JP4329081B2 - Metal-coated optical fiber, manufacturing method thereof, and optical component - Google Patents
Metal-coated optical fiber, manufacturing method thereof, and optical component Download PDFInfo
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本発明は、金属被覆された光ファイバに関するものである。より詳しくは、光ファイバの芯線の表面が金属膜で被覆された金属被覆光ファイバに関するものである。 The present invention relates to a metal-coated optical fiber. More specifically, the present invention relates to a metal-coated optical fiber in which the surface of the core wire of the optical fiber is coated with a metal film.
大容量の情報を高速で送受信するために、光通信システムが注目されている。光通信システムにおいて光の伝搬路として用いられる光ファイバは、その中心部に光を伝搬させるコアと、コアの周囲に形成されて且つコアよりも屈折率の小さいクラッド層を備える。通常、コアとクラッドは石英ガラス製であり、芯線と呼ばれる。芯線の周囲には、折れや水分による特性劣化を防ぐために、樹脂製の保護被覆が形成される。 In order to transmit and receive a large amount of information at high speed, an optical communication system has attracted attention. An optical fiber used as a light propagation path in an optical communication system includes a core for propagating light to the center thereof, and a cladding layer formed around the core and having a refractive index smaller than that of the core. Usually, the core and the clad are made of quartz glass and are called core wires. A resin protective coating is formed around the core wire in order to prevent characteristic deterioration due to breakage or moisture.
一方、光部品は光ファイバの伝送路の途中に配置され、光の送受、挿入、分岐などを行うものである。光部品は、光の送受、挿入、分岐などの機能を担う光素子と、その端部が光素子に対向する光ファイバと、それらを収納するための筐体から構成されている。光素子と光ファイバとの位置関係は光部品の機能が最も効率よく発現するように決められる。たとえば、光送信器は、光素子であるレーザーダイオードから出射される光が光ファイバに挿入されるときの光強度が最も大きくなるように、光ファイバとレーザーダイオードとの位置関係が決められる。この位置関係が変わると、送信される光強度が弱くなってしまう不具合となる。光部品において光素子と光ファイバの位置関係は重要であり、さまざまな使用環境下でこの位置関係が殆ど変わらないことが望まれる。 On the other hand, the optical component is disposed in the middle of the optical fiber transmission path, and performs transmission / reception, insertion, branching, etc. of light. The optical component is composed of an optical element that performs functions such as light transmission / reception, insertion, and branching, an optical fiber whose end faces the optical element, and a housing for housing them. The positional relationship between the optical element and the optical fiber is determined so that the function of the optical component is expressed most efficiently. For example, in the optical transmitter, the positional relationship between the optical fiber and the laser diode is determined so that the light intensity when the light emitted from the laser diode, which is an optical element, is inserted into the optical fiber is maximized. If this positional relationship changes, the transmitted light intensity becomes weak. In an optical component, the positional relationship between the optical element and the optical fiber is important, and it is desired that the positional relationship hardly changes under various usage environments.
従来、光素子と光ファイバの固定には、樹脂製の接着剤が用いられてきた。光ファイバは保護被覆が除去されて露出した芯線がセラミックス製のフェルールに貫入されて、貫入孔との隙間を樹脂製接着剤によって埋められ固定される。樹脂製接着剤を硬化させる方法として、熱を加えるもの、自然放置するもの、紫外線を照射するものなどがあるが、総じて透湿性が高く、湿気に弱いという欠点がある。このため、高湿度環境下では位置ズレを起こしてしまい、光部品としての正常な動作を行うことが困難となる。 Conventionally, resin adhesives have been used for fixing optical elements and optical fibers. In the optical fiber, the exposed core wire with the protective coating removed is inserted into a ceramic ferrule, and the gap with the penetration hole is filled and fixed with a resin adhesive. There are methods for curing resin adhesives, such as those that apply heat, those that are allowed to stand naturally, and those that irradiate ultraviolet rays. However, they generally have a drawback of high moisture permeability and weakness to moisture. For this reason, a positional shift occurs in a high humidity environment, and it is difficult to perform a normal operation as an optical component.
光ファイバが光部品筐体内部に貫入する貫入孔との隙間が樹脂製接着剤によって埋められ光ファイバが固定され、光部品が封止される場合も同様の問題を抱える。すなわち、高湿度環境下では、樹脂製接着剤で封止した箇所から光部品内部に水分が侵入し、位置ズレを起こすなどして正常な動作が困難となる。 A similar problem occurs when the optical fiber is fixed by sealing a gap between the optical fiber penetrating into the optical component housing with a resin adhesive and the optical fiber is fixed. That is, in a high humidity environment, moisture enters the optical component from the location sealed with the resin adhesive, causing a positional shift and making normal operation difficult.
かかる樹脂製接着剤の固定・封止に替わって、ハンダによる固定・封止も提案されている（特許文献１）。しかし、光ファイバの材質は、保護被覆は樹脂、芯線は石英ガラスであるため、そのままでは良好なハンダ接合を得にくい。そこで保護被覆を除去して、露出した光ファイバの芯線の表面を金属膜で被覆し、その金属膜とハンダ接合させることが行われている。 Instead of fixing / sealing such a resin adhesive, fixing / sealing with solder has also been proposed (Patent Document 1). However, since the protective coating is made of resin and the core wire is made of quartz glass, it is difficult to obtain a good solder joint as it is. Therefore, the protective coating is removed, and the exposed surface of the core of the optical fiber is coated with a metal film and soldered to the metal film.
光ファイバの芯線の表面に金属膜を形成させる方法として、メッキ法、イオンプレーティング法、スパッタ法が挙げられる。このうちイオンプレーティング法やスパッタ法では、全周に渡って均一な金属膜を得ることが難しく、光ファイバの保護被覆が高温となって変形してしまう不都合が生じる。これに対してメッキ法（例えば、特許文献１、特許文献２）は、全周にわたって均一な金属膜を得やすいため好適な金属膜形成方法と言える。 Examples of the method for forming a metal film on the surface of the core wire of the optical fiber include a plating method, an ion plating method, and a sputtering method. Among these, the ion plating method and the sputtering method have a disadvantage that it is difficult to obtain a uniform metal film over the entire circumference, and the protective coating of the optical fiber is deformed at a high temperature. On the other hand, the plating method (for example, Patent Document 1 and Patent Document 2) can be said to be a suitable metal film forming method because it is easy to obtain a uniform metal film over the entire circumference.
しかし、メッキ法のうち、電解メッキ法は、光ファイバの芯線が非導電性の石英ガラスでできているため、導通のためのカーボン層を設けたり、無電解メッキ層などを予め形成する（特許文献１）などの必要があり、作製工程が増えて工程が複雑になってしまう。一方、無電解メッキ法、例えばＮｉ−Ｐメッキでは、形成される金属膜のＰ濃度によって特性が変わることが知られている。この場合Ｐ濃度が高いと膜応力が小さくなり、密着性において有利となる。しかし、一方、金属膜のＰ濃度が高いとハンダ接合の密着性が低下するという問題があった。無電解メッキを施した後に電界メッキを施す方法（特許文献１）も、結局は工程を複雑なものとしてしまう。 However, among the plating methods, the electrolytic plating method is such that an optical fiber core wire is made of non-conductive quartz glass, so that a carbon layer for conduction is provided or an electroless plating layer is formed in advance (patent) Document 1) and the like are necessary, which increases the number of manufacturing steps and complicates the steps. On the other hand, in the electroless plating method such as Ni-P plating, it is known that the characteristics change depending on the P concentration of the formed metal film. In this case, if the P concentration is high, the film stress becomes small, which is advantageous in adhesion. On the other hand, however, when the P concentration of the metal film is high, there is a problem that the adhesion of the solder joint is lowered. The method of applying electroplating after applying electroless plating (Patent Document 1) also ultimately complicates the process.
このように、光ファイバと金属膜の良好な密着性と良好なハンダ接合性を簡易な工程で両立することは困難であった。本発明は、従来の上記問題点を解決し、光ファイバと金属膜との密着性、ハンダ接合性、共に優れた金属被覆光ファイバ、およびその製造方法を提供しようとするものである。 Thus, it has been difficult to achieve both good adhesion between the optical fiber and the metal film and good solderability in a simple process. The present invention is intended to solve the above-mentioned conventional problems and to provide a metal-coated optical fiber excellent in both adhesion and solder bonding between an optical fiber and a metal film, and a method for producing the same.
光ファイバの芯線表面の少なくとも一部に、前記芯線表面に接して形成される第１の無電解Ｎｉメッキ層と、前記第１の無電解Ｎｉメッキ層の上に形成される第２の無電解Ｎｉメッキ層とを有し、前記第１の無電解Ｎｉメッキ層のＰ濃度は６.５質量％以上であり、前記第２の無電解Ｎｉメッキ層のＰ濃度は６.５質量％未満であることを特徴とする。前記第１の無電解Ｎｉメッキ層のＰ濃度を高くして６.５質量％以上とすることで、内部応力を低減し良好な密着性を実現することができる。一方、第２の無電解Ｎｉメッキ層のＰ濃度を低くして６.５質量％未満とすることによって、良好なハンダ接合を得ることができる。 A first electroless Ni plating layer formed on at least a part of the core wire surface of the optical fiber in contact with the core wire surface, and a second electroless film formed on the first electroless Ni plating layer. The first electroless Ni plating layer has a P concentration of 6.5% by mass or more, and the second electroless Ni plating layer has a P concentration of less than 6.5% by mass. It is characterized by being. By increasing the P concentration of the first electroless Ni plating layer to 6.5 mass% or more, it is possible to reduce internal stress and achieve good adhesion. On the other hand, by reducing the P concentration of the second electroless Ni plating layer to less than 6.5% by mass, good solder joint can be obtained.
さらに、前記第１の無電解Ｎｉメッキ層の厚さは、０．２μｍ以上であることが好ましい。第１の無電解Ｎｉメッキ層の厚さを０．２μｍ以上とすることで、光ファイバとの良好な密着性を得ることができる。厚さが０．２μｍ未満であると、前記第２の無電解Ｎｉメッキ層の内部応力の影響を受け、剥離などの密着性不良を引き起こす。安定して良好な密着性を得るためには、より好ましくは、０．３μｍ以上である。また、前記第1の無電解Ｎｉメッキ層の厚さは、それが大きくなりすぎると、生産性が低下するほか、メッキ膜全体に占める第１の無電解メッキ層の割合が大きくなり、ハンダ密着性を阻害するため、１μｍ以下であることが好ましい。 Furthermore, the thickness of the first electroless Ni plating layer is preferably 0.2 μm or more. By setting the thickness of the first electroless Ni plating layer to 0.2 μm or more, good adhesion to the optical fiber can be obtained. When the thickness is less than 0.2 μm, it is affected by internal stress of the second electroless Ni plating layer and causes adhesion failure such as peeling. In order to stably obtain good adhesion, the thickness is more preferably 0.3 μm or more. In addition, if the thickness of the first electroless Ni plating layer becomes too large, the productivity is lowered, and the ratio of the first electroless plating layer to the entire plating film is increased, so that the solder adhesion is increased. In order to inhibit the property, the thickness is preferably 1 μm or less.
さらに、前記第２の無電解Ｎｉメッキ層の厚さは、０．８μｍ以上であることが好ましい。ハンダ接合を行うとき、金属膜の中でハンダと合金を形成する層の厚さはおよそ０．８μｍであり、前記第２の無電解Ｎｉメッキ層の厚さを０．８μｍ以上とすれば、ハンダと反応して合金を形成する部分を、実質的に前記第２の無電解Ｎｉメッキ層だけとすることが可能である。前記第２の無電解Ｎｉメッキ層はＰ濃度が低いので良好なハンダ接合を形成することができる。逆に前記第２の無電解Ｎｉメッキ層の厚さを０．８μｍ未満とすれば、前記第１の無電解Ｎｉメッキ層もハンダと反応して合金を形成する。第１の無電解Ｎｉメッキ層はＰ濃度が高く、Ｐを含有する異相を析出しやすいので、良好なハンダ接合を得ることが困難となる。また、前記第２の無電解Ｎｉメッキ層の厚さは、それを必要以上に大きくすることは生産性の低下につながるため、好ましくは１０μｍ以下とする。 Furthermore, the thickness of the second electroless Ni plating layer is preferably 0.8 μm or more. When performing solder bonding, the thickness of the layer forming the solder and alloy in the metal film is about 0.8 μm, and the thickness of the second electroless Ni plating layer is 0.8 μm or more, The portion that reacts with the solder to form an alloy can be substantially only the second electroless Ni plating layer. Since the second electroless Ni plating layer has a low P concentration, a good solder joint can be formed. Conversely, if the thickness of the second electroless Ni plating layer is less than 0.8 μm, the first electroless Ni plating layer also reacts with solder to form an alloy. Since the first electroless Ni plating layer has a high P concentration and tends to precipitate a heterogeneous phase containing P, it is difficult to obtain a good solder joint. Further, the thickness of the second electroless Ni plating layer is preferably 10 μm or less because increasing the thickness more than necessary leads to a decrease in productivity.
さらに、前記第２の無電解Ｎｉメッキ層の上にＡｕメッキ膜が形成されていることが好ましい。Ａｕはハンダの濡れ性がよく、さらに良好なハンダ接合を得ることができる。 Furthermore, it is preferable that an Au plating film is formed on the second electroless Ni plating layer. Au has good wettability of solder and can provide a better solder joint.
本発明の光部品は、光ファイバを用いており、前記光ファイバは上記本発明のいずれかの金属被覆光ファイバであり、前記金属被覆光ファイバはその金属被覆部分において前記光部品にハンダ固定されていることを特徴とする。ハンダ固定された光ファイバは、接着剤などの樹脂で固定した場合よりも、高湿度下の位置ズレが起きにくいため、光部品の耐環境の信頼性を向上させることができる。 The optical component of the present invention uses an optical fiber, and the optical fiber is any one of the metal-coated optical fibers of the present invention, and the metal-coated optical fiber is solder-fixed to the optical component at the metal-coated portion. It is characterized by. Since the solder-fixed optical fiber is less likely to be displaced under high humidity than when it is fixed with a resin such as an adhesive, the reliability of the environment resistance of the optical component can be improved.
さらに、本発明の別の光部品は、筐体と前記筐体内部に貫入する光ファイバを有する光部品であって、前記光ファイバは上記本発明のいずれかの金属被覆光ファイバであり、前記筐体は光ファイバ貫入部に金属部を有し、前記貫入部と前記金属被覆光ファイバとの隙間が、前記金属被覆光ファイバの金属被覆部分においてハンダ封止されていることを特徴とする。前記貫入部と前記金属被覆光ファイバとの隙間がハンダによって閉塞、封止されるので、樹脂で封止される場合よりも、光部品内部に湿気や外気が侵入しにくくなる。このため、光ファイバの位置ズレが生じにくく、また発光素子、受光素子の特性劣化を防ぐことができる。 Furthermore, another optical component of the present invention is an optical component having a casing and an optical fiber penetrating into the casing, and the optical fiber is the metal-coated optical fiber of any of the present invention, The housing has a metal portion at the optical fiber penetration portion, and a gap between the penetration portion and the metal-coated optical fiber is solder-sealed at a metal-coated portion of the metal-coated optical fiber. Since the gap between the penetrating portion and the metal-coated optical fiber is closed and sealed with solder, moisture and outside air are less likely to enter the optical component than when sealed with resin. For this reason, it is hard to produce the position shift of an optical fiber, and it can prevent the characteristic deterioration of a light emitting element and a light receiving element.
また、本発明の金属被覆光ファイバの製造方法は、光ファイバの芯線の表面の少なくとも一部を露出させる工程と、前記光ファイバを１種のＰ濃度を有する無電解Ｎｉメッキ浴に浸す無電解Ｎｉメッキ工程とを有し、前記無電解Ｎｉメッキ工程におけるＮｉメッキの成長速度を０．１μｍ／分以上とすることにより、光ファイバの芯線に接して形成される第１の無電解Ｎｉメッキ層と、前記第１の無電解Ｎｉメッキ層の上に形成され、Ｐ濃度が前記第１の無電解Ｎｉメッキ層のＰ濃度よりも小さい第２の無電解Ｎｉメッキ層とを形成することを特徴とする。前記無電解Ｎｉ工程におけるＮｉメッキの成長速度を０．１μｍ／分以上とすることにより、１種のＰ濃度を有する無電解Ｎｉメッキ浴で、Ｐ濃度の高い第１の無電解メッキ層とＰ濃度の低い第２の無電解メッキ層を有する密着性とハンダ接合性に優れる金属被覆光ファイバを提供することができ、製造工程の簡素化、低コスト化が可能となる。 The method for producing a metal-coated optical fiber according to the present invention includes a step of exposing at least a part of the surface of the core of the optical fiber, and an electroless method in which the optical fiber is immersed in an electroless Ni plating bath having one kind of P concentration. A first electroless Ni plating layer formed in contact with the core of the optical fiber by setting the Ni plating growth rate in the electroless Ni plating step to 0.1 μm / min or more. And a second electroless Ni plating layer formed on the first electroless Ni plating layer and having a P concentration lower than the P concentration of the first electroless Ni plating layer. And By setting the growth rate of Ni plating in the electroless Ni process to 0.1 μm / min or more, an electroless Ni plating bath having one kind of P concentration, and the first electroless plating layer having a high P concentration and P A metal-coated optical fiber having a low-concentration second electroless plating layer and excellent adhesion and solderability can be provided, and the manufacturing process can be simplified and the cost can be reduced.
また、本発明の金属被覆光ファイバの製造方法は、金属被覆光ファイバの製造方法であって、光ファイバの芯線の表面の少なくとも一部を露出させる工程と、前記光ファイバを１種のＰ濃度を有する無電解Ｎｉメッキ浴に浸す無電解Ｎｉメッキ工程とを有し、前記無電解Ｎｉメッキ工程の初期のメッキ浴温度を、終期のメッキ浴温度よりも低くすることにより、光ファイバの芯線に接して形成される第１の無電解Ｎｉメッキ層と、前記第１の無電解Ｎｉメッキ層の上に形成され、Ｐ濃度が前記第１の無電解Ｎｉメッキ層のＰ濃度よりも小さい第２の無電解Ｎｉメッキ層とを形成することを特徴とする。１種のＰ濃度を有する無電解Ｎｉメッキ浴で、Ｐ濃度の高い第１の無電解メッキ層とＰ濃度の低い第２の無電解メッキ層を有する密着性とハンダ接合性に優れる金属被覆光ファイバを提供することができ、製造工程の簡素化、低コスト化が可能となる。 The method for producing a metal-coated optical fiber according to the present invention is a method for producing a metal-coated optical fiber, the step of exposing at least a part of the surface of the core wire of the optical fiber; An electroless Ni plating step soaked in an electroless Ni plating bath, and the initial plating bath temperature of the electroless Ni plating step is made lower than the final plating bath temperature, thereby forming an optical fiber core wire. A first electroless Ni plating layer formed in contact with the first electroless Ni plating layer; a second P concentration lower than the P concentration of the first electroless Ni plating layer; The electroless Ni plating layer is formed. An electroless Ni plating bath having one kind of P concentration, and a metal-coated light having excellent adhesion and solder bonding, having a first electroless plating layer having a high P concentration and a second electroless plating layer having a low P concentration. A fiber can be provided, and the manufacturing process can be simplified and the cost can be reduced.
さらに、前記無電解Ｎｉメッキ浴は、被メッキ体がＮｉである場合に形成される無電解Ｎｉメッキ層のＰ濃度が３.５質量％以上、かつ６.５質量％未満となる無電解Ｎｉメッキ浴であることを特徴とする。前記無電解Ｎｉメッキ浴として、被メッキ体がＮｉである場合に形成される無電解Ｎｉメッキ層のＰ濃度が３.５質量％以上、かつ６.５質量％未満となるメッキ液を採用して、金属被覆光ファイバの製造を行えば、光ファイバの芯線に接して形成される第１の無電解Ｎｉメッキ層と、前記第１の無電解Ｎｉメッキ層の上に形成され、Ｐ濃度が前記第１の無電解Ｎｉメッキ層のＰ濃度よりも小さい第２の無電解Ｎｉメッキ層とを形成することができる。かかる方法により、第１の無電解Ｎｉメッキ層のＰ濃度を６.５質量％以上とすることが可能となり、内部応力が小さく、良好な密着性を実現できる。また、第２の無電解Ｎｉメッキ層のＰ濃度は、６.５質量％未満となり、Ｐ濃度が低いため良好なハンダ接合を得ることができる。 Further, the electroless Ni plating bath includes an electroless Ni plating layer in which the P concentration of the electroless Ni plating layer formed when the object to be plated is Ni is 3.5 mass% or more and less than 6.5 mass%. It is a plating bath. As the electroless Ni plating bath, a plating solution in which the P concentration of the electroless Ni plating layer formed when the object to be plated is Ni is 3.5% by mass or more and less than 6.5% by mass is used. When the metal-coated optical fiber is manufactured, the first electroless Ni plating layer formed in contact with the core of the optical fiber and the first electroless Ni plating layer are formed, and the P concentration is A second electroless Ni plating layer smaller than the P concentration of the first electroless Ni plating layer can be formed. By this method, the P concentration of the first electroless Ni plating layer can be made 6.5% by mass or more, the internal stress is small, and good adhesion can be realized. Further, the P concentration of the second electroless Ni plating layer is less than 6.5% by mass, and since the P concentration is low, a good solder joint can be obtained.
本発明によれば、密着性とハンダ接合性の両方に優れた金属被覆を有する金属被覆光ファイバおよびそれを簡易に製造できる方法を提供することができる。また、本発明の金属被覆光ファイバを用いた光部品では、該光ファイバをハンダ固定することにより位置ズレを防止する一方、ハンダ封止することにより気密性を向上させることができる。 ADVANTAGE OF THE INVENTION According to this invention, the metal-coated optical fiber which has a metal coating excellent in both adhesiveness and solder joint property, and the method of manufacturing it easily can be provided. Moreover, in the optical component using the metal-coated optical fiber of the present invention, the optical fiber can be prevented from being displaced by fixing the optical fiber, and the hermeticity can be improved by soldering.
本発明では、光ファイバの芯線表面の少なくとも一部に、前記芯線表面に接して第１の無電解Ｎｉメッキ層、前記第１の無電解Ｎｉメッキ層の上に第２の無電解Ｎｉメッキ層を形成する。そして前記第２の無電解Ｎｉメッキ層のＰ濃度が前記第１の無電解Ｎｉメッキ層のＰ濃度よりも小さいものとする。該構成を採用する理由を以下説明する。「無電解めっき 基礎と応用 電気鍍金研究会編 日刊工業新聞社」によれば、Ｐの濃度（質量％）と膜内の内部応力の関係は以下の通りである。Ｐ濃度が９質量％未満では引っ張り応力が発生し、Ｐ濃度が７質量％未満では３０ｋｇ／ｍｍ２（２９.４ｋＰａ）を超える引っ張り応力となる、さらにＰ濃度が６.５質量％未満では特に大きな引っ張り応力が発生する。逆にＰ濃度が６.５質量％以上では引っ張り応力が小さくなり、さらにＰ濃度が減り９〜１６質量％となると５ｋｇ／ｍｍ２（４.９ｋＰａ）未満の圧縮応力が発生する。Ｐ濃度が６.５質量％以上では内部応力は４０ｋｇ／ｍｍ２（３９.２ｋＰａ）以下であり、剥離、クラックが生じにくく、下地である光ファイバの芯線との密着性が良好な金属被覆光ファイバが得られることとなる。 In the present invention, at least a part of the surface of the core wire of the optical fiber is in contact with the surface of the core wire, the first electroless Ni plating layer, and the second electroless Ni plating layer on the first electroless Ni plating layer. Form. The P concentration of the second electroless Ni plating layer is lower than the P concentration of the first electroless Ni plating layer. The reason for adopting this configuration will be described below. According to “Electroless Plating Fundamentals and Applications, Nikkan Kogyo Shimbun Co., Ltd.”, the relationship between P concentration (% by mass) and internal stress in the film is as follows. When the P concentration is less than 9% by mass, a tensile stress is generated. When the P concentration is less than 7% by mass, the tensile stress exceeds 30 kg / mm 2 (29.4 kPa). Further, when the P concentration is less than 6.5% by mass, A large tensile stress is generated. Conversely, when the P concentration is 6.5% by mass or more, the tensile stress decreases, and when the P concentration decreases to 9 to 16% by mass, a compressive stress of less than 5 kg / mm 2 (4.9 kPa) is generated. When the P concentration is 6.5% by mass or more, the internal stress is 40 kg / mm 2 (39.2 kPa) or less, it is difficult to cause peeling and cracking, and the metal-coated light has good adhesion to the core of the optical fiber as the base. A fiber will be obtained.
一方、金属膜のＰ濃度が高いとハンダ接合の密着性が低下する。ハンダ接合を行うと、金属膜中のＮｉはハンダと合金を形成するが、金属膜中のＰはハンダと合金を形成することができず、Ｎｉとハンダとの合金層と金属膜との間に異相となって析出する。このＰを含有する異相は結合力が弱く、結果としてハンダ接合の接合強度を低下させてしまうのである。逆に、Ｐ濃度が低くすることによって、異相の生成を抑制し、良好な接合を得ることができる。したがって、光ファイバに接している第１の無電解Ｎｉメッキ層のＰ濃度を高くし、第2の無電解Ｎｉメッキ層のＰ濃度を低くすることによって、密着性、ハンダ接合性に優れた金属被覆光ファイバを得ることができる。上述のように、特に前記第１の無電解Ｎｉメッキ層のＰ濃度を６.５質量％以上、前記第２の無電解Ｎｉメッキ層のＰ濃度は６.５質量％未満とすることが好ましい。より好ましくは、前記第１の無電解Ｎｉメッキ層のＰ濃度は６.５質量％以上、かつ９.５質量％未満である。内部応力を低くするためには、第１の無電解Ｎｉメッキ層のＰ濃度は高いことが好ましいが、１種のＰ濃度を有する無電解Ｎｉメッキ浴で第１、第２の無電解メッキ層を形成する場合には、第１の無電解Ｎｉメッキ層のＰ濃度を高くしすぎると、第２の無電解Ｎｉメッキ層のＰ濃度を６.５質量％未満として、高いハンダ接合性を得ることが困難となる。この場合、第２の無電解メッキ層のＰ濃度は３.５質量％以上、かつ６.５質量％未満が好ましい。高いハンダ接合性を得る観点からは、さらに好ましくは、前記第１の無電解Ｎｉメッキ層のＰ濃度は６.５質量％以上、かつ８.５質量％未満、前記第２の無電解Ｎｉメッキ層のＰ濃度は３.５質量％以上、かつ５.５質量％未満である。 On the other hand, when the P concentration of the metal film is high, the adhesiveness of solder bonding is lowered. When solder bonding is performed, Ni in the metal film forms an alloy with the solder, but P in the metal film cannot form an alloy with the solder, and between the alloy layer of Ni and solder and the metal film. To form a different phase. This heterogeneous phase containing P has a weak bonding force, and as a result, the bonding strength of solder bonding is lowered. Conversely, by reducing the P concentration, it is possible to suppress the generation of heterogeneous phases and obtain good bonding. Therefore, by increasing the P concentration of the first electroless Ni plating layer in contact with the optical fiber and decreasing the P concentration of the second electroless Ni plating layer, a metal having excellent adhesion and solderability. A coated optical fiber can be obtained. As described above, the P concentration of the first electroless Ni plating layer is preferably 6.5% by mass or more, and the P concentration of the second electroless Ni plating layer is preferably less than 6.5% by mass. . More preferably, the P concentration of the first electroless Ni plating layer is 6.5% by mass or more and less than 9.5% by mass. In order to reduce the internal stress, it is preferable that the P concentration of the first electroless Ni plating layer is high, but the first and second electroless plating layers are used in an electroless Ni plating bath having one kind of P concentration. When the P concentration of the first electroless Ni plating layer is too high, the P concentration of the second electroless Ni plating layer is set to less than 6.5% by mass, and high solderability is obtained. It becomes difficult. In this case, the P concentration of the second electroless plating layer is preferably 3.5% by mass or more and less than 6.5% by mass. More preferably, from the viewpoint of obtaining high solderability, the first electroless Ni plating layer has a P concentration of 6.5% by mass or more and less than 8.5% by mass, and the second electroless Ni plating. The P concentration of the layer is 3.5% by mass or more and less than 5.5% by mass.
また、析出速度の違いから、前記第１の無電解Ｎｉメッキ層と前記第２の無電解Ｎｉメッキ層は組織も異なる。析出速度の遅い前記第１の無電解Ｎｉメッキ層は柱状晶を有し、析出速度の速い前記第２の無電解Ｎｉメッキ層はチル晶またはアモルファス相を有する。 Further, the first electroless Ni plating layer and the second electroless Ni plating layer have different structures due to the difference in deposition rate. The first electroless Ni plating layer having a low precipitation rate has columnar crystals, and the second electroless Ni plating layer having a high precipitation rate has a chill crystal or an amorphous phase.
前記第１の無電解Ｎｉメッキ層と前記第２の無電解Ｎｉメッキ層を形成させる方法として、１種の無電解Ｎｉメッキ浴を用いることが、本発明の特徴の一つである。これは、１種の無電解Ｎｉメッキ浴を用いつつ、金属被覆光ファイバに好適な無電解Ｎｉメッキ層構成を実現できるという新規な知見に基づく。この場合、メッキ析出速度の差によるＰ濃度変化を利用するのが、簡便であり最適である。Ｎｉメッキの析出速度が速くなると、Ｐ濃度は低下する。前記Ｎｉメッキの析出速度は０.１μｍ／分以上とすることが好ましい。光ファイバの芯線に接する部分の第１の無電解Ｎｉメッキ層の析出速度に対して、第２の無電解メッキ層の析出速度を速くするためには、０.１３μｍ／分以上の析出速度とすることがより好ましい。一方、析出速度が速くなりすぎると、第１の無電解メッキ層のＰ濃度が低くなってしまうので、析出速度は０.２μｍ／分以下が好ましい。また、析出速度は、メッキ処理の温度によって、制御することができる。浴の温度は、６０〜９０℃の範囲が好ましい。６０℃未満であると、めっき反応が進行しなくなるためにメッキ膜が得られず、９０℃超であるとメッキ液の分解が促進される。第１の無電解メッキ膜と第２の無電解メッキ膜とで析出速度に差を設けて、前者の析出速度を上げるためには、メッキ工程の初期と終期とで温度差を設け、メッキ初期の温度を低く、終期の温度を高くすることが好ましい。この場合メッキ初期の温度は６０℃以上、かつ７０℃未満とし、メッキ終期の温度は７０℃以上、かつ９０℃以下とすることが好ましい。かかる温度差は、２段階等の段階的に制御するほか、連続的に制御してもよい。このように、析出速度の違いにより、Ｎｉ濃度の異なる２層の無電解Ｎｉメッキ層の形成を制御することができるのである。また、Ｐ濃度の高い第1の無電解Ｎｉメッキ層を形成するためには、メッキの前処理としてＰｄ等の触媒処理を施すことが好ましい。 As a method for forming the first electroless Ni plating layer and the second electroless Ni plating layer, it is one of the features of the present invention to use one kind of electroless Ni plating bath. This is based on a novel finding that an electroless Ni plating layer configuration suitable for a metal-coated optical fiber can be realized while using one type of electroless Ni plating bath. In this case, it is simple and optimal to use the change in P concentration due to the difference in plating deposition rate. As the deposition rate of Ni plating increases, the P concentration decreases. The deposition rate of the Ni plating is preferably 0.1 μm / min or more. In order to increase the deposition rate of the second electroless plating layer relative to the deposition rate of the first electroless Ni plating layer in the portion in contact with the core of the optical fiber, a deposition rate of 0.13 μm / min or more is required. More preferably. On the other hand, if the deposition rate is too high, the P concentration of the first electroless plating layer will be low, so the deposition rate is preferably 0.2 μm / min or less. The deposition rate can be controlled by the temperature of the plating process. The temperature of the bath is preferably in the range of 60 to 90 ° C. When the temperature is lower than 60 ° C., the plating reaction does not proceed, so that a plating film cannot be obtained. When the temperature is higher than 90 ° C., decomposition of the plating solution is promoted. In order to increase the former deposition rate by providing a difference in deposition rate between the first electroless plating film and the second electroless plating film, a temperature difference is provided between the initial stage and the final stage of the plating process. It is preferable to lower the temperature and raise the final temperature. In this case, the initial plating temperature is preferably 60 ° C. or higher and lower than 70 ° C., and the final plating temperature is preferably 70 ° C. or higher and 90 ° C. or lower. Such a temperature difference may be controlled stepwise such as in two steps or continuously. Thus, the formation of two electroless Ni plating layers having different Ni concentrations can be controlled by the difference in deposition rate. In order to form the first electroless Ni plating layer having a high P concentration, it is preferable to perform a catalyst treatment such as Pd as a pretreatment for plating.
前記無電解Ｎｉメッキ浴として、通常のＮｉ−Ｐメッキに比べて、Ｐ濃度の低いメッキを用いる。被メッキ体がＮｉである場合に形成される無電解Ｎｉメッキ層のＰ濃度が３.５質量％以上、かつ６.５質量％未満となるメッキ液を採用して、金属被覆光ファイバの製造を行えば、光ファイバの芯線に接して形成される第１の無電解Ｎｉメッキ層と、前記第１の無電解Ｎｉメッキ層の上に形成され、Ｐ濃度が前記第１の無電解Ｎｉメッキ層のＰ濃度よりも小さい第２の無電解Ｎｉメッキ層とを形成することができる。かかる方法により、第１の無電解Ｎｉメッキ層のＰ濃度を６.５質量％以上とすることが可能となり、内部応力が小さく、良好な密着性を実現できる。また、第２の無電解Ｎｉメッキ層のＰ濃度は、６.５質量％未満となり、Ｐ濃度が低いため良好なハンダ接合を得ることができる。前記無電解Ｎｉメッキ浴として、被メッキ体がＮｉである場合に形成される無電解Ｎｉメッキ層のＰ濃度が３.５質量％以上、５.５質量％未満となるメッキ液を用いることが、前記第１の無電解Ｎｉメッキ層のＰ濃度を６.５質量％以上、かつ８.５質量％未満、前記第２の無電解Ｎｉメッキ層のＰ濃度を３.５質量％以上、かつ５.５質量％未満とするうえでより好ましい。 As the electroless Ni plating bath, plating having a lower P concentration than that of normal Ni-P plating is used. Production of a metal-coated optical fiber by employing a plating solution in which the P concentration of the electroless Ni plating layer formed when the object to be plated is Ni is 3.5% by mass or more and less than 6.5% by mass. Are formed on the first electroless Ni plating layer formed in contact with the core of the optical fiber, and the first electroless Ni plating layer is formed on the first electroless Ni plating layer. A second electroless Ni plating layer smaller than the P concentration of the layer can be formed. By this method, the P concentration of the first electroless Ni plating layer can be made 6.5% by mass or more, the internal stress is small, and good adhesion can be realized. Further, the P concentration of the second electroless Ni plating layer is less than 6.5% by mass, and since the P concentration is low, good solder bonding can be obtained. As the electroless Ni plating bath, a plating solution in which the P concentration of the electroless Ni plating layer formed when the object to be plated is Ni is 3.5% by mass or more and less than 5.5% by mass is used. The P concentration of the first electroless Ni plating layer is 6.5 mass% or more and less than 8.5 mass%, the P concentration of the second electroless Ni plating layer is 3.5 mass% or more, and It is more preferable to make it less than 5.5% by mass.
無電解Ｎｉメッキ処理としては、本発明において特に限定する以外は、通常の無電解Ｎｉメッキ処理の方法を用いることができる。 As the electroless Ni plating treatment, a normal electroless Ni plating treatment method can be used unless otherwise limited in the present invention.
また、無電解Ｎｉメッキの上にはさらにＡｕ被覆、特にＡｕメッキを施すことが好ましい。Ａｕはハンダとの濡れ性がよく、ハンダ接合性の向上に寄与するほか、Ｎｉ層の酸化を防止する。Ａｕメッキは、置換型無電解Ａｕメッキ、無電解Ａｕメッキなどの方法で形成すればよい。 Further, it is preferable to apply Au coating, particularly Au plating, on the electroless Ni plating. Au has good wettability with solder, contributes to improvement of solder jointability, and prevents oxidation of the Ni layer. The Au plating may be formed by a method such as substitutional electroless Au plating or electroless Au plating.
本発明に係る前述の金属被覆光ファイバをその金属被覆部分において光部品にハンダ固定すること、または光ファイバ貫入部を有する光部品の筐体との隙間をハンダ封止することによって、耐湿性などの信頼性を向上し、発光素子、受光素子の特性劣化を防いだ光部品を提供できる。ここでいう光部品とは、光ファイバを用いているものであれば特に限定するものではないが、具体的に次のようなものが挙げられる。例えば、ＬＤモジュール（Laser Diode Module）のように発光素子の光を先球光ファイバにより外部に送り出す装置、光ファイバ同士を突き合わせ若しくは移動させて光路を切り替えるファイバ駆動型光スイッチ、光路内でミラーを回転若しくは移動させて光路を切り替えるミラー駆動型光スイッチ、ミラーの代わりにプリズムを動かして光路を切り替えるプリズム駆動型光スイッチ、導波路と外部の光ファイバと結合させる導波路型光スイッチ、マイクロミラーをマトリクス状に２次元配置して光路を切り替えるＭＥＭＳ型光スイッチ、マイクロミラーアレイ同士を３次元的に対向させることにより光路を切り替えるＭＥＭＳ型光スイッチ、誘電体多層膜によって一部の光を透過させ、その強度を検出する光パワーモニタ、空気中に出射した光の光路中にファラデー回転子を挿入した光アイソレータおよび光サーキュレータ、光吸収体を挿入した光減衰器などである。 The above-mentioned metal-coated optical fiber according to the present invention is solder-fixed to the optical component at the metal-coated portion, or the gap between the optical component housing having the optical fiber penetrating portion is solder-sealed, and so on. Can be provided, and an optical component can be provided in which deterioration of characteristics of the light emitting element and the light receiving element is prevented. The optical component here is not particularly limited as long as it uses an optical fiber, but specific examples include the following. For example, a device that sends light from a light emitting element to the outside by a tip-end optical fiber, such as an LD module (Laser Diode Module), a fiber-driven optical switch that switches optical paths by abutting or moving optical fibers, and a mirror in the optical path A mirror-driven optical switch that switches the optical path by rotating or moving, a prism-driven optical switch that switches the optical path by moving a prism instead of a mirror, a waveguide-type optical switch that couples a waveguide with an external optical fiber, and a micromirror A MEMS type optical switch that switches two-dimensionally in a matrix and switches the optical path, a MEMS type optical switch that switches the optical path by causing the micromirror arrays to face each other three-dimensionally, a part of light is transmitted through the dielectric multilayer film, Optical power monitor that detects its intensity, light emitted into the air An optical isolator and an optical circulator was inserted Faraday rotator in the optical path, an optical attenuator inserted the light absorber and the like.
以下、本発明に係わる実施例を説明する。ただし、これら実施例により本発明が限定されるものではない。なお、類似の部品については同じ符号で説明する。
（実施例１）
図１に本実施例の金属被覆光ファイバの模式図を示す。光ファイバの先端の保護被覆（径２５０μｍ）を剥離除去して、芯線（径１２５μｍ）を露出させた（図１（ａ））。保護被覆の剥離除去は、被覆除去器（株式会社フジクラ社製高強度ホットジャケットストリッパー：ＨＴＳ−１２）を用いた。露出した芯線の長さはおよそ３ｍｍとした。芯線表面に残存する保護被覆片を取り除いた後、露出した芯線を水酸化カリウム水溶液およびフッ化水素アンモニウム水溶液に順次に浸漬させ、アルカリ洗浄と酸エッチングを行った。なお、アルカリ洗浄と酸エッチングの間には、十分な流水洗浄を行った。以下に説明する浸漬工程間でも同様に十分な流水洗浄を行った。
Embodiments according to the present invention will be described below. However, the present invention is not limited to these examples. Similar parts will be described with the same reference numerals.
Example 1
FIG. 1 shows a schematic diagram of a metal-coated optical fiber of this example. The protective coating (diameter 250 μm) at the tip of the optical fiber was peeled and removed to expose the core wire (diameter 125 μm) (FIG. 1A). For removal of the protective coating, a coating remover (high strength hot jacket stripper: HTS-12 manufactured by Fujikura Co., Ltd.) was used. The length of the exposed core wire was about 3 mm. After removing the protective covering piece remaining on the surface of the core wire, the exposed core wire was sequentially immersed in an aqueous potassium hydroxide solution and an aqueous ammonium hydrogen fluoride solution, followed by alkali cleaning and acid etching. In addition, sufficient flowing water cleaning was performed between the alkali cleaning and the acid etching. Similarly, sufficient running water washing was performed between the dipping steps described below.
続いて、カップリング剤等を含む溶液（例えば、メルテックス社製メルプレート コンディショナー １１０１）に浸漬させて芯線表面を増感させ、ついで塩化パラジウム水溶液に浸漬させて芯線表面に触媒Ｐｄを付加させた後、無電解Ｎｉメッキ液に浸漬させて、無電解Ｎｉメッキ膜を形成させた（図１（ｂ））。メッキ浴の温度はメッキ工程初期で６８℃、メッキ工程終期で７５℃、浸漬時間は１５分であった。 Subsequently, the core wire surface was sensitized by immersing in a solution containing a coupling agent or the like (for example, Melplate Conditioner 1101 manufactured by Meltex), and then immersed in an aqueous palladium chloride solution to add catalyst Pd to the core wire surface. Thereafter, it was immersed in an electroless Ni plating solution to form an electroless Ni plating film (FIG. 1B). The temperature of the plating bath was 68 ° C. at the beginning of the plating process, 75 ° C. at the end of the plating process, and the immersion time was 15 minutes.
第１の無電解Ｎｉメッキ層と第２の無電解Ｎｉメッキ層の、２層の無電解Ｎｉメッキ膜を形成させる方法として、メッキ析出速度の差によるＰ濃度変化を利用した。採用した無電解Ｎｉメッキ液は、被メッキ体がＮｉであるときに形成させるＮｉメッキ層のＰ濃度が４質量％のものを用いた。つまり、本実施例においては、芯線表面がＮｉメッキで覆われた後に形成される前記第２の無電解Ｎｉメッキ層のＰ濃度が４質量％となる。第２の無電解Ｎｉメッキ層の膜厚は１．６μｍであった。また、無電解Ｎｉメッキ膜の上にさらに０．０５μｍ厚さの置換型無電解Ａｕメッキを施した。膜厚は、メッキ断面をＳＥＭ観察し４箇所の平均をもってメッキ層の膜厚とした。また、Ｐの濃度はＳＥＭ／ＥＤＸで測定した。 As a method of forming two electroless Ni plating films, a first electroless Ni plating layer and a second electroless Ni plating layer, a change in P concentration due to a difference in plating deposition rate was used. As the electroless Ni plating solution employed, a Ni plating layer formed when the object to be plated is Ni has a P concentration of 4% by mass. That is, in this embodiment, the P concentration of the second electroless Ni plating layer formed after the core wire surface is covered with Ni plating is 4% by mass. The film thickness of the second electroless Ni plating layer was 1.6 μm. Further, substitutional electroless Au plating with a thickness of 0.05 μm was further applied on the electroless Ni plating film. The thickness of the plating layer was determined by SEM observation of the plating cross section and the average of the four locations. The concentration of P was measured by SEM / EDX.
一方、無電解Ｎｉメッキ膜の初期析出過程では、芯線表面はまだＮｉメッキ膜で覆われておらず、触媒Ｐｄが露出している。Ｐｄ上での無電解Ｎｉメッキ膜の析出速度は、Ｎｉ上に比べて速くＰ濃度が変化して低下する。本実施例では、芯線表面付近にＰ濃度が７質量％の第１の無電解Ｎｉメッキ層が形成された。第１の無電解Ｎｉメッキ層の膜厚は０．４μｍであり、前記第２の無電解Ｎｉメッキ層と合せた無電解Ｎｉメッキ層全体での析出速度は、０.１３μｍ／分であった。また、ＳＥＭ観察した結果を図２に、その模式図を図３に示すが、光ファイバ表面に接する第１の無電解Ｎｉメッキ層は柱状晶であり、該柱状晶の上の第２の無電解Ｎｉメッキ層はアモルファス相であった。 On the other hand, in the initial deposition process of the electroless Ni plating film, the surface of the core wire is not yet covered with the Ni plating film, and the catalyst Pd is exposed. The deposition rate of the electroless Ni plating film on Pd is lower than that on Ni, and the P concentration changes and decreases. In this example, a first electroless Ni plating layer having a P concentration of 7% by mass was formed near the surface of the core wire. The film thickness of the first electroless Ni plating layer was 0.4 μm, and the deposition rate of the entire electroless Ni plating layer combined with the second electroless Ni plating layer was 0.13 μm / min. . Further, FIG. 2 shows the result of SEM observation, and FIG. 3 shows a schematic diagram thereof. The first electroless Ni plating layer in contact with the optical fiber surface is a columnar crystal, and the second non-electrolytic Ni plating layer on the columnar crystal. The electrolytic Ni plating layer was an amorphous phase.
このようにメッキ析出速度の差を利用して、芯線表面上に、Ｐ濃度の大きい第1のＮｉメッキ層とＰ濃度の小さい第２のＮｉメッキ層を形成した。これを試料Ａとする。この試料Ａをハンダ接合させ、引張り試験の破断強度をもって、接合強度を調べたところ、良好な接合強度を示した。これは、第２の無電解Ｎｉメッキ層のＰ濃度が４質量％と低く、Ｐ異相の形成が少なかったためと考えられる。また、膜厚は１．６μｍであり、ハンダとの合金層の厚さ０．８μｍよりも厚い。合金となるのは実質的に第２の無電解Ｎｉメッキ層だけであり、Ｐ濃度の高い第１の無電解Ｎｉメッキ層は反応しないので、Ｐを含有する異相が少なく良好なハンダ接合となったと考えられる。また、金属被複ファイバ１００個に対する粘着テープによる密着力試験でも、剥れはなく、強固な密着性を示した。これは、第１の無電解Ｎｉメッキ層のＰ濃度が７質量％であり、内部応力が小さかったためと考えられる。 Thus, using the difference in plating deposition rate, a first Ni plating layer having a high P concentration and a second Ni plating layer having a low P concentration were formed on the surface of the core wire. This is designated as sample A. When this sample A was soldered and the joint strength was examined with the breaking strength of the tensile test, it showed a good joint strength. This is presumably because the P concentration of the second electroless Ni plating layer was as low as 4% by mass and there was little formation of P heterogeneous phase. Further, the film thickness is 1.6 μm, which is thicker than the thickness of the alloy layer with solder of 0.8 μm. The alloy is essentially only the second electroless Ni plating layer, and the first electroless Ni plating layer having a high P concentration does not react, so that it is possible to obtain a good solder joint with few different phases containing P. It is thought. Further, even in an adhesion test using an adhesive tape for 100 metal-coated fibers, there was no peeling and a strong adhesion was shown. This is presumably because the P concentration of the first electroless Ni plating layer was 7% by mass and the internal stress was small.
（比較例１）
被メッキ体がＮｉであるときに形成させるＮｉメッキ層のＰ濃度が１質量％の無電解Ｎｉメッキ液を用いた以外は実施例１と同様にして金属被覆光ファイバを作製したところ、芯線表面上に、Ｐ濃度が４質量％の第１の無電解Ｎｉメッキ層（厚さ０．４μｍ）が形成され、前記第１の無電解Ｎｉメッキ層の上に、Ｐ濃度が１質量％の第２の無電解Ｎｉメッキ層（厚さ１．６μｍ）が形成された。作製した金属被覆光ファイバを試料Ｂとする。この試料Ｂをハンダ接合させたところ、良好な接合強度を示した。一方、金属被複ファイバ１００個に対する粘着テープによる密着力試験では、１５個の剥れが発生し、密着性が低かった。これは、第２の無電解Ｎｉメッキ層のＰ濃度が１質量％と低くＰを含有する異相の生成が少なかったため、ハンダ接合は良好なものとなったが、第１の無電解Ｎｉメッキ層のＰ濃度が４質量％であり、内部応力が大きく密着性は低くなったためと考えられる。
(Comparative Example 1)
A metal-coated optical fiber was produced in the same manner as in Example 1 except that an electroless Ni plating solution having a P concentration of 1% by mass of the Ni plating layer formed when the object to be plated was Ni was produced. A first electroless Ni plating layer (thickness 0.4 μm) having a P concentration of 4% by mass is formed thereon, and a first electroless Ni plating layer having a P concentration of 1% by mass is formed on the first electroless Ni plating layer. Two electroless Ni plating layers (thickness 1.6 μm) were formed. The produced metal-coated optical fiber is designated as Sample B. When this sample B was soldered, good bonding strength was exhibited. On the other hand, in the adhesion test using the adhesive tape to 100 metal-coated fibers, 15 pieces were peeled off and the adhesion was low. This is because the P concentration of the second electroless Ni plating layer was as low as 1% by mass and the generation of heterogeneous phases containing P was small, so that the solder joint was good, but the first electroless Ni plating layer This is considered to be because the P concentration was 4 mass%, the internal stress was large, and the adhesion was low.
（比較例２）
被メッキ体がＮｉであるときに形成させるＮｉメッキ層のＰ濃度が８質量％の無電解Ｎｉメッキ液を用いた以外は実施例１と同様にして、金属被覆光ファイバを作製したところ、芯線表面上に、Ｐ濃度が１１質量％の第１の無電解Ｎｉメッキ層（厚さ０．４μｍ）が形成し、前記第１の無電解Ｎｉメッキ層の上に、Ｐ濃度が８質量％の第２の無電解Ｎｉメッキ層（厚さ１．６μｍ）が形成された。作製した金属被覆光ファイバを試料Ｃとする。この試料Ｃをハンダ接合したところ、破断し、接合強度が弱かった。一方、粘着テープによる密着力試験では、剥れはなく良好な密着性を示した。第１の無電解Ｎｉメッキ層のＰ濃度が１１質量％と低く密着性は良好なものとなったが、第２の無電解Ｎｉメッキ層のＰ濃度が８質量％と高く、Ｐ異相が多く生成したため、ハンダ接合強度は弱くなったものと考えられる。
(Comparative Example 2)
A metal-coated optical fiber was produced in the same manner as in Example 1 except that an electroless Ni plating solution having a P concentration of 8 mass% for the Ni plating layer formed when the object to be plated was Ni was produced. A first electroless Ni plating layer (thickness 0.4 μm) having a P concentration of 11 mass% is formed on the surface, and a P concentration of 8 mass% is formed on the first electroless Ni plating layer. A second electroless Ni plating layer (thickness 1.6 μm) was formed. The produced metal-coated optical fiber is designated as sample C. When this sample C was soldered, it was broken and the bonding strength was weak. On the other hand, the adhesion test using an adhesive tape showed good adhesion without peeling. The first electroless Ni plating layer has a low P concentration of 11% by mass and good adhesion, but the second electroless Ni plating layer has a high P concentration of 8% by mass and many P heterogeneous phases. Since it was generated, it is considered that the solder joint strength was weakened.
以上のように、被メッキ体がＮｉであるときに形成させるＮｉメッキ層のＰ濃度を３.５〜６.５質量％の範囲とし、第１の無電解Ｎｉメッキ層のＰ濃度を６.５質量％以上、第２の無電解Ｎｉメッキ層のＰ濃度を６.５質量％未満とすることによって、ハンダ接合性と密着性がともに良好な金属被複光ファイバが得られた。 As described above, the P concentration of the Ni plating layer formed when the object to be plated is Ni is in the range of 3.5 to 6.5% by mass, and the P concentration of the first electroless Ni plating layer is 6. By setting the P concentration of the second electroless Ni plating layer to 5% by mass or more and less than 6.5% by mass, a metal-coated optical fiber having both good solderability and good adhesion was obtained.
（実施例２）
芯線表面上に、Ｐ濃度が７質量％の第１の無電解Ｎｉメッキ層（厚さ０．４μｍ）を形成し、前記第１の無電解Ｎｉメッキ層の上に、Ｐ濃度が４質量％の第２の無電解Ｎｉメッキ層（厚さ１．６μｍ）を形成した金属被覆光ファイバ４（試料Ａ）を用いて、光部品用金属筐体５を作製した。これを金属筐体ａとする。図４に前記金属筐体の光ファイバ貫入部分の模式図を示す。前記金属筐体ａの孔６（径５００μｍ）に金属被覆光ファイバを貫入させ、前記金属被覆光ファイバ４の金属被覆３と前記孔６との隙間に溶融したハンダ７を流し込んで、前記隙間を封止した。金属被覆光ファイバ４の金属被覆３はハンダ７と合金を形成し、ハンダ接合を形成した。前記隙間の封止部の気密性を調べるために、８０℃に加熱したフロリナート液に金属筐体Aを浸漬させて封止部からの気泡発生の有無を確認した。８０℃に加熱するのは、金属筐体内の気圧を上昇させ封止部から気泡が発生しやすくさせるためである。金属被覆光ファイバ（試料Ａ）を用いて作製した２０個の金属筐体Ａを８０℃フロリナート液に浸漬させたところ、２０個すべてで封止部から気泡発生がなかった。封止部の気密性が良好であることが確認された。
(Example 2)
A first electroless Ni plating layer (thickness 0.4 μm) having a P concentration of 7% by mass is formed on the surface of the core wire, and the P concentration is 4% by mass on the first electroless Ni plating layer. Using the metal-coated optical fiber 4 (sample A) on which the second electroless Ni plating layer (thickness: 1.6 μm) was formed, a metal housing 5 for optical components was produced. This is a metal casing a. FIG. 4 shows a schematic view of the optical fiber penetration portion of the metal casing. A metal-coated optical fiber is inserted into the hole 6 (diameter 500 μm) of the metal casing a, and molten solder 7 is poured into the gap between the metal coating 3 of the metal-coated optical fiber 4 and the hole 6. Sealed. The metal coating 3 of the metal-coated optical fiber 4 formed an alloy with the solder 7 to form a solder joint. In order to examine the airtightness of the sealing portion in the gap, the metal casing A was immersed in a fluorinate solution heated to 80 ° C. to confirm whether bubbles were generated from the sealing portion. The reason for heating to 80 ° C. is to increase the atmospheric pressure in the metal casing and to easily generate bubbles from the sealing portion. When 20 metal casings A produced using a metal-coated optical fiber (sample A) were immersed in an 80 ° C. fluorinate solution, no bubbles were generated from the sealing portion in all 20. It was confirmed that the sealing part had good airtightness.
（比較例３、４）
比較のために、芯線表面上に、Ｐ濃度が４質量％の第１の無電解Ｎｉメッキ層（厚さ０．４μｍ）を形成し、前記第１の無電解Ｎｉメッキ層の上に、Ｐ濃度が１質量％の第２の無電解Ｎｉメッキ層（厚さ１．６μｍ）を形成した金属被覆光ファイバ（試料Ｂ）、および芯線表面上に、Ｐ濃度が１１質量％の第１の無電解Ｎｉメッキ層（厚さ０．４μｍ）を形成し、前記第１の無電解Ｎｉメッキ層の上に、Ｐ濃度が８質量％の第２の無電解Ｎｉメッキ層（厚さ１．６μｍ）を形成した金属被覆光ファイバを用いて、光部品用金属筐体を作製した。これらをそれぞれ金属筐体ｂ（比較例３）および金属筐体ｃ（比較例４）とする。実施例２と同様に、それぞれ２０個ずつの金属筐体ｂと金属筐体ｃを８０℃フロリナート液に浸漬させたところ、金属筐体Ｂでは３個、金属筐体Ｃでは４個の封止部から気泡が発生した。封止部の気密が不十分であることが確認された。金属筐体Ｂでは金属被覆と芯線との密着強度不足、金属筐体Ｃではハンダ接合時のハンダ濡れ性不足により、封止部に隙間が発生してしまったと考えられる。
(Comparative Examples 3 and 4)
For comparison, a first electroless Ni plating layer (thickness 0.4 μm) having a P concentration of 4 mass% is formed on the surface of the core wire, and P is formed on the first electroless Ni plating layer. A metal-coated optical fiber (sample B) on which a second electroless Ni plating layer (thickness 1.6 μm) having a concentration of 1% by mass is formed, and a first non-conductive layer having a P concentration of 11% by mass on the surface of the core wire. An electrolytic Ni plating layer (thickness 0.4 μm) is formed, and a second electroless Ni plating layer (thickness 1.6 μm) having a P concentration of 8 mass% is formed on the first electroless Ni plating layer. A metal casing for an optical component was manufactured using the metal-coated optical fiber formed with the. These are respectively referred to as a metal casing b (Comparative Example 3) and a metal casing c (Comparative Example 4). As in Example 2, 20 metal casings b and 20 metal casings c were each immersed in 80 ° C. fluorinate solution. As a result, three metal casings B and four metal casings C were sealed. Bubbles were generated from the part. It was confirmed that the sealing portion was not sufficiently airtight. It is considered that a gap was generated in the sealing portion due to insufficient adhesion strength between the metal coating and the core wire in the metal casing B, and insufficient solder wettability during solder joining in the metal casing C.
１：芯線 ２：保護被覆 ３：金属被覆 ４：金属被覆光ファイバ
５：金属筐体 ６：孔 ７：ハンダ ８：光ファイバ芯線
９：第１の無電解Ｎｉメッキ層 １０：第２の無電解Ｎｉメッキ層
1: Core wire 2: Protective coating 3: Metal coating 4: Metal coated optical fiber 5: Metal housing 6: Hole 7: Solder 8: Optical fiber core wire 9: First electroless Ni plating layer 10: Second electroless Ni plating layer
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