JP2022103538A - Nickel electroplating film, and plating structure - Google Patents

Nickel electroplating film, and plating structure Download PDF

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JP2022103538A
JP2022103538A JP2020218234A JP2020218234A JP2022103538A JP 2022103538 A JP2022103538 A JP 2022103538A JP 2020218234 A JP2020218234 A JP 2020218234A JP 2020218234 A JP2020218234 A JP 2020218234A JP 2022103538 A JP2022103538 A JP 2022103538A
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plating film
plating
film
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electrolytic plating
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JP7061247B1 (en
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薫 野村
Kaoru Nomura
岳彦 鈴木
Takehiko Suzuki
貴文 松岡
Takafumi Matsuoka
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Matsuda Sangyo Co Ltd
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Matsuda Sangyo Co Ltd
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Priority to TW110124466A priority patent/TWI787896B/en
Priority to JP2022506652A priority patent/JP7096955B1/en
Priority to PCT/JP2021/047335 priority patent/WO2022145290A1/en
Priority to CN202180065149.6A priority patent/CN116324002A/en
Priority to TW110148835A priority patent/TWI790062B/en
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C13/00—Alloys based on tin
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/48—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor
    • H01L23/50—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor for integrated circuit devices, e.g. power bus, number of leads

Abstract

To provide a Ni plating film excellent in solder wettability, and a plating structure comprising the Ni plating film.SOLUTION: The nickel electroplating film containing 0.01 wt.% or more and 1.0 wt.% or less of phosphorous, has a film thickness of 0.1 μm or more and 10 μm or less when the content of phosphorous is 0.01 wt.% or more and less than 0.05 wt.%, has a film thickness of 0.06 μm and 10 μm or less when the content of phosphorous is 0.05 wt.% or more and less than 0.2 wt.%, and has a film thickness of 0.01 μm or more and 10 μm or less when the content of phosphorous is 0.2 wt.% or more and 1.0 wt.% or less.SELECTED DRAWING: None

Description

本発明は、ニッケル電解めっき皮膜及び該めっき皮膜を備えためっき構造体に関し、特に、ＩＣやＬＳＩなどの半導体パッケージにおけるワイヤボンディングなどの接合部のめっき皮膜に関する。 The present invention relates to a nickel electrolytic plating film and a plating structure provided with the plating film, and more particularly to a plating film of a joint portion such as wire bonding in a semiconductor package such as an IC or LSI.

ＩＣやＬＳＩなどの半導体パッケージにおいて半導体素子を基板上に実装する方法として、バンプと呼ばれる突起状の端子によって電気的に接続するフリップチップという方法と、リードフレームを用いて外部配線と電気的に接続する（ワイヤボンディング）方法が知られている。フリップチップ実装に関しては、例えば、特許文献１～４には、半導体素子の接続端子部にＮｉ／Ｐｄ／Ａｕの無電解めっき皮膜を形成し、その上に、はんだバンプを形成することが開示されている。 As a method of mounting a semiconductor element on a substrate in a semiconductor package such as an IC or LSI, there is a method called a flip chip that is electrically connected by a protruding terminal called a bump, and a method of electrically connecting to an external wiring by using a lead frame. (Wire bonding) is known. Regarding flip chip mounting, for example, Patent Documents 1 to 4 disclose that a Ni / Pd / Au electroless plating film is formed on a connection terminal portion of a semiconductor element, and a solder bump is formed on the electroless plating film. ing.

一方、ワイヤボンディングに関して、本出願人は以前、電解めっきによって形成したＧｅ－Ｎｉ／Ｐｄ／Ａｕの三層からなるめっき構造に関する発明を提供した（特許文献５）。また、電解めっきによって、Ｎｉ／Ｐｄ－Ｐ／Ａｕ皮膜を形成する技術も知られている（特許文献６）。上記のめっき皮膜は電解めっき又は無電解めっきによって形成することが可能であるが、電解めっきと無電解めっきとは、各々メリットとデメリットがあるため、被めっき物に応じて使い分けられるのが通常である。 On the other hand, regarding wire bonding, the applicant has previously provided an invention relating to a plating structure composed of three layers of Ge—Ni / Pd / Au formed by electrolytic plating (Patent Document 5). Further, a technique for forming a Ni / Pd-P / Au film by electrolytic plating is also known (Patent Document 6). The above plating film can be formed by electrolytic plating or electroless plating, but since electroplating and electroless plating have advantages and disadvantages, they are usually used properly according to the object to be plated. be.

特開平１１－３４５８９６号公報Japanese Unexamined Patent Publication No. 11-345896 特開２００６－１７９７９７号公報Japanese Unexamined Patent Publication No. 2006-179977 国際公開第２００６／１１２２１５号International Publication No. 2006/11215 特開２０１６－１６２７７０号公報Japanese Unexamined Patent Publication No. 2016-162770 特開２００９－２２８０２１号公報Japanese Unexamined Patent Publication No. 2009-228021 特開２０１２－２４１２６０号公報Japanese Unexamined Patent Publication No. 2012-241260

リードフレームの表面処理法の一つとして、Ｐｄ－ＰＰＦ（Ｐｒｅ Ｐｌａｔｅｄ Ｆｒａｍｅ）という手法がある（特許文献６、参照）。これは、銅系のリードフレームの全面に、Ｎｉ／Ｐｄ／Ａｕの三層めっきを施したものであり、これによって、はんだ濡れ性を向上させることができ、十分な接合性能を得ることができるというものである。このＰｄ－ＰＰＦリードフレームにおけるコスト削減の試みとして、ＡｕやＰｄなどの貴金属皮膜の薄膜化が推し進められている。 As one of the surface treatment methods for lead frames, there is a method called Pd-PPF (Pre Plated Frame) (see Patent Document 6). This is a copper-based lead frame on which the entire surface is plated with three layers of Ni / Pd / Au, whereby the solder wettability can be improved and sufficient bonding performance can be obtained. That is. As an attempt to reduce costs in this Pd-PPF lead frame, thinning of precious metal films such as Au and Pd is being promoted.

貴金属めっき皮膜の薄膜化は、はんだ濡れ性を損なわないようにしなければならない。この効果を維持できているかの判定は、めっき皮膜に対して加熱処理後のはんだ濡れ性を評価することで行われている。例えば、特許文献５に記載されているように、めっき皮膜を形成した試験片を加熱処理後、はんだ浴に浸漬し、濡れ応力値がゼロになるまでの時間（ゼロクロスタイム：ＺＴＣ）を測定し、この時間が十分に短ければ、はんだ濡れ性を保っているとみなすことができる。 The thinning of the noble metal plating film must not impair the solder wettability. Whether or not this effect can be maintained is determined by evaluating the solder wettability of the plating film after the heat treatment. For example, as described in Patent Document 5, after heat-treating the test piece on which the plating film is formed, the test piece is immersed in a solder bath, and the time until the wet stress value becomes zero (zero cross time: ZTC) is measured. If this time is short enough, it can be considered that the solder wettability is maintained.

現在の技術では、Ａｕ、Ｐｄめっき皮膜は数ｎｍ～数十ｎｍでも十分なはんだ濡れ性を維持できるまでになっており、貴金属めっき皮膜の薄膜化によるコスト低減は限界に達している。一方、Ｎｉめっき膜については、未だ改善の余地があり、Ｎｉめっき膜の特性（はんだ濡れ性）を改善することで薄膜化を可能とし、タクトタイムの短縮によるさらなるコスト低減が期待できる。本発明は、このような問題に鑑みてなされたものであって、その目的は、はんだ濡れ性に優れた、Ｎｉめっき皮膜及び該Ｎｉめっき皮膜を備えためっき構造体を提供することを課題とする。 With the current technology, Au and Pd plating films can maintain sufficient solder wettability even at several nm to several tens of nm, and cost reduction by thinning the noble metal plating film has reached the limit. On the other hand, there is still room for improvement in the Ni-plated film, and by improving the characteristics (solder wetting property) of the Ni-plated film, it is possible to make the film thinner, and further cost reduction can be expected by shortening the tact time. The present invention has been made in view of such a problem, and an object of the present invention is to provide a Ni plating film having excellent solder wettability and a plating structure provided with the Ni plating film. do.

上記課題を解決するために、本発明者は鋭意研究を行った結果、Ｎｉ電解めっき皮膜に所定量のＰ（リン）を含有させることにより、はんだ濡れ性に優れたＮｉ電解めっき皮膜を形成することができるとの知見が得られ、本発明を完成するに至った。前記課題は、以下に示す手段によって解決される。 In order to solve the above problems, the present inventor has conducted diligent research to form a Ni electrolytic plating film having excellent solder wettability by containing a predetermined amount of P (phosphorus) in the Ni electrolytic plating film. It was found that this can be done, and the present invention has been completed. The problem is solved by the means shown below.

１）リンを０．０１ｗｔ％以上１．０ｗｔ％以下含有するニッケル電解めっき皮膜であり、リンの含有量が０．０１ｗｔ％以上０．０５ｗｔ％未満のとき、前記ニッケル電解めっき皮膜の膜厚が０．１μｍ以上１０μｍ以下であり、リンの含有量が０．０５ｗｔ％以上０．２ｗｔ％未満のとき、前記ニッケル電解めっき皮膜の膜厚が０．０６μｍ以上１０μｍ以下であり、リンの含有量が０．２ｗｔ％以上１．０ｗｔ％以下のとき、前記ニッケル電解めっき皮膜の膜厚が０．０１μｍ以上１０μｍ以下であるニッケル電解めっき皮膜。
２）ニッケル電解めっき皮膜と、ニッケル電解めっき皮膜の上に形成されたパラジウムめっき皮膜と、パラジウムめっき皮膜の上に形成された金めっき皮膜、の３層からなるめっき構造体であって、前記ニッケル電解めっき皮膜が上記１）に記載のニッケル電解めっき皮膜であるめっき構造体。
３）ニッケル電解めっき皮膜と、ニッケル電解めっき皮膜の上に形成されたパラジウムめっき皮膜、の２層からなるめっき構造体であって、前記ニッケル電解めっき皮膜が上記１）に記載のニッケル電解めっき皮膜であるめっき構造体。
４）ニッケル電解めっき皮膜と、ニッケル電解めっき皮膜の上に形成された金めっき皮膜、の２層からなるめっき構造体であって、前記ニッケル電解めっき皮膜が上記１）に記載のニッケル電解めっき皮膜であるめっき構造体。
５）上記２）～４）のいずれか一に記載のめっき構造体を備えたリードフレーム。 1) A nickel electrolytic plating film containing 0.01 wt% or more and 1.0 wt% or less of phosphorus, and when the phosphorus content is 0.01 wt% or more and less than 0.05 wt%, the film thickness of the nickel electrolytic plating film is When it is 0.1 μm or more and 10 μm or less and the phosphorus content is 0.05 wt% or more and less than 0.2 wt%, the thickness of the nickel electrolytic plating film is 0.06 μm or more and 10 μm or less, and the phosphorus content is A nickel electrolytic plating film having a thickness of 0.01 μm or more and 10 μm or less when the thickness is 0.2 wt% or more and 1.0 wt% or less.
2) A plating structure consisting of three layers of a nickel electrolytic plating film, a palladium plating film formed on the nickel electrolytic plating film, and a gold plating film formed on the palladium plating film. A plating structure in which the electrolytic plating film is the nickel electrolytic plating film according to 1) above.
3) A plating structure consisting of two layers, a nickel electrolytic plating film and a palladium plating film formed on the nickel electrolytic plating film, wherein the nickel electrolytic plating film is the nickel electrolytic plating film according to 1) above. The plating structure that is.
4) A plating structure consisting of two layers, a nickel electrolytic plating film and a gold plating film formed on the nickel electrolytic plating film, wherein the nickel electrolytic plating film is the nickel electrolytic plating film according to 1) above. The plating structure that is.
5) A lead frame provided with the plating structure according to any one of 2) to 4) above.

本発明によれば、はんだ濡れ性に優れたＮｉ電解めっき皮膜を得ることができるという優れた効果を有する。また、良好なはんだ濡れ性を維持しつつ、Ｎｉめっき電解皮膜の薄膜化を達成することができるという優れた効果を有する。めっき皮膜の成膜工程において、特に成膜時間がかかっているのは、Ｎｉめっき皮膜であることから、Ｎｉめっき皮膜を薄膜化することで、タクトタイムの大幅な短縮につなげることができる。 According to the present invention, it has an excellent effect that a Ni electrolytic plating film having excellent solder wettability can be obtained. Further, it has an excellent effect that the thinning of the Ni-plated electrolytic film can be achieved while maintaining good solder wettability. In the process of forming a plating film, it is the Ni plating film that takes a particularly long time to form, so thinning the Ni plating film can lead to a significant reduction in tact time.

無電解めっきは、電気を使用しないため、電気の流れに左右されることなく、均一にめっきすることができる一方、化学反応を用いて皮膜を形成するため、皮膜を形成する速度が遅く、また、めっき浴を化学的に安定させる必要があり、薬液やめっき槽の維持管理にコストがかかるということがある。このような事情から、リードフレームの全面にめっき皮膜を形成する場合には、通常、電解めっきによって、めっき皮膜を形成することが行われる。 Since electroless plating does not use electricity, it can be plated uniformly without being affected by the flow of electricity, but because it forms a film using a chemical reaction, the rate of forming the film is slow and it is also possible. , It is necessary to chemically stabilize the plating bath, and maintenance of the chemical solution and the plating tank may be costly. Under these circumstances, when a plating film is formed on the entire surface of the lead frame, the plating film is usually formed by electrolytic plating.

本発明者は、このような電解めっき皮膜におけるはんだ濡れ性改善について鋭意研究したところ、Ｎｉ電解めっき皮膜に所定量のＰ（リン）を含有させることにより、めっき皮膜のはんだ濡れ性を向上させることができることを見出した。特にＮｉめっき皮膜を薄くした場合であっても、十分なはんだ濡れ性を維持することができることを見出した。これによって、Ｎｉめっき皮膜の薄膜化によるタクトタイムを短縮でき、コストの低減が見込まれる。 The present inventor has earnestly studied the improvement of solder wettability in such an electrolytic plating film, and found that the solder wettability of the plating film is improved by containing a predetermined amount of P (phosphorus) in the Ni electrolytic plating film. I found that I could do it. In particular, it has been found that sufficient solder wettability can be maintained even when the Ni plating film is thinned. As a result, the tact time due to the thinning of the Ni plating film can be shortened, and the cost is expected to be reduced.

本発明の実施形態に係るＮｉ電解めっき皮膜は、Ｐ（リン）を０．０１ｗｔ％以上、１．０ｗｔ％以下含有することを特徴とする。Ｎｉめっき皮膜中のリン含有量を上記の範囲とすることにより、Ｎｉめっき皮膜のはんだ濡れ性を良好なものとすることができる。一方、リン含有量が０．０１ｗｔ％未満であると、はんだ濡れ性向上の効果が得られず、また、リン含有量が１．０ｗｔ％を超えると、はんだ濡れ性は逆に低下する。好ましくはリン含有量が０．０８ｗｔ％以上０．８ｗｔ％以下、より好ましくはリン含有量が０．１８ｗｔ％以上０．６１ｗｔ％以下とする。 The Ni electrolytic plating film according to the embodiment of the present invention is characterized by containing 0.01 wt% or more and 1.0 wt% or less of P (phosphorus). By setting the phosphorus content in the Ni plating film within the above range, the solder wettability of the Ni plating film can be improved. On the other hand, if the phosphorus content is less than 0.01 wt%, the effect of improving the solder wettability cannot be obtained, and if the phosphorus content exceeds 1.0 wt%, the solder wettability is conversely lowered. The phosphorus content is preferably 0.08 wt% or more and 0.8 wt% or less, and more preferably the phosphorus content is 0.18 wt% or more and 0.61 wt% or less.

Ｐ（リン）を含有したＮｉ電解めっき皮膜を走査型電子顕微鏡で観察すると、リン含有量の増加に伴って、Ｎｉ電解めっき皮膜の粒子が微細化する傾向が見られた。また、このＮｉ電解めっき皮膜を加熱すると加熱前と比較して結晶が拡大していたが、リン含有量が高いほど、結晶拡大が抑制されている様子が見られた。このような結晶微細化は粒界にリンが濃縮して、結晶成長を阻害したためと考えられる。はんだ濡れ性の低下は下地金属（Ｃｕ又はＣｕ合金など）がめっき皮膜最表面まで拡散し、大気に曝されて酸化することが原因であると考えられているが、このような粒界に濃縮したリンが、下地金属の拡散を抑制して、はんだ濡れ性の低下を抑制していると考えられる。 When the Ni electrolytic plating film containing P (phosphorus) was observed with a scanning electron microscope, the particles of the Ni electrolytic plating film tended to become finer as the phosphorus content increased. Further, when the Ni electrolytic plating film was heated, the crystals expanded as compared with those before heating, but it was observed that the higher the phosphorus content, the more the crystal expansion was suppressed. It is considered that such crystal refinement is due to the concentration of phosphorus at the grain boundaries and inhibition of crystal growth. It is thought that the decrease in solder wettability is caused by the fact that the base metal (Cu or Cu alloy, etc.) diffuses to the outermost surface of the plating film and is exposed to the atmosphere to oxidize. It is considered that the resulting phosphorus suppresses the diffusion of the base metal and suppresses the deterioration of the solder wettability.

Ｎｉ電解めっき皮膜の膜厚は、リンの含有量との関係で決定することができ、リンの含有量が０．０１ｗｔ％以上０．０５ｗｔ％未満のとき、前記ニッケル電解めっき皮膜の膜厚が０．１μｍ以上１０μｍ以下であり、リンの含有量が０．０５ｗｔ％以上０．２ｗｔ％未満のとき、前記ニッケル電解めっき皮膜の膜厚が０．０６μｍ以上１０μｍ以下であり、リンの含有量が０．２ｗｔ％以上１．０ｗｔ％以下のとき、前記ニッケル電解めっき皮膜の膜厚が０．０１μｍ以上１０μｍ以下とする。
本実施形態のＮｉ電解めっき皮膜は、Ｎｉ電解めっき皮膜の膜厚を１μｍ以下と薄膜化した場合であっても、良好なはんだ濡れ性を確保することができる点で、特に優れているといえる。 The film thickness of the Ni electrolytic plating film can be determined in relation to the phosphorus content, and when the phosphorus content is 0.01 wt% or more and less than 0.05 wt%, the film thickness of the nickel electrolytic plating film is When it is 0.1 μm or more and 10 μm or less and the phosphorus content is 0.05 wt% or more and less than 0.2 wt%, the thickness of the nickel electrolytic plating film is 0.06 μm or more and 10 μm or less, and the phosphorus content is When it is 0.2 wt% or more and 1.0 wt% or less, the thickness of the nickel electrolytic plating film is 0.01 μm or more and 10 μm or less.
It can be said that the Ni electrolytic plating film of the present embodiment is particularly excellent in that good solder wettability can be ensured even when the film thickness of the Ni electrolytic plating film is reduced to 1 μm or less. ..

リンの含有量が０．０１ｗｔ％以上０．０５ｗｔ％未満のとき、Ｎｉめっき皮膜の膜厚が０．１μｍよりも薄いと、下地金属（Ｃｕ又はＣｕ合金）の拡散防止効果が弱くなり、表面にＣｕの酸化物が形成し、はんだ濡れ性が低下する。
また、リンの含有量が０．０５ｗｔ％以上０．２ｗｔ％未満のとき、Ｎｉめっき皮膜の膜厚が０．０６μｍよりも薄いと、下地金属（Ｃｕ又はＣｕ合金）の拡散防止効果が弱くなり、表面にＣｕの酸化物が形成し、はんだ濡れ性が低下する。
さらに、リンの含有量が０．２ｗｔ％以上１．０ｗｔ％以下のとき、前記ニッケル電解めっき皮膜の膜厚が０．０１μｍよりも薄いと、上記と同様、下地金属の拡散防止機能が弱くなり、はんだ濡れ性が低下する。
好ましくは膜厚が０．０６μｍ以上、より好ましくは膜厚が０．１μｍ以上、さらに好ましくは膜厚が０．２μｍ以上である。
なお、Ｎｉ電解めっき皮膜の膜厚が厚いほど、はんだ濡れ性が高くなるが、必要以上に膜厚が厚いと、余分なＮｉを付着させることとなり、コストが増加する。したがって膜厚は１０μｍ以下とし、より好ましくは５μｍ以下、さらに好ましくは１μｍ以下、最も好ましくは０．５μｍ以下である。 When the phosphorus content is 0.01 wt% or more and less than 0.05 wt%, if the thickness of the Ni plating film is thinner than 0.1 μm, the diffusion prevention effect of the base metal (Cu or Cu alloy) is weakened, and the surface surface is weakened. Cu oxide is formed on the surface, and the solder wettability is lowered.
Further, when the phosphorus content is 0.05 wt% or more and less than 0.2 wt%, if the thickness of the Ni plating film is thinner than 0.06 μm, the diffusion prevention effect of the base metal (Cu or Cu alloy) becomes weak. , Cu oxide is formed on the surface, and the solder wettability is lowered.
Further, when the phosphorus content is 0.2 wt% or more and 1.0 wt% or less and the film thickness of the nickel electrolytic plating film is thinner than 0.01 μm, the diffusion prevention function of the base metal is weakened as described above. , Solder wettability is reduced.
The film thickness is preferably 0.06 μm or more, more preferably 0.1 μm or more, and further preferably 0.2 μm or more.
The thicker the film thickness of the Ni electrolytic plating film, the higher the solder wettability. However, if the film thickness is thicker than necessary, excess Ni will be attached and the cost will increase. Therefore, the film thickness is 10 μm or less, more preferably 5 μm or less, further preferably 1 μm or less, and most preferably 0.5 μm or less.

本発明の実施形態に係るめっき構造体は、以下の構造を採用することができる。
３層構造：（基板）／Ｎｉめっき皮膜／Ｐｄめっき皮膜／Ａｕめっき皮膜（最表面）
２層構造：（基板）／Ｎｉめっき皮膜／Ｐｄめっき皮膜（最表面）
２層構造：（基板）／Ｎｉめっき皮膜／Ａｕめっき皮膜（最表面）
ここで、上記Ｎｉめっき皮膜は、本実施形態に係るＰ含有Ｎｉ電解めっき皮膜である。上記いずれのめっき皮膜も電解めっき皮膜によって形成することができる。また、Ｐｄめっき皮膜は純Ｐｄだけでなく、Ｐｄ合金であってもよい。上記めっき構造体は、用途や要求特性によって選択することができる。最表面に形成されるＡｕめっき皮膜やＰｄめっき皮膜は、Ｎｉめっき皮膜の酸化防止やＮｉの表面への拡散防止を主な目的としている。 The following structure can be adopted as the plating structure according to the embodiment of the present invention.
3-layer structure: (Substrate) / Ni plating film / Pd plating film / Au plating film (outermost surface)
Two-layer structure: (board) / Ni plating film / Pd plating film (outermost surface)
Two-layer structure: (Substrate) / Ni plating film / Au plating film (outermost surface)
Here, the Ni plating film is the P-containing Ni electrolytic plating film according to the present embodiment. Any of the above plating films can be formed by an electrolytic plating film. Further, the Pd plating film may be not only pure Pd but also a Pd alloy. The plating structure can be selected according to the application and required characteristics. The Au plating film and Pd plating film formed on the outermost surface have the main purpose of preventing oxidation of the Ni plating film and preventing diffusion of Ni onto the surface.

本発明の他の実施形態は、上記めっき構造体を備えたリードフレームである。リードフレームは、銅又は銅合金から構成されることが多い。このようなリードフレーム上に本実施形態に係るめっき構造体を形成することにより、ワイヤボンディングやはんだ付けにおいて、優れた接合が可能となる。なお、本実施形態に係るめっき構造体は、リードフレームだけではなく、フリップチップ実装で使用されるはんだパッド部分に形成することも可能であり、同様に優れた接合が得られることが推測できる。 Another embodiment of the present invention is a lead frame provided with the above-mentioned plated structure. Lead frames are often composed of copper or copper alloys. By forming the plating structure according to the present embodiment on such a lead frame, excellent bonding is possible in wire bonding and soldering. The plating structure according to the present embodiment can be formed not only on the lead frame but also on the solder pad portion used in flip chip mounting, and it can be inferred that similarly excellent bonding can be obtained.

ところで、被めっき物によっては、Ｎｉ／Ｐｄ／Ａｕのめっき膜を無電解めっきによって形成することも行われている。無電解めっきの場合には、めっき液中の還元剤としてリン化合物が使用されることがあり、その場合、Ｎｉ皮膜にはＰ（リン）が必然的に含まれることなる。リン化合物以外の還元剤を使用することで、Ｐ含有量が０ｗｔ％のＮｉ皮膜を形成することも可能であるが、還元剤由来のため、Ｎｉ皮膜中のＰ含有量を２ｗｔ％以下で制御することは非常に困難である。 By the way, depending on the object to be plated, a Ni / Pd / Au plating film may be formed by electroless plating. In the case of electroless plating, a phosphorus compound may be used as a reducing agent in the plating solution, and in that case, P (phosphorus) is inevitably contained in the Ni film. It is possible to form a Ni film with a P content of 0 wt% by using a reducing agent other than a phosphorus compound, but since it is derived from a reducing agent, the P content in the Ni film is controlled to 2 wt% or less. It's very difficult to do.

本実施形態に係るＮｉめっき皮膜は、リン化合物を含むニッケルめっき浴を用いて、電解めっきにより形成することができる。リン化合物として、次亜リン酸、亜リン酸、リン酸などを用いることができる。また、他のリンを含有した化合物でも代替可能である。ニッケルめっき浴は、ワット浴、スルファミン浴、クエン酸浴などを用いることができる。また、他のニッケルを含有するめっき浴でも代替可能である。上記に示したリン化合物やニッケルめっき浴は例示的なものであって、限定的なものではない。
Ｎｉめっき浴中のニッケル塩の量は、金属換算で４０～１２５ｇ／Ｌとすることができる。また、リン化合物の量は、リン換算で５～３００ｍｇ／Ｌとすることができる。上記に示したニッケル塩の量やリン化合物の量は例示的なものであって、開示した範囲に限定する意図はないことを理解されたい。 The Ni plating film according to this embodiment can be formed by electrolytic plating using a nickel plating bath containing a phosphorus compound. As the phosphorus compound, hypophosphoric acid, phosphoric acid, phosphoric acid and the like can be used. Further, other phosphorus-containing compounds can be substituted. As the nickel plating bath, a watt bath, a sulfamic acid bath, a citric acid bath and the like can be used. Further, a plating bath containing other nickel can be used as an alternative. The phosphorus compounds and nickel plating baths shown above are exemplary and not limited.
The amount of nickel salt in the Ni plating bath can be 40 to 125 g / L in terms of metal. The amount of the phosphorus compound can be 5 to 300 mg / L in terms of phosphorus. It should be understood that the amounts of nickel salts and phosphorus compounds shown above are exemplary and are not intended to be limited to the disclosed scope.

Ｎｉ電解めっき条件は以下の通りとすることができる。但し、この電解めっき条件は例示的なものであって、Ｎｉ電解めっきを実施するための多くの処理システムや処理装置が存在し、その処理システムや処理装置に応じて、電解めっき条件の変更を行ってもよいことは明らかである。したがって、開示する電解めっき条件に限定する意図はないことに注意されたい。
陰極電流密度： １～１０Ａ／ｄｍ２
電解時間： ５～３０ｍｉｎ
ｐＨ： ３～６
浴温： ３０～６０℃
カソード： 銅又は銅合金
アノード： ニッケル The Ni electrolytic plating conditions can be as follows. However, this electrolytic plating condition is an example, and there are many processing systems and processing devices for carrying out Ni electrolytic plating, and the electrolytic plating conditions can be changed according to the processing system and processing device. It is clear that you can go. Therefore, it should be noted that there is no intention to limit to the disclosed electroplating conditions.
Cathode current density: 1-10A / dm 2
Electrolysis time: 5 to 30 min
pH: 3-6
Bath temperature: 30-60 ° C
Cathode: Copper or copper alloy Anode: Nickel

Ｐｄめっき皮膜およびＡｕめっき皮膜については、公知のめっき浴、公知の電解めっき条件を用いて、形成することができる（例えば、特許文献５）。 The Pd plating film and the Au plating film can be formed by using a known plating bath and known electrolytic plating conditions (for example, Patent Document 5).

次に、本発明の実施例及び比較例について説明する。なお、以下の実施例はあくまで代表的な例を示しているもので、本願発明は、これらの実施例に制限される必要はなく、明細書の記載される技術思想の範囲で解釈されるべきものである。 Next, Examples and Comparative Examples of the present invention will be described. It should be noted that the following examples show only representative examples, and the invention of the present application does not have to be limited to these examples and should be interpreted within the scope of the technical idea described in the specification. It is a thing.

＜評価サンプルの作製について＞
Ｃｕ合金からなるリードフレームに、前処理として、電解脱脂（液温：６８℃、電流密度：１０Ａ／ｄｍ２、浸漬時間：６０秒）を行い、次いで、酸洗浄（５ｖｏｌ．％硫酸、３０秒）を行い、その後、純水で洗浄した。前処理したリードフレームに、順次、以下のめっき条件にて、Ｎｉめっき、Ｐｄめっき、Ａｕめっき、を施した。このとき、Ｎｉめっき液中のＰ濃度を変化させて、評価サンプルを調整した。 <Preparation of evaluation sample>
The lead frame made of Cu alloy is subjected to electrolytic degreasing (liquid temperature: 68 ° C., current density: 10 A / dm 2 , immersion time: 60 seconds) as a pretreatment, and then pickled (5 vol.% Sulfuric acid, 30 seconds). ), And then washed with pure water. The pretreated lead frames were sequentially subjected to Ni plating, Pd plating, and Au plating under the following plating conditions. At this time, the evaluation sample was adjusted by changing the P concentration in the Ni plating solution.

（Ｎｉめっき条件）
めっき浴： リン化合物を含む無光沢ワット浴
Ｎｉ濃度： ６６ｇ／Ｌ
Ｐ濃度： ０～２００ｍｇ／Ｌ
電流密度： ５Ａ／ｄｍ２
浴温： ５０℃
ｐＨ： ４
狙い膜厚： ０．１３μｍ (Ni plating conditions)
Plating bath: Matte watt bath containing phosphorus compound Ni concentration: 66 g / L
P concentration: 0-200 mg / L
Current density: 5A / dm 2
Bath temperature: 50 ° C
pH: 4
Target film thickness: 0.13 μm

（Ｐｄめっき条件）
めっき浴： パラジウムめっき液（松田産業株式会社製：パラシグマＵＦ）
Ｐｄ濃度： ３ｇ／Ｌ
電流密度： ０．５Ａ／ｄｍ２
浴温： ４０℃
ｐＨ： ６．５
狙い膜厚： ０．０２５μｍ
アノード： 酸化イリジウム (Pd plating conditions)
Plating bath: Palladium plating solution (manufactured by Matsuda Sangyo Co., Ltd .: Parasigma UF)
Pd concentration: 3 g / L
Current density: 0.5A / dm 2
Bath temperature: 40 ° C
pH: 6.5
Target film thickness: 0.025 μm
Anode: Iridium oxide

（Ａｕめっき条件）
めっき浴： 金めっき液（松田産業株式会社製：オーロシグマＦ）
Ａｕ濃度： ２ｇ／Ｌ
電流密度： ２Ａ／ｄｍ２
浴温： ４５℃
ｐＨ： ４
狙い膜厚： ０．００５μｍ
アノード： 酸化イリジウム (Au plating conditions)
Plating bath: Gold plating solution (manufactured by Matsuda Sangyo Co., Ltd .: Aurora Sigma F)
Au concentration: 2 g / L
Current density: 2A / dm 2
Bath temperature: 45 ° C
pH: 4
Target film thickness: 0.005 μm
Anode: Iridium oxide

（リン含有量の測定）
各評価サンプルのＮｉめっき皮膜中のリン含有量の測定は、高周波誘導結合プラズマ（ＩＣＰ）発光分光分析装置を用いて測定した。 (Measurement of phosphorus content)
The phosphorus content in the Ni plating film of each evaluation sample was measured using a radio frequency inductively coupled plasma (ICP) emission spectrophotometer.

（はんだ濡れ性の評価）
各評価サンプルを所定の温度条件（４００℃±２℃）で時間保持することによって、高温の熱履歴を加えた後、はんだ浴（６３％－Ｓｎ、３７％－Ｐｂ、液温：２３０℃±５℃）に浸漬してから、該はんだ浴より受ける力がゼロになるまでの所要時間（ゼロクロスタイム）を測定し、はんだ濡れ性を評価した。ゼロクロスタイムは、短いほどはんだ濡れ性に優れていることを意味する。はんだ浴への浸漬条件は、浸漬深さを１ｍｍ、浸漬速度を２ｍｍ／秒、浸漬時間を５秒とし、はんだ付け促進剤として、Ｒ－ｔｙｐｅフラックス（非活性タイプ）を用いた。 (Evaluation of solder wettability)
After adding a high-temperature thermal history by holding each evaluation sample under a predetermined temperature condition (400 ° C ± 2 ° C) for a long time, a solder bath (63% -Sn, 37% -Pb, liquid temperature: 230 ° C ± The time required from immersion in 5 ° C. to zero the force received from the solder bath (zero cross time) was measured, and the solder wettability was evaluated. Zero cross time means that the shorter the time, the better the solder wettability. The dipping conditions in the solder bath were a dipping depth of 1 mm, a dipping speed of 2 mm / sec, and a dipping time of 5 seconds, and R-type flux (inactive type) was used as the soldering accelerator.

＜Ｎｉめっき膜のＰ含有量の評価＞
Ｎｉ皮膜中に含まれるＰ含有量とゼロクロスタイムの関係を表１に示す。表１に示す通り、リンを加えることで、はんだ濡れ性が改善されることが確認された。特にリン含有量が０．１ｗｔ％以上、０．８ｗｔ％以下の場合、はんだ濡れ性が大幅に改善されていた。なお、一般にＰｄフリーはんだの方が、Ｐｄ－Ｓｎはんだよりもはんだ濡れ性が悪いものであるが、Ｐｄフリーはんだ（Ｓｎ－３．０Ａｇ－０．５Ａｕ）を用いた場合でも、はんだ濡れ性に問題がないことを確認している。 <Evaluation of P content of Ni plating film>
Table 1 shows the relationship between the P content contained in the Ni film and the zero cross time. As shown in Table 1, it was confirmed that the solder wettability was improved by adding phosphorus. In particular, when the phosphorus content was 0.1 wt% or more and 0.8 wt% or less, the solder wettability was significantly improved. In general, Pd-free solder has poorer solder wettability than Pd-Sn solder, but even when Pd-free solder (Sn-3.0Ag-0.5Au) is used, the solder wettability is improved. I have confirmed that there are no problems.

Figure 2022103538000001
Figure 2022103538000001

＜Ｎｉめっき膜の薄膜化の評価＞
Ｎｉめっき液中のＰ濃度を５．４ｍｇ／Ｌ、１０．９ｍｇ／Ｌ、３２．７ｍｇ／Ｌ、７６．３ｍｇ／Ｌ、１１９．９ｍｇ／Ｌとし、Ｎｉめっき膜厚を表２の通りに変化させた以外は、上記と同様のめっき条件で、評価サンプルを作製した。そして、各種サンプルに対して、上記と同様の条件ではんだ濡れ性を評価した。なお、めっき膜厚が０．１３μｍについては、表１の結果をそのまま引用したものである。その結果を表２に示す。表２に示す通り、Ｎｉめっき皮膜の膜厚が１．０μｍ以下であっても、良好なはんだ濡れ性を維持できていることが確認できた。なお、Ｎｉめっき膜の膜厚を厚くするほど、はんだ濡れ性が向上することから、膜厚０．３μｍ超については、実施例に示していないが、はんだ濡れ性が問題ないことを確認している。 <Evaluation of thinning of Ni plating film>
The P concentration in the Ni plating solution was 5.4 mg / L, 10.9 mg / L, 32.7 mg / L, 76.3 mg / L, 119.9 mg / L, and the Ni plating film thickness was changed as shown in Table 2. An evaluation sample was prepared under the same plating conditions as above, except that the plating conditions were the same as above. Then, the solder wettability of various samples was evaluated under the same conditions as above. For the plating film thickness of 0.13 μm, the results in Table 1 are quoted as they are. The results are shown in Table 2. As shown in Table 2, it was confirmed that good solder wettability could be maintained even when the film thickness of the Ni plating film was 1.0 μm or less. The thicker the film thickness of the Ni plating film, the better the solder wettability. Therefore, although the film thickness of more than 0.3 μm is not shown in the examples, it is confirmed that there is no problem with the solder wettability. There is.

Figure 2022103538000002
Figure 2022103538000002

本発明は、はんだ濡れ性に優れたＮｉ電解めっき皮膜を得ることができるという優れた効果を有する。また、良好なはんだ濡れ性を維持しつつ、Ｎｉめっき電解皮膜の薄膜化を達成することができるという優れた効果を有する。本発明に係る電解めっき皮膜やめっき皮膜構造体は、リードフレーム、プリント配線板、リジッド基板、フレキシブル基板、テープキャリア、コネクタ、パワーデバイス、ワイヤー、ピン、等に有用である。
The present invention has an excellent effect that a Ni electrolytic plating film having excellent solder wettability can be obtained. Further, it has an excellent effect that the thinning of the Ni-plated electrolytic film can be achieved while maintaining good solder wettability. The electrolytic plating film and the plating film structure according to the present invention are useful for lead frames, printed wiring boards, rigid boards, flexible boards, tape carriers, connectors, power devices, wires, pins, and the like.

貴金属めっき皮膜の薄膜化は、はんだ濡れ性を損なわないようにしなければならない。この効果を維持できているかの判定は、めっき皮膜に対して加熱処理後のはんだ濡れ性を評価することで行われている。例えば、特許文献５に記載されているように、めっき皮膜を形成した試験片を加熱処理後、はんだ浴に浸漬し、濡れ応力値がゼロになるまでの時間（ゼロクロスタイム：ＺＣＴ）を測定し、この時間が十分に短ければ、はんだ濡れ性を保っているとみなすことができる。 The thinning of the noble metal plating film must not impair the solder wettability. Whether or not this effect can be maintained is determined by evaluating the solder wettability of the plating film after the heat treatment. For example, as described in Patent Document 5, after heat-treating the test piece on which the plating film is formed, the test piece is immersed in a solder bath, and the time until the wet stress value becomes zero (zero cross time: ZCT ) is measured. If this time is short enough, it can be considered that the solder wettability is maintained.

＜Ｎｉめっき膜のＰ含有量の評価＞
Ｎｉ皮膜中に含まれるＰ含有量とゼロクロスタイムの関係を表１に示す。表１に示す通り、リンを加えることで、はんだ濡れ性が改善されることが確認された。特にリン含有量が０．１ｗｔ％以上、０．８ｗｔ％以下の場合、はんだ濡れ性が大幅に改善されていた。なお、一般にＰｂフリーはんだの方が、Ｐｂ－Ｓｎはんだよりもはんだ濡れ性が悪いものであるが、Ｐｂフリーはんだ（Ｓｎ－３．０Ａｇ－０．５Ｃｕ）を用いた場合でも、はんだ濡れ性に問題がないことを確認している。 <Evaluation of P content of Ni plating film>
Table 1 shows the relationship between the P content contained in the Ni film and the zero cross time. As shown in Table 1, it was confirmed that the solder wettability was improved by adding phosphorus. In particular, when the phosphorus content was 0.1 wt% or more and 0.8 wt% or less, the solder wettability was significantly improved. In general, Pb -free solder has poorer solder wettability than Pb -Sn solder, but even when Pb -free solder (Sn-3.0Ag-0.5 Cu ) is used, solder wettability I have confirmed that there is no problem with.

Claims (5)

リンを０．０１ｗｔ％以上１．０ｗｔ％以下含有するニッケル電解めっき皮膜であり、リンの含有量が０．０１ｗｔ％以上０．０５ｗｔ％未満のとき、前記ニッケル電解めっき皮膜の膜厚が０．１μｍ以上１０μｍ以下であり、リンの含有量が０．０５ｗｔ％以上０．２ｗｔ％未満のとき、前記ニッケル電解めっき皮膜の膜厚が０．０６μｍ以上１０μｍ以下であり、リンの含有量が０．２ｗｔ％以上１．０ｗｔ％以下のとき、前記ニッケル電解めっき皮膜の膜厚が０．０１μｍ以上１０μｍ以下であるニッケル電解めっき皮膜。 A nickel electrolytic plating film containing 0.01 wt% or more and 1.0 wt% or less of phosphorus, and when the phosphorus content is 0.01 wt% or more and less than 0.05 wt%, the thickness of the nickel electrolytic plating film is 0. When the thickness is 1 μm or more and 10 μm or less and the phosphorus content is 0.05 wt% or more and less than 0.2 wt%, the thickness of the nickel electrolytic plating film is 0.06 μm or more and 10 μm or less, and the phosphorus content is 0. A nickel electrolytic plating film having a thickness of 0.01 μm or more and 10 μm or less when the thickness is 2 wt% or more and 1.0 wt% or less. ニッケル電解めっき皮膜と、ニッケル電解めっき皮膜の上に形成されたパラジウムめっき皮膜と、パラジウムめっき皮膜の上に形成された金めっき皮膜、の３層からなるめっき構造体であって、前記ニッケル電解めっき皮膜が請求項１に記載のニッケル電解めっき皮膜であるめっき構造体。 It is a plating structure consisting of three layers of a nickel electrolytic plating film, a palladium plating film formed on the nickel electrolytic plating film, and a gold plating film formed on the palladium plating film, and is the nickel electrolytic plating. A plating structure in which the film is the nickel electrolytic plating film according to claim 1. ニッケル電解めっき皮膜と、ニッケル電解めっき皮膜の上に形成されたパラジウムめっき皮膜、の２層からなるめっき構造体であって、前記ニッケル電解めっき皮膜が請求項１に記載のニッケル電解めっき皮膜であるめっき構造体。 It is a plating structure composed of two layers of a nickel electrolytic plating film and a palladium plating film formed on the nickel electrolytic plating film, and the nickel electrolytic plating film is the nickel electrolytic plating film according to claim 1. Plating structure. ニッケル電解めっき皮膜と、ニッケル電解めっき皮膜の上に形成された金めっき皮膜、の２層からなるめっき構造体であって、前記ニッケル電解めっき皮膜が請求項１に記載のニッケル電解めっき皮膜であるめっき構造体。 It is a plating structure composed of two layers of a nickel electrolytic plating film and a gold plating film formed on the nickel electrolytic plating film, and the nickel electrolytic plating film is the nickel electrolytic plating film according to claim 1. Plating structure. 請求項２～４のいずれか一項に記載のめっき構造体を備えたリードフレーム。
A lead frame comprising the plating structure according to any one of claims 2 to 4.
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US6037653A (en) * 1997-03-25 2000-03-14 Samsung Aerospace Industries, Ltd. Semiconductor lead frame having multi-layered plating layer including copper-nickel plating layer
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