JP6271130B2 - 複合材の製造方法 - Google Patents
複合材の製造方法 Download PDFInfo
- Publication number
- JP6271130B2 JP6271130B2 JP2013007628A JP2013007628A JP6271130B2 JP 6271130 B2 JP6271130 B2 JP 6271130B2 JP 2013007628 A JP2013007628 A JP 2013007628A JP 2013007628 A JP2013007628 A JP 2013007628A JP 6271130 B2 JP6271130 B2 JP 6271130B2
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- Prior art keywords
- molded
- cured
- primary
- temperature
- curing
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Images
Classifications
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- B29C66/73—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset
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- B29C66/7392—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of at least one of the parts being a thermoplastic
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- B29C66/80—General aspects of machine operations or constructions and parts thereof
- B29C66/84—Specific machine types or machines suitable for specific applications
- B29C66/843—Machines for making separate joints at the same time in different planes; Machines for making separate joints at the same time mounted in parallel or in series
- B29C66/8432—Machines for making separate joints at the same time mounted in parallel or in series
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- B29K2105/08—Condition, form or state of moulded material or of the material to be shaped containing reinforcements, fillers or inserts of continuous length, e.g. cords, rovings, mats, fabrics, strands or yarns
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Description
この一体成形法については、本出願人らの出願に係る特許第2647530号公報(特許文献1)に係るものが知られている。この成形法では、複合材の被成形品素材を、複合材一体成形用形状保持具で保持し、全体を一体で硬化させている。
この一体成形法は、被成形品素材の全体を一体で硬化するため、得られる複合材の強度において優れている。しかし、スティフナ素材が液状化した際のスティフナ形状の維持に必要な治具が複雑化しがちであり、工程上の負担が大きくなりがちであった。
このコボンド法では、予め硬化成形したパネル又はスティフナのいずれか一方と、硬化成形していないもう一方とを接着剤を介して設置し、オートクレーブで硬化させることとしている。
このコボンド法は、パネル又はスティフナのいずれか一方を事前に硬化しているために、製造にあたって、各被成形品素材の取扱性は良い。しかしながら、得られる複合材の強度が、スティフナとパネルとの接着剤による接着強度に依拠することとなるため、接着品質を高める工夫が必要である。
前記複合材が少なくとも二以上の被成形品素材から構成され、前記複合材を構成するための被成形品素材のうち少なくとも一を一次硬化させて準備し、前記一次硬化させた被成形品素材を、接着剤を介して、又は介さずに、前記複合材を構成するための他の被成形品素材に組み付けて組付体を準備し、前記一次硬化させた少なくとも一の被成形品素材のガラス転移点以上に前記組付体を加熱して、前記少なくとも一の被成形品素材をゴム状態とし、該被成形品素材と相接する接着剤又は前記被成形品素材と相接する前記他の被成形品素材を硬化過程で前記ゴム状態の被成形品素材と共存させ、前記一次硬化させた少なくとも一の被成形品素材を二次硬化させ、前記少なくとも一の被成形品素材と、前記他の被成形品素材とを一体化させることを特徴とする。
ここで、「他の被成形品素材」については、接着剤を介しない場合は、接着剤と同様の反応硬化過程を経て、「少なくとも一の被成形品素材」と一体化する必要がある。しかし、接着剤を介する場合には、必ずしもその必要はなく、この場合、「他の被成形品素材」は、硬化状態によらず採用することができる。例えば、硬化完了後のものを採用することができる。また、材質も金属であっても良い。
(i)dT31=Tr3−Tg1≧30℃であり、かつTr2−Tg1>0℃である制御範囲。
(ii)前記(i)であって、かつdT21=Tr2−Tg1≧25℃である制御範囲。
(iii)前記(ii)であって、かつdT11=Tr1−Tg1≧20℃である制御範囲。
(iv)dT32=Tr3−Tg2≧10℃であり、かつTr2−Tg1>0℃である制御範囲。
(v)前記(iv)であって、かつdT22=Tr2−Tg2≧5℃である制御範囲。
(vi)前記(v)であって、かつdT12=Tr1−Tg2≧0℃である制御範囲。
(vii)dT33=Tr3−Tg3≧0℃であり、かつTr2−Tg1>0℃である制御範囲。
(viii)dT23=Tr2−Tg3≧0℃である制御範囲。
(ix)dT13=Tr1−Tg3≧0℃である制御範囲。
(x)dT13=Tr1−Tg3≧10℃である制御範囲。
ただし、Tg1、Tg2、Tg3、Tr1、Tr2、Tr3は、以下の通りの温度である。
Tg1: 一次硬化させた被成形品素材の貯蔵弾性率の低下開始ポイントの温度
Tg2: 一次硬化させた被成形品素材のガラス状態からゴム状態の相転移の中間付近の温度(tanδ(=損失弾性率/貯蔵弾性率)がピークを示す温度)
Tg3: 一次硬化させた被成形品素材の貯蔵弾性率の低下終了ポイントの温度
Tr1: 一次硬化させた被成形品素材と相接する接着剤又は一次硬化させた被成形品素材と相接する他の被成形品素材の反応開始ポイントの温度
Tr2: 一次硬化させた被成形品素材と相接する接着剤又は一次硬化させた被成形品素材と相接する他の被成形品素材の反応温度
Tr3: 一次硬化させた被成形品素材と相接する接着剤又は一次硬化させた被成形品素材と相接する他の被成形品素材の反応終了ポイントの温度
本発明に係る複合材の製造方法は、他の実施の形態で、前記スティフナ素材を、連鎖硬化型樹脂を用いた繊維強化樹脂で構成することができる。
本実施の形態に係る複合材の製造方法は、少なくとも以下の工程を実施するものである。
(1)一次硬化させたスティフナ素材を準備する。ここで、この一次硬化させたスティフナ素材は、「少なくとも一の一次硬化させた被成形品素材」に対応するものである。
(2)パネル素材を準備する。このパネル素材は、「前記複合材を構成するための他の被成形品素材」に対応する。なお、パネル素材は、スティフナ素材の準備と同時、又はスティフナ素材の準備の前後のいずれのタイミングでも準備することができる。
(3)一次硬化させたスティフナ素材に、パネル素材を、接着剤を介して組み付け、組付体とする。
(4)組付体を、一次硬化させたスティフナ素材のガラス転移点以上に加熱して、スティフナ素材をゴム状態とし、スティフナ素材と相接する接着剤の硬化過程で前記ゴム状態の素材と共存させ、スティフナ素材を二次硬化させ、スティフナ素材とパネル素材とを一体化する。
また、パネル素材も、スキン、外板、外皮、表皮、バルクヘッド(圧力隔壁)用パネル等のように称されることもある。
図1に示すように、成形治具(成形型)1に中子型2と繊維基材(プリフォーム)3を配置する。
本発明では、成形治具1を用い、RTM成形方法によって、スティフナ素材を成形する。ただし、RTM成形方法に限定されるものではない。例えば、オートクレーブ成形法を用いることもできる。
さらに、必要に応じて、中子型2と繊維基材3との間にも、ピールプライ等の離型材(図示省略)を配置してもよい。または、中子型2の表面を離型処理してもよい。または、中子型2を離型材料で構成してもよい。
必要により、繊維基材3を所定の位置に固定するための構造を、繊維基材3に接する中子型2及び成形治具1に設けてもよい。例えば、図1では、上蓋5、下蓋6、枠型7、又は中子型2に設けてもよい。成形治具1内に、中子型2とともに繊維基材3を配置したら、上蓋5と下蓋6を閉じる。なお、型を閉じた後、必要に応じて、プレス等により成形治具1を挟み込み、外側から圧力をかける。
また、必要に応じて、成形治具1を熱板プレス等によって加温してもよい。加温する場合は、含浸温度や乾燥温度等の所定の温度まで加温する。
なお、一次硬化(半硬化)に留まるように制御することについては、後にさらに詳述する。
成形治具1を冷却することで、成形治具1の取り扱いや、その中から中子型2及び繊維強化樹脂の取り出しが、安全かつ容易に行えるとともに、一次硬化状態の制御も容易となる。 樹脂材が硬化したら、成形治具1から、スティフナ素材を取り出す。
また、パネル素材は、炭素繊維基材を2〜200積層したものに硬化前のマトリックス樹脂を含浸させたものとして準備することとしてもよい。炭素繊維基材には例えば炭素繊維織物等が用いられる。また、事前に数層分を積層し、纏められたプリフォームやノンクリンプファブリックを用いても良い。プリフォームやノンクリンプファブリックの積層枚数は事前に積層されている分を考慮して決定される。本工程は、前述したスティフナ素材と同様の工程を経てRTM成形によって準備することもできる。また、樹脂の含浸工程はスティフナ素材を組み付けた後に行うこともできる。
いずれの場合でも、接着剤を介さずにスティフナ素材に組み付けることもできる。
このステップでは、パネル素材を構成するプリプレグ12を治具上に載置する。そして、接着剤を介して、スティフナ素材13を、中子型2を保持した状態で組み付ける。バッギングフィルム14で被成形素材を覆い、内部を真空状態とする。なお、図中15は、封止材である。
なお、パネル素材と、スティフナ素材との関係を逆とし、パネル素材を一次硬化させて準備して本発明に係る複合材の製造方法とすることもできる。
図10の曲線Aに示すように、前述したスティフナ素材のような一次硬化(半硬化)させたものの粘弾性測定にての弾性率の温度依存性を測定すると、(室温から)温度上昇に伴い貯蔵弾性率が緩やかに低下して行く(ガラス状態、B部分)。そして、ある温度を越えると温度上昇に伴い急激に貯蔵弾性率が低下する(ガラス状態からゴム状態への状態変化、C部分。この状態転移点をガラス転移点と称し、この転移点の温度をガラス転移温度:Tgと称する。)。
なお、硬化するとTgは高温側にシフトする。
また、曲線Eは、接着剤の側のエネルギー曲線をモデル的に示したものである。
一般論として、硬化性樹脂における一次硬化[半硬化(状態)]とは、一般的に硬化が未了・不良の状態(硬化反応が完了していない状態)を意味する。
硬化が完了していない状態のものは全て半硬化状態ということができる。しかしながらが、同一の樹脂であっても硬化の程度(どの程度まで硬化が進んでいるか)により、様々な特性面(物理的特性、機械的特性、化学的特性)において全く異なる特性を発現し得る。
本発明で複合材の被成形品素材を一体化する場合において、一体化に用いる被成形品素材の硬化状態をTgの観点から制御し、本来、当該被成形品素材が硬化完了状態で有するTgよりも低いTgを有する状態であると同時に、一体化時の昇温過程においてマトリクス樹脂が液状となって流動することがない状態であって、かつ後述(<一次硬化(低Tg制御型硬化)状態の被成形品素材のTgと接着剤反応温度との相関・Tg制御ポイント>)する温度範囲に制御されたTgを有する硬化状態(低Tg制御型硬化状態)に制御された被成形品素材を一体化に用いることを特徴とする。
一次硬化(低Tg制御型硬化)状態の被成形品素材を得る上で重要となるのは、かかる被成形品素材のTgをどこに(どの温度に)制御するかがポイントとなる。このTgは、用いる接着剤等の接合部接触面相手材(接着剤又は他の被成形品素材)の反応温度との相関によって決定付けられる。すなわち、用いる被成形品素材の材種や接着剤種により、それぞれ、一次硬化完了時のTgや接着剤の反応温度が異なり様々である。しかし、一次硬化(低Tg制御型硬化)状態の被成形品素材のTgとしては、後述する接着剤の反応温度(Tr)との相関を示す限りにおいて、用いる被成形品素材の材種や接着剤種に依らず有効である。後述する例は、接着剤の例にて説明されている。しかし、Trは一次硬化(低Tg制御型硬化)状態の被成形品素材の接合部接触面相手材の反応温度を意味するものである。例えば、接合部接触面相手材が接着剤ではなく、プリプレグ材やRTM用マトリクス樹脂であった場合等はそれぞれの反応温度と読み替えることができる。
(1)貯蔵弾性率の低下開始ポイントTg1(ガラス状態側on set値)
これは、一次硬化状態の被成形品素材の粘弾性を測定することによって特定する。測定の一形態としては、供試体(平板)の上下をチャックで固定し、所定の昇温速度で熱を付与する。下部チャックに捩じりを付与し、上部チャックで捩じりをセンシングする。上下の差異を元にして弾性率の変化を算出する。
図11に示すように、貯蔵弾性率の低下開始ポイントは、加温初期のなだらかなB部分の線形外挿と、急激に弾性率が落ちるC部分の線形外挿の交点とする。剛性設計では、弾性率の変化が性能に影響するため、変化前の値を指標としており、この決め方で良い。
これも図11に示す。
これも一次硬化状態の被成形品素材の粘弾性を測定することによって特定する。
(3)貯蔵弾性率の低下終了ポイントTg3(ゴム状態側on set値、又は貯蔵弾性率の低下ピーク値)。
これも一次硬化状態の被成形品素材の粘弾性を測定することによって特定する。
図11に示すように、これは、急激に弾性率が落ちるC部分の線形外挿と、なだらかになったD部分の線形外挿との交点である。
(1)反応開始ポイントの温度Tr1[反応開始側on set値(DSC測定)]
図12に示すように、なだらかな部分Aと、急峻部分Bの外挿の交点である。
図12において、縦軸は、DSC測定(示差走査熱量測定)により測定した熱量(エネルギー)である。
(2)反応温度Tr2[反応ピーク温度(DSC測定)]
図12において、ピーク温度である。
(3)反応終了ポイントの温度Tr3[反応終了側on set値(DSC測定)]
図12に示すように、急峻なC部分と、なだらかなD部分との外挿の交点である。
(i)dT31=Tr3−Tg1≧30℃であり、かつTr2−Tg1>0℃である制御範囲。なお、「dT」の記号は、温度間の差を示すために用いている。以下の記述でも同様である。
(ii)より好ましくは、前記(i)であって、かつdT21=Tr2−Tg1≧25℃である制御範囲。
(iii)さらに好ましくは、前記(ii)であって、かつdT11=Tr1−Tg1≧20℃である制御範囲。
前記した(i)〜(iii)のTrとTgの温度差は大きい程好ましい。
(iv)dT32=Tr3−Tg2≧10℃であり、かつTr2−Tg1>0℃である制御範囲。
(v)より好ましくは、前記(iv)であって、かつdT22=Tr2−Tg2≧5℃である制御範囲。
(vi)さらに好ましくは、前記(v)であって、かつdT12=Tr1−Tg2≧0℃である制御範囲。
前記した(iv)〜(vi)のTrとTgの温度差は大きい程好ましい。
(vii)dT33=Tr3−Tg3 ≧ 0℃であり、かつTr2−Tg1>0℃である制御範囲。
(viii)より好ましくは、dT23=Tr2−Tg3≧0℃である制御範囲。
(ix)さらに好ましくは、dT13=Tr1−Tg3≧0℃である制御範囲。
(x)最も好ましくは、dT13=Tr1−Tg3≧10℃である制御範囲。
前記した(vii)〜(x)のTrとTgの温度差は大きい程好ましい。
一次硬化(低Tg制御型硬化)状態の成形条件の確立方法の例を示す。
ただし、これに限定されるものではなく、重要なのは前述の硬化状態が得られることである。
一次硬化(低Tg制御型硬化)状態としたい被成形品素材に用いる材料のDSC測定を実施し、硬化(反応)開始温度Tp1を測定する。
ここで、Tp1は硬化(反応)開始ポイント[反応開始側on set値(DSC測定)]であって、図16に示すように、なだらかな部分Aと、急峻部分Bの外挿の交点と定義する。
一次硬化(低Tg制御型硬化)状態としたい被成形品素材の成形において、成形温度と保持時間を硬化開始温度Tp1で30分保持にて成形し、この被成形品素材のTg(仮Tg)を粘弾性にて測定する。
このTg(仮Tg)と接着剤について測定された前記Tr(Tr1、Tr2、Tr3)を比較し、TgとTrについて規定した前記制御値[制御範囲(i)〜(x)]に入っているかを吟味する。上記Tg(仮Tg)が前記制御値[制御範囲(i)〜(x)]内にない場合や、前記制御値[制御範囲(i)〜(x)]で目標とする範囲に入っていない場合であって、高すぎる場合は、再度、成形条件を硬化開始温度−10℃するか、保持時間を半分の15分保持にするか(又はその両方)の条件にて複合材を成形し、再度、Tg(仮Tg)を計測する。上記Tg計測中に液状化する場合(及び上記Tg(仮Tg)が低すぎる場合)は、再度、成形条件を、硬化開始温度を+10℃するか、保持時間を倍の1時間保持するか(又はその両方)の条件にて複合材を成形し、再度、Tg(仮Tg)を計測する。
その他の方法として、目標とするTgを成形時の保持温度の目安として使用する方法等もある。
何れの方法を用いても通常、数回の試験にて一次硬化(低Tg制御型硬化)状態の成形条件の確立が可能である。
接合のための成形プロセスにおいて、昇温条件としてTg1以上Tr3以下の温度範囲にステップ(温度保持)を設けることも有用である。ステップを設ける温度範囲(Tg及びTr)としては、Tg側の温度範囲は、好ましくはTg2以上であり、さらに好ましくはTg3以上である。一方、Tr側の温度範囲は、好ましくはTr2以下であり、さらに好ましくはTr1以下である。
2 中子型
3 繊維基材
4 キャビティ
5 上蓋
6 下蓋
7 枠型
8 封止材
9 離型材
10 真空配管
11 樹脂注入配管
12 プリプレグ
13 スティフナ素材
14 バッギングフィルム
15 封止材
16 組付体
17 オートクレーブ
18 スティフナ・パネル
Claims (3)
- 複合材の製造方法であって、前記複合材が少なくとも二以上の被成形品素材から構成され、
前記複合材を構成するための被成形品素材のうち少なくとも一を一次硬化させて準備し、
前記一次硬化させた被成形品素材を、接着剤を介して、又は介さずに、前記複合材を構成するための他の被成形品素材に組み付けて組付体を準備し、
前記一次硬化させた少なくとも一の被成形品素材のガラス転移点以上に前記組付体を加熱して、前記少なくとも一の被成形品素材をゴム状態とし、該被成形品素材と相接する接着剤又は前記被成形品素材と相接する前記他の被成形品素材を硬化過程で前記ゴム状態の被成形品素材と共存させ、前記一次硬化させた少なくとも一の被成形品素材を二次硬化させ、前記少なくとも一の被成形品素材と、前記他の被成形品素材とを一体化させること
を含み、
以下の通りの温度Tg1、Tg2、Tg3、Tr1、Tr2、Tr3を求め
Tg1: 一次硬化させた被成形品素材の貯蔵弾性率の低下開始ポイントの温度
Tg2: tanδ(=損失弾性率/貯蔵弾性率)がピークを示す温度
Tg3: 一次硬化させた被成形品素材の貯蔵弾性率の低下終了ポイントの温度
Tr1: 一次硬化させた被成形品素材と相接する接着剤又は一次硬化させた被成形品素材と相接する他の被成形品素材の硬化反応開始ポイントの温度
Tr2: 一次硬化させた被成形品素材と相接する接着剤又は一次硬化させた被成形品素材と相接する他の被成形品素材の硬化反応温度
Tr3: 一次硬化させた被成形品素材と相接する接着剤又は一次硬化させた被成形品素材と相接する他の被成形品素材の硬化反応終了ポイントの温度)
前記一次硬化させた被成形品素材のガラス転移点Tgと、該被成形品素材と相接する接着剤又は前記被成形品素材と相接する前記他の被成形品素材の反応温度Trとを以下の(i)〜(x)のいずれかの条件を満足するように設定するようにしたことを特徴とする複合材の製造方法。
(i)dT31=Tr3−Tg1≧30℃であり、かつTr2−Tg1>0℃である制御範囲。
(ii)前記(i)であって、かつdT21=Tr2−Tg1≧25℃である制御範囲。
(iii)前記(ii)であって、かつdT11=Tr1−Tg1≧20℃である制御範囲。
(iv)dT32=Tr3−Tg2≧10℃であり、かつTr2−Tg1>0℃である制御範囲。
(v)前記(iv)であって、かつdT22=Tr2−Tg2≧5℃である制御範囲。
(vi)前記(v)であって、かつdT12=Tr1−Tg2≧0℃である制御範囲。
(vii)dT33=Tr3−Tg3≧0℃であり、かつTr2−Tg1>0℃である制御範囲。
(viii)dT23=Tr2−Tg3≧0℃である制御範囲。
(ix)dT13=Tr1−Tg3≧0℃である制御範囲。
(x)dT13=Tr1−Tg3≧10℃である制御範囲。 - 前記複合材がスティフナ素材と、パネル素材とから成る複合材であって、スティフナ素材を一次硬化させることを特徴とする請求項1に記載の複合材の製造方法。
- 前記スティフナ素材を、連鎖硬化型樹脂を用いた繊維強化樹脂で構成する請求項2に記載の複合材の製造方法。
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US10436758B2 (en) * | 2017-06-16 | 2019-10-08 | Xerox Corporation | Method and apparatus for determining an ultraviolet (UV) cure level |
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