JP2008285727A - Electrolytic copper foil with high tensile-strength, and manufacturing method therefor - Google Patents
Electrolytic copper foil with high tensile-strength, and manufacturing method therefor Download PDFInfo
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Abstract
Description
本発明は、製箔後において高い抗張力を維持する高抗張力電解銅箔及びその製造方法に関するものである。 The present invention relates to a high tensile strength electrolytic copper foil that maintains a high tensile strength after foil production and a method for producing the same.
HDDサスペンション、各種コネクタ部等に銅配線が使用されている。これらの用途ではその使用環境上、高い抗張力が求められる。 Copper wiring is used for HDD suspensions, various connector parts, and the like. In these applications, high tensile strength is required in the usage environment.
HDDサスペンション、各種コネクタ部等の銅配線部に銅箔が使用されるが、近年高密度実装が進みより薄い銅箔が求められている。銅箔には圧延銅箔と電解銅箔があるが、その製造方法上、圧延銅箔は薄くするにつれて生産性が落ちるので高コストとなるが電解銅箔は薄くするにつれて生産性が上がり低コストとなる。また、電解銅箔の方が圧延銅箔よりも幅広化が可能である。よって、HDDサスペンション、各種コネクタ部等の銅配線部への用途として電解銅箔への需要が高まってきている。 Copper foils are used for copper wiring parts such as HDD suspensions and various connector parts, but in recent years, high density mounting has progressed and thinner copper foils are required. There are two types of copper foil: rolled copper foil and electrolytic copper foil, but due to its manufacturing method, the productivity decreases as the thickness of the rolled copper foil decreases, but the cost increases as the thickness of the electrolytic copper foil increases. It becomes. Further, the electrolytic copper foil can be wider than the rolled copper foil. Therefore, the demand for electrolytic copper foil is increasing as a use for copper wiring parts such as HDD suspensions and various connector parts.
しかしながら、現在製造されている電解銅箔は製箔完了時点では高い抗張力を有するが、製箔後の銅箔を常温維持し、あるいは後工程における200〜300℃程度の加熱処理によって製箔直後の高い抗張力が維持できなくなり、上記のHDDサスペンション、各種コネクタ部等の銅配線部に使用するのに十分な高い抗張力が維持できないため、これらの用途には採用できない状況にあった。この原因は、製箔直後の微細な結晶状態から、低い抗張力となる粗大な結晶状態へと再結晶を起こし軟化してしまうためである。 However, the electrolytic copper foil currently produced has high tensile strength at the time of completion of foil production, but the copper foil after foil production is maintained at room temperature or heat treatment at about 200 to 300 ° C. in the subsequent process is performed immediately after the foil production. The high tensile strength cannot be maintained, and the high tensile strength sufficient for use in the above-described HDD suspension and various copper wiring portions cannot be maintained. This is because recrystallization occurs from a fine crystal state immediately after foil formation to a coarse crystal state having a low tensile strength and softens.
本発明は、従来の製造方法の電解銅箔では困難であった製箔完了時から次の製造工程に移るまでの常温保管、または次工程における200〜300℃程度の加熱処理によっても軟化せず高い抗張力を維持する電解銅箔、並びにその製造方法を提供することを目的とする。 The present invention is not softened even at room temperature storage from the time of completion of foil production to the next production process, or heat treatment at about 200 to 300 ° C. in the next process, which was difficult with the electrolytic copper foil of the conventional production method. It aims at providing the electrolytic copper foil which maintains high tensile strength, and its manufacturing method.
本発明の電解銅箔は、銅箔の製箔完了時から該銅箔の特性安定時以降の25℃で測定した抗張力が400N/mm2以上である高抗張力電解銅箔である。 The electrolytic copper foil of the present invention is a high-strength electrolytic copper foil having a tensile strength of 400 N / mm 2 or more measured at 25 ° C. after the completion of copper foil production and after the stabilization of the characteristics of the copper foil.
好ましくは、前記特性安定に要する時間が製箔完了時から48時間以降、更に好ましくは72時間以降である。 Preferably, the time required for the characteristic stabilization is 48 hours or more, more preferably 72 hours or more after the completion of foil production.
本発明の電解銅箔は、銅箔の製箔を完了し、該銅箔の特性が安定した後、該銅箔を300℃で1時間加熱処理し、該加熱処理後に25℃で測定した抗張力が400N/mm2以上である高抗張力電解銅箔である。 The electrolytic copper foil of the present invention is a tensile strength measured at 25 ° C. after heat treatment at 300 ° C. for 1 hour after the copper foil is completed and the properties of the copper foil are stabilized. Is a high tensile strength electrolytic copper foil having 400 N / mm 2 or more.
好ましくは、前記特性が安定するまでに要する時間が製箔完了時から48時間以降、更に好ましくは72時間以降である。 Preferably, the time required for the above characteristics to stabilize is 48 hours or more, more preferably 72 hours or more after the completion of foil production.
本発明の電解銅箔の製造方法は、銅箔の製箔完了時から該銅箔の特性安定時以降の25℃で測定した抗張力が400N/mm2以上である電解銅箔を、少なくとも平均分子量が100以上の有機化合物の濃度が100ppm以上である硫酸銅浴を用いて製箔する高抗張力電解銅箔の製造方法である。 The method for producing an electrolytic copper foil of the present invention comprises at least an average molecular weight of an electrolytic copper foil having a tensile strength of 400 N / mm 2 or more measured at 25 ° C. after the completion of copper foil production and after stabilization of the characteristics of the copper foil. Is a method for producing a high tensile strength electrolytic copper foil in which a copper sulfate bath having a concentration of 100 or more organic compounds is 100 ppm or more.
本発明の電解銅箔の製造方法は、銅箔の製箔を完了し、該銅箔の特性が安定した後、該銅箔を300℃で1時間加熱処理し、該加熱処理後に25℃で測定した抗張力が400N/mm2以上である電解銅箔を、少なくとも平均分子量が100以上の有機化合物の濃度が100ppm以上である硫酸銅浴を用いて製箔する高抗張力電解銅箔の製造方法である。 The manufacturing method of the electrolytic copper foil of the present invention is as follows. After the copper foil is completed and the characteristics of the copper foil are stabilized, the copper foil is heat-treated at 300 ° C. for 1 hour, and at 25 ° C. after the heat treatment. In the method for producing a high tensile strength electrolytic copper foil, an electrolytic copper foil having a measured tensile strength of 400 N / mm 2 or more is formed using a copper sulfate bath having a concentration of an organic compound having an average molecular weight of 100 or more and 100 ppm or more. is there.
好ましくは、前記硫酸銅浴は有機硫黄系化合物を含有し、前記少なくとも平均分子量が100以上である有機化合物を前記有機硫黄系化合物の100倍以上の濃度で含む硫酸銅浴を用いて製造する高抗張力電解銅箔の製造方法である。 Preferably, the copper sulfate bath contains an organic sulfur-based compound, and is manufactured using a copper sulfate bath containing the organic compound having an average molecular weight of 100 or more at a concentration 100 times or more that of the organic sulfur-based compound. It is a manufacturing method of a tensile strength electrolytic copper foil.
本発明によれば製箔完了時から次の製造工程に移るまでの常温保管時、または後工程における200〜300℃程度の加熱処理においても400N/mm2以上の高い抗張力を維持する電解銅箔を提供することができる。 According to the present invention, an electrolytic copper foil that maintains a high tensile strength of 400 N / mm 2 or more during normal temperature storage from the completion of foil production to the next production process, or in heat treatment at about 200 to 300 ° C. in the subsequent process. Can be provided.
本発明において電解銅箔の厚みは1μm以上300μm以下が好適である。銅箔の厚みが1μmより薄いと製造時に電解ドラムからうまく剥がせず、例え剥がせたとしてもシワなどが入りうまく巻き取れないため現実的ではない。また、300μm以上の厚みにおいては電解製箔は好ましくなく、現実的でないためである。 In the present invention, the thickness of the electrolytic copper foil is preferably 1 μm or more and 300 μm or less. If the thickness of the copper foil is less than 1 μm, it will not be peeled off from the electrolytic drum at the time of manufacture, and even if it is peeled off, wrinkles will enter and it will not wind up well, which is not realistic. Moreover, in the thickness of 300 micrometers or more, it is because electrolytic foil is not preferable and is not realistic.
本発明において、電解銅箔を製造するには、銅めっきの浴として硫酸銅めっき浴を用いる。本発明では硫酸銅めっき液に添加剤として少なくとも平均分子量が100以上の有機化合物を混入する。平均分子量が100以上の有機化合物の添加量は100ppm以上が好ましい。この濃度は従来のこの種添加剤の添加量を大きく上回る量である。
なた、電解浴には一般に有機硫黄系化合物が混入されている。本発明の抗張力銅箔を製造する電解浴においては、平均分子量が100以上の有機化合物の濃度は有機硫黄系化合物の濃度に対する比率を100倍以上大きくしている。
In the present invention, to produce an electrolytic copper foil, a copper sulfate plating bath is used as a copper plating bath. In the present invention, at least an organic compound having an average molecular weight of 100 or more is mixed in the copper sulfate plating solution as an additive. The addition amount of the organic compound having an average molecular weight of 100 or more is preferably 100 ppm or more. This concentration is much larger than the conventional amount of this kind additive.
In general, an organic sulfur compound is mixed in the electrolytic bath. In the electrolytic bath for producing the tensile strength copper foil of the present invention, the concentration of the organic compound having an average molecular weight of 100 or more increases the ratio to the concentration of the organic sulfur compound by 100 times or more.
このように、平均分子量が100以上の有機化合物の濃度を濃くすると、銅箔中へ取り込まれる不純物の量が多くなる。その結果、結晶粒界に不純物が多量に分散し、結晶成長を抑制することとなる。そのため、製箔完了後常温で保持しても、また、後工程における200〜300℃での加熱処理後も高い抗張力を維持させることが可能となる。 As described above, when the concentration of the organic compound having an average molecular weight of 100 or more is increased, the amount of impurities taken into the copper foil is increased. As a result, a large amount of impurities are dispersed in the crystal grain boundary, and crystal growth is suppressed. Therefore, even if it hold | maintains at normal temperature after completion of foil manufacture, it becomes possible to maintain a high tensile strength also after the heat processing at 200-300 degreeC in a post process.
本発明で用いる硫酸銅めっき浴組成とめっき条件の一実施例を表1に示す。
なお、表1には従来の硫酸銅めっき浴の組成とめっき条件を比較例として併記する。
Table 1 shows an example of the copper sulfate plating bath composition and plating conditions used in the present invention.
In Table 1, the composition and plating conditions of a conventional copper sulfate plating bath are also shown as comparative examples.
上記電解銅箔を製造する硫酸銅めっき浴には添加剤として少なくとも平均分子量が100以上である1種以上の有機化合物を添加する。少なくとも平均分子量が100以上である有機化合物としては膠、高分子界面活性剤、含窒素有機化合物等が使用できる。平均分子量が100未満の有機化合物では、求める添加剤の効果は期待できない。膠は一般に市販されているものが使用できるが、特に低分子量のものが好ましい。高分子界面活性剤としてはヒドロキシエチルセルロース、ポリエチレングリコール、ポリプロピレングリコール、ポリエチレングリコールジメチルエーテル、ポリエチレンオキシド等が挙げられる。含窒素有機化合物としてはポリエチレンイミン、ポリアクリル酸アミド等が挙げられる。 At least one organic compound having an average molecular weight of 100 or more is added as an additive to the copper sulfate plating bath for producing the electrolytic copper foil. As an organic compound having at least an average molecular weight of 100 or more, glue, a polymer surfactant, a nitrogen-containing organic compound, or the like can be used. For organic compounds having an average molecular weight of less than 100, the desired additive effect cannot be expected. As the glue, commercially available ones can be used, but those having a low molecular weight are particularly preferred. Examples of the polymer surfactant include hydroxyethyl cellulose, polyethylene glycol, polypropylene glycol, polyethylene glycol dimethyl ether, and polyethylene oxide. Examples of the nitrogen-containing organic compound include polyethyleneimine and polyacrylic acid amide.
平均分子量が100以上である有機化合物の添加量は100ppm以上が好ましく、更に好ましくは500ppm以下である。少なくとも平均分子量が100以上である有機化合物の添加量が100ppm未満では製箔した銅箔中へ取り込まれる不純物の量が不足し目的とする高抗張力性能の箔が得られない。また、500ppmを超えると添加量が過剰となり正常な製箔が困難になるばかりでなくコスト、電解浴としての安定性の面からも好ましくない。 The addition amount of the organic compound having an average molecular weight of 100 or more is preferably 100 ppm or more, more preferably 500 ppm or less. If the addition amount of the organic compound having an average molecular weight of 100 or more is less than 100 ppm, the amount of impurities taken into the copper foil that has been made is insufficient, and the desired high tensile strength foil cannot be obtained. On the other hand, if it exceeds 500 ppm, the amount added is excessive and normal foil production becomes difficult, and this is not preferable from the viewpoint of cost and stability as an electrolytic bath.
上記電解銅箔を製造する硫酸銅めっき浴への添加剤として少なくとも平均分子量が100以上である1種以上の有機化合物と有機硫黄系化合物を添加する。
添加する有機硫黄系化合物としては3-メルカプト-1-プロパンスルホン酸、ビス(3−スルホプロピル)ジスルフィド等が挙げられる。平均分子量が100以上である有機化合物の添加量は100ppm以上が好ましく、更に有機硫黄系化合物の100倍以上の濃度となるように添加する。具体的には有機硫黄系化合物を1〜5ppm、少なくとも平均分子量が100以上である有機化合物を100〜500ppmの範囲で比率を変えて添加する。有機硫黄系化合物は1ppm未満となると過少となり目的の性能の箔の製造が困難となる。また、5ppmを超えると共に添加する有機化合物の濃度が500ppmを超えて過剰となり正常な製箔が困難になるばかりでなくコスト、液の安定性の面からも好ましくない。
As an additive to the copper sulfate plating bath for producing the electrolytic copper foil, at least one organic compound having an average molecular weight of 100 or more and an organic sulfur compound are added.
Examples of the organic sulfur compound to be added include 3-mercapto-1-propanesulfonic acid and bis (3-sulfopropyl) disulfide. The addition amount of the organic compound having an average molecular weight of 100 or more is preferably 100 ppm or more, and is further added so that the concentration is 100 times or more that of the organic sulfur compound. Specifically, an organic sulfur compound is added in an amount of 1 to 5 ppm, and an organic compound having an average molecular weight of at least 100 is added in a range of 100 to 500 ppm. If the amount of the organic sulfur compound is less than 1 ppm, the amount becomes too small, making it difficult to produce a foil having the desired performance. Further, when the concentration exceeds 5 ppm, the concentration of the organic compound to be added exceeds 500 ppm, which makes it difficult to produce a normal foil, and is not preferable from the viewpoint of cost and liquid stability.
以下、本発明を実施例に基づき説明するが、本発明はこれらに限定されるものではない。 EXAMPLES Hereinafter, although this invention is demonstrated based on an Example, this invention is not limited to these.
<実施例1〜5>
表2に示す組成の硫酸銅めっき液(以後電解液という)を活性炭フィルターに通して清浄処理した。次いで、この電解液に表3に示す添加剤をそれぞれの濃度となるように添加して実施例1〜5の製箔用電解液を調整した。なお、本実施例1〜5において使用した添加剤は有機硫黄系化合物は3-メルカプト-1-プロパンスルホン酸ナトリウム(MPS)、少なくとも平均分子量が100以上である有機化合物は膠(PBF)(株式会社ニッピ製)である。このようにして調製した電解液を用い、アノードには貴金属酸化物被膜チタン電極、陰極にはチタン製回転ドラムを用いて、表3に示す電解条件の下に電解製箔によって銅箔を製造した。
<Examples 1-5>
A copper sulfate plating solution (hereinafter referred to as an electrolytic solution) having the composition shown in Table 2 was passed through an activated carbon filter for cleaning treatment. Subsequently, the additive shown in Table 3 was added to this electrolyte solution so that it might become each density | concentration, and the electrolyte solution for foil manufacture of Examples 1-5 was adjusted. The additive used in Examples 1 to 5 is an organic sulfur compound, sodium 3-mercapto-1-propanesulfonate (MPS), and an organic compound having an average molecular weight of 100 or more is glue (PBF) (stock) Company Nippi). Using the electrolytic solution thus prepared, a copper foil was produced by electrolytic foil under the electrolysis conditions shown in Table 3, using a noble metal oxide-coated titanium electrode for the anode and a titanium rotating drum for the cathode. .
<比較例1〜5>
表2に示す組成の電解液を活性炭フィルターに通して清浄処理した。次いで、この電解液に表3に示す添加剤をそれぞれの濃度となるように添加して比較例1〜5の製箔用電解液を調整した。このようにして調製した電解液を用い、実施例1〜5と同様に、アノードには貴金属酸化物被膜チタン電極、陰極にはチタン製回転ドラムを用いて、表3に示す電解条件の下に電解製箔によって銅箔を製造した。
<Comparative Examples 1-5>
The electrolytic solution having the composition shown in Table 2 was passed through an activated carbon filter for cleaning treatment. Subsequently, the additive shown in Table 3 was added to this electrolyte so that it might become each density | concentration, and the electrolyte solution for foil manufacture of Comparative Examples 1-5 was adjusted. Using the electrolytic solution thus prepared, as in Examples 1 to 5, using a noble metal oxide-coated titanium electrode for the anode and a titanium rotating drum for the cathode, the electrolytic conditions shown in Table 3 were used. Copper foil was manufactured by electrolytic foil.
<抗張力、伸びの測定>
実施例1〜5及び比較例1〜5で製造した電解銅箔にいて製箔完了時から24時間後、48時間後、72時間後、96時間後、及び72時間後に窒素雰囲気中300℃1時間加熱処理後の25℃における抗張力と伸びをJIS Z 2201:1998に基づいて引張試験機を用いて測定した。結果を表4、表5に示す。
<Measurement of tensile strength and elongation>
In the electrolytic copper foils produced in Examples 1 to 5 and Comparative Examples 1 to 5, 24 hours, 48 hours, 72 hours, 96 hours, and 72 hours after completion of the foil production, in a nitrogen atmosphere at 300 ° C. The tensile strength and elongation at 25 ° C. after the time heat treatment were measured using a tensile tester based on JIS Z 2201: 1998. The results are shown in Tables 4 and 5.
<抗張力の評価>
抗張力は表4から明らかなように実施例1〜5、比較例1〜5ともに製箔完了時から短くとも48時間後には常温における再結晶とそれに伴う抗張力の低下は収拾するとみなすことができる。実施例1〜5では添加剤として少なくとも平均分子量が100以上である有機化合物(PBF)を有機硫黄系化合物(MPS)の100倍以上の濃度で含む硫酸銅浴を用いて製造することで、48時間経過後も400N/mm2以上の高抗張力を維持する電解銅箔が得られている。
一方、添加剤として少なくとも平均分子量が100以上である有機化合物(PBF)を有機硫黄系化合物(MPS)の10倍程度の濃度で含む硫酸銅浴を用いて製造した比較例1〜5では、いずれにおいても製箔完了時から48時間程度までは400N/mm2以上の抗張力を維持しているが、48時間経過後では抗張力が400N/mm2以下となっている。
<Evaluation of tensile strength>
As is apparent from Table 4, in Examples 1 to 5 and Comparative Examples 1 to 5, it can be considered that the recrystallization at room temperature and the accompanying decrease in the tensile strength are collected after 48 hours from the completion of the foil production. In Examples 1 to 5, it is produced by using a copper sulfate bath containing an organic compound (PBF) having an average molecular weight of 100 or more as an additive at a concentration 100 times or more that of an organic sulfur compound (MPS). An electrolytic copper foil that maintains a high tensile strength of 400 N / mm 2 or more after the elapse of time has been obtained.
On the other hand, in Comparative Examples 1 to 5 manufactured using a copper sulfate bath containing an organic compound (PBF) having an average molecular weight of 100 or more as an additive at a concentration about 10 times that of the organic sulfur compound (MPS), Also, the tensile strength of 400 N / mm 2 or more is maintained for about 48 hours from the completion of foil production, but after 48 hours, the tensile strength is 400 N / mm 2 or less.
また、表5に常温における72時間後の抗張力とこの銅箔を300℃で1時間加熱処理した後自然冷却し、25℃に達した時点で測定した抗張力とを比較して示している。表5から明らかなように実施例1〜5は製箔完了時から72時間の抗張力に比較して、72時間後に300℃1時間加熱処理後の抗張力はやや低下しているが、いずれにおいても400N/mm2以上の抗張力を維持している。これに対して、比較例1〜5は製箔完了時から72時間後で既に抗張力が400N/mm2以下であり、この銅箔を72時間後に300℃1時間加熱処理するとかなり抗張力は低下している。 Table 5 shows a comparison between the tensile strength after 72 hours at room temperature and the tensile strength measured when the copper foil was naturally cooled after being heated at 300 ° C for 1 hour and reached 25 ° C. As is clear from Table 5, Examples 1 to 5 are slightly lower in tensile strength after heat treatment at 300 ° C. for 1 hour after 72 hours compared to the tensile strength for 72 hours from the completion of foil production. The tensile strength of 400 N / mm 2 or more is maintained. In contrast, in Comparative Examples 1 to 5, the tensile strength is already 400 N / mm 2 or less after 72 hours from the completion of the foil production, and when this copper foil is heated at 300 ° C. for 1 hour after 72 hours, the tensile strength is considerably lowered. ing.
<伸びの評価>
製箔後の常温での伸びは表4に示すように実施例1〜5、比較例1〜5共に同じような傾向を示すが、表5に示すように製箔完了時から72時間後の伸びと、72時間後に300℃1時間加熱処理後の伸びは、実施例1〜5はほとんど変化がないが、比較例1〜5は72時間後に300℃1時間加熱処理すると伸び率は大きくなっている。
即ち、実施例の伸び特性は熱処理によっても安定しているため、寸法精度を要求される製品に好適に採用することができる。
<Evaluation of elongation>
As shown in Table 4, the elongation at normal temperature after foil production shows the same tendency in Examples 1 to 5 and Comparative Examples 1 to 5, but as shown in Table 5, 72 hours after the completion of foil production. Elongation and elongation after heating treatment at 300 ° C. for 1 hour after 72 hours have almost no change in Examples 1 to 5, but Comparative Examples 1 to 5 increase the elongation rate when heat treatment is performed at 300 ° C. for 1 hour after 72 hours. ing.
That is, since the elongation characteristics of the examples are stable even by heat treatment, it can be suitably used for products that require dimensional accuracy.
上述したように本発明は、製箔後も安定した伸び特性を示し、高い抗張力を維持する電解銅箔を提供することができ、HDDサスペンション、各種コネクタ部等の銅配線として好適に使用することができる優れた効果を有する。 As described above, the present invention can provide an electrolytic copper foil that exhibits a stable elongation characteristic even after foil formation and maintains high tensile strength, and can be suitably used as a copper wiring for HDD suspensions, various connector portions, and the like. Has an excellent effect.
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