JP7269243B2 - 繊維強化樹脂複合体およびその製造方法、ならびに繊維強化樹脂複合体用不織布 - Google Patents
繊維強化樹脂複合体およびその製造方法、ならびに繊維強化樹脂複合体用不織布 Download PDFInfo
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- JP7269243B2 JP7269243B2 JP2020530093A JP2020530093A JP7269243B2 JP 7269243 B2 JP7269243 B2 JP 7269243B2 JP 2020530093 A JP2020530093 A JP 2020530093A JP 2020530093 A JP2020530093 A JP 2020530093A JP 7269243 B2 JP7269243 B2 JP 7269243B2
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Images
Classifications
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- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
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- B29B15/08—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00 of reinforcements or fillers
- B29B15/10—Coating or impregnating independently of the moulding or shaping step
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/003—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts characterised by the matrix material, e.g. material composition or physical properties
- B29C70/0035—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts characterised by the matrix material, e.g. material composition or physical properties comprising two or more matrix materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/02—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising combinations of reinforcements, e.g. non-specified reinforcements, fibrous reinforcing inserts and fillers, e.g. particulate fillers, incorporated in matrix material, forming one or more layers and with or without non-reinforced or non-filled layers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/02—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising combinations of reinforcements, e.g. non-specified reinforcements, fibrous reinforcing inserts and fillers, e.g. particulate fillers, incorporated in matrix material, forming one or more layers and with or without non-reinforced or non-filled layers
- B29C70/021—Combinations of fibrous reinforcement and non-fibrous material
- B29C70/025—Combinations of fibrous reinforcement and non-fibrous material with particular filler
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/06—Fibrous reinforcements only
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- B29C70/16—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of substantial or continuous length
- B29C70/20—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of substantial or continuous length oriented in a single direction, e.g. roofing or other parallel fibres
- B29C70/202—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of substantial or continuous length oriented in a single direction, e.g. roofing or other parallel fibres arranged in parallel planes or structures of fibres crossing at substantial angles, e.g. cross-moulding compound [XMC]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/40—Shaping or impregnating by compression not applied
- B29C70/50—Shaping or impregnating by compression not applied for producing articles of indefinite length, e.g. prepregs, sheet moulding compounds [SMC] or cross moulding compounds [XMC]
- B29C70/504—Shaping or impregnating by compression not applied for producing articles of indefinite length, e.g. prepregs, sheet moulding compounds [SMC] or cross moulding compounds [XMC] using rollers or pressure bands
- B29C70/506—Shaping or impregnating by compression not applied for producing articles of indefinite length, e.g. prepregs, sheet moulding compounds [SMC] or cross moulding compounds [XMC] using rollers or pressure bands and impregnating by melting a solid material, e.g. sheet, powder, fibres
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Description
本発明の強化繊維3については、特に制限されず、例えば、炭素繊維、ガラス繊維、炭化ケイ素繊維、アルミナ繊維、セラミック繊維、玄武岩繊維、各種メタル繊維(例えば、金、銀、銅、鉄、ニッケル、チタン、ステンレス)等の無機繊維や、全芳香族ポリエステル系繊維、ポリフェニレンサルファイド繊維、アラミド繊維、ポリスルフォンアミド繊維、フェノール樹脂繊維、ポリイミド繊維、及びフッ素繊維等の有機繊維を挙げることができる。なお、これらの繊維は、単独で、あるいは2種以上を組み合わせて用いてもよい。
本発明の繊維強化樹脂複合体1を構成する熱可塑性樹脂5は、後述の熱可塑性繊維8(即ち、熱可塑性樹脂からなる繊維)を溶解して得られるものである。この熱可塑性樹脂5の分子量分布は、特に制限されるものではないが、得られる繊維強化樹脂複合体1の成形性、及び力学物性の均一性を達成するとの観点から、重量平均分子量(Mw)と数平均分子量(Mn)との比で表記される分子量分布(Mw/Mn)が、2.3以下であることが好ましい。分子量分布が2.3を超える場合には、熱硬化性樹脂2の硬化工程にて、熱可塑性樹脂5の溶解性に斑が生じ、成形斑が起こることから、得られる繊維強化樹脂複合体1の外観や力学物性にバラツキが生じる場合がある。なお、重量平均分子量(Mw)、数平均分子量(Mn)、分子量分布は、例えば、サイズ排除クロマトグラフィー(SEC)の一種であるゲルパーミエーションクロマトグラフィー(GPC)により、ポリスチレン換算で算出することができる。
本発明の繊維強化樹脂複合体1を構成する熱可塑性樹脂5を形成するために用いられる熱可塑性繊維8の種類は特に制限されないが、例えば、ポリエーテルイミド系繊維、ポリエーテルケトンケトン系繊維、熱可塑性ポリイミド系繊維、半芳香族ポリアミド系繊維、ポリエーテルエーテルケトン系繊維、ポリフェニレンサルファイド系繊維、ポリスルフォン系繊維、ポリエーテルスルフォン系繊維、ポリカーボネート系繊維等が挙げられる。特に、高い耐熱性、耐水性が要求される航空宇宙、自動車、船舶等の輸送機器分野においては、これらの性能に優れるポリエーテルイミド系繊維、ポリスルフォン系繊維、ポリエーテルスルフォン系繊維が好ましく、中でも、ポリエーテルイミド系繊維がさらに好ましい。これらは単独で用いてもよく、2種以上の樹脂を組み合わせて用いてもよい。
本発明で用いる熱可塑性繊維8からなる繊維強化樹脂複合体用不織布(以下、単に「不織布」と略記することがある)9の製造方法は、特に限定されるものではなく、公知の方法を用いることができ、メルトブローン法、スパンレース法、ニードルパンチ法、スチームジェット法、乾式抄紙法、湿式抄紙法等が挙げられる。
本発明で用いる熱硬化性樹脂としては、従来、繊維強化樹脂複合体に使用されているものであれば、特に限定されず、例えば、エポキシ樹脂、ビニルエステル樹脂、フェノール樹脂、不飽和ポリエステル樹脂、シアネートエステル樹脂、ビスマレイミド樹脂、及びベンゾオキサジン樹脂等が挙げられる。このうち、耐熱性、力学特性、及び寸法安定性などの観点からエポキシ樹脂を好適に用いることができる。これらは単独で用いてもよく、2種以上の樹脂を組み合わせて用いてもよい。
次に、本発明の繊維強化樹脂複合体の製造方法の一例について説明する。図2~図3は本発明の繊維強化樹脂複合体の製造方法を説明するための断面図である。
繊維強化樹脂複合体1を製造する際には、まず、図2に示すように、強化繊維3からなる織物、編み物、及び引き揃え糸シート状物からなる群より選択された少なくとも1つの形態を有する布帛7に対して、上述の熱可塑性繊維8からなる不織布9を積層(即ち、布帛7間に、第三成分として、熱可塑性繊維8からなる不織布9を挿入)して、布帛7と不織布9からなる強化繊維基材10を作製する。なお、必要に応じて、強化繊維基材10を熱プレスしても良い。
強化繊維3からなる布帛7としては、織物、編物、不織布、及びUDシート(Unidirectional:繊維が一方向に引き揃えられている形態)などが挙げられる。これらのうち、複合体の力学特性の観点から、織物、編物、及びUDシートなどの連続繊維からなる布帛が好ましい。
次に、図3に示すように、液状のマトリクス樹脂である熱硬化性樹脂2を注入して、熱硬化性樹脂2を強化繊維基材10に含浸させる。
次に、熱硬化性樹脂2を含浸させた強化繊維基材10を、熱硬化性樹脂2の硬化温度まで、所定の昇温速度で加熱することにより、熱硬化性樹脂2を硬化させる。
上述のごとく、本発明の繊維強化樹脂複合体1は、優れた耐衝撃性を備えており、ASTM D7137に準拠して測定される衝撃後圧縮強度(CAI)が150MPa以上であることが好ましく、160MPa以上であることがより好ましく、170MPa以上であることが更に好ましい。衝撃後圧縮強度(CAI)の上限は特に限定されないが、通常500MPa以下であり、好ましくは400MPa以下であってもよく、より好ましくは300MPa以下程度であってもよい。
JIS L1913「一般不織布試験方法」のフラジール形法に準拠して測定した。
JIS L1913に準じ、縦20cm×横20cmの試料片を採取し、電子天秤にて質量を測定し、この質量を試験片の面積(0.04m2)で除して、単位面積当たりの質量を目付とした。
縦35cm×横25cmの複合体を作製し、その重量を複合体の面積(0.0875m2)で除して、単位面積当たりの質量を目付とした。
研磨した複合体の断面をマイクロスコープ(キーエンス製、商品名:VHX-5000)で撮影し、空隙部の面積比率を算出することにより、空隙率を算出した。より具体的には、研磨断面の二値化により、空隙部面積と充填部面積それぞれを算出し、下記式(1)により空隙率を算出した。
空隙率(%)=空隙部/(空隙部+充填部)×100 (1)
研磨した複合体の断面をマイクロスコープ(キーエンス製、商品名:VHX-5000)で撮影し、炭素繊維の面積比率を算出することにより、空隙率を算出した。より具体的には、研磨断面の二値化により、空隙部面積、樹脂部面積、及び繊維部面積それぞれを算出し、下記式(2)により、繊維体積比率を算出した。
繊維体積比率(%)=繊維部/(繊維部+樹脂部)×100 (2)
<繊維強化樹脂複合体の作製>
金属製のドラムに炭素繊維(三菱レイヨン(株)製、商品名:TR50S 12L)を開繊しながら巻き付け、赤外線ヒーターで加熱しながらロールで加圧することにより、炭素繊維を一方向のみに揃えたUD(Uni Direction)シートを得た。なお、得られたUDシートの目付は200g/m2であった。
まず、繊維強化樹脂複合体の樹脂層の剥離断面のSEM画像(3500倍)から、37.5μm×28μm四方の断面に相当する画像内において、熱可塑性樹脂からなる全粒子数を数えた。続いて、同画像内において熱可塑性樹脂からなる粒子の長径を計測し、粒子の長径が3μm以下の粒子数を数えた。そして、全粒子数に対する、粒子の長径が3μm以下の粒子数の割合を算出した。以上の結果を表1に示す。
ASTM-D7137に準拠して、耐衝撃性を評価した。より具体的には、24枚のUDシートが積層された複合体の厚み1mmあたり、6.67Jの落錘衝撃を与えた後、圧縮試験を行うことにより、衝撃後圧縮強度を測定した。以上の結果を表1に示す。
JIS L1907「吸水率」に準拠して測定した。より具体的には、12枚のUDシートが積層された複合体を120mm×25mmの短冊状に切り出し、80℃で24時間、真空乾燥した状態の重量(絶乾重量)と、70℃の熱水に14日間浸漬させ、表面の水分を拭いた状態の重量(吸水重量)を計測し、下記式(3)により、吸水率を算出した。以上の結果を表1に示す。
吸水率(%)={(吸水重量-絶乾重量)/絶乾重量}×100 (3)
JIS K7017に準拠して、曲げ強度、及び曲げ弾性率を測定した。より具体的には、12枚のUDシートが積層された複合体を120mm×25mmの短冊状に切り出し、80℃で24時間、真空乾燥したものに対し、曲げ試験を行うことにより、絶乾状態における曲げ強度、及び曲げ弾性率を測定した。また、上述の吸水率を測定した後のサンプルに対し、同様の曲げ試験を行うことにより、吸水状態における曲げ強度を測定した。以上の結果を表1に示す。
ポリエーテルイミド繊維からなる不織布として、目付が15g/m2、通気度が110cc/cm2/秒の不織布を使用したこと以外は、上述の実施例1と同様にして、繊維強化樹脂複合体を得た。
ポリエーテルイミド繊維からなる不織布として、目付が30g/m2、通気度が80cc/cm2/秒の不織布を使用したこと以外は、上述の実施例1と同様にして、繊維強化樹脂複合体を得た。
ポリエーテルイミド繊維からなる不織布として、目付が100g/m2、通気度が40cc/cm2/秒の不織布を使用したこと以外は、上述の実施例1と同様にして、繊維強化樹脂複合体を得た。
ポリエーテルイミド繊維からなる不織布を使用しなかったこと以外は、上述の実施例1と同様にして、繊維強化樹脂複合体を得た。
ポリエーテルイミド繊維からなる不織布の代わりに、ポリエーテルイミドフィルム(目付:8g/m2、通気度:0cc/cm2/秒)を使用したこと以外は、上述の実施例1と同様にして、繊維強化樹脂複合体を得た。
2 熱硬化性樹脂
3 強化繊維
4 強化繊維層
5 熱可塑性樹脂
6 樹脂層
7 布帛
8 熱可塑性繊維
9 不織布
10 強化繊維基材
Claims (6)
- 衝撃後圧縮強度が150MPa以上である、請求項1に記載の繊維強化樹脂複合体。
- 絶乾状態における曲げ強度が800MPa以上であり、曲げ弾性率が40GPa以上である、請求項1または請求項2に記載の繊維強化樹脂複合体。
- 吸水率が2.5%以下である、請求項1~請求項3のいずれか1項に記載の繊維強化樹脂複合体。
- 前記熱可塑性樹脂が、ポリエーテルイミド樹脂、ポリスルフォン樹脂、ポリエーテルスルフォン樹脂からなる群より選択される少なくとも一種である、請求項1~請求項4のいずれか1項に記載の繊維強化樹脂複合体。
- 熱硬化性樹脂と、前記熱硬化性樹脂中に積層された複数の強化繊維層と、前記複数の強化繊維層の層間における前記熱硬化性樹脂中に粒状に分散した熱可塑性樹脂とを備える繊維強化樹脂複合体の製造方法であって、
前記熱硬化性樹脂が、下記式で表されるビスフェノールA-ジグリシジルエーテル骨格に由来するエポキシ樹脂であり、
強化繊維からなる少なくとも2層の布帛の間に、熱可塑性繊維からなる不織布を積層して、強化繊維基材を得る積層工程、
前記強化繊維基材に熱硬化性樹脂を含浸する含浸工程、及び
前記熱硬化性樹脂を含浸した強化繊維基材を加熱して、前記熱可塑性樹脂からなる不織布を溶解し、熱硬化性樹脂を硬化する加熱・硬化工程、
を有する繊維強化樹脂複合体の製造方法。
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