WO2021172247A1 - 強化繊維ステッチ基材、プリフォーム材、及び繊維強化複合材料、並びにこれらの製造方法 - Google Patents
強化繊維ステッチ基材、プリフォーム材、及び繊維強化複合材料、並びにこれらの製造方法 Download PDFInfo
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- WO2021172247A1 WO2021172247A1 PCT/JP2021/006532 JP2021006532W WO2021172247A1 WO 2021172247 A1 WO2021172247 A1 WO 2021172247A1 JP 2021006532 W JP2021006532 W JP 2021006532W WO 2021172247 A1 WO2021172247 A1 WO 2021172247A1
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- Prior art keywords
- stitch
- fiber
- reinforcing fiber
- base material
- reinforced composite
- Prior art date
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
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- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
- B32B5/06—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer characterised by a fibrous or filamentary layer mechanically connected, e.g. by needling to another layer, e.g. of fibres, of paper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- 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
- B29B11/00—Making preforms
- B29B11/14—Making preforms characterised by structure or composition
- B29B11/16—Making preforms characterised by structure or composition comprising fillers or reinforcement
-
- 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
- B29C70/10—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres
- B29C70/16—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of substantial or continuous length
- B29C70/22—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of substantial or continuous length oriented in at least two directions forming a two dimensional structure
- B29C70/226—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of substantial or continuous length oriented in at least two directions forming a two dimensional structure the structure comprising mainly parallel filaments interconnected by a small number of cross threads
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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
-
- 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
- B29C70/42—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles
- B29C70/46—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles using matched moulds, e.g. for deforming sheet moulding compounds [SMC] or prepregs
- B29C70/48—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles using matched moulds, e.g. for deforming sheet moulding compounds [SMC] or prepregs and impregnating the reinforcements in the closed mould, e.g. resin transfer moulding [RTM], e.g. by vacuum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/12—Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
-
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Abstract
Description
1. 強化繊維ステッチ基材
本発明の強化繊維ステッチ基材は、強化繊維シートがステッチ糸によりステッチされて成る。本発明において、ステッチ糸は、極性基を有する有機化合物が付着したステッチ糸である。このようなステッチ糸を使用することにより、ステッチ糸の単糸と繊維強化複合材料を構成するマトリクス樹脂との界面において、特に冷熱衝撃に起因する局所的な応力を減少させることができる。そのため、得られる繊維強化複合材料において、ステッチ糸に起因するマイクロクラックの形成を抑制できる。
本発明において、ステッチ糸は、極性基を有する有機化合物が付着したステッチ糸である。極性基を有する有機化合物が付着したステッチ糸を用いることにより、ステッチ糸の単糸と繊維強化複合材料を構成する熱硬化性樹脂との界面において、特に冷熱衝撃に起因する界面剥離の発生と、それに続く局所的な応力集中を減少させることができる。そのため、このようなステッチ糸を強化繊維ステッチ基材に用いることで、得られる繊維強化複合材料において、ステッチ糸に起因するマイクロクラックの形成を抑制できる。
M=1/Σ(樹脂iの重量分率/樹脂iの分子量) ・・・(1)
なお、iは1からkまでの自然数であり、kは有機化合物の種類数である。
1-2. 強化繊維シート
本発明において用いる強化繊維シートは、炭素繊維、ガラス繊維、アラミド繊維、ボロン繊維、金属繊維等の通常の繊維強化材に用いる材料が使用できる。中でも炭素繊維が好ましい。繊維方向の線膨張係数(CTEf)が-10×10-6~10×10-6/Kの範囲にある強化繊維を用いることが好ましい。
本発明の強化繊維ステッチ基材を用いて繊維強化複合材料を成型する場合には、強化繊維ステッチ基材をそのまま用いることもできるが、取扱い性、作業性の観点から強化繊維ステッチ基材を積重して予備成形したプリフォーム材を用いることが好ましい。
本発明の繊維強化複合材料は、本発明の強化繊維ステッチ基材と、マトリクス樹脂組成物とを含んで成る。繊維強化複合材料は、強化繊維ステッチ基材と、マトリクス樹脂組成物と、を複合化した状態で成形させることにより作製される。本発明の強化繊維ステッチ基材に、マトリクス樹脂組成物を含侵させ、ステッチ基材とマトリクス樹脂組成物が複合化した状態で成形させることにより作製される。繊維強化複合材料の作製方法としては、特に制限はなく、強化繊維基材にあらかじめマトリクス樹脂組成物を含侵させたプリプレグを成形してもよく、レジントランスファー成形法(RTM法)や、レジンフィルムインフュージョン成形法(RFI法)等により成形と同時に強化繊維基材とマトリクス樹脂組成物とを複合化しても良い。本発明の強化繊維ステッチ基材は、RTM法やRFI法による成形方法により好ましく用いることができる。マトリクス樹脂の線膨張係数(CTEm)としては、40×10-6~70×10-6/Kが好ましい。
・ステッチ糸1:EMS-CHEMIE社製 ポリアミド繊維 Grilon(登録商標) K-178 23T4 繊度:23dTex 単糸数:4本
・ステッチ糸2:KBセーレン株式会社製 液晶ポリエステル繊維 ゼクシオン(登録商標)28T6 繊度:28dTex 単糸数:6本
・ステッチ糸3:旭化成株式会社製 銅アンモニアレーヨン繊維(セルロース繊維) ベンベルグ(登録商標)33T24 繊度:33dTex 単糸数:24本
・油剤1:芳香族エポキシ化合物 「jER-827」(登録商標)(三菱ケミカル株式会社製 ビスフェノールA型エポキシ樹脂 エポキシ基数:2個 エポキシ当量:180~190g/Eq)の50wt%アセトン溶液(ビスフェノールA型エポキシとアセトンとの重量比が1:1になるように混合)
・油剤2:脂肪族エポキシ化合物 「デナコール」(登録商標)EX832 (ナガセケムテックス(株)製 ポリオキシエチレンジグリシジルエーテル エポキシ基数:2個 エポキシ当量:284g/Eq、ポリオキシエチレン基の平均重合度n:9)の5wt%水溶液(ポリオキシエチレンジグリシジルエーテルと水との重量比が1:19になるように混合)
・油剤3:脂肪族エポキシ化合物 「デナコール」(登録商標)EX832 (ナガセケムテックス(株)製 ポリオキシエチレンジグリシジルエーテル エポキシ基数:2個 エポキシ当量:284g/Eq、ポリオキシエチレン基の平均重合度n:9)の50wt%水溶液(ポリオキシエチレンジグリシジルエーテルと水との重量比が1:1になるように混合)
・油剤4:脂肪族エポキシ化合物 「デナコール」(登録商標)EX861 (ナガセケムテックス(株)製 ポリオキシエチレンジグリシジルエーテル エポキシ基数:2個 エポキシ当量:551g/Eq、ポリオキシエチレン基の平均重合度n:23)の5wt%水溶液(ポリオキシエチレンジグリシジルエーテルと水との重量比が1:19になるように混合)
・油剤5:脂肪族ポリエーテル化合物 「アデカポリエーテル」(登録商標)P1000 (株式会社ADEKA製 ポリプロピレンポリオール(ポリオキシアルキレン骨格を有する化合物) 分子量:1000、水酸基数:2個)の10wt%エタノール溶液(ポリプロピレンポリオールとエタノールとの重量比が1:9になるように混合)
強化繊維として、炭素繊維束“テナックス(登録商標)”HTS40-12K (帝人(株)製、引張強度4.2GPa、引張弾性率240GPa、線膨張係数:-0.5×10-6/K)を用いた。
繊維強化複合材料のマトリクス樹脂として、アミン硬化型エポキシ樹脂を利用した。その組成は以下の通りである。また、硬化物の線膨張係数は、55×10-6/Kであった。
(エポキシ樹脂)
・テトラグリシジル-4,4’-ジアミノジフェニルメタン (ハンツマン・ジャパン株式会社製 Araldite(登録商標) MY721) 20質量部
・トリグリシジル-p-アミノフェノール (ハンツマン・ジャパン株式会社製 Araldite(登録商標) MY0510) 30質量部
・トリグリシジル-m-アミノフェノール (ハンツマン・ジャパン株式会社製 Araldite(登録商標) MY0610) 30質量部
・ビスフェノールF-ジグリシジルエーテル型エポキシ樹脂 (ハンツマン・ジャパン株式会社製 Araldite(登録商標) PY306) 20質量部
[硬化剤]
・4,4’-ジアミノ-3,3’-ジイソプロピル-5,5’-ジメチルジフェニルメタン (ロンザジャパン株式会社製 Lonzacure(登録商標)M-MIPA) 67質量部
(1) 冷熱衝撃試験
冷熱衝撃試験機(エスペック株式会社製 TSA-73EH-W)を用い、繊維強化複合材料に1000回の冷熱サイクルを与えた。冷熱サイクルの1サイクルは、15分間-55℃の平坦域、それに続く70℃の温度に達する15分間の温度変化域、それに続く15分間70℃の平坦域、それに続く-55℃の温度に戻る15分間の温度変化域から成るよう設定し、かかるサイクルを1000回繰り返した。
前記冷熱衝撃試験後の繊維強化複合材料試験片の内部における断面の亀裂数を顕微鏡観察により計測した。顕微鏡として株式会社キーエンス製 VHX-5000を用い、200倍拡大にて観察を行った。具体的には、冷熱衝撃試験後の試験片(幅80mm*長さ50mm*厚さ5mm)を幅40mm*長さ25mmの4等分に切断し、厚み方向の切断面を鏡面研磨し、長辺及び短辺それぞれを観察面とした。顕微鏡観察の微小亀裂の観察範囲は50mm2以上とし、計測された亀裂数を積層数と観察面の幅で割ることでクラック密度の値を算出することができる。クラック密度の単位は個/(cm・ply)である。長辺及び短辺の観察から得られたクラック密度の値は平均化し、最終的なクラック密度とした。
ステッチ糸に対する処理剤の付着量は以下の方法により測定した。エタノールとベンゼンの混合液を溶剤としてソックスレー抽出法により、ステッチ糸より処理剤を抽出した後、処理剤の含まれる溶液を乾燥し、得られた固形分を秤量することによって求めた。
処理剤付着量[M(質量%)]=(M3-M2)/M1×100
ステッチ糸として、ステッチ糸1を用いた。有機溶剤によりステッチ糸を洗浄し、ステッチ糸の表面に付着している繊維用油剤を除去した。ステッチ糸の洗浄は、有機溶剤としてエタノールとベンゼンの混合液を用い、ソックスレー抽出器を用いて12時間の循環洗浄により行った。洗浄後のステッチ糸は真空乾燥機で12時間の乾燥処理を行った。次いで、繊維用油剤を除去したステッチ糸を処理剤溶液中に連続的に浸漬し、処理剤を付与した。処理剤溶液として油剤1を用いた。次いで、ローラーにて余分な水分を除去した後、熱風乾燥器を用いて、ステッチ糸を100℃で1時間乾燥させた。乾燥後の処理剤付着量は、2.8wt%であった。
ステッチ糸としてステッチ糸1を用いた。ステッチ糸に対して、有機溶剤による洗浄及び処理剤の付与を行わなかった以外は、実施例1と同様にして、強化繊維ステッチ基材及び繊維強化複合材料を得た。得られた繊維強化複合材料を用いてクラック密度を測定した。その結果、クラックの発生が確認され、クラック密度は、0.46個/(cm・ply)と実施例1と比較して高いものであった。
ステッチ糸として、ステッチ糸2を用いた以外は、実施例1と同様にして、強化繊維ステッチ基材及び繊維強化複合材料を得た。ステッチ糸の処理剤付着量は1.2wt%であった。得られた繊維強化複合材料を用いてクラック密度を測定した。その結果、クラック密度は、0.09個/(cm・ply)ととても低く、クラック発生の少ない繊維強化複合材料であった。
ステッチ糸としてステッチ糸2を用いた。ステッチ糸に対して、有機溶剤による洗浄及び処理剤の付与を行わなかった以外は、実施例2と同様にして、強化繊維ステッチ基材及び繊維強化複合材料を得た。得られた繊維強化複合材料を用いてクラック密度を測定した。その結果、クラックの発生が確認され、クラック密度は、0.24個/(cm・ply)と実施例2と比較して高いものであった。
ステッチ糸として、ステッチ糸3を用いた以外は、実施例1と同様にして、強化繊維ステッチ基材及び繊維強化複合材料を得た。ステッチ糸の処理剤付着量は4.9wt%であった。得られた繊維強化複合材料を用いてクラック密度を測定した。結果を表1に記載した。得られた繊維強化複合材料のクラック密度は、0.10個/(cm・ply)ととても低く、クラック発生の少ない繊維強化複合材料が得られた。
処理剤として油剤2を用いた以外は、実施例3と同様にして、強化繊維ステッチ基材及び繊維強化複合材料を得た。ステッチ糸の処理剤付着量は、2.4wt%であった。得られた繊維強化複合材料を用いてクラック密度を測定した。結果を表1に記載した。得られた繊維強化複合材料のクラック密度は、0.20個/(cm・ply)と低く、クラック発生の少ない繊維強化複合材料が得られた。
処理剤として油剤3を用いた以外は、実施例3と同様にして、強化繊維ステッチ基材及び繊維強化複合材料を得た。ステッチ糸の処理剤付着量は5.8wt%であった。得られた繊維強化複合材料を用いてクラック密度を測定した。結果を表1に記載した。得られた繊維強化複合材料のクラック密度は、0.13個/(cm・ply)ととても低く、クラック発生の少ない繊維強化複合材料が得られた。
処理剤として油剤4を用いた以外は、実施例3と同様にして、強化繊維ステッチ基材及び繊維強化複合材料を得た。ステッチ糸の処理剤付着量は1.8wt%であった。得られた繊維強化複合材料を用いてクラック密度を測定した。結果を表1に記載した。得られた繊維強化複合材料のクラック密度は、0.19個/(cm・ply)ととても低く、クラック発生の少ない繊維強化複合材料が得られた。
処理剤として油剤5を用いた以外は、実施例3と同様にして、強化繊維ステッチ基材及び繊維強化複合材料を得た。ステッチ糸の処理剤付着量は1.2wt%であった。得られた繊維強化複合材料を用いてクラック密度を測定した。結果を表1に記載した。得られた繊維強化複合材料のクラック密度は、0.28個/(cm・ply)と低く、クラック発生の少ない繊維強化複合材料が得られた。
ステッチ糸としてステッチ糸3を用いた。ステッチ糸に対して、有機溶剤による洗浄及び処理剤の付与を行わなかった以外は、実施例3と同様にして、強化繊維ステッチ基材及び繊維強化複合材料を得た。得られた繊維強化複合材料を用いてクラック密度を測定した。結果を表1に記載した。比較例3で得られた繊維強化複合材料では、クラックの発生が確認され、クラック密度は、0.54個/(cm・ply)と実施例3~7と比較してとても高いものであった。
Claims (12)
- 強化繊維から成る強化繊維シートがステッチ糸によりステッチされて成る強化繊維ステッチ基材であって、
前記ステッチ糸が、極性基を有する有機化合物が付着したステッチ糸であることを特徴とする強化繊維ステッチ基材。 - 前記強化繊維シートが、一方向に引き揃えられた強化繊維から成る強化繊維シートである請求項1に記載の強化繊維ステッチ基材。
- 前記強化繊維シートが、一方向に引き揃えられた強化繊維からなる強化繊維シートが、繊維軸方向を互いに変えて順次積層された強化繊維シートである請求項1または2に記載の強化繊維ステッチ基材。
- 前記極性基を有する有機化合物が、ポリオキシアルキレン骨格を有する化合物である請求項1~3のいずれか1項に記載の強化繊維ステッチ基材。
- 前記極性基を有する有機化合物が、エポキシ基を有する化合物である請求項1~4のいずれか1項に記載の強化繊維ステッチ基材。
- 前記ステッチ糸が、極性基を有する有機化合物がステッチ糸の質量に対して0.1~10wt%付着したステッチ糸である請求項1~5のいずれか1項に記載の強化繊維ステッチ基材。
- 前記ステッチ糸が、180℃で2時間加熱し冷却した後の繊維軸方向の線膨張係数が-1~70×10-6/Kのステッチ糸である請求項1~6のいずれか1項に記載の強化繊維ステッチ基材。
- 強化繊維から成る強化繊維シートを、極性基を有する有機化合物が付着したステッチ糸でステッチすることを特徴とする強化繊維ステッチ基材の製造方法。
- 請求項1~7の何れか1項に記載の強化繊維ステッチ基材と、前記強化繊維ステッチ基材100質量部に対して1~20質量部のバインダー樹脂と、を含むプリフォーム材。
- 請求項1~7の何れか1項に記載の強化繊維ステッチ基材と、バインダー樹脂と、を加圧下で加熱するプリフォーム材の製造方法。
- 請求項1~7の何れか1項に記載の強化繊維ステッチ基材と、前記強化繊維ステッチ基材100質量部に対して20~60質量部のマトリクス樹脂組成物と、を含む繊維強化複合材料。
- 請求項1~7の何れか1項に記載の強化繊維ステッチ基材に、マトリクス樹脂を含侵させる繊維強化複合材料の製造方法。
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