JP2015141152A - Evaluation method of resin film - Google Patents
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本発明は、銅張積層板のベースフィルムとして使用される樹脂フィルムの評価方法に関し、特にポリイミドフィルムに代表される樹脂フィルムの脱水による寸法変化率を熱機械分析の測定結果に基づいて評価する方法に関する。 The present invention relates to a method for evaluating a resin film used as a base film of a copper-clad laminate, and in particular, a method for evaluating a dimensional change rate due to dehydration of a resin film represented by a polyimide film based on a measurement result of thermomechanical analysis. About.
ポリイミドフィルムは優れた耐熱性を有している上、機械的、電気的、および化学的特性において他のプラスチック材料に比べて遜色ないことから、例えばプリント配線板（ＰＷＢ）、フレキシブルプリント配線板（ＦＰＣ）、テープ自動ボンディング用テープ（ＴＡＢ）、チップオンフィルム（ＣＯＦ）等の電子部品用の絶縁基板材料として多用されている。これらＰＷＢ、ＦＰＣ、ＴＡＢ、及びＣＯＦは、一般にベースフィルムとしてのポリイミドフィルムの少なくとも片面に金属導体層として銅をめっき等で被覆し、得られた銅被覆ポリイミド基板の金属導体層に配線をパターニング加工することによって作製することができる。 The polyimide film has excellent heat resistance and is not inferior to other plastic materials in mechanical, electrical, and chemical characteristics. For example, a printed wiring board (PWB), a flexible printed wiring board ( It is widely used as an insulating substrate material for electronic components such as FPC), tape automatic bonding tape (TAB), and chip on film (COF). These PWB, FPC, TAB, and COF are generally coated with copper as a metal conductor layer on at least one side of a polyimide film as a base film, and wiring is patterned on the metal conductor layer of the obtained copper-coated polyimide substrate. It can produce by doing.
このような銅被覆ポリイミド基板に代表される銅張積層板の品質の評価方法としては、例えば非特許文献１に、ＴＭＡ（Ｔｈｅｒｍｏ Ｍｅｃｈａｎｉｃａｌ Ａｎａｌｙｓｉｓ）装置を用いて銅張積層板のベースフィルムの寸法変化率を測定し、これにより銅張積層板の品質を評価する手法が記載されている。この手法は、銅張積層板の全面銅はくをエッチングにより除去し、得られたプラスチックフィルムに複数の穴を開けてＴＭＡ装置で加熱処理を行い、この加熱処理の前後での穴間隔の変化を測定して寸法変化率を算出するものである。また、非特許文献２には、包装用延伸ポリプレンフィルムを加熱処理した時の寸法変化率を測定する手法が記載されている。 As a method for evaluating the quality of a copper-clad laminate typified by such a copper-coated polyimide substrate, for example, Non-Patent Document 1 describes a dimensional change of a base film of a copper-clad laminate using a TMA (Thermo Mechanical Analysis) apparatus. A technique for measuring the rate and thereby evaluating the quality of the copper clad laminate is described. In this method, the copper foil on the copper clad laminate is removed by etching, a plurality of holes are made in the obtained plastic film, and heat treatment is performed with a TMA apparatus, and the change in the hole interval before and after the heat treatment is performed. Is used to calculate the dimensional change rate. Non-Patent Document 2 describes a method of measuring a dimensional change rate when a stretched stretched polypropylene film for heat treatment is heat-treated.
上記した非特許文献１、２の樹脂フィルムの評価方法は、いずれも常温の樹脂フィルムに対して特定の温度及び時間で加熱処理した時に生ずる寸法変化率を測定して評価するものであるが、樹脂フィルムには一般的に水分が含まれており、これが加熱によって脱水した時にどの程度寸法変化に影響を及ぼすかについては把握することができなかった。 The above-mentioned evaluation methods for the resin films of Non-Patent Documents 1 and 2 are to measure and evaluate the rate of dimensional change that occurs when heat treatment is performed at a specific temperature and time for a normal temperature resin film, The resin film generally contains moisture, and it has not been possible to grasp how much this affects the dimensional change when dehydrated by heating.
例えば、分子鎖に親水基であるカルボニル基を持つ樹脂フィルムは高い吸水性を有しているため、上記した寸法変化率の測定の際の昇温により樹脂フィルムに吸水されていた水分が脱水し、この脱水による収縮挙動が樹脂フィルムの寸法変化率の測定結果に影響を及ぼすことがあった。本発明は上記した従来の問題に鑑みてなされたものであり、樹脂フィルムを加熱した時に生じる脱水による寸法変化率への影響を評価する方法を提供することを目的としている。 For example, since a resin film having a carbonyl group that is a hydrophilic group in the molecular chain has high water absorption, the water absorbed in the resin film is dehydrated due to the temperature rise during the measurement of the dimensional change rate described above. The shrinkage behavior due to dehydration sometimes affects the measurement result of the dimensional change rate of the resin film. The present invention has been made in view of the above-described conventional problems, and an object of the present invention is to provide a method for evaluating the influence on the dimensional change rate due to dehydration that occurs when a resin film is heated.
上記目的を達成するため、本発明に係る樹脂フィルムの寸法安定性の評価方法は、評価対象となる樹脂フィルムから２枚の試験片を切り出し、前処理として一方には吸湿処理を他方には１００℃以上１５０℃以下まで昇温させる乾燥処理を施した後、各々熱機械分析装置を用いて室温から所定の温度まで昇温させることで寸法変化率の温度による変化を測定し、前記吸湿処理した試験片の寸法変化率から前記乾燥処理した試験片の寸法変化率を温度毎に差し引くことで脱水による寸法変化率を算出することを特徴としている。 In order to achieve the above object, the method for evaluating the dimensional stability of a resin film according to the present invention cuts out two test pieces from a resin film to be evaluated, and performs a moisture absorption treatment on one side and a moisture absorption treatment on the other side as a pretreatment. After performing a drying process of raising the temperature from 150 ° C. to 150 ° C., the temperature change was measured from room temperature to a predetermined temperature using a thermomechanical analyzer, and the moisture absorption treatment was performed. The dimensional change rate due to dehydration is calculated by subtracting the dimensional change rate of the dried test piece for each temperature from the dimensional change rate of the test piece.
本発明によれば、樹脂フィルムを加熱した時に生じる脱水による寸法変化率をＴＭＡ装置を用いて簡易に評価することができ、これによりフレキシブルプリント配線板等に用いる銅張積層板のベースフィルムの寸法安定性に関して脱水による影響が考慮されたより詳細な知見を得ることができる。 According to the present invention, the rate of dimensional change due to dehydration that occurs when a resin film is heated can be easily evaluated using a TMA apparatus, whereby the dimensions of the base film of a copper-clad laminate used for flexible printed wiring boards and the like. More detailed knowledge regarding the effect of dehydration in consideration of stability can be obtained.
以下、本発明の樹脂フィルムの評価方法の一具体例について説明する。この本発明の一具体例の樹脂フィルムの評価方法は、一般に厚み０.２〜１ｍｍの長尺状樹脂フィルムを評価対象としており、特にフレキシブルプリント配線板等に用いる銅張積層板用のベースフィルムとして使用される長尺状のポリイミドフィルムの評価に適している。評価に際して先ず長尺状樹脂フィルムから幅２〜６ｍｍ×長さ１５〜５０ｍｍ程度の２枚の同サイズの矩形のフィルム片を切り出して試験片とする。 Hereinafter, a specific example of the resin film evaluation method of the present invention will be described. This method for evaluating a resin film according to one specific example of the present invention is generally intended to evaluate a long resin film having a thickness of 0.2 to 1 mm, and particularly a base film for a copper-clad laminate used for a flexible printed wiring board or the like. It is suitable for evaluation of long polyimide films used as At the time of evaluation, first, two rectangular film pieces of the same size having a width of 2 to 6 mm and a length of 15 to 50 mm are cut out from the long resin film to obtain test pieces.
これら２枚の試験片を切り出す際は、それらの長手方向が両方とも長尺状プラスチックフィルムの平面上において同じ向きを向いているように切り出すのが好ましい。例えば、２枚の矩形の試験片の長手方向が両方とも長尺状プラスチックフィルムのＴＤ（Ｔｒａｎｓｖｅｒｓｅ Ｄｉｒｅｃｔｉｏｎ）方向を向くように切り出すのが好ましい。 When cutting out these two test pieces, it is preferable to cut them out so that their longitudinal directions are both in the same direction on the plane of the long plastic film. For example, it is preferable to cut out the two rectangular test pieces so that both of the longitudinal directions thereof are directed to the TD (Transverse Direction) direction of the long plastic film.
このようにして切り出した２枚の試験片のうちの一方は、所定の温度及び湿度条件の雰囲気下に所定の時間曝すことにより吸湿処理を施す。この吸湿処理は、限定するものではないが、恒温恒湿槽内で行うのが望ましい。２枚の試験片のうちの他方は、水の沸点である１００℃以上で好ましくは１５０℃以下の温度まで昇温させる乾燥処理を施す。これにより樹脂フィルムに残留している水分を除去する。その後、高温の試験片に対しては必要に応じて冷却を行って室温に戻す。このようにして前処理された両試験片に対して、各々熱機械分析装置（ＴＭＡ：Ｔｈｅｒｍｏ−Ｍｅｃｈａｎｉｃａｌ Ａｎａｌｙｓｉｓ）装置を用いて所定の引っ張り荷重をかけながら室温から好ましくは１５０℃以上２００℃以下の温度、より好ましくは約１８０℃まで昇温させる。 One of the two test pieces cut out in this way is subjected to moisture absorption treatment by exposure to an atmosphere of a predetermined temperature and humidity condition for a predetermined time. Although this moisture absorption process is not limited, it is desirable to perform in a constant temperature and humidity tank. The other of the two test pieces is subjected to a drying process in which the temperature is raised to a temperature of 100 ° C. or higher, preferably 150 ° C. or lower, which is the boiling point of water. As a result, moisture remaining on the resin film is removed. Then, it cools as needed with respect to a hot test piece, and returns to room temperature. The two specimens pretreated in this way are each subjected to a predetermined tensile load using a thermo-mechanical analyzer (TMA: Thermo-Mechanical Analysis) apparatus, and preferably from 150 ° C. to 200 ° C. from room temperature. The temperature is raised, more preferably to about 180 ° C.
これにより、吸湿処理された試験片及び乾燥処理された試験片の寸法変化率の温度による変化プロフィールがそれぞれ得られる。そして、これら吸湿処理された試験片の寸法変化率から乾燥処理された試験片の寸法変化率を温度毎に差し引くことで脱水による寸法変化率を算出することができる Thereby, the change profile with the temperature of the dimensional change rate of the test piece which carried out the moisture absorption process and the test piece which carried out the dry process is each obtained. The dimensional change rate due to dehydration can be calculated by subtracting the dimensional change rate of the dried test piece from the dimensional change rate of the moisture-absorbed test piece for each temperature.
なお、上記した熱機械分析は、不活性ガス雰囲気下にて実施するのが好ましい。酸素を含むガス雰囲気ではおおよそ１００℃以上の温度でプラスチックフィルムが酸化されて変質するおそれがあるからである。また、吸湿処理や乾燥処理を施した試験片はすばやくＴＭＡ装置で試験を行うのが好ましい。吸湿処理された試験片の乾燥が進んだり、乾燥処理された試験片に再度水分が吸着したりするのを抑えることができ、寸法変化率をより正確に測定することが可能になるからである。 The thermomechanical analysis described above is preferably performed in an inert gas atmosphere. This is because in a gas atmosphere containing oxygen, the plastic film may be oxidized and deteriorated at a temperature of about 100 ° C. or higher. Moreover, it is preferable that the test piece which performed the moisture absorption process and the drying process test quickly with a TMA apparatus. This is because it is possible to suppress drying of the moisture-absorbed test piece and to prevent moisture from adsorbing again to the dried test piece, and to measure the dimensional change rate more accurately. .
試験片の引っ張り荷重は３ｇ以上７ｇ未満が好ましく、５ｇがより好ましい。この荷重が３ｇ未満では試験片の保持が不十分になりやすく、振動によるノイズが加わって測定精度が低下するおそれがある。一方、荷重が７ｇを超えると試験片が過剰に引っ張られるため、精度の高い測定ができなくなるおそれがある。更に、上記昇温の際は毎分２０℃以上で昇温させるのが望ましい。この昇温速度が毎分２０℃未満では各温度での保持時間が長くなりすぎるため、脱水による寸法変化率を正しく算出できなくなるおそれがある。 The tensile load of the test piece is preferably 3 g or more and less than 7 g, more preferably 5 g. If the load is less than 3 g, the test piece is likely to be insufficiently held, and noise due to vibration may be added to reduce measurement accuracy. On the other hand, if the load exceeds 7 g, the test piece is pulled excessively, so that there is a possibility that measurement with high accuracy cannot be performed. Furthermore, it is desirable to raise the temperature at 20 ° C. or more per minute when the temperature is raised. If this rate of temperature rise is less than 20 ° C. per minute, the holding time at each temperature will be too long, and the dimensional change rate due to dehydration may not be calculated correctly.
［実施例１］
東レ・デュポン株式会社製の長尺状のポリイミドフィルム（商品名：カプトン１５０ＥＮ）から２枚の同サイズの矩形の試験片をそれらの長手方向が長尺状のポリイミドフィルムのＴＤ方向を向くように切り出し、それらのうちの一方の試験片に対して恒温恒湿槽にて２３℃、相対湿度８５％の雰囲気に９６時間曝露させる吸湿処理を行った。また、もう一方の試験片に対しては、試験片の温度を１００℃まで昇温させて残留水分を除去した後、２５℃まで温度を下げる乾燥処理を行った。
[Example 1]
Two rectangular test pieces of the same size from a long polyimide film (trade name: Kapton 150EN) manufactured by Toray DuPont Co., Ltd. so that the longitudinal direction thereof faces the TD direction of the long polyimide film The sample was cut out and subjected to a moisture absorption treatment in which one of the test pieces was exposed to an atmosphere of 23 ° C. and 85% relative humidity for 96 hours in a constant temperature and humidity chamber. Further, the other test piece was subjected to a drying treatment in which the temperature of the test piece was raised to 100 ° C. to remove residual moisture, and then the temperature was lowered to 25 ° C.
これら吸湿処理及び乾燥処理がそれぞれ施された両試験片を各々ブルカー・エイエックス（株）製のＴＭＡ装置４０３０ＳＡに取り付けた。各試験片をＴＭＡ装置の測定チャックに取り付ける際は、ＴＤ方向に５ｇの引っ張り荷重がかかるようにした。そして、雰囲気温度を毎分２０℃の昇温速度で３０℃から１８０℃まで昇温させて１８０℃で３０分間保持する加熱処理を行いながら寸法変化率を測定した。なお、寸法変化率の測定の際はＴＭＡ装置内を窒素雰囲気にした。また、雰囲気温度は試験片から約５ｍｍ離れた場所に設置した熱電対で測定した。 Both test pieces subjected to the moisture absorption treatment and the drying treatment were respectively attached to a TMA apparatus 4030SA manufactured by Bruker Ax Co., Ltd. When attaching each test piece to the measurement chuck of the TMA apparatus, a tensile load of 5 g was applied in the TD direction. And the dimensional change rate was measured, performing the heat processing which heated up atmospheric temperature from 30 degreeC to 180 degreeC with the temperature increase rate of 20 degreeC / min, and hold | maintained at 180 degreeC for 30 minutes. In the measurement of the dimensional change rate, the inside of the TMA apparatus was made a nitrogen atmosphere. The ambient temperature was measured with a thermocouple installed at a location about 5 mm away from the test piece.
このようにして行った加熱処理の際の昇温パターン及びそれに伴って生じた寸法変化率の測定結果を、乾燥処理が施された試験片については図１（ａ）に、吸湿処理が施された試験片については図１（ｂ）にそれぞれ示す。これら図１（ａ）及び（ｂ）の横軸には加熱により雰囲気温度が３０℃に達してからの経過時間が示されている。なお、寸法変化率は、（（ｌ１−ｌ０）／ｌ０）×１００で求めることができる。ここで、ｌ０は変形前の試験片の長さ、はｌ１変形後の試験片の長さを示す。 The temperature rise pattern during the heat treatment performed in this way and the measurement result of the dimensional change rate that accompanies it are shown in FIG. The test specimens are shown in FIG. 1A and 1B show the elapsed time after the atmospheric temperature reaches 30 ° C. by heating. The dimensional change rate can be obtained by ((l 1 −l 0 ) / l 0 ) × 100. Here, l 0 indicates the length of the test piece before deformation, and l 1 indicates the length of the test piece after deformation.
そして、脱水による寸法変化率を求めるべく、図１（ｂ）に示す吸湿処理が施された試験片の寸法変化率から図１（ａ）に示す乾燥処理が施された試験片の寸法変化率を温度毎に差し引いた。その結果を加熱処理の際の昇温パターンと共に図１（ｃ）に示す。この図１（ｃ）のグラフから、実施例１の条件で吸湿させたポリイミドフィルムは、３０℃から１８０℃までの昇温時の脱水により約０.０５％収縮することが分かる。 Then, in order to obtain the dimensional change rate due to dehydration, the dimensional change rate of the test piece subjected to the drying process shown in FIG. 1A from the dimensional change rate of the test piece subjected to the moisture absorption process shown in FIG. Was subtracted for each temperature. The result is shown in FIG.1 (c) with the temperature rising pattern in the case of heat processing. From the graph of FIG. 1C, it can be seen that the polyimide film absorbed under the conditions of Example 1 contracts by about 0.05% due to dehydration when the temperature is raised from 30 ° C. to 180 ° C.
［実施例２］
恒温恒湿槽の相対湿度を８５％に代えて５５％にした以外は実施例１と同様にして試験片を吸湿させた。そして、この吸湿させた試験片に対して実施例１と同様にしてＴＭＡ装置で加熱処理を行った。この加熱処理の際の昇温パターン及びそれに伴って生じた寸法変化率の測定結果を図２（ａ）に示す。また、脱水による寸法変化率を求めるべく、図２（ａ）に示す吸湿処理が施された試験片の寸法変化率から上記実施例１の図１（ａ）に示す乾燥処理が施された試験片の寸法変化率を温度毎に差し引いた。その結果を加熱処理の際の昇温パターンと共に図２（ｂ）に示す。この図２（ｂ）のグラフから、実施例２の条件で吸湿させたポリイミドフィルムは、３０℃から１８０℃までの昇温時の脱水により約０.０３５％収縮することが分かる。
[Example 2]
The test piece was absorbed in the same manner as in Example 1 except that the relative humidity of the constant temperature and humidity chamber was changed to 55% instead of 85%. And it heat-processed with the TMA apparatus like Example 1 with respect to this moisture-absorbed test piece. FIG. 2 (a) shows the temperature rise pattern during the heat treatment and the measurement result of the rate of dimensional change caused thereby. Moreover, in order to obtain | require the dimensional change rate by spin-drying | dehydration, the test which performed the drying process shown in FIG. 1 (a) of the said Example 1 from the dimensional change rate of the test piece which performed the moisture absorption process shown in FIG. 2 (a). The dimensional change rate of the piece was subtracted for each temperature. The result is shown in FIG. 2 (b) together with the temperature rising pattern during the heat treatment. From the graph of FIG. 2 (b), it can be seen that the polyimide film absorbed under the conditions of Example 2 contracts by about 0.035% by dehydration when the temperature is raised from 30 ° C. to 180 ° C.
［実施例３］
カプトン１５０ＥＮに代えて宇部興産株式会社製のポリイミドフィルム（商品名：ユーピレックス２５Ｓ）を用いた以外は実施例１と同様にして、吸湿処理及び乾燥処理がそれぞれ施された２枚の試験片に対して各々ＴＭＡ装置で加熱処理を行った。この加熱処理の際の昇温パターン及びそれに伴って生じた寸法変化率の測定結果を、乾燥処理が施された試験片については図３（ａ）に、吸湿処理が施された試験片については図３（ｂ）にそれぞれ示す。
[Example 3]
In the same manner as in Example 1 except that a polyimide film (trade name: Upilex 25S) manufactured by Ube Industries, Ltd. was used instead of Kapton 150EN, two specimens subjected to moisture absorption treatment and drying treatment were used. Each was heat-treated with a TMA apparatus. FIG. 3 (a) shows the temperature rise pattern during the heat treatment and the measurement result of the dimensional change rate that accompanies it. FIG. 3 (a) shows the test piece subjected to the drying treatment, and FIG. Each is shown in FIG.
また、脱水による寸法変化率を求めるべく、図３（ｂ）に示す吸湿処理が施された試験片の寸法変化率から図３（ａ）に示す乾燥処理が施された試験片の寸法変化率を温度毎に差し引いた。その結果を加熱処理の際の昇温パターンと共に図３（ｃ）に示す。この図３（ｃ）のグラフから、実施例３の条件で吸湿させたポリイミドフィルムは、３０℃から１８０℃までの昇温時の脱水により約０.０４％収縮することが分かる。 Further, in order to obtain the dimensional change rate due to dehydration, the dimensional change rate of the test piece subjected to the drying treatment shown in FIG. 3A from the dimensional change rate of the test piece subjected to the moisture absorption treatment shown in FIG. Was subtracted for each temperature. The result is shown in FIG.3 (c) with the temperature rising pattern in the case of heat processing. From the graph of FIG. 3 (c), it can be seen that the polyimide film absorbed under the conditions of Example 3 contracts by about 0.04% due to dehydration when the temperature is raised from 30 ° C. to 180 ° C.
［実施例４］
恒温恒湿槽の相対湿度を８５％に代えて５５％にした以外は実施例３と同様にして試験片を吸湿させた。そして、この吸湿させた試験片に対して実施例１と同様にしてＴＭＡ装置で加熱処理を行った。この加熱処理の際の昇温パターン及びそれに伴って生じた寸法変化率の測定結果を図４（ａ）に示す。また、脱水による寸法変化率を求めるべく、この図４（ａ）に示す吸湿処理が施された試験片の寸法変化率から上記実施例３の図３（ａ）に示す乾燥処理が施された試験片の寸法変化率を温度毎に差し引いた。その結果を加熱処理の際の昇温パターンと共に図４（ｂ）に示す。この図４（ｂ）のグラフから、実施例４の条件で吸湿させたポリイミドフィルムは、３０℃から１８０℃までの昇温時の脱水により約０.０２５％収縮することが分かる。
[Example 4]
The test piece was absorbed in the same manner as in Example 3 except that the relative humidity of the constant temperature and humidity chamber was changed to 55% instead of 85%. And it heat-processed with the TMA apparatus like Example 1 with respect to this moisture-absorbed test piece. FIG. 4 (a) shows the temperature rise pattern during the heat treatment and the measurement result of the rate of dimensional change caused thereby. Further, in order to obtain the dimensional change rate due to dehydration, the drying process shown in FIG. 3A of Example 3 was performed from the dimensional change rate of the test piece subjected to the moisture absorption process shown in FIG. 4A. The dimensional change rate of the test piece was subtracted for each temperature. The result is shown in FIG.4 (b) with the temperature rising pattern in the case of heat processing. From the graph of FIG. 4 (b), it can be seen that the polyimide film absorbed under the conditions of Example 4 shrinks by about 0.025% by dehydration when the temperature is raised from 30 ° C. to 180 ° C.
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| CN105444705A (en) * | 2015-11-24 | 2016-03-30 | 苏州生益科技有限公司 | Laminated board size stability test method |
| JP2018069578A (en) * | 2016-10-28 | 2018-05-10 | 住友金属鉱山株式会社 | Both side plated laminate, and method for producing both side plated laminate |
| JP7136400B1 (en) * | 2021-12-23 | 2022-09-13 | 昭和電工マテリアルズ株式会社 | Physical property measuring method, member evaluation method, electronic component device manufacturing method, electronic component device material manufacturing method, and physical property measuring system |
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| JP7136400B1 (en) * | 2021-12-23 | 2022-09-13 | 昭和電工マテリアルズ株式会社 | Physical property measuring method, member evaluation method, electronic component device manufacturing method, electronic component device material manufacturing method, and physical property measuring system |
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