JP2008229995A - Manufacturing method of laminate - Google Patents
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Abstract
【課題】高い寸法安定性の要求される回路基板用金属張積層板に好適に使用される積層体につき、製造工程で発生する外観不良（フクレ）を抑えて安定的に製造できる積層体の製造方法を提供。
【解決手段】液晶ポリマーフィルムの両側に金属箔を有する積層体を製造する方法において、第１工程で該液晶ポリマーフィルムと該金属箔とを熱圧着して形成した搬送可能な積層体を、第２工程で搬送させながら加熱処理を行った後、第３工程で加圧雰囲気状態及び加熱状態にする炉又は装置を用いて、圧力を１．５×１０5〜３．０×１０6Ｐａの範囲にすると共に加熱温度を該液晶ポリマーの融点より３０℃低い温度以上にして処理を行うことを特徴とする。
【選択図】図１[PROBLEMS] To manufacture a laminate that can be stably manufactured by suppressing appearance defects (flattening) that occur in a manufacturing process for a laminate suitably used for a metal-clad laminate for a circuit board that requires high dimensional stability. Provide a way.
In a method of manufacturing a laminate having metal foil on both sides of a liquid crystal polymer film, a transportable laminate formed by thermocompression bonding the liquid crystal polymer film and the metal foil in a first step is provided. After carrying out heat treatment while transporting in two steps, the pressure is set to 1.5 × 10 5 to 3.0 × 10 6 Pa using a furnace or apparatus that is brought into a pressurized atmosphere state and a heated state in the third step. It is characterized in that the treatment is carried out at a heating temperature of 30 ° C. lower than the melting point of the liquid crystal polymer.
[Selection] Figure 1
Description
本発明は、樹脂フィルムと金属箔との積層体の製造方法に関するものであり、より詳細には、光学的異方性の溶融相を形成し得る液晶ポリマーからなるフィルム（以下、液晶ポリマーフィルムともいう。）と金属箔とを重ね合わせてなる積層体の製造方法に関する。 The present invention relates to a method for producing a laminate of a resin film and a metal foil. More specifically, the present invention relates to a film composed of a liquid crystal polymer capable of forming an optically anisotropic melt phase (hereinafter also referred to as a liquid crystal polymer film). It is related with the manufacturing method of the laminated body which overlaps and metal foil.
一般に液晶ポリマーフィルムは、高耐熱性、吸湿寸法安定性、高周波特性等に優れた材料として知られている。液晶ポリマーフィルムのこのような特性に着目し、これを電子回路基板の絶縁材料に用いることが検討されてきている。電子回路基板に用いる場合、液晶ポリマーフィルムと銅箔に代表される金属箔との積層体が配線基板用積層体として適している。 In general, a liquid crystal polymer film is known as a material excellent in high heat resistance, hygroscopic dimensional stability, high frequency characteristics, and the like. Focusing on such characteristics of the liquid crystal polymer film, it has been studied to use it as an insulating material for an electronic circuit board. When used for an electronic circuit board, a laminate of a liquid crystal polymer film and a metal foil represented by copper foil is suitable as a laminate for a wiring board.
従来、液晶ポリマーフィルムと金属箔とからなる積層体を製造する技術としては、熱プレス装置を使用していた。代表的な具体例としては、熱プレス装置の上下の熱板間に所定の大きさに裁断された液晶ポリマーフィルムと金属箔を重ねて置き、真空状態で加熱圧着する方法が挙げられる。しかしながら、この方式はバッチ式であるため、剥離強さ等において均一な品質の積層体を製造することができないという問題があり、また、積層体一枚あたりの生産速度が遅くなって、コストが高くなるという欠点を有する。 Conventionally, a hot press apparatus has been used as a technique for producing a laminate composed of a liquid crystal polymer film and a metal foil. As a typical example, there is a method in which a liquid crystal polymer film cut to a predetermined size and a metal foil are placed between upper and lower hot plates of a hot press apparatus and heat-pressed in a vacuum state. However, since this method is a batch method, there is a problem that it is not possible to produce a laminated body having a uniform quality in terms of peel strength, etc., and the production speed per laminated body is slowed, resulting in a cost reduction. It has the disadvantage of becoming expensive.
そこで、低コストでありながら生産速度を高めるために、積層体を連続的に製造する方法が提案されている（例えば、特許文献１を参照）。液晶ポリマーフィルムと金属箔とを重ね合わせて、加圧ロールの間を通過させることにより、フィルムと該金属箔とを液晶ポリマーの融点より８０℃低い温度から融点より５℃低い温度までの範囲内の温度で圧着した状態で、加圧ロールを通過させるものである。また、液晶ポリマーの融点より８０℃低い温度から融点より５℃低い温度までの範囲内の表面温度を有する少なくとも１個のロールを含む加熱・加圧ロールの間を通過させることにより、該フィルムと該金属箔とを圧着するとしている。 Therefore, in order to increase the production speed at a low cost, a method for continuously producing a laminate has been proposed (see, for example, Patent Document 1). By overlapping the liquid crystal polymer film and the metal foil and passing between the pressure rolls, the film and the metal foil are within a range from a temperature 80 ° C. lower than the melting point of the liquid crystal polymer to a temperature 5 ° C. lower than the melting point. The pressure roll is allowed to pass through in a state where it is pressure-bonded at the temperature. And passing the film between a heating and pressing roll containing at least one roll having a surface temperature in a range from a temperature lower than the melting point of the liquid crystal polymer by 80 ° C. to a temperature lower than the melting point by 5 ° C. It is assumed that the metal foil is pressure-bonded.
また、寸法安定性に優れた回路基板用金属張積層板を高い生産性で提供するために、上述の液晶ポリマーフィルムと金属箔の熱圧着を行う第１工程と、第１工程で得られた積層体を、液晶ポリマーフィルムの融点以上で加熱処理する第２工程とを備えた製造方法が提案されている（例えば、特許文献２を参照）。特許文献２は、上記第１工程の加熱ロール間で熱可塑性液晶ポリマーフィルムと金属箔を圧着させる場合、熱可塑性液晶ポリマーフィルムに張力がかかり、その分子の変動が起こり易くなり、同フィルムを用いた金属張積層板ではフィルム表面において、加熱に伴い分子配向の変化が起こり易くなる。このため、上記の第２工程を実施することにより、等方性および寸法安定性の良好な金属張積層板が得られるとしている。 Moreover, in order to provide the metal-clad laminate for circuit boards excellent in dimensional stability with high productivity, the first step of thermocompression bonding of the liquid crystal polymer film and the metal foil was obtained in the first step. A manufacturing method has been proposed that includes a second step of heat-treating the laminate at a temperature equal to or higher than the melting point of the liquid crystal polymer film (for example, see Patent Document 2). In Patent Document 2, when the thermoplastic liquid crystal polymer film and the metal foil are pressure-bonded between the heating rolls in the first step, tension is applied to the thermoplastic liquid crystal polymer film, and the molecules easily change. In the conventional metal-clad laminate, the molecular orientation easily changes with heating on the film surface. For this reason, it is said that a metal-clad laminate having good isotropy and dimensional stability can be obtained by performing the second step.
さらに、第１工程、第２工程を終了させた後、後段の第３工程として、熱処理と冷却固化を複数回繰り返し、熱処理の都度、液晶ポリマーの融点が変化するのに合わせて、熱処理温度を変える熱処理方法が提案されている（例えば、特許文献３を参照）。そして、このような第３工程の熱処理によって、優れた耐熱性と耐摩耗性を有する積層体を得ることができるとしているが、金属箔／液晶ポリマーフィルム／金属箔のような両面金属張積層板の加熱において、同フィルムからのアウトガスが原因で積層体表面に外観不良（フクレ）が発生するという問題があった。 Furthermore, after finishing the first step and the second step, as the third step in the subsequent stage, the heat treatment and cooling solidification are repeated a plurality of times. A heat treatment method to be changed has been proposed (see, for example, Patent Document 3). And it is said that a laminate having excellent heat resistance and wear resistance can be obtained by the heat treatment in the third step, but a double-sided metal-clad laminate such as metal foil / liquid crystal polymer film / metal foil. In this heating, there was a problem that appearance defects (bulges) occurred on the surface of the laminate due to outgas from the film.
本発明は、高い寸法安定性の要求される回路基板用金属張積層板に好適に使用される積層体につき、製造工程で発生する外観不良（フクレ）を抑えて安定的に製造できる積層体の製造方法を提供することを目的とする。 The present invention relates to a laminate suitably used for a metal-clad laminate for circuit boards that requires high dimensional stability, and is a laminate that can be stably produced while suppressing appearance defects (blowing) that occur in the production process. An object is to provide a manufacturing method.
本発明者等は、上記課題を解決するために鋭意検討を重ねた結果、高耐熱化のための加熱工程を特定条件下で行うことで、上記課題を解決し得ることを見出し本発明を完成するに至った。すなわち、本発明は、液晶ポリマーフィルムの両側に金属箔を有する積層体を製造する方法において、
第１工程で該液晶ポリマーフィルムと該金属箔とを熱圧着して形成した搬送可能な積層体を、第２工程で搬送させながら加熱処理を行った後、第３工程で加圧雰囲気状態及び加熱状態にする炉又は装置を用いて、圧力を１．５×１０5〜３．０×１０6Ｐａの範囲にすると共に加熱温度を該液晶ポリマーの融点より３０℃低い温度以上にして処理を行うことを特徴とする積層体の製造方法である。
As a result of intensive studies to solve the above-mentioned problems, the present inventors have found that the above-mentioned problems can be solved by performing a heating process for increasing heat resistance under specific conditions, and the present invention has been completed. It came to do. That is, the present invention is a method for producing a laminate having metal foil on both sides of a liquid crystal polymer film,
The transportable laminate formed by thermocompression bonding the liquid crystal polymer film and the metal foil in the first step is subjected to heat treatment while being transported in the second step, and then in the pressurized atmosphere state and in the third step. Using a furnace or apparatus to be heated, the pressure is set in the range of 1.5 × 10 5 to 3.0 × 10 6 Pa and the heating temperature is set to 30 ° C. lower than the melting point of the liquid crystal polymer. It is the manufacturing method of the laminated body characterized by performing.
本発明の製造方法によれば、液晶ポリマーフィルムと金属箔とを熱圧着により積層した後に行われる所謂第３工程において、加圧雰囲気状態で熱処理を行うことで、フクレ等の発生のない外観の優れた積層体を生産性よく製造することが可能である。ここで製造された積層体は、液晶ポリマー保有の高耐熱性、吸湿寸法安定性、高周波特性等を損なうことなく、かつ金属箔との接着性にも優れていることから、例えばフレキシブル配線基板に代表される配線基板に用いられる積層体として有用である。 According to the production method of the present invention, in the so-called third step performed after laminating the liquid crystal polymer film and the metal foil by thermocompression bonding, by performing heat treatment in a pressurized atmosphere state, the appearance without occurrence of swelling or the like is obtained. It is possible to produce an excellent laminate with high productivity. The laminate produced here is not damaged by the high heat resistance, moisture absorption dimensional stability, high frequency characteristics, etc. possessed by the liquid crystal polymer, and is excellent in adhesion to metal foil. It is useful as a laminate used for a representative wiring board.
以下、必要に応じて添付図面を参照しながら本発明に係る積層体の製造方法を詳述する。以下に示す実施形態及び実施例により、本発明の積層体の製造方法を限定するものではない。 Hereinafter, the manufacturing method of the laminated body which concerns on this invention is explained in full detail, referring an accompanying drawing as needed. The following embodiments and examples do not limit the production method of the laminate of the present invention.
本発明は、光学的異方性の溶融相を形成する液晶ポリマーよりなるフィルムと金属箔とを重ね合わせて積層体を製造する方法であるが、フィルム３と金属箔４、４’とを熱圧着して形成した巻き取り搬送可能な積層体とする第１工程（図１参照）と、積層体５を架橋搬送させながら加熱処理を行う第２工程（図２参照）と、第２工程を経た積層体を特定範囲で加圧雰囲気状態にし、該液晶ポリマーの融点より３０℃低い温度以上で加熱処理を行う第３工程（図３参照）を必須の製造工程とする。 The present invention is a method for producing a laminate by laminating a film made of a liquid crystal polymer that forms an optically anisotropic melt phase and a metal foil, and the film 3 and the metal foils 4 and 4 ′ are heated. A first step (see FIG. 1) for forming a laminate that can be wound and conveyed formed by pressure bonding, a second step (see FIG. 2) in which heat treatment is performed while the laminate 5 is cross-linked and conveyed, and a second step. The third step (see FIG. 3) in which the laminated body is subjected to a pressurized atmosphere in a specific range and subjected to heat treatment at a temperature 30 ° C. lower than the melting point of the liquid crystal polymer is an essential manufacturing step.
先ず、本発明に係る積層体の製造方法の第１工程は、フィルムと金属箔とを熱圧着して積層体を形成する限り、従来からの公知の熱圧着工程を使用することができる。例えば、本発明の第１工程で均一な品質の積層体を安定的に得るためには、図１に示すように、光学的異方性の溶融相を形成する液晶ポリマーよりなるフィルム３と金属箔４、４’とを重ね合わせて加圧ロール１、１’の間を通過させることによりフィルム３と金属箔４、４’とを積層する。特に、フィルム３と金属箔４、４’とを加圧ロール１、１’の間に通過させる工程で、加圧ロール１、１’の外部に適宜加熱手段２を設けて、フィルム１、金属箔４、４’及び加圧ロール１、１’を加熱又は保温することが望ましい。 First, the 1st process of the manufacturing method of the laminated body which concerns on this invention can use the conventionally well-known thermocompression bonding process, as long as a film and metal foil are thermocompression-bonded and a laminated body is formed. For example, in order to stably obtain a laminate of uniform quality in the first step of the present invention, as shown in FIG. 1, a film 3 made of a liquid crystal polymer that forms an optically anisotropic molten phase and a metal The film 3 and the metal foils 4, 4 ′ are laminated by overlapping the foils 4, 4 ′ and passing between the pressure rolls 1, 1 ′. In particular, in the step of passing the film 3 and the metal foils 4 and 4 ′ between the pressure rolls 1 and 1 ′, the heating means 2 is appropriately provided outside the pressure rolls 1 and 1 ′, and the film 1 and metal It is desirable to heat or keep the foils 4, 4 ′ and the pressure rolls 1, 1 ′.
フィルム３は、光学的異方性の溶融相を形成する液晶ポリマーからなるものである。光学的異方性の溶融相を形成する液晶ポリマーは、サーモトロピック液晶高分子とも呼ばれている。光学的に異方性を形成する溶融相を形成する高分子は、当業者にはよく知られているように加熱装置を備えた偏光顕微鏡直行ニコル下で溶融状態の試料を観察したときに偏光を透過する高分子である。 The film 3 is made of a liquid crystal polymer that forms an optically anisotropic melt phase. A liquid crystal polymer that forms an optically anisotropic melt phase is also called a thermotropic liquid crystal polymer. As is well known to those skilled in the art, a polymer that forms a melt phase that forms optical anisotropy is polarized when observing a sample in a molten state under a direct microscope with a polarizing microscope equipped with a heating device. Is a polymer that permeates.
フィルム３の液晶ポリマーの原料は、特に限定されるものではないが、以下に例示する（１）〜（４）に分類される化合物およびその誘導体から導かれる公知のサーモトロピック液晶ポリエステル及びポリエステルアミドを挙げることができる。但し、高分子液晶を形成するためには、各々の原料化合物の組合せに適宜な範囲がある。
（１）芳香族又は脂肪族ジヒドロキシ化合物
（２）芳香族又は脂肪族ジカルボン酸
（３）芳香族ヒドロキシカルボン酸
（４）芳香族ジアミン、芳香族ヒドロキシアミンまたは芳香族アミノカルボン酸
The raw material of the liquid crystal polymer of the film 3 is not particularly limited, but known thermotropic liquid crystal polyesters and polyesteramides derived from the compounds (1) to (4) and derivatives thereof exemplified below. Can be mentioned. However, in order to form a polymer liquid crystal, there is an appropriate range for each combination of raw material compounds.
(1) Aromatic or aliphatic dihydroxy compounds (2) Aromatic or aliphatic dicarboxylic acids (3) Aromatic hydroxycarboxylic acids (4) Aromatic diamines, aromatic hydroxyamines or aromatic aminocarboxylic acids
これらの原料化合物から得られる液晶ポリマーの代表例として下記式に示す構造単位を有する共重合体を挙げることができる。 Typical examples of the liquid crystal polymer obtained from these raw material compounds include a copolymer having a structural unit represented by the following formula.
液晶ポリマーフィルムは、耐熱性、加工性の点で、以下の測定法における融点温度が２００〜４００℃、特に２５０〜３５０℃の範囲を有するものが好ましい。ここで、上記の液晶ポリマーフィルムの融点とは、熱圧着に供するフィルムを１０℃／分の昇温速度で加熱した時での示差走査熱量測定法（ＤＳＣ）における融解ピーク温度をいう。尚、フィルムは、フィルムの特性を損なわない範囲で、滑剤、酸化防止剤、充填剤などが配合されていても良い。 The liquid crystal polymer film preferably has a melting point temperature of 200 to 400 ° C., particularly 250 to 350 ° C. in the following measurement methods in terms of heat resistance and workability. Here, melting | fusing point of said liquid crystal polymer film means the melting peak temperature in a differential scanning calorimetry method (DSC) when the film used for thermocompression bonding is heated at the temperature increase rate of 10 degree-C / min. The film may be blended with a lubricant, an antioxidant, a filler and the like as long as the characteristics of the film are not impaired.
液晶ポリマーフィルムは、押出成型して得られる。任意の押出成型法が適用できるが、周知のＴダイ法、ラミネート体延伸法、インフレーション法などが工業的に有利である。特にインフレーション法やラミネート体延伸法では、フィルムの機械軸方向（ＭＤ方向）だけでなく、これと直行する方向（ＴＤ方向）にも応力が加えられるため、ＭＤ方向とＴＤ方向における機械的性質のバランスのとれたフィルムが得られる。 The liquid crystal polymer film is obtained by extrusion molding. Although any extrusion molding method can be applied, the known T-die method, laminate stretching method, inflation method and the like are industrially advantageous. In particular, in the inflation method and the laminate stretching method, stress is applied not only in the mechanical axis direction of the film (MD direction) but also in the direction orthogonal to the film direction (TD direction). A balanced film is obtained.
液晶ポリマーフィルムの好ましい厚み範囲は、５００μｍ以下であり、より好ましくは１０〜２５０μｍ、特に好ましくは１５〜６０μｍである。フィルム厚みが、５００μｍを超えるとフィルムが剛直になりロール状に巻き取ることが困難になるなど取り扱いが困難となる。また、フィルム厚みが、１０μｍに満たないと、フィルムが容易に裂け、取り扱いが困難となる恐れがある。 A preferable thickness range of the liquid crystal polymer film is 500 μm or less, more preferably 10 to 250 μm, and particularly preferably 15 to 60 μm. When the film thickness exceeds 500 μm, the film becomes rigid and difficult to handle, such as being difficult to wind in a roll. On the other hand, if the film thickness is less than 10 μm, the film may be easily torn and difficult to handle.
金属箔４、４’の材質は、本発明において特に制限はない。金、銀、銅、ステンレス、ニッケル、アルミニウムなどが例示される。好ましく用いられる金属箔としては、銅箔、ステンレス箔が挙げられる。銅箔としては、圧延法や電気分解法によって製造されるいずれのものでも使用することができる。金属箔には液晶ポリマーフィルムとの接着力を確保することなどを目的として、粗化処理などの物理的表面処理あるいは酸洗浄などの化学的表面処理を本発明の効果が損なわない範囲で施していても良い。 The material of the metal foil 4, 4 'is not particularly limited in the present invention. Examples include gold, silver, copper, stainless steel, nickel, and aluminum. Examples of metal foils that are preferably used include copper foils and stainless steel foils. As the copper foil, any copper foil manufactured by a rolling method or an electrolysis method can be used. The metal foil is subjected to physical surface treatment such as roughening treatment or chemical surface treatment such as acid cleaning for the purpose of ensuring the adhesive strength with the liquid crystal polymer film, as long as the effect of the present invention is not impaired. May be.
金属箔の好ましい厚さ範囲は、５〜１５０μｍであり、より好ましくは６〜７０μｍ、特に好ましくは９〜１８μｍの範囲である。金属箔の厚みを薄くすることは、ファインパターンを形成可能であるという点からは好ましいが、その厚さが薄くなりすぎると、製造工程で金属箔にしわが生じたりする他、配線基板として回路形成した場合にも配線の破断が生じたり回路基板の信頼性が低下する恐れがある。一方、金属箔の厚みが厚くなると、金属箔をエッチング加工する際、回路側面にテーパーが生じ、ファインパターン形成に不利が生じる。 A preferable thickness range of the metal foil is 5 to 150 μm, more preferably 6 to 70 μm, and particularly preferably 9 to 18 μm. Although it is preferable to reduce the thickness of the metal foil from the point that a fine pattern can be formed, if the thickness is too thin, the metal foil may be wrinkled in the manufacturing process, and a circuit may be formed as a wiring board. In such a case, the wiring may be broken or the reliability of the circuit board may be lowered. On the other hand, when the thickness of the metal foil is increased, the side surface of the circuit is tapered when the metal foil is etched, which is disadvantageous for fine pattern formation.
液晶ポリマーフィルム３と金属箔４、４’との熱圧着は、加圧ロール間１、１’で行われ、通常、一対の加圧ロールが使用される。一対の加圧ロール１、１’は、ゴムロール、金属ロール、樹脂被覆金属ロール等を挙げることができる。加圧ロール１、１’による圧着時の圧力は、幅方向に均一に加圧できる範囲であれば、特に限定されないが、５〜２００ｋＮ／ｍであることが好ましく、１０〜４０ｋＮ／ｍであることがより好ましい。 The thermocompression bonding between the liquid crystal polymer film 3 and the metal foils 4 and 4 ′ is performed between the pressure rolls 1 and 1 ′, and usually a pair of pressure rolls is used. Examples of the pair of pressure rolls 1 and 1 ′ include a rubber roll, a metal roll, and a resin-coated metal roll. Although the pressure at the time of press-bonding by the pressure rolls 1 and 1 ′ is not particularly limited as long as it can be uniformly pressed in the width direction, it is preferably 5 to 200 kN / m, and preferably 10 to 40 kN / m. It is more preferable.
加圧ロールが金属ロールを構成部分として有する場合、その内部を内部加熱手段で加熱することが好ましい。例えば、誘電加熱方式や熱媒循環方式の加熱機構を備えた金属ロール部分を有する加熱・加圧ロールを用いることが好ましい。 When a pressure roll has a metal roll as a component, it is preferable to heat the inside with an internal heating means. For example, it is preferable to use a heating / pressurizing roll having a metal roll portion provided with a heating mechanism of a dielectric heating system or a heat medium circulation system.
本発明の製造方法の第１工程は種々の公知の工程を採用することができる。しかし、図１に示すような以下の特徴のある第１工程を実施することにより、品質的に安定した巻き取り搬送可能な積層体を第２工程へ提供することができる。 Various known processes can be adopted as the first process of the production method of the present invention. However, by carrying out the first step having the following characteristics as shown in FIG. 1, a laminate that can be wound up and transported stably in quality can be provided to the second step.
図１において加熱手段２は、加圧ロール１、１’の全体を覆う加熱ブースである。加熱・加圧ロールの表面は、ロール外部より加熱または保温されることが好ましい。加熱または保温の方法としては、ブース内に加圧ロールを配置する方法が好ましい。 In FIG. 1, the heating means 2 is a heating booth that covers the entire pressure rolls 1, 1 ′. The surface of the heating / pressurizing roll is preferably heated or kept warm from the outside of the roll. As a method of heating or keeping warm, a method of disposing a pressure roll in the booth is preferable.
加熱ブース２の構造は、加圧ロールの全体を囲む密閉構造とし、さらに断熱材で覆われていることが好ましい。ブース内は加熱され、指定した範囲の温度を一定に保つようにすることが好ましい。ブース内の加熱の方法は特に限定されないが、熱風循環ブロアやセラミックヒーターなどが好ましく適用できる。また、ブース内にファンを設置してもよい。金属箔の通紙作業や掃除のために、ブースの一部が開放できる構造が好ましい。 The structure of the heating booth 2 is preferably a sealed structure that surrounds the entire pressure roll and is further covered with a heat insulating material. It is preferable that the inside of the booth is heated so that the temperature within a specified range is kept constant. The heating method in the booth is not particularly limited, but a hot air circulation blower, a ceramic heater, or the like can be preferably applied. Moreover, you may install a fan in a booth. A structure in which a part of the booth can be opened is preferable for the paper passing work and cleaning of the metal foil.
次に、本発明に係る積層体の製造方法の第２工程について、図２に従って説明する。
第１工程での巻き取り搬送可能積層体は、一旦、ロール状に巻き取った後に第２工程に使用しても良く、また第１工程から直接第２工程に適用しても良い。
Next, the 2nd process of the manufacturing method of the laminated body concerning this invention is demonstrated according to FIG.
The laminate that can be wound and conveyed in the first step may be used in the second step after being wound up in a roll, or may be applied directly from the first step to the second step.
本発明では、積層体幅が７０〜１２００ｍｍの範囲が適しており、２００〜６４０ｍｍの範囲がより好ましい。積層体幅が７０ｍｍ未満では、積層体の寸法特性がばらつくことが少なく、第２工程での効果が少ない。一方、積層体幅が１２００ｍｍを超える場合は、ロールなどを含めた設備的な部材の寸法が過大となり、温度制御も難しくなる傾向にある。 In this invention, the range whose laminated body width is 70-1200 mm is suitable, and the range which is 200-640 mm is more preferable. When the laminated body width is less than 70 mm, the dimensional characteristics of the laminated body are less likely to vary, and the effect in the second step is small. On the other hand, when the laminated body width exceeds 1200 mm, the dimensions of equipment members including rolls are excessive, and temperature control tends to be difficult.
図２に示すように、本発明の第２工程は、第１工程の搬送可能な積層体５を、その幅方向（図の紙面の手前から奧方向）をほぼ水平に維持しほぼ水平に架橋搬送させながら、液晶ポリマーの融点より１０℃低い温度以上で加熱処理を行うことが好ましい。また、第２工程の加熱処理温度の上限は、液晶ポリマーの融点より１０℃高い温度以下であることが好ましい。このような加熱処理により、第１工程の加熱ロール間で金属箔との圧着時に生じるポリマーフィルムの張力、その分子の変動、及び表面における加熱に伴い分子配向の変化等が解消し、等方性および寸法安定性の良好な積層板となる。尚、上記融点との関係の温度未満では積層体の加工性が十分でなく、また上記融点との関係の温度を超えると、フィルムに溶融が生じてくるため好ましくない。 As shown in FIG. 2, in the second step of the present invention, the laminate 5 that can be transported in the first step is maintained substantially horizontally in the width direction (from the front side of the drawing to the heel direction) and is bridged almost horizontally. It is preferable to perform the heat treatment at a temperature that is 10 ° C. lower than the melting point of the liquid crystal polymer while being conveyed. Moreover, it is preferable that the upper limit of the heat processing temperature of a 2nd process is below the temperature 10 degreeC higher than melting | fusing point of a liquid crystal polymer. By such heat treatment, the tension of the polymer film generated at the time of pressure bonding with the metal foil between the heating rolls in the first step, the fluctuation of the molecule, and the change in the molecular orientation with the heating on the surface are eliminated, and isotropic And it becomes a laminate with good dimensional stability. If the temperature is lower than the temperature related to the melting point, the processability of the laminate is not sufficient, and if it exceeds the temperature related to the melting point, the film is melted, which is not preferable.
第２工程において、加熱処理の手段は限定されないが、積層体に接触することなく、積層体を精度よく加熱処理することができるという観点から、加熱炉を使用することが好ましい。加熱炉を用いる場合、その種類は特に限定されるものではなく、熱風式加熱炉、熱風循環式加熱炉、赤外線ヒーター式加熱炉などが好ましいものとして例示される。 In the second step, the means for the heat treatment is not limited, but it is preferable to use a heating furnace from the viewpoint that the laminate can be accurately heat-treated without contacting the laminate. When using a heating furnace, the kind is not specifically limited, A hot air type heating furnace, a hot air circulation type heating furnace, an infrared heater type heating furnace, etc. are illustrated as a preferable thing.
本発明における第３工程では、積層体の製品としての耐熱性や均一化等の向上を目的として、上述の第２工程後に加圧加熱処理を行う。この際使用する装置は、加圧雰囲気状態及び加熱状態にできる炉であれば種類は特に限定されるものではなく、バッチ式炉（例えば、東海高熱工業社製ＴＪシリーズ）を用いると、安定した生産性が得られて好ましい。また、加熱方式に関しては、赤外線ヒーター式加熱炉、黒鉛ヒーター式加熱炉、金属線式加熱炉などが好ましいものとして例示される。尚、上記雰囲気状態を形成できるのであれば、バッチ炉でなく、フロー式装置であってもよい。 In the third step of the present invention, pressure heat treatment is performed after the second step for the purpose of improving the heat resistance and uniformity of the laminated product. The apparatus used in this case is not particularly limited as long as it is a furnace that can be in a pressurized atmosphere state and a heated state, and when a batch type furnace (for example, TJ series manufactured by Tokai High Heat Industry Co., Ltd.) is used, the apparatus is stable. Productivity is obtained and preferable. Moreover, regarding a heating system, an infrared heater type heating furnace, a graphite heater type heating furnace, a metal wire type heating furnace, etc. are illustrated as a preferable thing. In addition, as long as the said atmospheric state can be formed, a flow type apparatus may be used instead of a batch furnace.
第３工程で用いる炉は、第２工程で得られた積層体をロール状に巻き取るなどして加圧加熱状態にすることができるものであれば特に制限されるものではないが、炉容積が８〜５００Ｌの範囲が適しており、４０〜３００Ｌの範囲がより好ましい。炉容積が８Ｌ未満では、積層体を入れるには小さすぎる。一方、炉容積５００Ｌを超える場合は、設備的な部材の寸法が過大となり、温度制御も難しくなる傾向にある。 The furnace used in the third step is not particularly limited as long as the laminated body obtained in the second step can be wound into a roll shape, and the like, but is not limited. Is preferably in the range of 8 to 500 L, more preferably in the range of 40 to 300 L. If the furnace volume is less than 8 L, it is too small to contain the laminate. On the other hand, when the furnace volume exceeds 500 L, the size of equipment members is excessive, and temperature control tends to be difficult.
図３に示すように、本発明の第３工程は、例えば、第２工程の搬送可能な積層体５を、金属製のコアに巻き替えた後、ロール状態のまま装置内へ縦に置くことで可能となる。加圧加熱処理時の圧力は、１．５×１０5〜３．０×１０6Ｐａの範囲とすることが必要で、２．０×１０5〜１．５×１０6Ｐａの範囲が好ましい。 As shown in FIG. 3, in the third step of the present invention, for example, after the transportable laminate 5 in the second step is wound around a metal core, it is placed vertically in the apparatus in a roll state. Is possible. The pressure during the pressure heating treatment needs to be in the range of 1.5 × 10 5 to 3.0 × 10 6 Pa, and preferably in the range of 2.0 × 10 5 to 1.5 × 10 6 Pa. .
第３工程では、加熱処理と加圧雰囲気状態とを同時に開始することができ、特に、積層体５を上記圧力範囲で加圧雰囲気状態にした後、その加圧状態を保ったまま加熱処理をすることが好ましい。
この際の加熱処理温度は、液晶ポリマーの融点より３０℃低い温度以上である必要があり、１０〜２５℃低い温度の範囲が適しており、１５〜２０℃低い温度の範囲が好ましい。第３工程の加熱処理温度の上限は、液晶ポリマーの融点より１０℃高い温度以下であることが望ましい。これ以上の温度ではフィルムに溶融が生じる。また、加熱処理温度が液晶ポリマーの融点より３０℃低い温度未満では、積層体の耐熱性、加工性が良くならない。
In the third step, the heat treatment and the pressurized atmosphere state can be started at the same time. In particular, after the laminated body 5 is brought into the pressurized atmosphere state within the above pressure range, the heat treatment is performed while maintaining the pressurized state. It is preferable to do.
The heat treatment temperature in this case needs to be 30 ° C. or more lower than the melting point of the liquid crystal polymer, and a temperature range of 10 to 25 ° C. is suitable, and a temperature range of 15 to 20 ° C. is preferable. The upper limit of the heat treatment temperature in the third step is desirably 10 ° C. or higher than the melting point of the liquid crystal polymer. Above this temperature, the film will melt. On the other hand, if the heat treatment temperature is less than 30 ° C. lower than the melting point of the liquid crystal polymer, the heat resistance and workability of the laminate are not improved.
第３工程での加熱処理時間は６０〜２４０分の範囲が適しており、８０〜２００分の範囲が好ましい。第３工程の加熱処理時間が２４０分を超えるとフィルムに外観不良が生じる恐れがある。また、加熱処理温度が６０分未満では、積層体の耐熱性、加工性が良くならない。 The heat treatment time in the third step is suitably in the range of 60 to 240 minutes, and preferably in the range of 80 to 200 minutes. If the heat treatment time in the third step exceeds 240 minutes, the film may have a poor appearance. Further, when the heat treatment temperature is less than 60 minutes, the heat resistance and workability of the laminate are not improved.
第３工程の加熱処理は不活性ガス雰囲気下で行うのが適しており、窒素ガス雰囲気下で行うのが好ましい。空気中で加熱処理を行った場合、積層体表面が変色してしまう恐れがある。このような加圧加熱処理が行われた後、冷却して圧力を大気圧に戻し、積層体を取り出すことができる。 The heat treatment in the third step is suitably performed in an inert gas atmosphere, and is preferably performed in a nitrogen gas atmosphere. When heat treatment is performed in air, the surface of the laminate may be discolored. After such pressure heat treatment is performed, the laminate can be taken out by cooling to return the pressure to atmospheric pressure.
本発明の製造方法によって得られる積層体は、フクレのない良好な外観を有し、絶縁フィルム層が液晶ポリマーの有する、優れた機械的強度、電気特性及び耐熱性を保持しており、しかも該フィルム層が金属箔と常温条件下のみならず高温条件下においても強固に接着している。このため、ＦＰＣ、ＴＡＢ用テープ等を製造するための材料として有用である。 The laminate obtained by the production method of the present invention has a good appearance without blisters, and the insulating film layer has excellent mechanical strength, electrical properties and heat resistance possessed by the liquid crystal polymer, and The film layer is firmly bonded to the metal foil not only at room temperature but also at high temperature. Therefore, it is useful as a material for producing FPC, TAB tape and the like.
以上の最良の実施形態では積層体を１つの液晶ポリマーフィルムと１又は２つの金属箔との構造としている。しかしながら、本発明にあって製造される積層体は、少なくとも１層の液晶ポリマーフィルムと少なくとも２層の金属箔を含むものであればよく、例えば、下記Ｉ）に示した３層構造、ＩＩ）の４層構造、ＩＩＩ）の５層構造などを例示することができる。 In the above-mentioned best embodiment, the laminated body has a structure of one liquid crystal polymer film and one or two metal foils. However, the laminate produced in the present invention may be any layer as long as it includes at least one liquid crystal polymer film and at least two metal foils. For example, the three-layer structure shown in the following I), II) 4 layer structure, III) 5 layer structure, etc. can be illustrated.
Ｉ）金属箔／フィルム／金属箔
ＩＩ）金属箔／フィルム／フィルム／金属箔
ＩＩＩ）金属箔／フィルム／金属箔／フィルム／金属箔
I) Metal foil / film / metal foil II) Metal foil / film / film / metal foil III) Metal foil / film / metal foil / film / metal foil
以下、実施例によって本発明を具体的に説明するが、本発明はこれらの実施例によって何ら限定されるものではない。なお、実施例において得られた積層体の評価は以下の方法による。 EXAMPLES Hereinafter, although an Example demonstrates this invention concretely, this invention is not limited at all by these Examples. In addition, evaluation of the laminated body obtained in the Example is based on the following method.
＜積層体の評価方法＞
（１）外観：液晶ポリマーフィルムと金属箔とを圧着した積層体を目視により観察し、外観不良（フクレ）の有無を調べた。幅３４０ｍｍ、長さ４０ｍの積層体を作成し、同積層体中に目視可能なフクレが１つでもある場合を。フクレありと判断した。
（２）融点：示差走査熱量計（ＤＳＣ）を用いて、昇温速度１０℃／ｍｉｎで３６０℃まで昇温した際に観察される吸熱ピークの値をいう。
（３）熱変形開始温度：ＴＭＡ法（引張荷重５ｇ）にて測定した。
<Method for evaluating laminate>
(1) Appearance: A laminate obtained by press-bonding a liquid crystal polymer film and a metal foil was observed with the naked eye, and the presence or absence of an appearance defect (inflation) was examined. A case where a laminated body having a width of 340 mm and a length of 40 m is prepared, and there is at least one visible bulge in the laminated body. Judged that there was a bulge.
(2) Melting point: Refers to the value of the endothermic peak observed when the temperature is raised to 360 ° C. at a rate of temperature rise of 10 ° C./min using a differential scanning calorimeter (DSC).
(3) Thermal deformation start temperature: Measured by TMA method (tensile load 5 g).
（実施例１）
厚さ２５μｍの液晶ポリマーフィルム（商品名ベクスター、融点２８０℃）の両面に９μｍの厚みの電解銅箔を重ね合わせ、重ね合わせると同時に一対の加圧ロール間に１ｍ／分で連続的に供給した。ロール表面は、ロール内部の加熱機構により２６０℃に加熱した。加熱・加圧ロールはブース内に配置し、ブースは熱風循環ブロアにより２１０〜２１５℃に加熱した。
(Example 1)
A 9 μm thick electrolytic copper foil was superposed on both sides of a liquid crystal polymer film (trade name Bexter, melting point 280 ° C.) having a thickness of 25 μm and simultaneously supplied at a rate of 1 m / min between a pair of pressure rolls. . The roll surface was heated to 260 ° C. by a heating mechanism inside the roll. The heating / pressurizing roll was placed in a booth, and the booth was heated to 210 to 215 ° C. by a hot air circulation blower.
続く第２工程において、積層体を熱風式加熱炉により加熱処理を行った。この際、加熱処理は、熱風式加熱炉内を９６秒間通過させることで行ったが、炉内最高温度領域を液晶ポリマーの融点より１０℃低い温度とし、２．５ｍ／分で連続的に処理した。 In the subsequent second step, the laminate was subjected to a heat treatment using a hot air heating furnace. At this time, the heat treatment was performed by passing through the hot-air heating furnace for 96 seconds. The maximum temperature region in the furnace was 10 ° C. lower than the melting point of the liquid crystal polymer, and the treatment was continuously performed at 2.5 m / min. did.
続く第３工程において、窒素雰囲気の加熱炉中にロール状にした積層体を静置して加熱処理を行った。この際、加熱前に炉内窒素圧力を９．６×１０5Ｐａに設定し、設定圧力到達後に加圧状態を維持したまま加熱処理を行った。加熱処理は加熱炉内設置のヒーター温度を２６３℃に設定し、設定温度到達後にその温度を３時間保持し熱処理を施した。なお、液晶ポリマーフィルムと電解銅箔には、ロール状のものを原料とし、第１工程と第２工程をロール・ツウ・ロール方式で連続的に製造し、第３工程をバッチ式で製造した。得られた積層体の評価結果を表１に示す。 In the subsequent third step, the roll-shaped laminate was placed in a heating furnace in a nitrogen atmosphere and subjected to heat treatment. At this time, the nitrogen pressure in the furnace was set to 9.6 × 10 5 Pa before heating, and heat treatment was performed while maintaining the pressurized state after reaching the set pressure. In the heat treatment, the heater temperature installed in the heating furnace was set to 263 ° C., and after reaching the set temperature, the temperature was maintained for 3 hours and subjected to heat treatment. In addition, the liquid crystal polymer film and the electrolytic copper foil are made of a roll-shaped material, the first step and the second step are continuously manufactured by a roll-to-roll method, and the third step is manufactured by a batch method. . The evaluation results of the obtained laminate are shown in Table 1.
（比較例１）
実施例１と同様にして、第１工程を経た積層体とし、続く第２工程において、積層体を熱風式加熱炉により加熱処理を行った。
続く第３工程において、炉内窒素圧力を１．０×１０5Ｐａ（ほぼ１気圧）に設定したこと以外は実施例１と同様に行った。
(Comparative Example 1)
In the same manner as in Example 1, the laminated body was subjected to the first step, and in the subsequent second step, the laminated body was subjected to heat treatment using a hot air heating furnace.
In the subsequent third step, the same procedure as in Example 1 was performed except that the furnace nitrogen pressure was set to 1.0 × 10 5 Pa (approximately 1 atm).
（実施例２）
実施例１と同様にして、第１工程を経た積層体とし、続く第２工程において、積層体を熱風式加熱炉により加熱処理を行った。
続く第３工程において、炉内窒素圧力を２．０×１０5Ｐａに設定したこと以外は実施例１と同様に行った。
(Example 2)
In the same manner as in Example 1, the laminated body was subjected to the first step, and in the subsequent second step, the laminated body was subjected to heat treatment using a hot air heating furnace.
In the 3rd process which followed, it carried out like Example 1 except having set the nitrogen pressure in a furnace to 2.0 * 10 < 5 > Pa.
（実施例３）
実施例１と同様にして、第１工程を経た積層体とし、続く第２工程において、積層体を熱風式加熱炉により加熱処理を行った。
続く第３工程において、炉内窒素圧力を５．０×１０5Ｐａに設定したこと以外は実施例１と同様に行った。
(Example 3)
In the same manner as in Example 1, the laminated body was subjected to the first step, and in the subsequent second step, the laminated body was subjected to heat treatment using a hot air heating furnace.
In the 3rd process which followed, it carried out like Example 1 except having set the nitrogen pressure in a furnace to 5.0x10 < 5 > Pa.
本発明は積層体の製造方法は、高い寸法安定性の要求される回路基板用金属張積層板に好適に使用される積層体を、その製造工程における外観不良発生を抑えて安定的に製造できる産業上の利用可能性が高いものである。 According to the present invention, a laminate manufacturing method can stably manufacture a laminate suitably used for a metal-clad laminate for a circuit board that requires high dimensional stability while suppressing occurrence of appearance defects in the manufacturing process. The industrial applicability is high.
１、１’・・・加圧ロール
２・・・・・・加熱ブース（加熱手段）
３・・・・・・フィルム
４、４’・・・金属箔
５・・・・・・積層体
６・・・・・・架橋ロール
７・・・・・・加熱炉
８・・・・・・（ロール化）積層体
９・・・・・・ヒーター（加熱手段）
１０・・・・・加圧加熱炉
1, 1 '... pressure roll 2 ... heating booth (heating means)
3 ... Film 4, 4 '... Metal foil 5 ... Laminate 6 ... Crosslinking roll 7 ... Heating furnace 8 ...・ (Rolled) Laminate 9 ... Heater (heating means)
10 ... Pressure furnace
Claims (6)
第１工程で該液晶ポリマーフィルムと該金属箔とを熱圧着して形成した搬送可能な積層体を、第２工程で搬送させながら加熱処理を行った後、第３工程で加圧雰囲気状態及び加熱状態にする炉又は装置を用いて、圧力を１．５×１０5〜３．０×１０6Ｐａの範囲にすると共に加熱温度を該液晶ポリマーの融点より３０℃低い温度以上にして処理を行うことを特徴とする積層体の製造方法。 In a method for producing a laminate having a metal foil on both sides of a liquid crystal polymer film,
The transportable laminate formed by thermocompression bonding the liquid crystal polymer film and the metal foil in the first step is subjected to heat treatment while being transported in the second step, and then in the pressurized atmosphere state and in the third step. Using a furnace or apparatus to be heated, the pressure is set in the range of 1.5 × 10 5 to 3.0 × 10 6 Pa and the heating temperature is set to 30 ° C. lower than the melting point of the liquid crystal polymer. A method for producing a laminate, which is performed.
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| JP2007071762A JP2008229995A (en) | 2007-03-20 | 2007-03-20 | Manufacturing method of laminate |
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| JP2007071762A JP2008229995A (en) | 2007-03-20 | 2007-03-20 | Manufacturing method of laminate |
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| JP2016107507A (en) * | 2014-12-05 | 2016-06-20 | 株式会社クラレ | Metal-clad laminated sheet and method for producing the same |
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- 2007-03-20 JP JP2007071762A patent/JP2008229995A/en not_active Withdrawn
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| JP2016107507A (en) * | 2014-12-05 | 2016-06-20 | 株式会社クラレ | Metal-clad laminated sheet and method for producing the same |
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| WO2016170779A1 (en) * | 2015-04-20 | 2016-10-27 | 株式会社クラレ | Metal-clad laminate sheet manufacturing method, and metal-clad laminate sheet using same |
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| JPWO2017154811A1 (en) * | 2016-03-08 | 2019-01-31 | 株式会社クラレ | Method for producing metal-clad laminate and metal-clad laminate |
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| WO2017154811A1 (en) * | 2016-03-08 | 2017-09-14 | 株式会社クラレ | Method for producing metal-clad laminate, and metal-clad laminate |
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| CN113844149A (en) * | 2020-06-27 | 2021-12-28 | 普洛梅特库株式会社 | Method for producing laminate |
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