなるポリイミド樹脂と混合複合化す
ることにより、SiCウィスカーとポリイミド樹脂の強
固な接合をはかるものである。In order to solve the above problems, the present invention forms a film of polyimide resin on the surface of the SiC whiskers in advance, and then mixes and composites the film with the polyimide resin that serves as the matrix, thereby creating a strong bond between the SiC whiskers and the polyimide resin. It measures the
すなわち、本発明はポリイミド樹脂を有機溶媒に30g
/l以下の割合で溶解し、この溶液中にSiCウィスカ
ーを混合分散した後、が過乾燥してSiCウィスカーを
表面にポリイミド樹脂の被膜を形成し、このようにして
予めポリイミド樹脂の被膜を形成したSiCウィスカー
とマトリックスとなるポリイミド樹脂を有機分散媒に分
散、濾過乾燥して有機分散媒を除去し、得られる混合粉
末を熱圧成形することを構成的特徴とするSiCウィス
カー強化ポリイミド樹脂の製造方法である。That is, in the present invention, 30g of polyimide resin is added to an organic solvent.
After mixing and dispersing the SiC whiskers in this solution, the SiC whiskers are overdried to form a polyimide resin film on the surface of the SiC whiskers, thus forming a polyimide resin film in advance. Production of a SiC whisker-reinforced polyimide resin characterized by dispersing SiC whiskers and a polyimide resin as a matrix in an organic dispersion medium, filtering and drying to remove the organic dispersion medium, and hot-pressing the resulting mixed powder. It's a method.
有機溶媒は、ポリイミド樹脂を溶解し得るものであれば
よく、例えばアセトンやN、N−ジメチルポルムアミド
などが用いられる。ポリイミド樹脂は、これらの有機溶
媒中に309/l以下の割合で溶解させる。ポリイミド
樹脂の割合が30g/lを越えると溶液の粘度が上昇し
て撹拌混合が困難となり、SiCウィスカーと均質に分
散させ難いためである。また、SiCウィスカー表面に
被膜を形成するためには、ポリイミド樹脂を高濃度にす
る必要がないためである。この溶液中にSiCウィスカ
ーを混合分散させる場合、SiCウィスカーに対しポリ
イミド樹脂が05〜10重量%になるように設定するこ
とが好ましい。10重量%を越えるとポリイミド被膜の
結合によりSiCウィスカーが凝集し易いためであり、
0.5重量%を下回る場合はSiCウィスカー表面に均
質な被膜形成が困難となるからである。この場合、Si
Cウィスカーを予めシランカップリング剤などで表面処
理するとポリイミド樹脂との界面濡れ性を更に向上させ
ることができる。この混合分散液をか過して、濾過ケー
キを風乾もしくは加温して有機溶媒を除去することによ
り、ポリイミド樹脂の被膜を形成したSiCウィスカー
が得られる。The organic solvent may be any solvent as long as it can dissolve the polyimide resin, and examples thereof include acetone and N,N-dimethylpolamide. The polyimide resin is dissolved in these organic solvents at a ratio of 309/l or less. This is because if the proportion of the polyimide resin exceeds 30 g/l, the viscosity of the solution increases, making stirring and mixing difficult and making it difficult to homogeneously disperse it with SiC whiskers. This is also because it is not necessary to use a high concentration of polyimide resin in order to form a film on the surface of the SiC whisker. When mixing and dispersing SiC whiskers in this solution, it is preferable to set the amount of polyimide resin to be 05 to 10% by weight relative to the SiC whiskers. This is because if it exceeds 10% by weight, SiC whiskers tend to aggregate due to the bonding of the polyimide film.
This is because if it is less than 0.5% by weight, it will be difficult to form a homogeneous film on the surface of the SiC whisker. In this case, Si
If the surface of the C whiskers is previously treated with a silane coupling agent or the like, the interfacial wettability with the polyimide resin can be further improved. By filtering this mixed dispersion and removing the organic solvent by air drying or heating the filter cake, SiC whiskers having a polyimide resin coating formed thereon can be obtained.
次いで、マトリックスのポリイミド樹脂と前記被膜形成
SiCウィスカーをエタノールなどの有機分散媒中に分
散させ、が過乾燥して有機分散媒を除去することにより
、均質な混合粉末を得ることができる。ポリイミド樹脂
とSiCウィスカーの混合比は、複合材とした場合のV
f値を考慮して設定する。なお、有機分散媒の量は均質
分散さ仕るために分散液の粘度などを考慮して定めるが
、ポリイミド樹脂とSiCウィスカーの合計量に対して
5容量倍以上に設定することが好ましい。Next, a homogeneous mixed powder can be obtained by dispersing the matrix polyimide resin and the film-forming SiC whiskers in an organic dispersion medium such as ethanol, and over-drying to remove the organic dispersion medium. The mixing ratio of polyimide resin and SiC whiskers is V when used as a composite material.
Set by considering the f value. The amount of the organic dispersion medium is determined in consideration of the viscosity of the dispersion liquid in order to achieve homogeneous dispersion, but it is preferably set to 5 times the volume or more of the total amount of the polyimide resin and SiC whiskers.
このようにして得られる混合粉末は、モールド成形、射
出成形、押出成形などの手段により所定形状に熱圧成形
してSiCウィスカー強化ポリイミド樹脂を製造するこ
とができる。The mixed powder thus obtained can be hot-pressed into a predetermined shape by means such as molding, injection molding, extrusion molding, etc. to produce a SiC whisker-reinforced polyimide resin.
本発明は、予めポリイミド樹脂の被膜を形成させたSi
Cウィスカーを用いてポリイミド樹脂と混合し、この混
合粉末を熱圧成形するものであるから、SiCウィスカ
ー表面のポリイミド樹脂被膜を介してマトリックスとな
るポリイミド樹脂と速やかに、強固な接着構造が形成さ
れる。更にマトリックスのポリイミド樹脂とSiCウィ
スカー表面のポリイミド樹脂被膜は、均等に硬化反応が
進行するので優れた強度特性を有するポリイミド樹脂複
合材を製造することができる。The present invention is made of Si on which a polyimide resin coating has been formed in advance.
Since C whiskers are mixed with polyimide resin and the mixed powder is hot-press molded, a strong adhesive structure is quickly formed with the polyimide resin matrix through the polyimide resin coating on the surface of the SiC whiskers. Ru. Further, since the curing reaction proceeds evenly between the polyimide resin of the matrix and the polyimide resin coating on the surface of the SiC whisker, a polyimide resin composite material having excellent strength properties can be manufactured.
ポリイミド樹脂としてポリアミノビスマレイミド〔日本
ポリイミド(株)製ケルイミドl050、以下“PAB
I”と略記。〕を用い、有機溶媒としてはアセトンを
使用して濃度19/l、5g/lの溶液を調製した。こ
の溶液Ie中に直径01〜1μm、長さ30〜100μ
mのSiCウィスカー100gを入れて充分に撹拌混合
した。次いで吸引が過し、20時間風乾して溶媒アセト
ンを完全に除去した。このようにしてPABIの被膜を
形成したSiCウィスカーを得た。As a polyimide resin, polyamino bismaleimide (Kelimide 1050 manufactured by Nippon Polyimide Co., Ltd., hereinafter referred to as "PAB") is used as a polyimide resin.
A solution with a concentration of 19/l and 5 g/l was prepared using acetone as an organic solvent.
100 g of SiC whiskers were added thereto and thoroughly stirred and mixed. It was then vacuumed and air dried for 20 hours to completely remove the solvent acetone. In this way, SiC whiskers with a PABI film formed thereon were obtained.
このSiCウィスカー531?とPAB I 97gを
、有機分散媒としてエタノール4.5a中に入れ撹拌混
合して均質に分散させた後吸引′U5過し、15時間風
乾してエタノールを除去した。このようにして得られた
SiCウィスカーとPABIの均質な混合粉末をモール
ドに装填し、温度110℃、圧力200kg/am’で
3分間予備成形した後、温度260℃、圧力400 k
g/aR2で5分間モールド成形して、150X150
X3iuの成形体を製造した。This SiC whisker 531? and PABI (97 g) were placed in ethanol 4.5a as an organic dispersion medium, stirred and mixed to homogeneously disperse, filtered with suction 'U5, and air-dried for 15 hours to remove ethanol. The thus obtained homogeneous mixed powder of SiC whiskers and PABI was loaded into a mold and preformed at a temperature of 110°C and a pressure of 200 kg/am' for 3 minutes, followed by a temperature of 260°C and a pressure of 400 k.
Mold for 5 minutes at g/aR2, 150X150
A molded body of X3iu was manufactured.
この成形体の強度特性を測定して表−1に示した。The strength characteristics of this molded body were measured and shown in Table 1.
また比較のためにポリイミド樹脂の被膜形成処理をしな
いSiCウィスカーを使用した以外は実施例と同じ方法
で成形体を製造して、その強度特性を同表中に併記した
。For comparison, a molded body was manufactured in the same manner as in the example except that SiC whiskers without polyimide resin film formation treatment were used, and the strength characteristics of the molded body are also listed in the same table.
表−1
(注) *l JIS 6911−1979*
2 ASTM DI044−1978C9−171
000サイクル、荷重+0009*3 ASTM D
256−1984表−Iの結果から、本発明方法により
機械的強度や耐摩耗性の極めて優れたポリイミド樹脂複
合材が得られることが判明する。Table-1 (Note) *l JIS 6911-1979*
2 ASTM DI044-1978C9-171
000 cycles, load +0009*3 ASTM D
From the results shown in Table I of 256-1984, it is clear that a polyimide resin composite material having extremely excellent mechanical strength and abrasion resistance can be obtained by the method of the present invention.
上記説明で明らかなように本発明によれば、ポリイミド
樹脂とSiCウィスカーを強固に接着複合化することが
可能となるので、機械的強度や耐摩耗性の著しい向上を
はかることができる。したがって、このポリイミド樹脂
複合材は、高温下で使用される高強度構造部材として広
い用途分野において極めて有用性が高い。As is clear from the above description, according to the present invention, it is possible to firmly bond and composite polyimide resin and SiC whiskers, so that mechanical strength and abrasion resistance can be significantly improved. Therefore, this polyimide resin composite material is extremely useful in a wide range of application fields as a high-strength structural member used at high temperatures.
Claims (1)
で溶解し、この溶液中にSiCウィスカーを混合分散し
た後ろ過乾燥してSiCウィスカーを表面にポリイミド
樹脂の被膜を形成し、このようにして予めポリイミド樹
脂の被膜を形成したSiCウィスカーとマトリックスと
なるポリイミド樹脂を有機分散媒に分散、ろ過乾燥して
有機分散媒を除去し、得られる混合粉末を熱圧成形する
ことを特徴とする SiCウィスカー強化ポリイミド樹脂の製造方法。[Claims] 1. Polyimide resin is dissolved in an organic solvent at a ratio of 30 g/l or less, SiC whiskers are mixed and dispersed in this solution, and then overdried to form a polyimide resin coating on the SiC whisker surface. Then, the SiC whiskers on which a polyimide resin film has been formed in advance and the polyimide resin serving as a matrix are dispersed in an organic dispersion medium, filtered and dried to remove the organic dispersion medium, and the resulting mixed powder is hot-press molded. A method for producing a SiC whisker-reinforced polyimide resin, characterized by:
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP14711987A JPS63312328A (en) | 1987-06-15 | 1987-06-15 | Production of polyimide polymer reinforced with sic whisker |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP14711987A JPS63312328A (en) | 1987-06-15 | 1987-06-15 | Production of polyimide polymer reinforced with sic whisker |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS63312328A true JPS63312328A (en) | 1988-12-20 |
JPH042606B2 JPH042606B2 (en) | 1992-01-20 |
Family
ID=15422961
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP14711987A Granted JPS63312328A (en) | 1987-06-15 | 1987-06-15 | Production of polyimide polymer reinforced with sic whisker |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS63312328A (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8319299B2 (en) | 2009-11-20 | 2012-11-27 | Auman Brian C | Thin film transistor compositions, and methods relating thereto |
US8653512B2 (en) | 2009-11-20 | 2014-02-18 | E. I. Du Pont De Nemours And Company | Thin film transistor compositions, and methods relating thereto |
CN104810347A (en) * | 2015-03-18 | 2015-07-29 | 上海交通大学 | Silicon carbide whisker/polymer composite material patch panel and preparation method thereof |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS53121872A (en) * | 1977-04-01 | 1978-10-24 | Toho Rayon Co Ltd | Polymide resin reinforcing material and its preparation |
-
1987
- 1987-06-15 JP JP14711987A patent/JPS63312328A/en active Granted
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS53121872A (en) * | 1977-04-01 | 1978-10-24 | Toho Rayon Co Ltd | Polymide resin reinforcing material and its preparation |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8319299B2 (en) | 2009-11-20 | 2012-11-27 | Auman Brian C | Thin film transistor compositions, and methods relating thereto |
US8653512B2 (en) | 2009-11-20 | 2014-02-18 | E. I. Du Pont De Nemours And Company | Thin film transistor compositions, and methods relating thereto |
CN104810347A (en) * | 2015-03-18 | 2015-07-29 | 上海交通大学 | Silicon carbide whisker/polymer composite material patch panel and preparation method thereof |
Also Published As
Publication number | Publication date |
---|---|
JPH042606B2 (en) | 1992-01-20 |
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