JP2008119974A - Polyimide composite material sandwich panel and manufacturing method therefor - Google Patents
Polyimide composite material sandwich panel and manufacturing method therefor Download PDFInfo
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Abstract
Description
本発明は、長繊維強化付加型ポリイミドシート（硬化体）の間にコア材の発泡ポリイミドが挟まれて一体形成されたポリイミド複合材料からなるサンドイッチパネルに関する。 The present invention relates to a sandwich panel made of a polyimide composite material in which a foamed polyimide core material is sandwiched between long fiber reinforced addition type polyimide sheets (cured bodies).
軽量高剛性の構造材、断熱材、防振材、吸音材などが航空機や人工衛星などの航空・宇宙分野で嘱望されている。
しかしながら、３００℃以下で成型できる長繊維強化樹脂と３００℃以下の耐熱性を有する発泡体によるサンドイッチパネルは提案されているが、３００℃以上の耐熱性を有するサンドイッチパネルは従来の材料では実現できていない。
Lightweight and highly rigid structural materials, heat insulating materials, vibration-proofing materials, and sound-absorbing materials are desired in the aerospace field such as aircraft and artificial satellites.
However, sandwich panels made of long fiber reinforced resin that can be molded at 300 ° C. or lower and foams having heat resistance of 300 ° C. or lower have been proposed, but sandwich panels having heat resistance of 300 ° C. or higher cannot be realized with conventional materials. Not.
本発明の目的は、３００℃以上の耐熱性を有し軽量高剛性の構造材、断熱材、防振材或いは吸音材として利用可能なポリイミド複合材料からなるサンドイッチパネル、及びその製造方法を提供することである。 An object of the present invention is to provide a sandwich panel made of a polyimide composite material having a heat resistance of 300 ° C. or more and having a light weight and high rigidity, a heat insulating material, a vibration isolating material, or a sound absorbing material, and a method for manufacturing the same. That is.
即ち、本発明は、長繊維強化付加型ポリイミドシート（硬化体）の間にコア材の発泡ポリイミドが挟まれて一体形成されたポリイミド複合材料からなり耐熱性が３００℃以上の耐熱性を有するサンドイッチパネルに関する。 That is, the present invention is a sandwich having a heat resistance of 300 ° C. or more, comprising a polyimide composite material integrally formed by sandwiching a foamed polyimide of a core material between long fiber reinforced addition type polyimide sheets (cured bodies). Regarding panels.
また、本発明は、発泡ポリイミドの両側に長繊維に付加型ポリイミド前駆体を含浸したプリプレグを配置し、圧縮プレス機で加圧しながら３００℃以上の温度で加熱して長繊維強化付加型ポリイミドシート（硬化体）の間にコア材の発泡ポリイミドが挟まれて一体形成されたポリイミド複合材料からなるサンドイッチパネルを製造する製造方法に関する。 Moreover, this invention arrange | positions the prepreg which impregnated the addition type polyimide precursor to the long fiber on both sides of the foaming polyimide, and heats it at the temperature of 300 degreeC or more, pressing with a compression press machine, and a long fiber reinforcement addition type polyimide sheet The present invention relates to a manufacturing method for manufacturing a sandwich panel made of a polyimide composite material in which a foamed polyimide of a core material is sandwiched between (cured bodies).
本発明によって、３００℃以上の耐熱性を有し軽量高剛性の構造材、断熱材、防振材或いは吸音材として利用可能なポリイミド複合材料からなるサンドイッチパネル、及びその製造方法を得ることができる。このサンドイッチパネルは、特に航空・宇宙分野で好適に利用することができる。 According to the present invention, it is possible to obtain a sandwich panel made of a polyimide composite material having a heat resistance of 300 ° C. or more and having a light weight and high rigidity, a heat insulating material, a vibration isolating material, or a sound absorbing material, and a manufacturing method thereof. . This sandwich panel can be suitably used particularly in the aerospace field.
本発明のサンドイッチパネルは密度が０．３〜１ｇ／ｃｍ３が好ましい。また、コア材の発泡ポリイミド層の発泡倍率は２〜５０倍特に２〜２０倍が好ましい。
コア材の発泡ポリイミドは、Ｔｇが３００℃以上のポリイミドからなる発泡ポリイミドが好適であり、更に発泡ポリイミドのチップを再結着した再結着発泡ポリイミドを用いても構わない。
使用するプリプレグは長繊維クロスに付加型ポリイミド前駆体特にＰＥＰＡを用いた付加型ポリイミド前駆体を含浸したものが好適である。
長繊維としては、ガラス繊維、炭素繊維、無機繊維、アラミド繊維などの耐熱性繊維を用いることが好適である。
以下実施例によって本発明を説明する。なお、本発明は以下の実施例に限定されるものではない。
The sandwich panel of the present invention preferably has a density of 0.3 to 1 g / cm 3 . The expansion ratio of the foamed polyimide layer of the core material is preferably 2 to 50 times, particularly 2 to 20 times.
The foamed polyimide of the core material is preferably a foamed polyimide made of polyimide having a Tg of 300 ° C. or higher, and a rebound foamed polyimide obtained by rebinding a foamed polyimide chip may be used.
The prepreg used is preferably a long fiber cloth impregnated with an addition type polyimide precursor, particularly an addition type polyimide precursor using PEPA.
As long fibers, it is preferable to use heat-resistant fibers such as glass fibers, carbon fibers, inorganic fibers, and aramid fibers.
The following examples illustrate the invention. In addition, this invention is not limited to a following example.
以下の記載において、各略号は次の化合物を意味する。
ａ−ＢＰＤＡ：２，３，３’，４’−ビフェニルテトラカルボン酸二無水物
ＰＥＰＡ：４−（フェニルエチニル）無水フタル酸
ＴＰＥ−Ｒ：１，３−ビス（４−アミノフェノキシ）ベンゼン
ＰＰＤ：パラフェニレンジアミン
In the following description, each abbreviation means the following compound.
a-BPDA: 2,3,3 ′, 4′-biphenyltetracarboxylic dianhydride PEPA: 4- (phenylethynyl) phthalic anhydride TPE-R: 1,3-bis (4-aminophenoxy) benzene PPD: Paraphenylenediamine
ピリプレグの揮発分率（Ｖｃ）、樹脂含有率（Ｒｃ）の測定は、プリプレグの重量とそれを３７０℃で１時間加熱後の重量を測定して下式から求めた。
Ｖｃ（％）＝１００×［プリプレグの重量（ｇ）−３７０℃で１時間加熱後の重量（ｇ）］／［プリプレグの重量（ｇ）］
Ｒｃ（％）＝１００×［３７０℃で１時間加熱後の重量（ｇ）−繊維クロスの重量（ｇ）］／［３７０℃で１時間加熱後の重量（ｇ）］
なお、繊維クロスの重量はプリプレグの面積とＦＡＷの積として求めた。また、ＦＡＷは単位面積当りの繊維重量である。
The measurement of the volatile content (Vc) and resin content (Rc) of pyripreg was obtained from the following formula by measuring the weight of the prepreg and the weight after heating it at 370 ° C. for 1 hour.
Vc (%) = 100 × [weight of prepreg (g) -weight after heating at 370 ° C. for 1 hour (g)] / [weight of prepreg (g)]
Rc (%) = 100 × [weight after heating at 370 ° C. for 1 hour (g) −weight of fiber cloth (g)] / [weight after heating at 370 ° C. for 1 hour (g)]
The weight of the fiber cloth was determined as the product of the prepreg area and the FAW. FAW is the fiber weight per unit area.
コア材の密度、及びサンドイッチパネルの密度は、材料の寸法と重量より求めた。 The density of the core material and the density of the sandwich panel were determined from the size and weight of the material.
以下の例で用いた発泡ポリイミドとしては、
（１）宇部興産株式会社製発泡ポリイミド「ユーピレックスフォームＢＦ３０１」（密度：０．００６ｇ／ｃｍ３）
（２）再結着発泡ポリイミド（ボーデン社製チップ状ポリイミドフォーム「ポリイミドスポンジＵＦＣ」を３２０ｍｍ角の金型内に所定量入れ、室温下０．５ｔの荷重を掛けて一軸圧縮成型したもの）
を用いた。
As the foamed polyimide used in the following examples,
(1) Foamed polyimide “Upilex Foam BF301” manufactured by Ube Industries, Ltd. (density: 0.006 g / cm 3 )
(2) Rebound foamed polyimide (Boden chip polyimide foam "Polyimide sponge UFC" is placed in a 320mm square mold and uniaxially compression-molded under a load of 0.5t at room temperature)
Was used.
〔参考例１〕
攪拌機と還流管および窒素導入管を装着した１０００ｍｌの４つ口セパラブルフラスコに窒素気流下、酸成分としてａ−ＢＰＤＡ１１７．７ｇ（０.４００モル）、ＰＥＰＡ４９．７ｇ（０.２００モル）およびメタノール１３５．４ｇを投入し還流下５時間攪拌し均一液を得た。その後、室温まで冷却し攪拌しながらジアミン成分としてＴＰＥ−Ｒ４３．９ｇ（０.１５０モル）およびＰＰＤ３７．８ｇ（０.３５０モル）を投入し６０℃、６０分で均一に溶解して付加型ポリイミド前駆体溶液を得た。
[Reference Example 1]
In a 1000 ml four-necked separable flask equipped with a stirrer, a reflux tube and a nitrogen introduction tube, 117.7 g (0.400 mol) of a-BPDA, 49.7 g (0.200 mol) of PEPA and methanol as an acid component under a nitrogen stream 135.4 g was added and stirred for 5 hours under reflux to obtain a uniform solution. Thereafter, while cooling to room temperature and stirring, 43.9 g (0.150 mol) of TPE-R and 37.8 g (0.350 mol) of PPD were added as diamine components and dissolved uniformly at 60 ° C. for 60 minutes to add type polyimide. A precursor solution was obtained.
〔参考例２〕
参考例１の付加型ポリイミド前駆体溶液をＰＥＴフィルムに流延し、そこに３００ｍｍ×３００ｍｍの炭素繊維クロス（東レ社製Ｔ８００−１２Ｋ平織、ＦＡＷ３２０ｇ／ｍ２）を重ね、それを４０℃に加熱したホットプレートにＰＥＴフィルムの未流延側がホットプレート面側になるように置き炭素繊維クロス面から軽く押しながら溶液を含浸させた。そして、ＰＥＴフィルムより付加型ポリイミド前駆体溶液を含浸させた炭素繊維クロスを剥がし１００℃の熱風乾燥機内に吊るし３分間乾燥した。その後、乾燥機から取り出し２５μｍのＰＥＴフィルムにはさみ８０℃のプレスを用いて０．１ＭＰａで１分間加圧し炭素繊維に付加型ポリイミド前駆体を含浸したプリプレグを得た。得られたプリプレグは、タック性およびドレープ性を有していた。さらに、得られたプリプレグを１３５℃で３０分、１８０℃で３０分、２５０℃で３０分、３００℃で３０分、３７０℃で６０分熱処理し揮発分率（Ｖｃ）、樹脂含有率（Ｒｃ）を求めた。Ｖｃは１４％、Ｒｃは４０％であつた。
[Reference Example 2]
The addition type polyimide precursor solution of Reference Example 1 is cast on a PET film, and a 300 mm × 300 mm carbon fiber cloth (T800-12K plain weave, FAW 320 g / m 2 ) manufactured by Toray Industries, Inc. is stacked thereon and heated to 40 ° C. The hot plate was placed so that the non-cast side of the PET film became the hot plate surface side, and the solution was impregnated while gently pressing from the carbon fiber cloth surface. Then, the carbon fiber cloth impregnated with the addition-type polyimide precursor solution was peeled off from the PET film, suspended in a hot air dryer at 100 ° C., and dried for 3 minutes. Thereafter, the prepreg was taken out from the drier and was pressed at 0.1 MPa for 1 minute using an 80 ° C. press sandwiched between 25 μm PET films and carbon fibers were impregnated with an addition-type polyimide precursor. The obtained prepreg had tackiness and draping properties. Furthermore, the obtained prepreg was heat-treated at 135 ° C. for 30 minutes, 180 ° C. for 30 minutes, 250 ° C. for 30 minutes, 300 ° C. for 30 minutes, 370 ° C. for 60 minutes and volatile fraction (Vc), resin content (Rc ) Vc was 14% and Rc was 40%.
〔参考例３〕
参考例２の炭素繊維クロスをチラノ繊維クロス（宇部興産社製ＰＭ−Ｇ１５Ｈ１６ＥＬ、ＦＡＷ２７０ｇ／ｍ２）に変更した以外は同様操作を行い、チラノ繊維に付加型ポリイミド前駆体を含浸したプリプレグを得た。このプリプレグはタック性およびドレープ性を有していた。さらに、得られたプリプレグを１３５℃で３０分、１８０℃で３０分、２５０℃で３０分、３００℃で３０分、３７０℃で６０分熱処理し揮発分率（Ｖｃ）、樹脂含有率（Ｒｃ）を求めた。Ｖｃ：１６％，Ｒｃ：３９％であつた。
[Reference Example 3]
The same operation was performed except that the carbon fiber cloth of Reference Example 2 was changed to Tyranno fiber cloth (PM-G15H16EL manufactured by Ube Industries, FAW 270 g / m 2 ) to obtain a prepreg in which Tyranno fiber was impregnated with an addition type polyimide precursor. . This prepreg had tackiness and draping properties. Furthermore, the obtained prepreg was heat-treated at 135 ° C. for 30 minutes, 180 ° C. for 30 minutes, 250 ° C. for 30 minutes, 300 ° C. for 30 minutes, 370 ° C. for 60 minutes and volatile fraction (Vc), resin content (Rc ) Vc: 16%, Rc: 39%.
〔実施例１〕
サイズが３００×３００ｍｍで厚さが１７８ｍｍの発泡ポリイミド（ＢＦ３０１、密度：０．００６ｇ／ｃｍ３）の両側に、参考例２で得た炭素繊維に付加型ポリイミド前駆体を含浸したプリプレグを、さらにその両側に離型フィルム及び保護フィルムを配置し、それらを５ｍｍのスペーサーと共に、室温の一軸圧縮プレス機（ＮＦ−５０：神藤金属工業社製）にセットし、加圧なしでプレス機温度を２５０℃まで昇温させて１時間保持した。
一軸圧縮プレス機にセットしたときの、発泡ポリイミド、プリプレグ、離型フィルム及び保護フィルムの構成（積層順）は以下のとおりであり、図１に示したとおりである。
ＳＵＳ板
保護フィルム（ユーピレックス７５Ｓ：宇部興産社製）
離型フィルム（Ｒｅｌｅａｓｅ Ｅａｓｅ２３４ＴＦＰ−１：ＡｉｒＴｅｃｈ社製）
炭素繊維のプリプレグ
発泡ポリイミド
炭素繊維のプリプレグ
離型フィルム（Ｒｅｌｅａｓｅ Ｅａｓｅ２３４ＴＦＰ−１：ＡｉｒＴｅｃｈ社製）
保護フィルム（ユーピレックス７５Ｓ：宇部興産社製）
ＳＵＳ板
次いで、プレス圧力を７．５ＭＰａ（ゲージ圧）とし、プレス機温度を３７０℃まで昇温させ、３７０℃到達後、１時間保持してプリプレグを硬化させた。
成型後、加圧状態のまま、プレス機温度を１００℃まで冷却し、２枚の炭素繊維強化付加型ポリイミドシート（硬化体）の間にコア材の発泡ポリイミドが挟まれて一体形成されたポリイミド複合材料からなるサンドイッチパネルを取り出した。
このサンドイッチパネルは、厚さが５ｍｍ、密度が０．４９ｇ／ｃｍ３であり、コア材の発泡ポリイミドとその両側の繊維で強化されたポリイミド複合材料とが強固に接着して一体化されており、ボイドやしわなどがなくて良好な表面状態であった。
[Example 1]
A prepreg obtained by impregnating the carbon fiber obtained in Reference Example 2 with an addition-type polyimide precursor on both sides of a foamed polyimide (BF301, density: 0.006 g / cm 3 ) having a size of 300 × 300 mm and a thickness of 178 mm, A release film and a protective film are arranged on both sides, and they are set together with a 5 mm spacer in a uniaxial compression press machine (NF-50: manufactured by Kondo Metal Industry Co., Ltd.) at a room temperature. The temperature was raised to 0 ° C. and held for 1 hour.
The configuration (lamination order) of the foamed polyimide, prepreg, release film, and protective film when set in a uniaxial compression press is as follows, as shown in FIG.
SUS board protective film (Upilex 75S: manufactured by Ube Industries)
Release film (Release Ease 234TFP-1: manufactured by AirTech)
Carbon fiber prepreg Foamed polyimide Carbon fiber prepreg Release film (Release Ease 234TFP-1: AirTech)
Protective film (Upilex 75S: manufactured by Ube Industries)
SUS plate Subsequently, the press pressure was set to 7.5 MPa (gauge pressure), the press machine temperature was raised to 370 ° C., and after reaching 370 ° C., the prepreg was cured by holding for 1 hour.
After molding, the press machine temperature is cooled to 100 ° C. with the pressure applied, and the core foamed polyimide is sandwiched between two carbon fiber reinforced addition type polyimide sheets (cured bodies), and the polyimide is integrally formed. The sandwich panel made of the composite material was taken out.
This sandwich panel has a thickness of 5 mm and a density of 0.49 g / cm 3. The core foamed polyimide and the polyimide composite material reinforced with fibers on both sides are firmly bonded and integrated. There was no void or wrinkle, and the surface condition was good.
〔実施例２〕
用いた発泡ポリイミドの厚みを９０ｍｍとした以外は実施例１と同様に行って、２枚の炭素繊維強化付加型ポリイミドシート（硬化体）の間にコア材の発泡ポリイミドが挟まれて一体形成されたポリイミド複合材料からなるサンドイッチパネルを得た。
このサンドイッチパネルは、厚さが５ｍｍ、密度が０．３５／ｃｍ３であり、コア材の発泡ポリイミドとその両側の繊維で強化されたポリイミド複合材料とが強固に接着して一体化されており、ボイドやしわなどがなくて良好な表面状態であった。
[Example 2]
Except that the thickness of the foamed polyimide used was 90 mm, the same procedure as in Example 1 was carried out, and the core material foamed polyimide was sandwiched between two carbon fiber reinforced addition type polyimide sheets (cured bodies) to be integrally formed. A sandwich panel made of polyimide composite was obtained.
This sandwich panel has a thickness of 5 mm and a density of 0.35 / cm 3. The core foamed polyimide and the polyimide composite material reinforced with fibers on both sides are firmly bonded and integrated. There was no void or wrinkle, and the surface condition was good.
〔実施例３〕
発泡ポリイミドとしてサイズが３２０×３２０ｍｍで厚さが６．３ｍｍの再結着した発泡ポリイミド（密度０．２７ｇ／ｃｍ３）を用いた以外は、実施例１と同様に行って、２枚の炭素繊維強化付加型ポリイミドシート（硬化体）の間にコア材の発泡ポリイミドが挟まれて一体形成されたポリイミド複合材料からなるサンドイッチパネルを得た。
このサンドイッチパネルは、厚さが５ｍｍ、密度が０．４９／ｃｍ３であり、コア材の発泡ポリイミドとその両側の繊維で強化されたポリイミド複合材料とが強固に接着して一体化されており、ボイドやしわなどがなくて良好な表面状態であった。
Example 3
Two carbon sheets were obtained in the same manner as in Example 1 except that a re-bonded expanded polyimide (density 0.27 g / cm 3 ) having a size of 320 × 320 mm and a thickness of 6.3 mm was used as the expanded polyimide. A sandwich panel made of a polyimide composite material in which a foamed polyimide core material was sandwiched between fiber-reinforced additive-type polyimide sheets (cured bodies) was obtained.
This sandwich panel has a thickness of 5 mm and a density of 0.49 / cm 3. The core foamed polyimide and the polyimide composite material reinforced with fibers on both sides are firmly bonded and integrated. There was no void or wrinkle, and the surface condition was good.
〔実施例４〕
発泡ポリイミドとしてサイズが３２０×３２０ｍｍで厚さが１１．６ｍｍの再結着した発泡ポリイミド（密度０．３０ｇ／ｃｍ３）を用いた以外は、実施例１と同様に行って、２枚の炭素繊維強化付加型ポリイミドシート（硬化体）の間にコア材の発泡ポリイミドが挟まれて一体形成されたポリイミド複合材料からなるサンドイッチパネルを得た。
このサンドイッチパネルは、厚さが５ｍｍ、密度が０．９６／ｃｍ３であり、コア材の発泡ポリイミドとその両側の繊維で強化されたポリイミド複合材料とが強固に接着して一体化されており、ボイドやしわなどがなくて良好な表面状態であった。
Example 4
Two carbon sheets were produced in the same manner as in Example 1 except that re-bonded expanded polyimide (density 0.30 g / cm 3 ) having a size of 320 × 320 mm and a thickness of 11.6 mm was used as the expanded polyimide. A sandwich panel made of a polyimide composite material in which a foamed polyimide core material was sandwiched between fiber-reinforced additive-type polyimide sheets (cured bodies) was obtained.
This sandwich panel has a thickness of 5 mm and a density of 0.96 / cm 3. The core foamed polyimide and the polyimide composite material reinforced with fibers on both sides are firmly bonded and integrated. There was no void or wrinkle, and the surface condition was good.
〔実施例５〕
発泡ポリイミドとしてサイズが３２０×３２０ｍｍで厚さが６．０ｍｍの再結着した発泡ポリイミド（密度０．３２ｇ／ｃｍ３）の両側に、参考例３で得たチラノ繊維に付加型ポリイミド前駆体を含浸したプリプレグを使用した以外は、実施例１と同様に行って、２枚のチラノ繊維強化付加型ポリイミドシート（硬化体）の間にコア材の発泡ポリイミドが挟まれて一体形成されたポリイミド複合材料からなるサンドイッチパネルを得た。
このサンドイッチパネルは、厚さが５ｍｍ、密度が０．６３／ｃｍ３であり、コア材の発泡ポリイミドとその両側の繊維で強化されたポリイミド複合材料とが強固に接着して一体化されており、ボイドやしわなどがなくて良好な表面状態であった。
Example 5
Addition-type polyimide precursor to the Tyranno fiber obtained in Reference Example 3 on both sides of re-bonded foamed polyimide (density 0.32 g / cm 3 ) having a size of 320 × 320 mm and a thickness of 6.0 mm. Except for using the impregnated prepreg, the same procedure as in Example 1 was performed, and the polyimide composite in which the core foamed polyimide was sandwiched between two Tyranno fiber reinforced addition type polyimide sheets (cured bodies) was integrally formed A sandwich panel of materials was obtained.
This sandwich panel has a thickness of 5 mm and a density of 0.63 / cm 3. The core foamed polyimide and the polyimide composite material reinforced with fibers on both sides are firmly bonded and integrated. There was no void or wrinkle, and the surface condition was good.
〔実施例６〕
発泡ポリイミドとしてサイズが３２０×３２０ｍｍで厚さが１１．５ｍｍの再結着した発泡ポリイミド（密度０．３０ｇ／ｃｍ３）を用いた以外は、実施例５と同様に行って、２枚のチラノ繊維強化付加型ポリイミドシート（硬化体）の間にコア材の発泡ポリイミドが挟まれて一体形成されたポリイミド複合材料からなるサンドイッチパネルを得た。
このサンドイッチパネルは、厚さが５ｍｍ、密度が０．９８／ｃｍ３であり、コア材の発泡ポリイミドとその両側の繊維で強化されたポリイミド複合材料とが強固に接着して一体化されており、ボイドやしわなどがなくて良好な表面状態であった。
Example 6
Two Tyrannos were carried out in the same manner as in Example 5 except that a re-bonded foamed polyimide (density 0.30 g / cm 3 ) having a size of 320 × 320 mm and a thickness of 11.5 mm was used as the foamed polyimide. A sandwich panel made of a polyimide composite material in which a foamed polyimide core material was sandwiched between fiber-reinforced additive-type polyimide sheets (cured bodies) was obtained.
This sandwich panel has a thickness of 5 mm and a density of 0.98 / cm 3. The core foamed polyimide and the polyimide composite material reinforced with fibers on both sides are firmly bonded and integrated. There was no void or wrinkle, and the surface condition was good.
〔実施例７〕
発泡ポリイミドとしてサイズが３２０×３２０ｍｍで厚さが１１．０ｍｍの再結着した発泡ポリイミド（密度０．３３ｇ／ｃｍ３）を用い、１０ｍｍのスペーサーと共に、室温のプレス機にセットした以外は、実施例１と同様に行って、２枚の炭素繊維強化付加型ポリイミドシート（硬化体）の間にコア材の発泡ポリイミドが挟まれて一体形成されたポリイミド複合材料からなるサンドイッチパネルを得た。
このサンドイッチパネルは、厚さが１０ｍｍ、密度が０．４８／ｃｍ３であり、コア材の発泡ポリイミドとその両側の繊維で強化されたポリイミド複合材料とが強固に接着して一体化されており、ボイドやしわなどがなくて良好な表面状態であった。
Example 7
Except that the foamed polyimide used was a reattached foamed polyimide (density 0.33 g / cm 3 ) with a size of 320 × 320 mm and a thickness of 11.0 mm, and was set in a room temperature press with a 10 mm spacer. In the same manner as in Example 1, a sandwich panel made of a polyimide composite material in which a foamed polyimide core material was sandwiched between two carbon fiber reinforced addition type polyimide sheets (cured bodies) was obtained.
This sandwich panel has a thickness of 10 mm and a density of 0.48 / cm 3. The core foamed polyimide and the polyimide composite material reinforced with fibers on both sides are firmly bonded and integrated. There was no void or wrinkle, and the surface condition was good.
〔実施例８〕
サイズが３２０×３２０ｍｍで厚さが１３．０ｍｍの再結着した発泡ポリイミド（密度０．３３ｇ／ｃｍ３）２枚の両側及び間に、参考例２で得た炭素繊維に付加型ポリイミド前駆体を含浸したプリプレグを配置し、さらにその両側に離型フィルム及び保護フィルムを配置し、それらを１０ｍｍのスペーサーと共に、室温のプレス機にセットし、加圧なしでプレス機温度を２５０℃まで昇温させて１時間保持した。
プレス機にセットしたときの、発泡ポリイミド、プリプレグ、離型フィルム及び保護フィルムの構成（積層順）は以下のとおりとした。
ＳＵＳ板
保護フィルム（ユーピレックス７５Ｓ：宇部興産社製）
離型フィルム（Ｒｅｌｅａｓｅ Ｅａｓｅ２３４ＴＦＰ−１：ＡｉｒＴｅｃｈ社製）
炭素繊維のプリプレグ
発泡ポリイミド
炭素繊維のプリプレグ
発泡ポリイミド
炭素繊維のプリプレグ
離型フィルム（Ｒｅｌｅａｓｅ Ｅａｓｅ２３４ＴＦＰ−１：ＡｉｒＴｅｃｈ社製）
保護フィルム（ユーピレックス７５Ｓ：宇部興産社製）
ＳＵＳ板
次いで、実施例１と同様に成型を行い、コア材の発泡ポリイミドの間及び両側に３枚の炭素繊維強化付加型ポリイミドシート（硬化体）が一体成形させた複合材料からなるサンドイッチパネルを取り出した。
このサンドイッチパネルは、厚さが１０ｍｍ、密度が０．９０／ｃｍ３であり、コア材の発泡ポリイミドとその両側及び間の繊維で強化されたポリイミド複合材料とが強固に接着して一体化されており、ボイドやしわなどがなくて良好な表面状態であった。
Example 8
Addition-type polyimide precursor to the carbon fiber obtained in Reference Example 2 on both sides and between two sheets of re-bonded foamed polyimide (density 0.33 g / cm 3 ) having a size of 320 × 320 mm and a thickness of 13.0 mm A prepreg impregnated with selenium and a release film and protective film on both sides of the prepreg are set in a room temperature press with a 10 mm spacer, and the temperature of the press is increased to 250 ° C. without pressure. Held for 1 hour.
The configuration (lamination order) of the foamed polyimide, prepreg, release film, and protective film when set in a press was as follows.
SUS board protective film (Upilex 75S: manufactured by Ube Industries)
Release film (Release Ease 234TFP-1: manufactured by AirTech)
Carbon fiber prepreg Foamed polyimide Carbon fiber prepreg Foamed polyimide Carbon fiber prepreg Release film (Release Ease 234TFP-1: AirTech)
Protective film (Upilex 75S: manufactured by Ube Industries)
Next, a sandwich panel made of a composite material in which three carbon fiber reinforced addition type polyimide sheets (cured bodies) are integrally formed between the foamed polyimide of the core material and on both sides is molded in the same manner as in Example 1. I took it out.
This sandwich panel has a thickness of 10 mm and a density of 0.90 / cm 3 , and the foamed polyimide of the core material and the polyimide composite material reinforced with fibers on both sides and between them are firmly bonded and integrated. There was no void or wrinkle and the surface condition was good.
〔比較例１〕
用いた発泡ポリイミドの厚みを１６ｍｍとした以外は実施例１と同様に行って、２枚の炭素繊維強化付加型ポリイミドシート（硬化体）の間にコア材の発泡ポリイミドが挟まれて一体形成されたポリイミド複合材料からなるサンドイッチパネルを得た。
このサンドイッチパネルは、厚さが５ｍｍ、密度が０．２６／ｃｍ３であり、コア材の発泡ポリイミドとその両側の繊維で強化されたポリイミド複合材料とが強固に接着して一体化されていたが、ボイドが多く発生し、表面状態が悪かった。
[Comparative Example 1]
Except that the thickness of the foamed polyimide used was 16 mm, the same procedure as in Example 1 was carried out, and the core material foamed polyimide was sandwiched between the two carbon fiber reinforced addition type polyimide sheets (cured bodies) to be integrally formed. A sandwich panel made of polyimide composite was obtained.
The sandwich panel had a thickness of 5 mm and a density of 0.26 / cm 3 , and the core foamed polyimide and the polyimide composite material reinforced with the fibers on both sides were firmly bonded and integrated. However, many voids were generated and the surface condition was poor.
本発明によって、３００℃以上の耐熱性を有し軽量高剛性の構造材、断熱材、防振材或いは吸音材として利用可能なポリイミド複合材料からなるサンドイッチパネル、及びその製造方法を得ることができる。 According to the present invention, it is possible to obtain a sandwich panel made of a polyimide composite material having a heat resistance of 300 ° C. or more and having a light weight and high rigidity, a heat insulating material, a vibration isolating material, or a sound absorbing material, and a manufacturing method thereof. .
１：ＳＵＳ板
２：保護フィルム
３：離型フィルム
４：長繊維に付加型ポリイミド前駆体を含浸したプリプレグ
５：発泡ポリイミド
６：スペーサー
１０：繊維強化付加型ポリイミドシート（硬化体）
１１：発泡ポリイミド
1: SUS plate 2: protective film 3: release film 4: prepreg in which an addition type polyimide precursor is impregnated into a long fiber 5: foamed polyimide 6: spacer 10: fiber reinforced addition type polyimide sheet (cured body)
11: Foamed polyimide
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| JP2009274284A (en) * | 2008-05-13 | 2009-11-26 | Ube Ind Ltd | Heat-resistant sandwich panel comprising polyimide composite material and its method for manufacturing |
| JP2016149756A (en) * | 2015-02-09 | 2016-08-18 | 三菱電機株式会社 | Radome for aviation body and manufacturing method of the same |
| CN106142781A (en) * | 2015-03-30 | 2016-11-23 | 株洲时代新材料科技股份有限公司 | A kind of alternately stratiform complex sound insulation damping sheets |
| CN111590913A (en) * | 2020-04-29 | 2020-08-28 | 哈尔滨工程大学 | Polyimide heat-insulating sound-absorbing foam with high specific strength and processing method thereof |
| CN112060733A (en) * | 2020-08-14 | 2020-12-11 | 贵州航天建设工程有限公司 | Polyimide-phosphogypsum color steel sandwich board and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112060733A (en) * | 2020-08-14 | 2020-12-11 | 贵州航天建设工程有限公司 | Polyimide-phosphogypsum color steel sandwich board and preparation method thereof |
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