JP2002226927A - Ag ALLOY REFLECTION FILM FOR PLANAR DISPLAY DEVICE - Google Patents
Ag ALLOY REFLECTION FILM FOR PLANAR DISPLAY DEVICEInfo
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- JP2002226927A JP2002226927A JP2001024453A JP2001024453A JP2002226927A JP 2002226927 A JP2002226927 A JP 2002226927A JP 2001024453 A JP2001024453 A JP 2001024453A JP 2001024453 A JP2001024453 A JP 2001024453A JP 2002226927 A JP2002226927 A JP 2002226927A
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- film
- alloy
- reflectance
- reflective film
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、例えば液晶ディス
プレイ、プラズマディスプレイパネル（以下、ＰＤ
Ｐ）、フィールドエミッションディスプレイ（以下、Ｆ
ＥＤ）、エレクトロルミネッセンス（以下、ＥＬ）等の
平面表示装置において、高い光学反射率と耐食性が要求
されるＡｇ合金系反射膜に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a liquid crystal display, a plasma display panel (hereinafter, referred to as a PD).
P), field emission display (hereinafter F
The present invention relates to an Ag alloy-based reflective film that requires high optical reflectance and corrosion resistance in flat display devices such as ED) and electroluminescence (hereinafter, EL).
【０００２】[0002]
【従来の技術】従来、液晶表示装置は、バックライトと
して光源（ランプ）を内蔵し背面から照射することで高
い表示品質を有する透過型液晶ディスプレイが一般的で
あった。しかし、透過型液晶ディスプレイはバックライ
トの消費電力が大きく、電池駆動の携帯情報端末として
は使用時間が短くなると言う問題があった。このため、
近年、外光を効率よく利用しバックライトを基本的に使
用しない反射型液晶ディスプレイの開発が行われてい
る。このような反射型ディスプレイに用いる反射膜に
は、金属の中でも可視光域の反射率の高い元素であるＡ
ｌまたはＡｌ合金薄膜が多く用いられてきた。2. Description of the Related Art Conventionally, a liquid crystal display device generally includes a transmissive liquid crystal display having a high display quality by incorporating a light source (lamp) as a backlight and irradiating the light from the back. However, the transmissive liquid crystal display has a problem that the power consumption of the backlight is large and the use time of the portable information terminal driven by a battery is short. For this reason,
2. Description of the Related Art In recent years, a reflective liquid crystal display that efficiently uses external light and basically does not use a backlight has been developed. The reflective film used for such a reflective display includes A, which is an element having a high reflectance in the visible light region among metals.
1 or Al alloy thin films have been widely used.
【０００３】また、近年、液晶ディスプレイの表示品質
向上のため、その反射膜にはペーパーホワイトと呼ばれ
る高い反射と可視光域でフラットな反射特性が求められ
ている。このため、Ａｌより反射率の高いＡｇが注目さ
れている。In recent years, in order to improve the display quality of a liquid crystal display, the reflection film is required to have a high reflection called paper white and a flat reflection characteristic in a visible light region. For this reason, Ag having higher reflectivity than Al has attracted attention.
【０００４】[0004]
【発明が解決しようとする課題】上述のＡｌ系反射膜の
場合、液晶ディスプレイの製造工程中の加熱工程でヒロ
ック等が発生したり、また粒成長により反射率が低下す
る問題がある。このため、上記ヒロックや粒成長の抑制
のために、Ａｌに遷移金属であるＴｉ、Ｔａ等の耐食性
向上元素を添加するＡｌ合金が用いられている。このＡ
ｌ合金により液晶ディスプレイ製造時の反射率低減は抑
制できる。しかし、素材の反射率そのものが低下してし
まう問題がある。In the case of the above-mentioned Al-based reflective film, there is a problem that hillocks and the like are generated in a heating step in a manufacturing process of a liquid crystal display, and that the reflectance is lowered due to grain growth. For this reason, an Al alloy in which a transition metal such as Ti or Ta is added to Al to suppress the hillocks and grain growth is used. This A
With the use of the 1 alloy, the reduction of the reflectance during the production of the liquid crystal display can be suppressed. However, there is a problem that the reflectance itself of the material is reduced.
【０００５】一方、反射率の高いＡｇ反射膜の場合、液
晶ディスプレイ用の基板であるガラスやプラスチックに
対しての密着性が低く、プロセス中に剥がれが生じると
いう問題がある。さらに、この密着性が低いことに起因
し、ディスプレイの製造時の加熱工程等で膜が凝集し大
幅に反射率が低下すると共に、抵抗値が増加してしま
う。また、耐食性が低く、基板上に成膜した後、１日程
度大気に放置しただけで変色し、黄色味を帯びた反射特
性となる。そして、ディスプレイの製造時に使用する薬
液により腐食され、大幅に反射率が低下してしまう問題
があった。On the other hand, an Ag reflective film having a high reflectance has a problem that adhesion to glass or plastic, which is a substrate for a liquid crystal display, is low, and peeling occurs during the process. Further, due to the low adhesion, the film is aggregated in a heating step or the like at the time of manufacturing the display, so that the reflectance is greatly reduced and the resistance value is increased. In addition, it has low corrosion resistance, and after forming a film on a substrate, it is discolored only by being left in the air for about one day, and has a yellowish reflection characteristic. Then, there is a problem that the liquid crystal is corroded by a chemical used at the time of manufacturing the display, and the reflectance is greatly reduced.
【０００６】本発明の目的は、例えば反射型液晶ディス
プレイ、ＦＥＤ等のような平面表示装置において要求さ
れる高い反射率とプロセス中での耐熱性、耐食性、そし
て基板への密着性を兼ね備えたＡｇ合金系反射膜を提供
することにある。An object of the present invention is to provide Ag having both high reflectance required in a flat display device such as a reflection type liquid crystal display and an FED, heat resistance in a process, corrosion resistance, and adhesion to a substrate. An object of the present invention is to provide an alloy-based reflective film.
【０００７】[0007]
【課題を解決するための手段】本発明者らは、上記の課
題を解決するべく、鋭意検討を行った結果、Ａｇに、選
択した元素を加えた反射膜とすることにより、本来Ａｇ
の持つ高い反射率を低下させることなく耐熱性、耐食性
を向上し、さらに基板への密着性も改善できることを見
いだし、本発明に到達した。Means for Solving the Problems The inventors of the present invention have conducted intensive studies to solve the above-mentioned problems, and as a result, by forming a reflective film in which a selected element is added to Ag, the original Ag is obtained.
It has been found that the heat resistance and the corrosion resistance can be improved without lowering the high reflectance possessed by the compound, and that the adhesion to the substrate can be improved, and the present invention has been achieved.
【０００８】すなわち、本発明は、Ｃｅ、Ｎｄ、Ｓｍ、
Ｇｄ、Ｔｂ、Ｄｙから選ばれる１種以上の元素を０．２
〜５ａｔ（原子）％含み、残部実質的にＡｇからなるＡ
ｇ合金系反射膜である。That is, the present invention relates to Ce, Nd, Sm,
One or more elements selected from Gd, Tb and Dy
A containing at most 5 at (atomic)% and the balance being substantially Ag
It is a g-alloy reflective film.
【０００９】また、本発明のＡｇ合金系反射膜は、Ｔ
ｉ、Ｖ、Ｎｂ、Ｃｒ、Ｍｏ、Ｍｎから選ばれる１種以上
の元素を１〜１０ａｔ％含んでいてもよい。Further, the Ag alloy-based reflective film of the present invention has a T
It may contain 1 to 10 at% of one or more elements selected from i, V, Nb, Cr, Mo, and Mn.
【００１０】[0010]
【発明の実施の形態】本発明のＡｇ合金系反射膜の最も
重要な特徴は、Ｃｅ、Ｎｄ、Ｓｍ、Ｇｄ、Ｔｂ、Ｄｙか
ら選ばれる１種以上の元素を０．２〜５ａｔ％含み、残
部実質的にＡｇからなるところにある。BEST MODE FOR CARRYING OUT THE INVENTION The most important feature of the Ag alloy-based reflective film of the present invention is that it contains 0.2 to 5 at% of one or more elements selected from Ce, Nd, Sm, Gd, Tb and Dy, The balance is substantially composed of Ag.
【００１１】通常、純Ａｇを原料として反射膜を作製す
ると、膜としての反射率は高いものの、その反射膜を用
いて製品（例えば液晶ディスプレイなど）を作製する際
のプロセスにおいて反射率が低下してしまうという問題
があることは、上述の通りである。そこで、本発明で
は、ＡｇにＣｅ、Ｎｄ、Ｓｍ、Ｇｄ、Ｔｂ、Ｄｙから選
ばれる１種以上の元素を適量添加することにより、反射
膜の反射率を低下させることなく、場合によっては純Ａ
ｇより反射率の向上が図れた反射膜とすることができ
る。Usually, when a reflective film is produced using pure Ag as a raw material, the reflectivity as a film is high, but the reflectivity decreases in a process of producing a product (eg, a liquid crystal display) using the reflective film. As described above, there is the problem that the Therefore, in the present invention, by adding an appropriate amount of one or more elements selected from Ce, Nd, Sm, Gd, Tb, and Dy to Ag, the reflectivity of the reflective film may not be reduced, and pure A may be added in some cases.
It is possible to obtain a reflection film whose reflectance is improved more than g.
【００１２】また、例えば液晶ディスプレイ、有機ＥＬ
といった製品の製造工程では、その反射膜を形成した後
に何度かの加熱処理を伴う工程があり、その際の加熱工
程でもＡｇ反射膜は反射率が低下する。つまり、加熱に
よる膜成長や凝集等が起こり膜表面はより凹凸のある形
状となり、またボイドが発生する。そして、その加熱雰
囲気によっては膜表面が変色し、これも反射率の低下す
る原因となる。この場合であっても、本発明のＡｇ合金
系反射膜は、Ａｇに上述したＣｅ、Ｎｄ、Ｓｍ、Ｇｄ、
Ｔｂ、Ｄｙから選ばれる１種以上の元素を適量加えるこ
とにより、この加熱に伴う工程後でも高い反射率を維持
する。Also, for example, a liquid crystal display, an organic EL
In the manufacturing process of such a product, there is a process involving several heat treatments after the formation of the reflective film. Even in the heating process, the reflectance of the Ag reflective film is reduced. That is, film growth, aggregation, and the like occur due to heating, and the film surface has a more uneven shape, and voids are generated. Then, depending on the heating atmosphere, the film surface is discolored, which also causes a decrease in reflectance. Even in this case, the Ag alloy-based reflective film of the present invention provides the above-described Ce, Nd, Sm, Gd,
By adding an appropriate amount of at least one element selected from Tb and Dy, a high reflectance is maintained even after the step accompanying this heating.
【００１３】上記本発明のＣｅ、Ｎｄ、Ｓｍ、Ｇｄ、Ｔ
ｂ、Ｄｙは、その添加・含有量を合計で０．２〜５ａｔ
％とした。これは、０．２ａｔ％未満ではその含有によ
る耐熱性の改善効果がなく、５ａｔ％を超えると十分な
反射率を維持・確保できないためである。さらに高い耐
熱性と９５％以上の高い反射率を得るには１〜４ａｔ％
の含有が望ましい。The above Ce, Nd, Sm, Gd, T of the present invention
b and Dy are added and contained in a total amount of 0.2 to 5 at.
%. This is because if the content is less than 0.2 at%, there is no effect of improving heat resistance due to the content, and if it exceeds 5 at%, a sufficient reflectance cannot be maintained or secured. 1 to 4 at% to obtain higher heat resistance and higher reflectivity of 95% or more
Is desirable.
【００１４】本発明の上記元素種の含有による反射率の
維持または向上の理由は明確ではない。しかし、融点の
比較的低いＡｇの場合、本発明の選定したＣｅ、Ｎｄ、
Ｓｍ、Ｇｄ、Ｔｂ、Ｄｙの添加元素はＡｇと化合物を形
成し易く、粒界に析出することから、これがＡｇ粒界腐
食による酸化を防ぎ耐食性を向上させ、高い反射率を維
持できるものと考えられる。[0014] The reason for maintaining or improving the reflectance by containing the above-mentioned element species of the present invention is not clear. However, in the case of Ag having a relatively low melting point, Ce, Nd,
Since the added elements of Sm, Gd, Tb, and Dy easily form a compound with Ag and precipitate at the grain boundaries, they are considered to prevent oxidation due to Ag grain boundary corrosion, improve corrosion resistance, and maintain high reflectance. Can be
【００１５】また、粒界にＡｇの化合物が析出すること
により加熱工程での粒成長や凝集が抑制されるため、耐
熱性が向上する。そして、微細で平滑な表面の膜形態と
なるために反射率の低下を抑制できる。さらに、これら
元素種の添加により膜応力が低減される効果と、凝集抑
制の両方の効果により、密着性が改善されると考えられ
る。Further, since the Ag compound precipitates at the grain boundaries, the grain growth and aggregation in the heating step are suppressed, so that the heat resistance is improved. In addition, since the film has a fine and smooth surface, it is possible to suppress a decrease in reflectance. Further, it is considered that the adhesion is improved by both the effect of reducing the film stress and the effect of suppressing the aggregation by the addition of these element types.
【００１６】通常、スパッタ膜においては、その添加さ
れる元素は基地中に過飽和で固溶する。つまり、結晶格
子間に添加元素が過飽和に侵入することから、その格子
が乱れ、自由電子の動きが阻害されるために反射率が低
下する。しかし、添加元素が粒界析出物を形成する本発
明の場合、そのＡｇ粒内はＡｇ単独となり自由電子の動
きも阻害されず、高い反射率を維持できる。Usually, in a sputtered film, the added element is supersaturated and forms a solid solution in the matrix. That is, since the additional element invades into the supersaturation between the crystal lattices, the lattice is disturbed, and the movement of free electrons is inhibited, so that the reflectance is reduced. However, in the case of the present invention in which the additive element forms a grain boundary precipitate, the Ag inside the Ag grains becomes only Ag and the movement of free electrons is not inhibited, so that a high reflectance can be maintained.
【００１７】本発明のＡｇ合金系反射膜は、上記元素種
の１種以上を必須として含んだ上で、さらには、Ｔｉ、
Ｖ、Ｎｂ、Ｃｒ、Ｍｏ、Ｍｎから選ばれる１種以上の元
素を１〜１０ａｔ％含んでいてもよい。これらの元素が
含まれることにより、さらに耐食性が向上し、反射率の
低下を抑制する。The Ag alloy-based reflective film of the present invention contains at least one of the above-mentioned element types, and further contains Ti,
One or more elements selected from V, Nb, Cr, Mo, and Mn may be contained at 1 to 10 at%. By containing these elements, the corrosion resistance is further improved, and a decrease in reflectance is suppressed.
【００１８】上述の通り、本発明のＣｅ、Ｎｄ、Ｓｍ、
Ｇｄ、Ｔｂ、ＤｙはＡｇと化合物を形成し易く、その粒
界に析出することで粒界腐食を抑制し、これが耐食性を
向上させるものと考えられるが、例えばフラットディス
プレイの製造工程において使用される酸等の薬液に対す
る耐食性を確保するには十分でない場合がある。本発明
の選定するＴｉ、Ｖ、Ｎｂ、Ｃｒ、Ｍｏ、Ｍｎは強い耐
酸性を有し、また上記Ｃｅ、Ｎｄ、Ｓｍ、Ｇｄ、Ｔｂ、
Ｄｙとは固溶し難いため、膜表面や粒界に析出し、Ａｇ
合金膜全体を保護するとして、これが大幅に耐食性を向
上するものと考えられる。As described above, Ce, Nd, Sm,
Gd, Tb, and Dy are likely to form compounds with Ag and precipitate at the grain boundaries to suppress intergranular corrosion, which is thought to improve corrosion resistance. For example, they are used in flat display manufacturing processes. It may not be enough to ensure corrosion resistance to chemicals such as acids. Ti, V, Nb, Cr, Mo, and Mn selected by the present invention have strong acid resistance, and the above Ce, Nd, Sm, Gd, Tb,
Since Dy is unlikely to form a solid solution, it precipitates on the film surface and grain boundaries,
This is considered to significantly improve the corrosion resistance of the entire alloy film.
【００１９】加えて、Ｔｉ、Ｖ、Ｎｂ、Ｃｒ、Ｍｏ、Ｍ
ｎはガラスやプラスティック基板との密着性が良く、本
発明のＡｇ合金系反射膜に添加することで基板との密着
性を大幅に向上することが可能となる。In addition, Ti, V, Nb, Cr, Mo, M
n has good adhesion to glass or a plastic substrate, and when added to the Ag alloy-based reflective film of the present invention, it becomes possible to greatly improve the adhesion to the substrate.
【００２０】Ｔｉ、Ｖ、Ｎｂ、Ｃｒ、Ｍｏ、Ｍｎから選
ばれる１種以上の元素の含有量は、１ａｔ％未満では耐
食性改善効果が不十分であり、１０ａｔ％を超えると耐
食性は優れるが反射率が大幅に低下してしまう。このた
め、これらの元素の含有量は１〜１０ａｔ％とすること
が望ましい。好ましくは、１〜５ａｔ％である。If the content of at least one element selected from Ti, V, Nb, Cr, Mo, and Mn is less than 1 at%, the effect of improving corrosion resistance is insufficient, and if it exceeds 10 at%, corrosion resistance is excellent but reflection is high. The rate will drop significantly. Therefore, the content of these elements is desirably 1 to 10 at%. Preferably, it is 1 to 5 at%.
【００２１】本発明のＡｇ合金系反射膜は、安定した反
射率を得るために膜厚としては５０〜３００ｎｍとする
ことが好ましい。５０ｎｍ未満であると、膜の表面形態
が変化し易く、さらに例えば平面表示装置に用いた場合
に光が透過するために、反射率が低下する。一方、３０
０ｎｍを超える膜厚であると、反射率が大きく変化せ
ず、膜を形成する際に時間が掛かる。The Ag alloy-based reflective film of the present invention preferably has a thickness of 50 to 300 nm in order to obtain a stable reflectance. When the thickness is less than 50 nm, the surface morphology of the film is liable to change, and further, for example, when used for a flat panel display, light is transmitted, so that the reflectance is reduced. On the other hand, 30
When the film thickness exceeds 0 nm, the reflectance does not change significantly, and it takes time to form the film.
【００２２】また、本発明のＡｇ合金系反射膜を形成す
る場合、例えばターゲットを用いたスパッタリングで形
成する際に用いる基板として、ガラス基板、Ｓｉウェハ
ーを用いることが好適ではあるが、スパッタリングで薄
膜を形成できるものであればよく、例えば樹脂基板、金
属基板でもよい。When the Ag alloy-based reflective film of the present invention is formed, for example, a glass substrate or a Si wafer is preferably used as a substrate used for forming by sputtering using a target. Any material can be used as long as it can be formed, and for example, a resin substrate or a metal substrate may be used.
【００２３】[0023]
【実施例】（実施例１）Ａｇ合金系反射膜の目標組成と
実質的に同一となるようにターゲット材を作製し、機械
加工により直径１００ｍｍ、厚さ５ｍｍのターゲットを
作製した。そのターゲットを用いたスパッタリングによ
り、ガラス基板またはＳｉウェハー上に膜厚２００ｎｍ
のＡｇ合金系反射膜を形成し、光学反射率計を用いてそ
の反射率を測定した。EXAMPLES (Example 1) A target material was manufactured so as to have substantially the same target composition as the Ag alloy-based reflective film, and a target having a diameter of 100 mm and a thickness of 5 mm was manufactured by machining. By sputtering using the target, a film thickness of 200 nm is formed on a glass substrate or a Si wafer.
Was formed, and the reflectance was measured using an optical reflectometer.
【００２４】さらに、所定製品としての製造工程を経た
後での反射率を評価するために、上記作製したＡｇ合金
系反射膜を温度２５０℃の窒素ガス雰囲気で加熱処理
後、再度反射率を測定した。その熱処理による反射率の
変化も併せ、測定結果を表１に示す。Further, in order to evaluate the reflectance after the manufacturing process as a predetermined product, the Ag alloy-based reflection film prepared above was heated in a nitrogen gas atmosphere at a temperature of 250 ° C., and the reflectance was measured again. did. The measurement results are shown in Table 1 together with the change in reflectance due to the heat treatment.
【００２５】[0025]
【表１】 [Table 1]
【００２６】純Ａｇ膜（Ｎｏ．１）は、成膜時にて９９
％の反射率を有するが、加熱処理にて大幅に反射率が低
下している。一方、ＡｇにＣｅ、Ｎｄ、Ｓｍ、Ｇｄ、Ｔ
ｂ、Ｄｙから選ばれる１種以上の元素を含むＡｇ合金膜
は熱処理後の反射率の低下が抑制されており、その効果
は０．２ａｔ％以上の添加量で明確となっている。しか
し、その添加量が増加すると熱処理後の反射率の低下こ
そ少ないが、成膜時の反射率が低下し、５ａｔ％を超え
ると高い反射率が得難くなる。このため、本発明の上記
含有量は合計で０．２〜５ａｔ％とする。また、９５％
以上の反射率を安定して得るに、その含有量は０．５〜
３ａｔ％が望ましい。The pure Ag film (No. 1) was 99%
%, But the reflectance is significantly reduced by the heat treatment. On the other hand, Ag, Ce, Nd, Sm, Gd, T
The Ag alloy film containing one or more elements selected from b and Dy has a suppressed decrease in reflectance after heat treatment, and the effect is clear at an addition amount of 0.2 at% or more. However, when the amount of addition increases, the reflectance after heat treatment decreases only slightly, but the reflectance during film formation decreases, and when it exceeds 5 at%, it becomes difficult to obtain a high reflectance. For this reason, the content of the present invention is set to 0.2 to 5 at% in total. 95%
In order to stably obtain the above reflectance, the content is 0.5 to
3 at% is desirable.
【００２７】（実施例２）形成した所定の組成を有する
Ａｇ合金膜に実施例１と同条件の加熱処理を行ない、そ
の反射率を測定した。そして、さらに温度８０℃、湿度
９０％の環境に２４ｈ放置した際の反射率を測定した。
その環境試験による反射率の変化も併せ、測定結果を表
２に示す。Example 2 A heat treatment was performed on the formed Ag alloy film having a predetermined composition under the same conditions as in Example 1, and the reflectance was measured. Then, the reflectance when left for 24 hours in an environment at a temperature of 80 ° C. and a humidity of 90% was measured.
The measurement results are shown in Table 2 together with the change in reflectance due to the environmental test.
【００２８】[0028]
【表２】 [Table 2]
【００２９】純Ａｇ膜（Ｎｏ．３３）は、上記の環境試
験にて大幅に反射率が低下している。また、ＡｇにＴ
ｉ、Ｍｎ等のみを添加したＡｇ合金膜（Ｎｏ．４３〜４
８）の場合、上記の環境試験による反射率の低下こそ少
ないが、反射率そのものが低いことがわかる。それらに
対し、本発明のＡｇ合金膜は、環境試験による耐食性の
評価の上でも反射率の低下が少なく、高い反射率を維持
できることがわかる。The reflectivity of the pure Ag film (No. 33) has been significantly reduced in the above environmental test. In addition, T
Ag alloy film containing only i, Mn, etc. (Nos. 43 to 4)
In the case of 8), it can be seen that the reflectivity is reduced only slightly by the environmental test, but the reflectivity itself is low. On the other hand, it can be seen that the Ag alloy film of the present invention has a small decrease in reflectance and can maintain a high reflectance even in the evaluation of corrosion resistance by an environmental test.
【００３０】（実施例３）以下のプロセス試験により耐
食性の評価を行なった。実施例２に同組成のＡｇ合金膜
を形成して作製・熱処理した基板上に、東京応化製ＯＦ
ＰＲ−８００レジストをスピンコートにより形成した。
次にフォトマスクを用いて紫外線でレジストを露光後、
有機アルカリ現像液ＮＭＤ−３で現像し、レジストパタ
ーンを作製、希塩酸に３０秒間浸漬した後に浸漬部の反
射率を再度測定した。そのプロセス試験による反射率の
変化も併せ、測定結果を表３に示す。Example 3 The corrosion resistance was evaluated by the following process tests. An Ag alloy film of the same composition as in Example 2 was formed and heat-treated on a substrate, which was manufactured by Tokyo Ohka.
A PR-800 resist was formed by spin coating.
Next, after exposing the resist with ultraviolet light using a photomask,
The resist was developed with an organic alkali developer NMD-3 to form a resist pattern. After immersion in dilute hydrochloric acid for 30 seconds, the reflectance of the immersed portion was measured again. The measurement results are shown in Table 3 together with the change in reflectance due to the process test.
【００３１】[0031]
【表３】 [Table 3]
【００３２】純Ａｇ膜（Ｎｏ．３３）は、上記のプロセ
ス試験にて大幅に反射率が低下している。また、Ａｇに
Ｔｉ、Ｍｎ等のみを添加したＡｇ合金膜（Ｎｏ．４３〜
４８）の場合、上記のプロセス試験による反射率の低下
こそ少ないが、反射率そのものが低いことは述べた通り
である。それらに対し、Ａｇに所定量の希土類元素：Ｃ
ｅ、Ｎｄ、Ｓｍ、Ｇｄ、Ｔｂ、Ｄｙを添加した本発明の
Ａｇ合金膜は、プロセス試験による反射率の低下こそあ
るも、それであっても９０％以上の反射率を維持してい
る。そして、さらに所定量の遷移金属：Ｔｉ、Ｖ、Ｎ
ｂ、Ｃｒ、Ｍｏ、Ｍｎを加えた本発明のＡｇ合金膜は、
プロセス試験後にて高い反射率を維持できることがわか
る。The reflectivity of the pure Ag film (No. 33) is greatly reduced in the above process test. Ag alloy films obtained by adding only Ti, Mn, etc. to Ag (Nos. 43 to 43)
In the case of 48), as described above, the reflectivity itself is low although the reflectivity is not significantly reduced by the above process test. On the other hand, a predetermined amount of rare earth element: C
The Ag alloy film of the present invention to which e, Nd, Sm, Gd, Tb, and Dy are added maintains the reflectivity of 90% or more even though the reflectivity is lowered by the process test. And a predetermined amount of transition metal: Ti, V, N
The Ag alloy film of the present invention to which b, Cr, Mo, and Mn are added,
It can be seen that high reflectivity can be maintained after the process test.
【００３３】（実施例４）次に膜の密着性を評価する。
実施例２に同組成のＡｇ合金膜を形成して作製した基板
にて、その膜の基板との密着性を測定した。具体的に
は、膜表面にスコッチテープを貼り付け、斜め４５°方
向にテープを引き剥がした際に基板上に残った面積を２
０ｃｍ２あたりの面積率にて表わし、密着力として評価
した。結果を表４に示す。Example 4 Next, the adhesion of the film is evaluated.
Using a substrate prepared by forming an Ag alloy film having the same composition as in Example 2, the adhesion of the film to the substrate was measured. Specifically, a scotch tape was stuck on the film surface, and the area left on the substrate when the tape was peeled off at an angle of 45 ° was 2
It was expressed as the area ratio per 0 cm 2 and evaluated as the adhesion. Table 4 shows the results.
【００３４】[0034]
【表４】 [Table 4]
【００３５】純Ａｇ膜（Ｎｏ．３３）に比して、Ａｇに
所定量のＣｅ、Ｎｄ、Ｓｍ、Ｇｄ、Ｔｂ、Ｄｙを添加し
た本発明のＡｇ合金膜は大幅に密着性が改善されてい
る。そして、所定量のＴｉ、Ｖ、Ｎｂ、Ｃｒ、Ｍｏ、Ｍ
ｎをも加えた本発明のＡｇ合金膜では、さらに優れた密
着性が得られていることがわかる。Compared with the pure Ag film (No. 33), the Ag alloy film of the present invention in which a predetermined amount of Ce, Nd, Sm, Gd, Tb, and Dy are added to Ag has significantly improved adhesion. I have. Then, a predetermined amount of Ti, V, Nb, Cr, Mo, M
It can be seen that the Ag alloy film of the present invention to which n is added also has more excellent adhesion.
【００３６】[0036]
【発明の効果】本発明であれば、高い反射率と耐環境
性、耐薬品性、そして基板との密着性を改善したＡｇ合
金系反射膜を得ることが可能である。よって、携帯情報
端末等に用いられる低消費電力が要求される反射型液晶
ディスプレイ等の平面表示装置に有用であり、産業上の
価値は高い。According to the present invention, it is possible to obtain an Ag alloy-based reflective film having high reflectivity, improved environmental resistance, improved chemical resistance, and improved adhesion to a substrate. Therefore, it is useful for a flat display device such as a reflection type liquid crystal display which is used for a portable information terminal and requires low power consumption, and has high industrial value.
─────────────────────────────────────────────────────
────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成１４年２月２５日（２００２．２．２
５）[Submission Date] February 25, 2002 (2002.2.2)
5)
【手続補正１】[Procedure amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】発明の名称[Correction target item name] Name of invention
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【発明の名称】 平面表示装置用Ａｇ合金系反射膜Patent application title: Ag alloy-based reflective film for flat panel display
【手続補正２】[Procedure amendment 2]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】特許請求の範囲[Correction target item name] Claims
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【特許請求の範囲】[Claims]
【請求項２】ガラス基板またはＳｉウェハー上に形成さ
れた請求項１に記載の平面表示装置用Ａｇ合金系反射
膜。 2. A method according to claim 1, wherein said substrate is formed on a glass substrate or a Si wafer.
The Ag alloy-based reflection for a flat panel display according to claim 1.
film.
【請求項３】Ｔｉ、Ｖ、Ｎｂ、Ｃｒ、Ｍｏ、Ｍｎから選
ばれる１種以上の元素を１〜１０ａｔ％含むことを特徴
とする請求項１または２に記載の平面表示装置用Ａｇ合
金系反射膜。 Wherein Ti, V, Nb, Cr, Mo, flat display devices Ag alloy system according to claim 1 or 2, characterized in that it comprises 1～10At% one or more elements selected from Mn Reflective film.
【手続補正３】[Procedure amendment 3]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】０００１[Correction target item name] 0001
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【０００１】[0001]
【発明の属する技術分野】本発明は、例えば液晶ディス
プレイ、プラズマディスプレイパネル（以下、ＰＤ
Ｐ）、フィールドエミッションディスプレイ（以下、Ｆ
ＥＤ）、エレクトロルミネッセンス（以下、ＥＬ）等の
平面表示装置において、高い光学反射率と耐食性が要求
される平面表示装置用Ａｇ合金系反射膜に関するもので
ある。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a liquid crystal display, a plasma display panel (hereinafter, referred to as a PD).
P), field emission display (hereinafter F
The present invention relates to an Ag alloy-based reflective film for a flat display device which requires high optical reflectance and corrosion resistance in flat display devices such as ED) and electroluminescence (hereinafter, EL).
【手続補正４】[Procedure amendment 4]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】０００６[Correction target item name] 0006
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【０００６】本発明の目的は、例えば反射型液晶ディス
プレイ、ＦＥＤ等のような平面表示装置において要求さ
れる高い反射率とプロセス中での耐熱性、耐食性、そし
て基板への密着性を兼ね備えた平面表示装置用Ａｇ合金
系反射膜を提供することにある。An object of the present invention, for example, a reflective liquid crystal display, heat resistance in a high reflectivity and processes required in the flat display device such as FED or the like, corrosion and the plane having both adhesion to the substrate, An object of the present invention is to provide an Ag alloy-based reflective film for a display device .
【手続補正５】[Procedure amendment 5]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】０００８[Correction target item name] 0008
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【０００８】すなわち、本発明は、Ｃｅ、Ｎｄ、Ｓｍ、
Ｇｄ、Ｔｂ、Ｄｙから選ばれる１種以上の元素を０．２
〜５ａｔ（原子）％含み、残部実質的にＡｇからなる平
面表示装置用Ａｇ合金系反射膜である。That is, the present invention relates to Ce, Nd, Sm,
One or more elements selected from Gd, Tb and Dy
Wherein ～5At (atomic)%, the balance being substantially Ag Rights
An Ag alloy-based reflective film for a surface display device .
【手続補正６】[Procedure amendment 6]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】０００９[Correction target item name] 0009
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【０００９】また、本発明の平面表示装置用Ａｇ合金系
反射膜は、Ｔｉ、Ｖ、Ｎｂ、Ｃｒ、Ｍｏ、Ｍｎから選ば
れる１種以上の元素を１〜１０ａｔ％含んでいてもよ
い。Further , the Ag alloy-based reflective film for a flat panel display of the present invention may contain 1 to 10 at% of one or more elements selected from Ti, V, Nb, Cr, Mo and Mn.
【手続補正７】[Procedure amendment 7]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００１０[Correction target item name] 0010
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【００１０】[0010]
【発明の実施の形態】本発明の平面表示装置用Ａｇ合金
系反射膜の最も重要な特徴は、Ｃｅ、Ｎｄ、Ｓｍ、Ｇ
ｄ、Ｔｂ、Ｄｙから選ばれる１種以上の元素を０．２〜
５ａｔ％含み、残部実質的にＡｇからなるところにあ
る。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The most important feature of the Ag alloy-based reflective film for a flat panel display according to the present invention is Ce, Nd, Sm, and G.
at least one element selected from d, Tb and Dy
5 at%, with the balance substantially consisting of Ag.
【手続補正８】[Procedure amendment 8]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００１２[Correction target item name] 0012
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【００１２】また、例えば液晶ディスプレイ、有機ＥＬ
といった製品の製造工程では、その反射膜を形成した後
に何度かの加熱処理を伴う工程があり、その際の加熱工
程でもＡｇ反射膜は反射率が低下する。つまり、加熱に
よる膜成長や凝集等が起こり膜表面はより凹凸のある形
状となり、またボイドが発生する。そして、その加熱雰
囲気によっては膜表面が変色し、これも反射率の低下す
る原因となる。この場合であっても、本発明の平面表示
装置用Ａｇ合金系反射膜は、Ａｇに上述したＣｅ、Ｎ
ｄ、Ｓｍ、Ｇｄ、Ｔｂ、Ｄｙから選ばれる１種以上の元
素を適量加えることにより、この加熱に伴う工程後でも
高い反射率を維持する。Also, for example, a liquid crystal display, an organic EL
In a process of manufacturing such a product, there is a process involving several heat treatments after the formation of the reflective film, and the reflectance of the Ag reflective film is reduced even in the heating process. That is, film growth, aggregation, and the like are caused by heating, and the film surface has a more uneven shape, and voids are generated. Then, depending on the heating atmosphere, the film surface is discolored, which also causes a decrease in reflectance. Even in this case, the planar display of the present invention
The Ag alloy-based reflective film for the device is made of the above-described Ce, N
By adding an appropriate amount of at least one element selected from d, Sm, Gd, Tb, and Dy, a high reflectance is maintained even after this heating step.
【手続補正９】[Procedure amendment 9]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００１７[Correction target item name] 0017
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【００１７】本発明の平面表示装置用Ａｇ合金系反射膜
は、上記元素種の１種以上を必須として含んだ上で、さ
らには、Ｔｉ、Ｖ、Ｎｂ、Ｃｒ、Ｍｏ、Ｍｎから選ばれ
る１種以上の元素を１〜１０ａｔ％含んでいてもよい。
これらの元素が含まれることにより、さらに耐食性が向
上し、反射率の低下を抑制する。The Ag alloy-based reflective film of the present invention for a flat display device contains at least one of the above-mentioned element types, and further comprises one or more selected from Ti, V, Nb, Cr, Mo, and Mn. More than one kind of element may be contained at 1 to 10 at%.
By containing these elements, the corrosion resistance is further improved, and a decrease in reflectance is suppressed.
【手続補正１０】[Procedure amendment 10]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００１９[Correction target item name] 0019
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【００１９】加えて、Ｔｉ、Ｖ、Ｎｂ、Ｃｒ、Ｍｏ、Ｍ
ｎはガラスやプラスティック基板との密着性が良く、本
発明の平面表示装置用Ａｇ合金系反射膜に添加すること
で基板との密着性を大幅に向上することが可能となる。In addition, Ti, V, Nb, Cr, Mo, M
n has good adhesion to glass or a plastic substrate, and when added to the Ag alloy-based reflective film for a flat display device of the present invention, it becomes possible to greatly improve the adhesion to the substrate.
【手続補正１１】[Procedure amendment 11]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００２１[Correction target item name] 0021
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【００２１】本発明の平面表示装置用Ａｇ合金系反射膜
は、安定した反射率を得るために膜厚としては５０〜３
００ｎｍとすることが好ましい。５０ｎｍ未満である
と、膜の表面形態が変化し易く、さらに例えば平面表示
装置に用いた場合に光が透過するために、反射率が低下
する。一方、３００ｎｍを超える膜厚であると、反射率
が大きく変化せず、膜を形成する際に時間が掛かる。The Ag alloy-based reflective film for a flat panel display of the present invention has a thickness of 50 to 3 to obtain a stable reflectance.
It is preferably set to 00 nm. If it is less than 50 nm, the surface morphology of the film is liable to change, and furthermore, for example, when used in a flat panel display, light is transmitted, so that the reflectance decreases. On the other hand, if the thickness exceeds 300 nm, the reflectance does not change significantly, and it takes time to form the film.
【手続補正１２】[Procedure amendment 12]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００２２[Correction target item name] 0022
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【００２２】また、本発明の平面表示装置用Ａｇ合金系
反射膜を形成する場合、例えばターゲットを用いたスパ
ッタリングで形成する際に用いる基板として、ガラス基
板、Ｓｉウェハーを用いることが好適ではあるが、スパ
ッタリングで薄膜を形成できるものであればよく、例え
ば樹脂基板、金属基板でもよい。In the case of forming the Ag alloy-based reflective film for a flat panel display according to the present invention, it is preferable to use a glass substrate or a Si wafer as a substrate used for forming by sputtering using a target, for example. As long as a thin film can be formed by sputtering, a resin substrate or a metal substrate may be used.
Claims (2)
ら選ばれる１種以上の元素を合計で０．２〜５ａｔ％含
み、残部実質的にＡｇからなることを特徴とするＡｇ合
金系反射膜。1. An Ag alloy system comprising at least one element selected from the group consisting of Ce, Nd, Sm, Gd, Tb, and Dy in a total amount of 0.2 to 5 at%, and the balance substantially consisting of Ag. Reflective film.
選ばれる１種以上の元素を１〜１０ａｔ％含むことを特
徴とする請求項１に記載のＡｇ合金系反射膜。2. The Ag alloy-based reflective film according to claim 1, wherein the Ag alloy-based reflective film contains 1 to 10 at% of at least one element selected from Ti, V, Nb, Cr, Mo, and Mn.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001024453A JP3656898B2 (en) | 2001-01-31 | 2001-01-31 | Ag alloy reflective film for flat panel display |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001024453A JP3656898B2 (en) | 2001-01-31 | 2001-01-31 | Ag alloy reflective film for flat panel display |
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| Publication Number | Publication Date |
|---|---|
| JP2002226927A true JP2002226927A (en) | 2002-08-14 |
| JP3656898B2 JP3656898B2 (en) | 2005-06-08 |
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ID=18889593
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2001024453A Expired - Fee Related JP3656898B2 (en) | 2001-01-31 | 2001-01-31 | Ag alloy reflective film for flat panel display |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2857459A1 (en) * | 2003-07-07 | 2005-01-14 | Kobe Steel Ltd | AG ALLOY REFLECTING FILM FOR REFLECTORS AND REFLECTOR PROVIDED THEREWITH |
| WO2005056850A1 (en) * | 2003-12-10 | 2005-06-23 | Tanaka Kikinzoku Kogyo K.K. | Silver alloy excelling in performance of reflectance maintenance |
| EP1560704A4 (en) * | 2003-04-18 | 2006-09-06 | Target Technology Co Llc | Metal alloys for the reflective or the semi-reflective layer of an optical storage medium |
| WO2006132412A1 (en) * | 2005-06-10 | 2006-12-14 | Tanaka Kikinzoku Kogyo K.K. | Silver alloy for electrode, wiring and electromagnetic shielding |
| WO2006132416A1 (en) * | 2005-06-10 | 2006-12-14 | Tanaka Kikinzoku Kogyo K.K. | Silver alloy excellent in reflectance/transmittance maintaining characteristics |
| JP2007004166A (en) * | 2005-06-23 | 2007-01-11 | Samsung Electronics Co Ltd | Display substrate, its manufacturing method and display apparatus with same |
| US7189460B2 (en) | 2003-06-27 | 2007-03-13 | Asahi Glass Company, Limited | High reflectance mirror |
| EP1795950A1 (en) | 2005-12-06 | 2007-06-13 | Samsung Electronics Co., Ltd. | Liquid crystal display and manufacturing method therefor |
| WO2008018298A1 (en) * | 2006-08-10 | 2008-02-14 | Kabushiki Kaisha Kobe Seiko Sho | Ag ALLOY REFLECTIVE FILM FOR REFLECTOR, REFLECTOR, AND Ag ALLOY SPUTTERING TARGET FOR FORMATION OF Ag ALLOY REFLECTIVE FILM FOR REFLECTOR |
| EP1746590A3 (en) * | 2005-07-22 | 2009-04-08 | Kabushiki Kaisha Kobe Seiko Sho (Kobe Steel, Ltd.) | Silver alloy reflective films for optical information recording media, silver alloy sputtering targets therefor, and optical |
| WO2010089840A1 (en) * | 2009-02-06 | 2010-08-12 | Dewaki Kenji | Product having gadolinium-containing metal layer |
| US8841541B2 (en) | 2009-09-04 | 2014-09-23 | Mitsubishi Electric Corporation | Solar battery and method of manufacturing the same |
| US9080247B2 (en) | 2009-07-31 | 2015-07-14 | Shinji Dewaki | Tin-containing alloy plating bath, electroplating method using same, and substrate with the electroplating deposited thereon |
| US9574281B2 (en) | 2009-02-06 | 2017-02-21 | M-Tech Japan Co., Ltd. | Silver-containing alloy plating bath and method for electrolytic plating using same |
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2001
- 2001-01-31 JP JP2001024453A patent/JP3656898B2/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1560704A4 (en) * | 2003-04-18 | 2006-09-06 | Target Technology Co Llc | Metal alloys for the reflective or the semi-reflective layer of an optical storage medium |
| US7645500B2 (en) | 2003-04-18 | 2010-01-12 | Target Technology Company, Llc | Metal alloys for the reflective or the semi-reflective layer of an optical storage medium |
| US7189460B2 (en) | 2003-06-27 | 2007-03-13 | Asahi Glass Company, Limited | High reflectance mirror |
| FR2857459A1 (en) * | 2003-07-07 | 2005-01-14 | Kobe Steel Ltd | AG ALLOY REFLECTING FILM FOR REFLECTORS AND REFLECTOR PROVIDED THEREWITH |
| WO2005056850A1 (en) * | 2003-12-10 | 2005-06-23 | Tanaka Kikinzoku Kogyo K.K. | Silver alloy excelling in performance of reflectance maintenance |
| US7575714B2 (en) | 2003-12-10 | 2009-08-18 | Tanaka Kikinzoku Kogyo K.K. | Silver alloy excellent in reflectance maintenance property and method for producing an optical recording medium |
| JPWO2006132412A1 (en) * | 2005-06-10 | 2009-01-08 | 田中貴金属工業株式会社 | Silver alloy for electrode, wiring and electromagnetic shielding |
| WO2006132412A1 (en) * | 2005-06-10 | 2006-12-14 | Tanaka Kikinzoku Kogyo K.K. | Silver alloy for electrode, wiring and electromagnetic shielding |
| WO2006132416A1 (en) * | 2005-06-10 | 2006-12-14 | Tanaka Kikinzoku Kogyo K.K. | Silver alloy excellent in reflectance/transmittance maintaining characteristics |
| JPWO2006132416A1 (en) * | 2005-06-10 | 2009-01-08 | 田中貴金属工業株式会社 | Silver alloy with excellent reflectivity and transmittance maintenance characteristics |
| JP2007004166A (en) * | 2005-06-23 | 2007-01-11 | Samsung Electronics Co Ltd | Display substrate, its manufacturing method and display apparatus with same |
| US8169428B2 (en) | 2005-06-23 | 2012-05-01 | Samsung Electronics Co., Ltd. | Display substrate, method of manufacturing the same and display device having the same |
| EP1746590A3 (en) * | 2005-07-22 | 2009-04-08 | Kabushiki Kaisha Kobe Seiko Sho (Kobe Steel, Ltd.) | Silver alloy reflective films for optical information recording media, silver alloy sputtering targets therefor, and optical |
| US7695792B2 (en) | 2005-07-22 | 2010-04-13 | Kobe Steel, Ltd. | Silver alloy reflective films for optical information recording media, silver alloy sputtering targets therefor, and optical information recording media |
| JP2007156482A (en) * | 2005-12-06 | 2007-06-21 | Samsung Electronics Co Ltd | Display panel, liquid crystal display device including the same, and manufacturing method of same display panel |
| EP1795950A1 (en) | 2005-12-06 | 2007-06-13 | Samsung Electronics Co., Ltd. | Liquid crystal display and manufacturing method therefor |
| WO2008018298A1 (en) * | 2006-08-10 | 2008-02-14 | Kabushiki Kaisha Kobe Seiko Sho | Ag ALLOY REFLECTIVE FILM FOR REFLECTOR, REFLECTOR, AND Ag ALLOY SPUTTERING TARGET FOR FORMATION OF Ag ALLOY REFLECTIVE FILM FOR REFLECTOR |
| WO2010089840A1 (en) * | 2009-02-06 | 2010-08-12 | Dewaki Kenji | Product having gadolinium-containing metal layer |
| JPWO2010089840A1 (en) * | 2009-02-06 | 2012-08-09 | 謙治 出分 | Products with gadolinium-containing metal layers |
| US9574281B2 (en) | 2009-02-06 | 2017-02-21 | M-Tech Japan Co., Ltd. | Silver-containing alloy plating bath and method for electrolytic plating using same |
| US9080247B2 (en) | 2009-07-31 | 2015-07-14 | Shinji Dewaki | Tin-containing alloy plating bath, electroplating method using same, and substrate with the electroplating deposited thereon |
| US8841541B2 (en) | 2009-09-04 | 2014-09-23 | Mitsubishi Electric Corporation | Solar battery and method of manufacturing the same |
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