JP5218842B2 - Manufacturing method of jig for evaluation of plating smoothness - Google Patents
Manufacturing method of jig for evaluation of plating smoothness Download PDFInfo
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本発明は、めっき液の平滑化能力、特にフレキシブル配線用基板用めっき液の平滑化能力を評価するために用いる評価用冶具と、その評価用冶具の製造方法に関するものである。 The present invention relates to an evaluation jig used for evaluating the smoothing ability of a plating solution, in particular, the smoothing ability of a plating solution for a flexible wiring board, and a method for producing the evaluation jig.
フレキシブル配線基板（ＦＰＣとも称される）は、折り曲げ性が良いためハードディスクの読み書きヘッドやプリンターヘッド、デジタルカメラ内の屈折配線板用などとして広く用いられている。 A flexible wiring board (also referred to as FPC) is widely used as a read / write head for a hard disk, a printer head, a refractive wiring board in a digital camera, and the like because of its good bendability.
通常、フレキシブル配線基板には、基板表面が平滑であることが要求されている。そこで、基板の表面を形成するめっき層を如何に平坦に仕上げるかが重視され、平滑化能力（平滑性）を重視しためっき液の開発が行われている。 Usually, a flexible wiring board is required to have a smooth substrate surface. Therefore, emphasis is placed on how to flatten the plating layer forming the surface of the substrate, and a plating solution has been developed with an emphasis on smoothing ability (smoothness).
例えば、セラミック電子部品のめっき用浴用ではあるが、めっき成長を極力抑制することができ、かつ良好な平滑性を有するニッケル皮膜と良好なアノード溶解性を有するニッケルめっき液を得るために、ニッケルめっき液が、硫酸ニッケルを主成分とするニッケル塩と塩化ニッケル等のハロゲン化合物とホウ酸等のｐＨ緩衝剤とを含有し、ｐＨが２．２〜５．５に調整され、かつニッケルイオンのモル濃度ｘが１．７１ｍｏｌ／Ｌ以上であって、ニッケルイオンのモル濃度ｘとハロゲンイオンのモル濃度ｙとのモル濃度比ｘ／ｙが３．０＜ｘ／ｙ≦１０．０としたニッケルめっき液を提案している（例えば、特許文献１参照）。 For example, in order to obtain a nickel plating solution that can suppress plating growth as much as possible, and has good smoothness and good anodic solubility, although it is used for a plating bath for ceramic electronic parts. The liquid contains a nickel salt mainly composed of nickel sulfate, a halogen compound such as nickel chloride, and a pH buffer such as boric acid, the pH is adjusted to 2.2 to 5.5, and the molarity of nickel ions Nickel plating in which the concentration x is 1.71 mol / L or more and the molar concentration ratio x / y between the molar concentration x of nickel ions and the molar concentration y of halogen ions is 3.0 <x / y ≦ 10.0 The liquid is proposed (for example, refer patent document 1).
ところで、フレキシブル配線基板に使用される絶縁性フィルムは、ポリイミドフィルムが一般的に用いられるようになってきている。このポリイミドフィルムの表面に乾式めっき法で下地層を設け、この下地層に電気めっき法により平滑なめっき層を設け、パターニングしてめっき層を配線層に加工し、必要であれば配線層の該当部に金めっき等を施してフレキシブル配線基板が作製される。 By the way, as the insulating film used for the flexible wiring board, a polyimide film is generally used. A base layer is provided on the surface of this polyimide film by a dry plating method, a smooth plating layer is provided on the base layer by an electroplating method, and the plating layer is processed into a wiring layer by patterning. A flexible wiring board is produced by applying gold plating or the like to the part.
近年、このようなフレキシブル配線基板においても高密度化、高集積化が求められ、そのため、ポリイミドフィルム表面に設けられるめっき層は、その厚みが１０μｍに満たない薄さを要求されてきている。また、設ける配線幅も２５μｍに満たない幅のものが求められてきている。こうした状況において、めっき層表面の平滑度も１μｍ以下のオーダーで形成すべき重要なファクターとなってきている。
一方、通常ポリイミドフィルムの表面をμｍのオーダーで捉えた場合、決して平滑とは言えず、多数の数μｍオーダーでの凹凸が存在している。
On the other hand, when the surface of a polyimide film is usually captured on the order of μm, it cannot be said that the surface is smooth, and there are many irregularities on the order of several μm.
このような数μｍオーダーでの凹凸を有するポリイミドフィルムに、めっき層を設けて平坦な表面とする場合には、従来、乾式めっき法を用いて形成される下地層では、その厚みが極めて薄いためにポリイミドフィルムの表面凹凸を軽減することはできず、通常、その下地層の上に電気めっき法などを用いて、より厚みのあるめっき層を設けることで、ポリイミドフィルムの表面凹凸を解消し、平坦且つ平滑な表面を得ようとしている。 In the case of providing a flat surface by providing a plating layer on such a polyimide film having irregularities on the order of several μm, the thickness of an underlayer conventionally formed using a dry plating method is extremely thin. The surface unevenness of the polyimide film cannot be reduced, and usually by using an electroplating method or the like on the underlying layer, the surface unevenness of the polyimide film is eliminated by providing a thicker plating layer, We are trying to obtain a flat and smooth surface.
このため、下地層の上に設けるめっき層の形成時に、数μｍオーダーの表面凹凸を解消して、厚み１０μｍ程度において平滑な表面が得られるめっき層、即ちめっき液かどうかを事前に評価することができれば、操業上極めて有用であり、生産性の向上に大きく寄与する。 For this reason, when forming the plating layer provided on the underlayer, it is necessary to evaluate in advance whether the plating layer is a plating layer that eliminates surface irregularities on the order of several μm and obtains a smooth surface at a thickness of about 10 μm, that is, a plating solution. If it is possible, it will be extremely useful in operation and will greatly contribute to the improvement of productivity.
従来、めっき層の平滑性評価に用いられる方法には、基板に傷をつけてその上からめっきを行い、めっき層表面の平滑性を調べる方法が採られている。
しかしながら、この基板表面に傷をつけてめっきする方法では、実際の基板表面である数μｍオーダーの微細な凹凸を均一に再現することは困難であるため、めっき液の平滑性を比較する方法としては不適当である。
Conventionally, as a method used for evaluating the smoothness of a plating layer, a method has been adopted in which a substrate is scratched and plated from above to examine the smoothness of the surface of the plating layer.
However, in this method of plating with scratches on the substrate surface, it is difficult to uniformly reproduce the fine irregularities of the order of several μm, which is the actual substrate surface, so as a method for comparing the smoothness of the plating solutions Is inappropriate.
本発明はこのような状況に鑑みなされたものであり、数μｍ程度の凹凸を有する表面に厚み１０μｍ程度のめっき層を設けた場合に、得られるめっき層表面が平滑かどうかを判断しうる評価用冶具及びその製造方法の提供を目的とする。 This invention is made | formed in view of such a condition, and when the plating layer about 10 micrometers thick is provided in the surface which has an unevenness | corrugation about several micrometers, the evaluation which can judge whether the plating layer surface obtained is smooth It is intended to provide a jig for use and a manufacturing method thereof.
このような課題を解決する本発明の第１の発明は、めっき平滑性を評価するための評価用冶具の製造方法であって、その評価用冶具は表面に凹凸形状部を備える基板材料からなり、基板材料の表面に備わる凹凸形状部が、高さが１〜３μｍの凸形状部、あるいは深さが１〜３μｍの凹形状部であり、その凹凸形状部は、ナノインプリント法により形成されることを特徴とする評価用冶具の製造方法である。
なお、ナノインプリント法とは、ハンコを押すように、テンプレートを基板に押し当てることでナノオーダの微細加工を実現する技術である。
A first invention of the present invention that solves such a problem is a method of manufacturing an evaluation jig for evaluating plating smoothness, and the evaluation jig is made of a substrate material having a concavo-convex shape portion on the surface. The uneven shape portion provided on the surface of the substrate material is a convex shape portion having a height of 1 to 3 μm or a concave shape portion having a depth of 1 to 3 μm, and the uneven shape portion is formed by a nanoimprint method. This is a method for manufacturing an evaluation jig.
The nanoimprint method is a technology that realizes nano-order microfabrication by pressing a template against a substrate like pressing a hammer.
本発明の第２の発明は、めっき平滑性を評価するための評価用冶具の製造方法であって、この評価用冶具は表面に凹凸形状部を備える基板材料からなり、その凹凸形状部が、高さが１〜３μｍ、径が２〜２０μｍの凸形状部、あるいは深さが１〜３μｍ、径が２〜２０μｍの凹形状部であり、その凹凸形状部が、ナノインプリント法により形成したことを特徴とする評価用冶具の製造方法である。 2nd invention of this invention is a manufacturing method of the jig for evaluation for evaluating plating smoothness, Comprising : This jig for evaluation consists of a substrate material provided with an uneven shape part on the surface, The uneven shape part is height 1 to 3 [mu] m, diameter of concave portion convex portion or depth 1 to 3 [mu] m, diameter of 2 to 20 [mu] m of 2 to 20 [mu] m, that the concave-convex part is formed by nanoimprinting It is the manufacturing method of the jig for evaluation characterized.
更に、凸形状部または凹形状部の横断面は円、楕円、長円、多角形であり、また、その基板材料は熱可塑性の絶縁性樹脂フィルムが用いられる。 Furthermore, the cross section of the convex or concave portion is a circle, an ellipse, an ellipse, or a polygon, and a thermoplastic insulating resin film is used as the substrate material.
本発明において使用するフィルムは特に限定されないが、具体的にはポリエチレン、ポリプロピレン、ポリスチレン、ポリビニルアルコール、ポリエチレンテレフタレート、ポリブチレンテレフタレート、ポリ塩化ビニール、ＡＢＳ樹脂、ＰＭＭＡ樹脂、ＡＳ樹脂、ＣＯＣ樹脂、ＣＯＰ樹脂、アクリル樹脂、ポリアミド、ポリ塩化ビニリデン、ポリカーボネート、ポリエーテルイミド等の熱可塑性樹脂を用いることを特徴とするものである。 Although the film used in the present invention is not particularly limited, specifically, polyethylene, polypropylene, polystyrene, polyvinyl alcohol, polyethylene terephthalate, polybutylene terephthalate, polyvinyl chloride, ABS resin, PMMA resin, AS resin, COC resin, COP resin In addition, a thermoplastic resin such as an acrylic resin, polyamide, polyvinylidene chloride, polycarbonate, or polyetherimide is used.
本発明のめっき平滑性の評価用冶具は、フレキシブル配線用基板、特に従来から使用される絶縁性ポリイミドフィルム基板の表面を模擬した条件における、めっき層を形成するめっき液の平滑性を簡便に評価することで、使用するめっき液の適否の判定ばかりでなく、使用しているめっき液の平滑剤濃度の調整にも用いることができ、更にめっき液の添加成分によるめっき析出状態の微妙な変化を比較して有用なめっき液の提供を可能とするものである。 The plating smoothness evaluation jig of the present invention simply evaluates the smoothness of a plating solution for forming a plating layer under conditions simulating the surface of a flexible wiring substrate, particularly a conventionally used insulating polyimide film substrate. As a result, it can be used not only to determine the suitability of the plating solution used, but also to adjust the concentration of the smoothing agent in the plating solution being used. In comparison, it is possible to provide a useful plating solution.
以下に図を用いて、本発明のめっき液の平滑化能力を判定するための評価用冶具を詳細に説明する。
図１及び２は、本発明の評価用冶具の一実施例を示す図で、（ａ）は外観斜視図、（ｂ）はａ−ａ線断面図及びｂ−ｂ線断面図、（ｃ）は凹凸形状部を説明する拡大模式図である。
図３は、本発明の評価用冶具の製造方法を説明する図で、（ａ）、（ｂ）、（ｃ）の順に工程が進んで行き、（ｄ）に模式平面図で示す評価用冶具が作製される。
図１、２及び３において、１は評価用冶具、２は基板、３ａ、３ｂはそれぞれ凸形状部、凹形状部、１０は金型、１１は金型凸部、１２は金型凹部、ｈは凹凸形状部の高さ、Ｌは凹凸形状部の径である。
The evaluation jig for determining the smoothing ability of the plating solution of the present invention will be described below in detail with reference to the drawings.
1 and 2 are views showing an embodiment of an evaluation jig according to the present invention, wherein (a) is an external perspective view, (b) is a cross-sectional view taken along line aa and bb, and (c). These are the expansion schematic diagrams explaining an uneven | corrugated shaped part.
FIG. 3 is a diagram for explaining a method for manufacturing an evaluation jig according to the present invention, in which the steps proceed in the order of (a), (b), and (c), and the evaluation jig shown in a schematic plan view in (d). Is produced.
1, 2 and 3, 1 is an evaluation jig, 2 is a substrate, 3 a and 3 b are convex portions, concave portions, 10 is a mold, 11 is a mold convex portion, 12 is a mold concave portion, h Is the height of the uneven portion, and L is the diameter of the uneven portion.
図１及び２（ａ）、（ｂ）の実施例に示すように、本発明の評価用冶具は、凹形状部のみ、凸形状部のみ、或いは凹、凸形状部の両者を、本発明で規定する大きさで基板２の表面に備えたものである。 As shown in the examples of FIGS. 1 and 2 (a) and 2 (b), the evaluation jig according to the present invention has only a concave portion, only a convex portion, or both concave and convex portions. It is provided on the surface of the substrate 2 in a prescribed size.
形成する凹凸形状部の大きさは、実際のポリイミドフィルム基板の表面状態に近づけるために、図１及び２の（ｃ）に示すように、高さｈ（或いは深さｈ）は、１μｍから３μｍが良い。又、凹凸形状部の横断面形状である円、楕円、長円、多角形の径Ｌ、即ち円では直径、楕円では長径、四角形を除く多角形では外接円の直径で、２μｍから２０μｍが望ましく、四角形では短辺の長さ（所謂、幅）で、２０μｍ以下が望ましい。 The size of the concavo-convex shape portion to be formed is close to the actual surface state of the polyimide film substrate, so that the height h (or depth h) is 1 μm to 3 μm, as shown in FIGS. Is good. In addition, the diameter L of the circle, ellipse, ellipse, and polygon, which is the cross-sectional shape of the concavo-convex shape portion, is preferably 2 to 20 μm as the diameter of the circle, the long diameter as the ellipse, and the diameter of the circumscribed circle as the polygon excluding the rectangle In the case of a square, the length of the short side (so-called width) is preferably 20 μm or less.
基板２には、凹凸形状部を形成し易い樹脂フィルム、特に熱可塑性樹脂が望ましく、具体的にはポリエチレン、ポリプロピレン、ポリスチレン、ポリビニルアルコール、ポリエチレンテレフタレート、ポリブチレンテレフタレート、ポリ塩化ビニール、ＡＢＳ樹脂、ＰＭＭＡ樹脂、ＡＳ樹脂、ＣＯＣ樹脂、ＣＯＰ樹脂、アクリル樹脂、ポリアミド、ポリ塩化ビニリデン、ポリカーボネート、ポリエーテルイミド等の熱可塑性樹脂が好適である。 The substrate 2 is preferably a resin film that can easily form a concavo-convex shape, particularly a thermoplastic resin. Specifically, polyethylene, polypropylene, polystyrene, polyvinyl alcohol, polyethylene terephthalate, polybutylene terephthalate, polyvinyl chloride, ABS resin, PMMA A thermoplastic resin such as resin, AS resin, COC resin, COP resin, acrylic resin, polyamide, polyvinylidene chloride, polycarbonate, or polyetherimide is preferable.
めっきの平滑性の評価は、平滑性の最も良い状態では、基板表面の凹凸がめっきすることで、その凹凸が解消し平滑な状態になることで、その表面を走査電子顕微鏡（ＳＥＭ）或いは高倍率の光学顕微鏡による観察で評価する。また、凸部や凹部におけるめっきの析出状態がどのように変化するかについても、めっき層断面を観察することで情報が得られ、めっき液の選定が容易にできる。 The smoothness of the plating is evaluated by plating the unevenness of the substrate surface in a state where the smoothness is the best so that the unevenness is eliminated and becomes a smooth state, so that the surface can be scanned with a scanning electron microscope (SEM) or high Evaluation is carried out by observation with a magnification optical microscope. In addition, information on how the deposition state of the plating in the convex part and the concave part changes can be obtained by observing the cross section of the plating layer, and the plating solution can be easily selected.
本発明の評価用冶具の製造方法は、図３に製造工程の概略を示すナノインプリント法を用いると簡便に精度良く作製できる。
図３は、本発明の評価用冶具のナノインプリント法による製造方法の概略を示す模式図で、評価用冶具は、図３（ａ）、（ｂ）、（ｃ）の順に工程を踏んで、図３（ｄ）の模式平面図に示す評価用冶具１が作製される。図３において、１は評価用冶具、２は基板、３ｂは凹形状部、１０は金型である。
The evaluation jig manufacturing method of the present invention can be easily and accurately manufactured by using the nanoimprint method shown in FIG.
FIG. 3 is a schematic diagram showing an outline of a method for producing the evaluation jig of the present invention by the nanoimprint method. The evaluation jig follows the steps in the order of FIGS. 3 (a), (b), and (c). The evaluation jig 1 shown in the schematic plan view of 3 (d) is produced. In FIG. 3, 1 is an evaluation jig, 2 is a substrate, 3b is a concave portion, and 10 is a mold.
基板２に所定の凹形状部３ｂを作製できるような凸部１１を持つ金型１０と基板２をプレス成形機（図示せず）の所定位置に配置（図３（ａ））し、金型１０を基板２に押し当て、所定条件で圧縮、加熱、保持して基板２表面に凹形状部３ｂを形成する（図３（ｂ））、保持終了後、基板２から金型１０を離反（図３（ｃ））して評価用冶具１（図３（ｄ））が作製される。
この作製した評価用冶具１にスパッタ法などで、厚み０．１μｍ程度のＣｕの下地層を形成して評価試験に供される。
A mold 10 having a convex portion 11 capable of producing a predetermined concave shape portion 3b on the substrate 2 and the substrate 2 are arranged at predetermined positions of a press molding machine (not shown) (FIG. 3A), and the mold 10 is pressed against the substrate 2 and compressed, heated, and held under predetermined conditions to form a concave portion 3b on the surface of the substrate 2 (FIG. 3B). After the holding, the mold 10 is separated from the substrate 2 ( 3 (c)), the evaluation jig 1 (FIG. 3 (d)) is manufactured.
A Cu underlayer having a thickness of about 0.1 μm is formed on the produced evaluation jig 1 by a sputtering method or the like and used for an evaluation test.
以下、実施例を用いて、本発明をより詳細に説明する。
（実施例１）
基板として厚み１００μｍのＣＯＰ樹脂（シクロオレフィンポリマー）を用い、その表面に径１０μｍ、深さ２μｍの横断面が円形の凸形状部を形成する金型を用いて、プレス圧５ｔ／ｃｍ２で温度１６０℃で加熱しながら１０分間保持して凸形状部３ａを備える図４（ａ）に示すＣＯＰ樹脂基板の評価用冶具１を作製した。
Hereinafter, the present invention will be described in more detail with reference to examples.
Example 1
A COP resin (cycloolefin polymer) having a thickness of 100 μm is used as a substrate, and a die having a diameter of 10 μm and a depth of 2 μm having a circular cross-section is formed on the surface, and the pressure is 5 t / cm 2 and the temperature is increased. The jig 1 for evaluation of the COP resin substrate shown in FIG. 4 (a) provided with the convex portion 3a while being heated at 160 ° C. for 10 minutes was produced.
次に、この評価用冶具を用いて、銅めっき液の評価試験を行った。
先ず、この評価用冶具にスパッタ装置を用いて厚み０．１μｍのＣｕの下地層を形成して、評価試験に供した。
評価試験は、この評価用冶具の表面に電気めっき法により銅めっきを施し、その銅めっき層の表面状態を観察して評価した。
銅めっきは、硫酸銅９０ｇ／ｌ、硫酸１８０ｇ／ｌ、塩素５０ｐｐｍ、０．３ｇ／ｌのＰＥＧ（Ｐｏｌｙｅｔｈｙｌｅｎｅ Ｇｌｙｃｏｌ：ポリエチレングリコール）、０．５ｐｐｍのＳＰＳ（Ｂｉｓ（３‐ｓｕｌｆｏｐｒｏｐｙｌ）ｄｉｓｕｌｆｉｄｅ ：ビス（３‐スルホプロピル）ジスルフィド）、そして平滑性を向上させる添加剤として、１ｐｐｍのＪＧＢ（Ｊａｎｕｓ Ｇｒｅｅｎ Ｂ：ヤヌスグリーンＢ）、又は１ｐｐｍのチオ尿素を添加した銅めっき液を用い、浴温２５℃、電流密度２Ａ／ｄｍ２で行った。
Next, an evaluation test of a copper plating solution was performed using this evaluation jig.
First, a 0.1 μm-thick Cu underlayer was formed on this evaluation jig using a sputtering apparatus and subjected to an evaluation test.
In the evaluation test, the surface of this evaluation jig was subjected to copper plating by an electroplating method, and the surface state of the copper plating layer was observed and evaluated.
Copper plating is copper sulfate 90 g / l, sulfuric acid 180 g / l, chlorine 50 ppm, 0.3 g / l PEG (Polyethylene Glycol: polyethylene glycol), 0.5 ppm SPS (Bis (3-sulfopropyl) disulphide: screw (3 -Sulfopropyl) disulfide), and a copper plating solution containing 1 ppm JGB (Janus Green B) or 1 ppm thiourea as an additive for improving smoothness, bath temperature of 25 ° C., current It was carried out at a density 2A / dm 2.
銅めっき後、評価用冶具の表面状態をＳＥＭ観察した結果を図５（ａ）−（１）及び図６（ａ）−（１）に示す。
表面を観察した図５（ａ）−（２），（３）から、添加剤の種類による平滑性の微妙な差を見分けられる。また、断面を観察した図６（ａ）−（２），（３）から、表面の凹凸に対して添加剤の種類によってＣｕの析出の仕方が異なることが判る。
The results of SEM observation of the surface state of the evaluation jig after copper plating are shown in FIGS. 5 (a)-(1) and 6 (a)-(1).
From FIGS. 5 (a)-(2) and (3), which observe the surface, it is possible to distinguish a subtle difference in smoothness depending on the type of additive. Moreover, it can be seen from FIGS. 6 (a)-(2) and (3) in which the cross section is observed that the manner of precipitation of Cu differs depending on the type of additive with respect to the surface irregularities.
（実施例２）
基板として厚み１００μｍのポリエチレンテレフタレート（ＰＥＴ）フィルムを用い、その表面に径５μｍ、高さ２μｍの横断面が円形の凹部形状部を形成する金型を用いて、プレス圧５ｔ／ｃｍ２、１６０℃の温度に１０分間保持して凹形状部３ｂを備える図４（ｂ）に示すＰＥＴフィルム基板の評価用冶具１を作製した。
(Example 2)
A polyethylene terephthalate (PET) film having a thickness of 100μm as a substrate, the diameter 5μm on the surface, using a mold cross section of the height 2μm to form a circular recess-shaped portion, a press pressure 5t / cm 2, 160 ℃ An evaluation jig 1 for a PET film substrate shown in FIG. 4B, which was held at the temperature of 10 minutes and was provided with a concave portion 3b, was produced.
次に、この評価用冶具を用いて、銅めっき液の評価試験を行った。
先ず、この評価用冶具にスパッタ装置を用いて厚み０．１μｍのＣｕの下地層を形成して、評価試験に供した。
評価試験は、この評価用冶具の表面に電気めっき法により銅めっきを施し、その銅めっき層の表面状態を観察して評価した。
銅めっきは、硫酸銅９０ｇ／ｌ、硫酸１８０ｇ／ｌ、塩素５０ｐｐｍ、０．３ｇ／ｌのＰＥＧ（Ｐｏｌｙｅｔｈｙｌｅｎｅ Ｇｌｙｃｏｌ：ポリエチレングリコール）、０．５ｐｐｍのＳＰＳ（Ｂｉｓ（３‐ｓｕｌｆｏｐｒｏｐｙｌ）ｄｉｓｕｌｆｉｄｅ ：ビス（３‐スルホプロピル）ジスルフィド）、そして平滑性を向上させる添加剤として、１ｐｐｍのＪＧＢ（Ｊａｎｕｓ Ｇｒｅｅｎ Ｂ：ヤヌスグリーンＢ）、又は１ｐｐｍのチオ尿素を添加した銅めっき液を用い、浴温２５℃、電流密度２Ａ／ｄｍ２で行った。
Next, an evaluation test of a copper plating solution was performed using this evaluation jig.
First, a 0.1 μm-thick Cu underlayer was formed on this evaluation jig using a sputtering apparatus and subjected to an evaluation test.
In the evaluation test, the surface of this evaluation jig was subjected to copper plating by an electroplating method, and the surface state of the copper plating layer was observed and evaluated.
Copper plating is copper sulfate 90 g / l, sulfuric acid 180 g / l, chlorine 50 ppm, 0.3 g / l PEG (Polyethylene Glycol: polyethylene glycol), 0.5 ppm SPS (Bis (3-sulfopropyl) disulphide: screw (3 -Sulfopropyl) disulfide), and a copper plating solution containing 1 ppm JGB (Janus Green B) or 1 ppm thiourea as an additive for improving smoothness, bath temperature of 25 ° C., current It was carried out at a density 2A / dm 2.
銅めっき後、評価用冶具の表面状態をＳＥＭ観察した結果を図５（ｂ）−（１）及び図６（ｂ）−（１）に示す。
表面を観察した図５（ｂ）−（２），（３）から、添加剤の種類による平滑性の微妙な差を見分けられる。また、断面を観察した図６（ｂ）−（２），（３）から、表面の凹凸に対して添加剤の種類によってＣｕの析出の仕方が異なることが判る。
The results of SEM observation of the surface state of the evaluation jig after copper plating are shown in FIGS. 5 (b)-(1) and 6 (b)-(1).
5 (b)-(2) and (3) in which the surface is observed, a subtle difference in smoothness depending on the type of additive can be distinguished. Further, from FIGS. 6 (b)-(2) and (3) in which the cross section was observed, it can be seen that the manner of Cu precipitation differs depending on the type of additive with respect to the surface irregularities.
（実施例３）
基板として厚み１００μｍのポリスチレンフィルムを用い、その表面に幅１５μｍ、高さ２μｍの堤防形の凸形状部を形成する金型を用いて、プレス圧５ｔ／ｃｍ２、１６０℃の温度に１０分間保持して凸形状部３ｃを備える図４（ｃ）に示すポリスチレンフィルム基板の評価用冶具１を作製した。
(Example 3)
A polystyrene film having a thickness of 100 μm is used as a substrate, and a die having a bank-shaped convex part having a width of 15 μm and a height of 2 μm is used and held at a pressure of 5 t / cm 2 and a temperature of 160 ° C. for 10 minutes. Then, an evaluation jig 1 for a polystyrene film substrate shown in FIG.
次に、この評価用冶具を用いて、銅めっき液の評価試験を行った。
先ず、この評価用冶具にスパッタ装置を用いて厚み０．１μｍのＣｕの下地層を形成して、評価試験に供した。
評価試験は、この評価用冶具の表面に電気めっき法により銅めっきを施し、その銅めっき層の表面状態を観察して評価した。
銅めっきは、硫酸銅９０ｇ／ｌ、硫酸１８０ｇ／ｌ、塩素５０ｐｐｍ、０．３ｇ／ｌのＰＥＧ（Ｐｏｌｙｅｔｈｙｌｅｎｅ Ｇｌｙｃｏｌ：ポリエチレングリコール）、０．５ｐｐｍのＳＰＳ（Ｂｉｓ（３‐ｓｕｌｆｏｐｒｏｐｙｌ）ｄｉｓｕｌｆｉｄｅ ：ビス（３‐スルホプロピル）ジスルフィド）、そして平滑性を向上させる添加剤として、１ｐｐｍのＪＧＢ（Ｊａｎｕｓ Ｇｒｅｅｎ Ｂ：ヤヌスグリーンＢ）、又は１ｐｐｍのチオ尿素を添加した銅めっき液を用い、浴温２５℃、電流密度２Ａ／ｄｍ２で行った。
Next, an evaluation test of a copper plating solution was performed using this evaluation jig.
First, a 0.1 μm-thick Cu underlayer was formed on this evaluation jig using a sputtering apparatus and subjected to an evaluation test.
In the evaluation test, the surface of this evaluation jig was subjected to copper plating by an electroplating method, and the surface state of the copper plating layer was observed and evaluated.
Copper plating is copper sulfate 90 g / l, sulfuric acid 180 g / l, chlorine 50 ppm, 0.3 g / l PEG (Polyethylene Glycol: polyethylene glycol), 0.5 ppm SPS (Bis (3-sulfopropyl) disulphide: screw (3 -Sulfopropyl) disulfide), and a copper plating solution containing 1 ppm JGB (Janus Green B) or 1 ppm thiourea as an additive for improving smoothness, bath temperature of 25 ° C., current It was carried out at a density 2A / dm 2.
銅めっき後、評価用冶具の表面状態をＳＥＭ観察した結果を図５（ｃ）−（１）及び図６（ａ）−（１）に示す。
表面を観察した図５（ｃ）−（２），（３）から、添加剤の種類による平滑性の微妙な差を見分けられる。また、断面を観察した図６（ｃ）−（２），（３）から、表面の凹凸に対して添加剤の種類によってＣｕの析出の仕方が異なることが判る。
The results of SEM observation of the surface state of the evaluation jig after copper plating are shown in FIGS. 5 (c)-(1) and 6 (a)-(1).
5 (c)-(2) and (3) in which the surface is observed, a subtle difference in smoothness depending on the type of additive can be distinguished. Moreover, it can be seen from FIGS. 6 (c)-(2) and (3) in which the cross section is observed that the manner of precipitation of Cu differs depending on the type of additive with respect to the surface irregularities.
以上の実施例から明らかように、本発明の評価用冶具は、使用するめっき液の成分組成の違いによるめっき層の平滑性の評価に有用であることがわかる。また、実際の製品であるポリイミドフィルム表面の凹凸に近い評価用冶具を作製することができるため、量産化するときの条件に近い状態で評価でき、まためっき液に加える添加剤などの微妙な平滑性を評価できるため、めっき液を開発する上で非常に効果的な方法である。 As can be seen from the above examples, the evaluation jig of the present invention is useful for evaluating the smoothness of the plating layer due to the difference in the composition of the plating solution used. In addition, since an evaluation jig close to the unevenness on the surface of the polyimide film, which is an actual product, can be produced, it can be evaluated in a state close to the conditions for mass production and subtle smoothness such as additives to be added to the plating solution. Therefore, it is a very effective method for developing a plating solution.
１ 評価用冶具
２ 基板
３ａ 凸形状部
３ｂ 凹形状部
１０ 金型
１１ 金型凸部
１２ 金型凹部
DESCRIPTION OF SYMBOLS 1 Jig for evaluation 2 Board | substrate 3a Convex shape part 3b Concave shape part 10 Mold 11 Mold convex part 12 Mold recessed part
Claims (5)
前記評価用冶具は、表面に凹凸形状部を備える基板材料からなり、
前記基板材料の表面に備わる凹凸形状部が、高さが１〜３μｍの凸形状部、あるいは深さが１〜３μｍの凹形状部であり、
前記凹凸形状部が、ナノインプリント法により形成されることを特徴とする評価用冶具の製造方法。 A method for producing an evaluation jig for evaluating plating smoothness,
The evaluation jig is made of a substrate material having a concavo-convex shape portion on the surface,
The uneven portion provided on the surface of the substrate material is a convex portion having a height of 1 to 3 μm, or a concave portion having a depth of 1 to 3 μm .
The method for manufacturing an evaluation jig, wherein the uneven portion is formed by a nanoimprint method.
前記評価用冶具は、表面に凹凸形状部を備える基板材料からなり、
前記基板材料の表面に備わる凹凸形状部が、高さが１〜３μｍ、径が２〜２０μｍの凸形状部、あるいは深さが１〜３μｍ、径が２〜２０μｍの凹形状部であり、
前記凹凸形状部が、ナノインプリント法により形成されることを特徴とする評価用冶具の製造方法。 A method for producing an evaluation jig for evaluating plating smoothness ,
The evaluation jig is made of a substrate material having a concavo-convex shape portion on the surface,
The uneven portion provided on the surface of the substrate material is a convex portion having a height of 1 to 3 μm and a diameter of 2 to 20 μm, or a concave portion having a depth of 1 to 3 μm and a diameter of 2 to 20 μm .
The method for manufacturing an evaluation jig, wherein the uneven portion is formed by a nanoimprint method.
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