Creep Characteristics of Liquid Crystal Polymer Film

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(Journal of the Society of Materials Science, Japan), Vol. 59, No. 8, pp. 645-652, Aug. 2010 Creep Characteristics of Liquid Crystal Polymer Film by Hideyuki KANAYAMA, Shengde ZHANG, Masao SAKANE, Tadashi NAGASAWA and Kaoru KOBAYASHI This paper studies the creep characteristic of a liquid crystal polymer (LCP) thin film. Tensile creep tests were performed using three directional specimens at three testing temperatures. Creep curves consisted of mainly transient creep and almost no steady and accelerated creep stages were found. The minimum creep strain rate and rupture lifetime were significantly influenced by the specimen direction and testing temperature. This paper developed a new method of correlating the minimum creep strain rate independent of the specimen direction and testing temperature. This paper also developed a correlation method of creep rupture lifetime independent of the specimen direction and testing temperature. Key words : Liquid crystal polymer, Thin film, Creep, Anisotropy, Monkman-Grant equation, Larson- Miller parameter 1 1) ON/OFF 2) 3), 4) 5) 8) 8) 9), 10) 5) 7) 2 2 Fig. 1 30μm 423K LCP LCP 5), 6) 5) 7) LCP X X 50kV 200mA CuKα 1.5418Å LCP 13 50mm 2 Fig. 2 Fig. 1 Structural formula of LCP film sheet. 21 10 13 Received Oct. 13, 2009 2010 The Society of Materials Science, Japan 525-8577 Integrated Sci. and Eng., Graduate School of Sci. and Eng., Ritsumeikan Univ., Nojihigashi, Kusatsu, 525-8577 525-8577 Dept. of Mech. Eng., Ritsumeikan Univ., Nojihigashi, Kusatsu, 525-8577 520-2362 KYOCERASLC Tech. Corp., Ichimiyake, Yasu, 520-2362

11996 10.7.21 3:15 PM ページ 646 646 金山英幸 張 聖徳 坂根政男 長澤 忠 小林 馨 Fig. 2 X-ray diffraction pattern of LCP film sheet. TD 方向に明瞭な回折パターンが観察できたが MD 方 向では回折パターンがほとんど観察できなかった この ことから MD 方向に主鎖方向が高配向していることがわ 5), 11) かる Fig. 3 に本研究で用いた LCP 薄膜試験片の形状 寸 法を示す 試験片は平行部長さ 30mm 同幅 5mm のも のをレーザーで切出したものである クリープ変形およ びクリープ破断時間の LCP 薄膜の配向状態による異方性 を検討するため 本研究では Fig. 4 に示すように θ = 0 45 および 90 の 3 方向から切出した試験片を用い た ここで θ は MD 方向と試験片の軸方向との角度で ある Fig. 2 の結果から 切出し角度 θ は主鎖方向が高 Fig. 5 Schematic of creep testing machine for thin film specimens. 配向している方向からの角度に対応している 本試験には Fig. 5 に示す荷重容量 200N のクリープ 12) 荷重負荷方式は重錘②による直荷式 試験装置を用いた である 試験片①の変位は試験片に連結されたプルロッ ドに取り付けたプレート⑥の変位を 2 つの差動トランス ⑤を用いて計測した 試験片の加熱には電気抵抗炉③ (100W) と電気炉内の温度分布改善のために補助ヒータ ④ (8.6W) を用いた 試験期間中の温度変動は ± 0.1K 以 内であった 大気中で 353K 373K および 393K の 3 温度レベルで クリープ試験を実施した クリープ試験は 試験片温度が Fig. 3 Shape and dimensions of the film specimen (mm). 設定値に到達後 16 24 時間の均熱時間後に開始した 3 試験結果および考察 3 1 クリープ変形特性 本研究で得られたクリープ曲線の一例を 3 つの切出し 角度 試験温度が 353K について Fig. 6 (a) (c)に示す いずれの結果も クリープ試験の最終データ点は 60 秒毎 の計測の最終点である Fig. 6 (a) (c)からわかるよう に 明瞭な遷移域が荷重負荷直後に 3 つの切出し角度 ともに観察される クリープ曲線から得られたひずみ速度と時間の関係を Fig. 7 (a) (c)に示す ひずみ速度は隣り合う 11 点のク リープ曲線のデータを用いて最小二乗法で 2 次関数の係 13) Fig. 7 (a) 数を求め 11 点の中央点の微分係数とした (c)のひずみ速度線図では ひずみ速度は時間経過に伴っ て単調に減少した また ひずみ速度が一定値を示す明 Fig. 4 Sampling directions of specimen from LCP film sheet. 瞭な定常域は観察されなかった 以上のことから 主鎖

647 Fig. 6 Creep curves in three directions at 353K. Fig. 7 Strain rate with time in three directions at 353K. LCP 3 Fig. 7 Fig. 8 (a) (c) 3 22.5 θ = 0 θ = 45 90 θ = 45 θ = 0 3 θ = 90 θ = 45 3 LCP

648 [MPa] Q [J/mol] R [8.31J/(mol K)] T [K] α β Q α (1) σ β 1/T Fig. 9 (a) Q α α Fig. 9 (b) Fig. 9 (b) α θ (2) LCP (3) Table 1 Material constants in Eq. (3). Fig. 8 Correlation of minimum strain rate with stress in three directions. 20K 2 LCP (1) (1) ε min [%/h] σ Fig. 9 Calculation method of material constants in Eq. (3).

649 (2) (3) (3) A β γ Q Table 1 (3) Q Q = 318 10 3 J/mol 40 80 10 3 J/mol 14) 300 10 3 J/mol 15) Fig. 10 (3) 1 10 10 LCP (3) 3 2 Fig. 11 (a) (c) 3 θ = 0 θ = 45 90 θ = 45 θ = 0 4 θ = 90 θ = 45 4 LCP 20K 2 Fig. 11 Variation of time to rupture with stress for three types of specimens. Fig. 10 Correlation of minimum strain rate in experiments with that estimated by Eq. (3). Fig. 12 θ = 0 θ = 45 90 353K 373K

650 Table 2 Constants in Monkman-Grant equation. Fig. 12 Variation of creep rupture elongation with stress for three types of specimens at three temperatures. 16) 393K 393K LCP 353K 373K (3) Larson-Miller 17) 353K 393K Fig. 13 3 LCP (4) Monkman-Grant 18) (4) Table 2 (4) m C MG m 1.05 1 18) C MG C MG 18) Table 2 C MG Fig. 12 C MG 3 3 Fig. 11 LCP (5) Larson-Miller 17) (5) T [K] t r [hr] C LM Fig. 14 Larson- Miller Larson-Miller C LM θ = 0 3 C LM = 47.8 Larson-Miller (6) σ (3) exp (γ θ ) (3) (6) θ = 0 σ = σ σ (7) Fig. 13 Correlation of time to rupture with minimum strain rate. Fig. 14 Correlation of time to rupture with Larson- Miller parameter.

651 (6) (7) β γ Table 1 (7) Fig. 15 Fig. 16 (7) Larson-Miller θ = 0 5 5 Larson-Miller LCP 4 (1) 353K 373K 393K LCP (2) X LCP MD (3) LCP 10 (4) LCP LCP Larson-Miller 5 Fig. 15 Correlation of time to rupture with equivalent stress. Fig. 16 Correlation of time to rupture using the equivalent stress and Larson-Miller parameter. 1 ) Y. Tsukada, Introduction of build-up printed circuit board (1998) The Nikkan Kogyo Shinbun, LTD. 2 ) M. Sakane, New challenges for thermo-mechanical fatigue III : Thermo-mechanical fatigue in electronic devices, Journal of the Society of Materials Science, Japan, Vol.56, No.3, pp.302-308 (2007). 3 ) T. Mori, Super low thermal expansion curable polyamide insulating resin, Journal of Japan Institute of Electronics Packaging, Vol.10, No.2, pp.116-119 (2007). 4 ) L. Valette and R. Wiechmann, High-performance substrate from new epoxy resin and enhanced copper foil, Circuit World, Vol.30, No.4, pp.20-26 (2004). 5 ) N. Koide and K. Sakamoto, Liquid crystal polymer (1988) Kyoritsu Shuppan Co., LTD. 6 ) T. Kamiya and T. Shimizu, Liquid crystal polymer new age (1991) Kogyo Chosakai Publishing, Inc. 7 ) The Society of Materials Science, Japan, Engineering materials, fourth edition, pp.333-337 (2000) The Society of Materials Science, Japan. 8 ) M. Onodera, Flexible printed circuit- Liquid crystal polymer, Japan Institute of Electronics Packing, Vol.8, No.2, pp.90-94 (2005). 9 ) A. E. Akinay, W. Brostow, V. M. Castano, R. Maksimov and P. Olszynski, Time-temperature correspondence prediction of stress relaxation of polymeric materials from a minimum of data, Polymer, Vol.43, No.13, pp.3593-3600 (2002).

652 10) A. E. Akinay, W. Brostow, V. M. Castano and R. Maksimov, Prediction of long-term service performance of polymeric materials from short-term tests : Creep and prediction of the stress shift factor of a longitudinal polymer liquid crystal, Polymer Engineering and Science, Vol.41, No.6, pp.997-981 (2001). 11) N. Koide, Development of Liquid crystal polymer (2001) CMC Publishing Co., LTD. 12) A. Takada, H. Danjo, M. Sakane, Y. Tsukada and H. Nishimura, Development of miniature creep testing for solders, Transactions of the Japan Society of Mechanical Engineers, Vol.69, No.683, A, pp.1082-1087 (2003). 13) The Society of Materials Science, Japan, Standard creep testing for solders (2004) The Society of Materials Science, Japan. 14) A. Takada, M. Sakane and Y. Tsukada, Creep and creep rupture properties of Sn-8Zn-3Bi solder, Journal of the Society of Materials Science, Japan, Vol.56, No.2, pp.129-135 (2007). 15) The Society of Materials Science, Japan, Strength and fracture of materials, pp.145-146 (2000) The Society of Materials Science, Japan. 16) S. Taira, High temperature strength of metal material (1968) Yokendo Co., LTD. 17) F. R. Larson and J. Miller, A time-temperature relationship for rupture and creep stresses, Transactions of the American Society of Mechanical Engineers, Vol.74, No.5, pp.765-775 (1952). 18) F. C. Monkman and N. J. Grant, An empirical relationship between rupture-life and minimum creep rate in creep-rupture tests, Proceedings of American Society for Testing and Materials, Vol.56, pp.593-620 (1956).

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