JP2007072427A - Reflection film for reflection plate excellent in corrosion resistance and sputtering target for forming reflection film for reflection plate excellent in corrosion resistance - Google Patents
Reflection film for reflection plate excellent in corrosion resistance and sputtering target for forming reflection film for reflection plate excellent in corrosion resistance Download PDFInfo
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この発明は、投光機、輻射暖房器具、自動車のヘッドライトなど光を照射または拡散させるための各種照明器具の反射板に使用される反射膜に関するものであり、さらにこの反射膜を形成するためのアルミニウム合金からなるスパッタリングターゲットに関するものである。 The present invention relates to a reflective film used for a reflector of various lighting fixtures for irradiating or diffusing light, such as a projector, a radiant heater, and a headlight of an automobile, and further for forming the reflective film. The present invention relates to a sputtering target made of an aluminum alloy.
従来、投光機、輻射暖房器具、自動車のヘッドライトの反射板や各種照明器具の反射板にはＪＩＳ１０５０、ＪＩＳ１０７０、ＪＩＳ１０８０、ＪＩＳ１０８５などの純度９９．８５質量％以上の純Ａｌ板、またはＦｅ：０．０５〜０．１５質量％、Ｃｕ：０．０６〜０．１５質量％、Ｔｉ：０．００４〜０．０４質量％を含有し、不純物としてＳｉ，ＭｇおよびＭｎがそれぞれ０．０８質量％以下であり、残部がＡｌおよび不可避不純物であるＡｌ合金からなるアルミニウム合金板が使用されている（特許文献１参照）。
しかし、一般に、純ＡｌまたはＡｌ合金は両性金属であるために酸およびアルカリに対して非常に弱い。そのために純Ａｌ板またはＡｌ合金板を各種反射板として使用した場合、短期間で反射率が低下するなどの問題点があった。かかる反射率の低下を防止するために、従来は前記純Ａｌ板またはＡｌ合金板からなる反射面の表面に透明な合成樹脂の皮膜を形成したり陽極酸化処理を行って表面に薄い酸化膜を形成したりして腐食による反射率の低下を防止していた。しかし、前記合成樹脂皮膜を形成したり陽極酸化処理を行って表面にアルミニウムの酸化膜を形成すると純Ａｌ板またはＡｌ合金板の反射率の低下は避けられず、したがって、反射板としての特性が劣ることは避けられなかった。
さらに、純Ａｌ板またはＡｌ合金板を使用して各種反射板を作製するには、鏡面仕上げされた純Ａｌ板またはＡｌ合金板を所定の形状に絞り加工などの成形加工を施して作製するが、成形加工中に反射面に傷が付いたり加工ムラが発生することがある。これら成形加工後に発生した傷や加工ムラを除去するためにさらにバフ研磨を行う必要があった。
However, in general, pure Al or an Al alloy is an amphoteric metal and is very weak against acids and alkalis. Therefore, when a pure Al plate or an Al alloy plate is used as various reflectors, there is a problem that the reflectance is reduced in a short period of time. In order to prevent such a decrease in reflectance, conventionally, a transparent synthetic resin film is formed on the surface of the reflective surface made of the pure Al plate or the Al alloy plate, or a thin oxide film is formed on the surface by anodizing treatment. It was formed to prevent a decrease in reflectance due to corrosion. However, when an aluminum oxide film is formed on the surface by forming the above synthetic resin film or anodizing treatment, a decrease in the reflectance of a pure Al plate or an Al alloy plate is inevitable. Inferiority was inevitable.
Furthermore, in order to produce various reflectors using a pure Al plate or an Al alloy plate, a mirror-finished pure Al plate or Al alloy plate is produced by subjecting it to a predetermined shape such as drawing. During the molding process, the reflective surface may be scratched or uneven processing may occur. In order to remove the scratches and processing irregularities generated after the molding process, it was necessary to perform further buffing.
本発明者らは、前記従来の純Ａｌ板またはＡｌ合金板で作製した反射板がかかえるこれら問題点を解決すべく研究を行なった。その結果、
（イ）純度９９．９９質量％以上の高純度Ａｌに純度：９９．９質量％以上のＭｇ：０．１〜１５質量％を添加して溶解し鋳造し熱間加工し機械加工することによりＭｇ：０．１〜１５質量％を含有し、残部がＡｌおよび不可避不純物からなり、前記不可避不純物は１００ｐｐｍ以下に規定されているＡｌ−Ｍｇ系のＡｌ合金製ターゲットを作製し、このターゲットを用いてスパッタリングすることにより得られたＡｌ合金スパッタリング膜は、表面にバリア膜が形成され、それによって酸およびアルカリに対する耐腐食性が向上し、このＡｌ合金スパッタリング膜を反射膜として使用すると、長期にわたって反射率が低下することは無い、
（ロ）各種反射板の構造を有する基板の表面に形成されたスパッタリング膜は、成形加工されることが無いので製造中に傷が付く心配が無く、表面研磨を行う必要が無い、などの研究結果が得られたのである。
The present inventors have studied to solve these problems associated with the reflector made of the conventional pure Al plate or Al alloy plate. as a result,
(B) Purity: 99.9% by mass or more of Mg: 0.1-15% by mass added to high purity Al having a purity of 99.99% by mass or more, melting, casting, hot working and machining Mg: 0.1 to 15% by mass, the balance is made of Al and inevitable impurities, and the inevitable impurities are defined as 100 ppm or less, and an Al—Mg-based Al alloy target is prepared, and this target is used. The Al alloy sputtering film obtained by sputtering in this way forms a barrier film on the surface, thereby improving the corrosion resistance against acids and alkalis. When this Al alloy sputtering film is used as a reflection film, it is reflected over a long period of time. The rate will never drop,
(B) Research that sputtering films formed on the surface of substrates with various reflector structures are not molded, so there is no risk of scratching during production, and there is no need for surface polishing. The result was obtained.
この発明は、かかる研究結果に基づいて成されたものであって、
（１）Ｍｇ：０．１〜１５質量％を含有し、残部がＡｌおよび不可避不純物からなり、前記不可避不純物は１００ｐｐｍ以下に規定されている組成のアルミニウム合金からなる耐腐食性に優れた反射板用反射膜、に特徴を有するものである。
The present invention has been made based on such research results,
(1) Mg: 0.1 to 15% by mass, with the balance being made of Al and inevitable impurities, the inevitable impurities being made of an aluminum alloy having a composition defined as 100 ppm or less and having excellent corrosion resistance The reflective film has a feature.
前記（１）記載の耐腐食性に優れた反射板用反射膜は、この反射板用反射膜と同じ成分組成のターゲットを用いてスパッタリングすることにより形成される。したがって、この発明は、
（２）Ｍｇ：０．１〜１５質量％を含有し、残部がＡｌおよび不可避不純物からなり、前記不可避不純物は１００ｐｐｍ以下に規定されている組成のアルミニウム合金からなる耐腐食性に優れた反射板用反射膜形成のためのスパッタリングターゲット、に特徴を有するものである。
The reflective film for a reflective plate excellent in corrosion resistance described in (1) is formed by sputtering using a target having the same component composition as the reflective film for a reflective plate. Therefore, the present invention
(2) Mg: 0.1 to 15% by mass, with the balance being made of Al and inevitable impurities, the inevitable impurities being made of an aluminum alloy having a composition defined as 100 ppm or less and having excellent corrosion resistance It has the characteristics in the sputtering target for reflective film formation.
この発明の反射板用反射膜を形成するためのスパッタリングターゲットは、原料として純度：９９.９質量％以上のＭｇおよび希土類元素を用意し、まず、高純度Ａｌを高真空または不活性ガス雰囲気中で溶解して不純物が可及的に少ない高純度Ａｌ溶湯を作製し、得られた高純度Ａｌ溶湯にＭｇを所定の含有量となるように添加し、その後、真空または不活性ガス雰囲気中で鋳造してインゴットを作製し、これらインゴットを熱間加工したのち機械加工することにより製造することができる。 A sputtering target for forming a reflective film for a reflector according to the present invention is prepared by preparing Mg and rare earth elements having a purity of 99.9% by mass or more as raw materials. To prepare a high-purity Al molten metal with as little impurities as possible, and add Mg to the obtained high-purity Al molten metal to a predetermined content, and then in a vacuum or an inert gas atmosphere An ingot can be produced by casting, and these ingots can be hot-worked and then machined.
次に、この発明の反射板用反射膜およびこの反射板用反射膜を形成するためのスパッタリングターゲットにおける成分組成を前記の如く限定した理由を説明する。 Next, the reason why the component composition in the reflective film for the reflective plate of the present invention and the sputtering target for forming the reflective film for the reflective plate is limited as described above will be described.
Ｍｇ：
Ｍｇ成分は、Ａｌに固溶し、Ａｌ合金からなる反射板用反射膜の表面に緻密で透明な不働態膜を形成することにより高反射率を維持したまま耐腐食性を向上させる成分であるが、Ｍｇを０．１質量％未満含んでも所望の効果が得られず、一方、１５質量％を越えて含有すると、ターゲット製造時に割れが発生するようになるので好ましくない。
Mg:
The Mg component is a component that improves the corrosion resistance while maintaining a high reflectivity by forming a dense and transparent passive film on the surface of the reflective film for a reflector made of an Al alloy by dissolving in Mg. However, even if Mg is contained in an amount of less than 0.1% by mass, the desired effect cannot be obtained. On the other hand, if the content exceeds 15% by mass, cracks occur during target production, which is not preferable.
したがって、この発明の反射板用反射膜およびこの反射板用反射膜を形成するためのスパッタリングターゲットに含まれるＭｇ成分の含有量を０.１〜１５質量％(一層好ましくは１〜１０質量％)に定めた。 Therefore, the content of the Mg component contained in the reflective film for reflector of the present invention and the sputtering target for forming the reflective film for reflector is 0.1 to 15% by mass (more preferably 1 to 10% by mass). Determined.
不可避不純物：
この発明のスッパタリングして得られた反射板用反射膜およびこの反射板用反射膜を形成するためのスパッタリングターゲットに含まれる不可避不純物は少ないほど好ましく、反射板用反射膜およびこの反射板用反射膜を形成するためのスパッタリングターゲットに含まれる不可避不純物は１００ｐｐｍ以下であることが必要である。その理由は、反射板用反射膜およびこの反射板用反射膜を形成するためのスパッタリングターゲットに含まれる不可避不純物が１００ｐｐｍを越えると、耐腐食性が急激に悪化するからである。
Inevitable impurities:
The smaller the inevitable impurities contained in the reflecting film for reflecting plate obtained by the sputtering of the present invention and the sputtering target for forming the reflecting film for reflecting plate are preferable, the reflecting film for reflecting plate and the reflecting plate for reflecting plate are preferred. The inevitable impurities contained in the sputtering target for forming the film must be 100 ppm or less. The reason is that if the inevitable impurities contained in the reflecting film for the reflecting plate and the sputtering target for forming the reflecting film for the reflecting plate exceed 100 ppm, the corrosion resistance deteriorates rapidly.
この発明の反射板用反射膜を反射面に形成した反射板は、従来の純Ａｌ板またはＡｌ合金板を用いて作製した反射板に比べて、大気中に長期間暴露されても経時変化による反射面の反射率の低下が少なく、長期にわたって使用できる。 The reflecting plate having the reflecting film for the reflecting plate of the present invention formed on the reflecting surface is subject to change over time even if it is exposed to the atmosphere for a long time, compared to a reflecting plate produced using a conventional pure Al plate or Al alloy plate. There is little decrease in the reflectance of the reflecting surface, and it can be used for a long time.
原料として、純度：９９.９９質量％以上の高純度Ａｌ、純度：９９.９質量％以上のＡｌを用意し、さらに純度：９９.９質量％以上のＭｇを用意した。
まず、純度：９９.９９質量％以上の高純度Ａｌを高周波真空溶解炉にて真空中で溶解したのち炉内圧力が大気圧となるまでＡｒガスを充填し、前記ＭｇをＡｌ溶湯に添加し、その後、黒鉛製鋳型に鋳造することによりインゴットを作製した。得られたインゴットを４３０℃、２時間加熱した後、熱間圧延し、機械加工することにより直径：１２５ｍｍ、厚さ：５ｍｍの寸法を有し、表１に示される成分組成を有する本発明ターゲット１〜１０を製造した。
また、表１に示される比較例ターゲット１、２は純度：９９．９９質量％以上の高純度Ａｌを用い、比較例ターゲット３、４は純度：９９．９質量％以下の低純度Ａｌを用いた以外は本発明ターゲット１〜１０の製造条件と同じ条件で製造した。さらに、表１に示される従来ターゲット１はＪＩＳＡ１０５０を用いて製造した。
なお、表１に示される不可避不純物としてはＳｉ，Ｆｅ，Ｃｕ，Ｍｎ，Ｚｎ，ＴｉをＩＣＰ法にて分析し、検出下限を下まわる場合は０ｐｐｍとし、各分析値の合計で示した。ＪＩＳＡ１０５０で作製した従来ターゲット１に含まれるＭｇの値はＩＣＰ法にて分析した値である。
As raw materials, high purity Al with a purity of 99.99% by mass or more, Al with a purity of 99.9% by mass or more, and Mg with a purity of 99.9% by mass or more were prepared.
First, after purifying high purity Al having a purity of 99.99% by mass or higher in a high-frequency vacuum melting furnace in a vacuum, Ar gas is charged until the pressure in the furnace reaches atmospheric pressure, and the Mg is added to the molten Al. Thereafter, an ingot was produced by casting into a graphite mold. The obtained ingot was heated at 430 ° C. for 2 hours, then hot-rolled and machined to have a diameter: 125 mm, a thickness: 5 mm, and a target of the present invention having the component composition shown in Table 1 1-10 were manufactured.
Moreover, the comparative example targets 1 and 2 shown in Table 1 use high-purity Al with a purity of 99.99% by mass or more, and the comparative targets 3 and 4 use low-purity Al with a purity of 99.9% by mass or less. It manufactured on the same conditions as the manufacturing conditions of this invention target 1-10 except having been. Furthermore, the conventional target 1 shown in Table 1 was manufactured using JISA1050.
As inevitable impurities shown in Table 1, Si, Fe, Cu, Mn, Zn, and Ti were analyzed by ICP method. When the lower limit of detection was exceeded, 0 ppm was used, and the total of each analysis value was shown. The value of Mg contained in the conventional target 1 produced by JISA1050 is a value analyzed by the ICP method.
これら表１に示される本発明ターゲット１〜１０、比較ターゲット１〜４および従来ターゲット１をそれぞれ無酸素銅製のバッキングプレートにはんだ付けし、これを直流マグネトロンスパッタ装置に装着し、真空排気装置にて直流マグネトロンスパッタ装置内を１×１０-4Ｐａまで排気した後、Ａｒガスを導入して１．０Ｐａのスパッタガス圧とし、続いて直流電源にてターゲットに１００Ｗの直流スパッタ電力を印加し、前記ターゲットに対抗しかつ７０ｍｍの間隔を設けてターゲットと平行に配置した縦：３０ｍｍ、横：３０ｍｍ、厚さ：０．５ｍｍの無アルカリガラス基板と前記ターゲットの間にプラズマを発生させ、表２〜３に示される成分組成を有し、厚さ：１００ｎｍを有する本発明反射膜１〜１０、比較反射膜１〜４および従来反射膜１を形成した。 The present invention targets 1 to 10, the comparative targets 1 to 4 and the conventional target 1 shown in Table 1 are each soldered to a backing plate made of oxygen-free copper, and this is mounted on a DC magnetron sputtering device, and is evacuated by a vacuum exhaust device. After evacuating the DC magnetron sputtering apparatus to 1 × 10 −4 Pa, Ar gas is introduced to a sputtering gas pressure of 1.0 Pa, and then a DC sputtering power of 100 W is applied to the target with a DC power source. A plasma is generated between a non-alkali glass substrate having a length of 30 mm, a width of 30 mm, and a thickness of 0.5 mm arranged opposite to the target and parallel to the target at a distance of 70 mm, and Table 2 3 of the present invention having the composition shown in FIG. 3 and having a thickness of 100 nm, comparative reflective films 1 to 4 and comparative reflective films 1 to 4 The formation of the coming reflection film 1.
このようにして形成した厚さ：１００ｎｍを有する本発明反射膜１〜１０、比較反射膜１〜４および従来反射膜１について、下記の試験を行った。
（ａ）Ａｌ合金反射膜の初期反射率試験
作製した直後の本発明反射膜１〜１０、比較反射膜１〜４および従来反射膜１の各反射率を分光光度計により測定し、その結果を表２〜３に示した。
The following tests were performed on the reflective films 1 to 10 of the present invention, the comparative reflective films 1 to 4 and the conventional reflective film 1 having a thickness of 100 nm formed as described above.
(A) Initial reflectance test of Al alloy reflective film The reflectances of the present reflective films 1 to 10, the comparative reflective films 1 to 4, and the conventional reflective film 1 immediately after production were measured with a spectrophotometer, and the results were obtained. It showed in Tables 2-3.
（ｂ）耐アルカリ性試験
本発明反射膜１〜１０、比較反射膜１〜４および従来反射膜１をそれぞれ１％ＮａＯＨ溶液に１２０秒間浸漬したのち取出して、蛍光灯下における室内照度３２０ルックスの環境にて反射膜を蛍光灯側に向けるようにかざし、光の透過の有無を目視にて観察する光透過試験を行い、その結果を表２〜３に示した。
(B) Alkali resistance test The reflective films 1 to 10 of the present invention, the comparative reflective films 1 to 4 and the conventional reflective film 1 are each immersed in a 1% NaOH solution for 120 seconds and then taken out, and the environment has an indoor illumination of 320 lux under a fluorescent lamp. The light transmission test was conducted by visually observing the presence or absence of light transmission by holding the reflective film facing the fluorescent lamp side, and the results are shown in Tables 2-3.
（ｃ）耐酸性試験
本発明反射膜１〜１０、比較反射膜１〜４および従来反射膜１をそれぞれ１％Ｈ２ＳＯ４溶液に１０分間浸漬したのち取出して、蛍光灯下における室内照度３２０ルックスの環境にて反射膜を蛍光灯側に向けるようにかざし、光の透過の有無を目視にて観察する光透過試験を行い、その結果を表２〜３に示した。
(C) Acid resistance test The reflective films 1 to 10, the comparative reflective films 1 to 4 and the conventional reflective film 1 of the present invention are each immersed in a 1% H 2 SO 4 solution for 10 minutes and then taken out, and the room illuminance 320 under a fluorescent lamp is taken out. In a Lux environment, the reflective film was held so as to face the fluorescent lamp side, and a light transmission test was performed to visually observe the presence or absence of light transmission. The results are shown in Tables 2-3.
（ｄ）耐湿性試験
本発明反射膜１〜１０、比較反射膜１〜４および従来反射膜１をそれぞれ温度：４０℃、相対湿度：８５％の恒温恒湿槽に１００時間保持したのち取出して反射率を分光光度計により波長：６５０ｎｍにて測定し、その結果を表２に示した。
(D) Moisture resistance test The reflective films 1 to 10, comparative reflective films 1 to 4 and the conventional reflective film 1 of the present invention are each held for 100 hours in a constant temperature and humidity chamber having a temperature of 40 ° C. and a relative humidity of 85%. The reflectance was measured with a spectrophotometer at a wavelength of 650 nm, and the results are shown in Table 2.
表１〜３に示される結果から、この発明の本発明ターゲット１〜１０を用いてスパッタリングを行うことにより得られた本発明反射膜１〜１０は、従来ターゲット１を用いてスパッタリングを行うことにより得られた従来反射膜１に比べて、初期反射率に大差が無いが、本発明反射膜１〜１０は従来反射膜１に比べて耐アルカリ性試験および耐酸性試験において耐食性が高く、また耐湿性試験後の反射率の低下が少ないことがわかる。しかし、この発明の範囲から外れてＭｇ、希土類元素および不可避不純物を含む比較ターゲット１〜４を用いて作製した反射膜は、ターゲット製造時に割れが生じたり、初期反射率が著しく低下したり各種試験後に膜が腐食され光を透過したりして好ましくない特性が現れることが分かる。
From the results shown in Tables 1 to 3, the present reflective films 1 to 10 obtained by performing sputtering using the present inventive targets 1 to 10 of the present invention are performed by performing sputtering using the conventional target 1. Although the initial reflectance is not significantly different from the obtained conventional reflective film 1, the reflective films 1 to 10 of the present invention have higher corrosion resistance and higher moisture resistance in the alkali resistance test and acid resistance test than the conventional reflective film 1. It can be seen that the decrease in reflectance after the test is small. However, the reflective film produced using the comparative targets 1 to 4 containing Mg, rare earth elements and inevitable impurities outside the scope of the present invention is cracked during the production of the target, the initial reflectivity is remarkably lowered, and various tests are performed. It can be seen that undesirable characteristics appear after the film is corroded and transmits light.
Claims (2)
Mg: 0.1 to 15% by mass, with the balance being made of Al and inevitable impurities, the inevitable impurities being made of an aluminum alloy having a composition defined as 100 ppm or less, and having excellent corrosion resistance A sputtering target for forming a reflective film for a reflector.
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| JP2006044737A JP2007072427A (en) | 2005-03-10 | 2006-02-22 | Reflection film for reflection plate excellent in corrosion resistance and sputtering target for forming reflection film for reflection plate excellent in corrosion resistance |
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| JP2005066916 | 2005-03-10 | ||
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| JP2006044737A JP2007072427A (en) | 2005-03-10 | 2006-02-22 | Reflection film for reflection plate excellent in corrosion resistance and sputtering target for forming reflection film for reflection plate excellent in corrosion resistance |
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| JP2007072427A true JP2007072427A (en) | 2007-03-22 |
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| JP2010287565A (en) * | 2009-05-14 | 2010-12-24 | Mitsubishi Materials Corp | Al ALLOY-REFLECTING ELECTRODE FILM FOR FORMING ANODE LAYER OF TOP-EMISSION TYPE ORGANIC EL ELEMENT |
| JP2012068608A (en) * | 2010-02-01 | 2012-04-05 | Kobe Steel Ltd | Reflective film laminate |
| JP2013225051A (en) * | 2012-04-23 | 2013-10-31 | Kobe Steel Ltd | Reflective film laminate and method of manufacturing the same |
| US20170253951A1 (en) * | 2012-12-26 | 2017-09-07 | Posco | Steel sheet coated with aluminum-magnesium |
| JP2020032686A (en) * | 2018-08-31 | 2020-03-05 | 北川工業株式会社 | Optical laminate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2010287565A (en) * | 2009-05-14 | 2010-12-24 | Mitsubishi Materials Corp | Al ALLOY-REFLECTING ELECTRODE FILM FOR FORMING ANODE LAYER OF TOP-EMISSION TYPE ORGANIC EL ELEMENT |
| JP2012068608A (en) * | 2010-02-01 | 2012-04-05 | Kobe Steel Ltd | Reflective film laminate |
| JP2013225051A (en) * | 2012-04-23 | 2013-10-31 | Kobe Steel Ltd | Reflective film laminate and method of manufacturing the same |
| US20170253951A1 (en) * | 2012-12-26 | 2017-09-07 | Posco | Steel sheet coated with aluminum-magnesium |
| US10619228B2 (en) * | 2012-12-26 | 2020-04-14 | Posco | Steel sheet coated with aluminum-magnesium |
| JP2020032686A (en) * | 2018-08-31 | 2020-03-05 | 北川工業株式会社 | Optical laminate |
| JP7084031B2 (en) | 2018-08-31 | 2022-06-14 | 北川工業株式会社 | Optical laminate |
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