JP4801279B2 - Sputtering target material - Google Patents
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Description
【０００１】
【発明の属する技術分野】
本発明は、高い反射率を維持しながら耐食性、特に耐ハロゲン性、耐酸化性、耐硫化性を向上させた薄膜形成用スパッタリングターゲット材、およびこのスパッタリングターゲット材を用いて形成された薄膜に関する。
【０００２】
【従来の技術及びその課題】
ＣＤ（Compact Disc）、ＤＶＤ（Digital Versatile Disc）等の光学記録媒体に使用されている反射膜や、反射型ＳＴＮ（Super Twist Nemａtic）液晶表示装置、有機ＥＬ（Electro luminescence）表示装置等の表示装置に使用されている光反射性導電膜には、一般に、ＡｌやＡｌ合金が使用されている。
【０００３】
上記の光学記録媒体や液晶表示装置、有機ＥＬ表示装置などの用途に使用される光反射性薄膜は、一般に、所望とする性質をもつスパッタリングターゲット材を作製し、そのスパッタリングターゲット材を使用してＲＦ（高周波）スパッタリング法やＤＣ（直流）スパッタリング法により成膜することにより製造されている。
【０００４】
上記の方法で製造されるＡｌやＡｌ合金からなる薄膜は、ある程度の反射率を有しかつ電気抵抗が低く、しかも、表層に不動態皮膜を形成するため、空気中においても安定した耐食性を有するが、ＡｌやＡｌ合金からなる薄膜の反射率は、例えば波長が７００nmの光の場合８０％程度であり、高反射率が要求される用途に対しては充分に満足できるものではない。
【０００５】
そのため、高い反射率を有する薄膜が要求される、例えばＣＤ−ＲやＤＶＤに代表される光ディスク媒体には、スパッタリングターゲット材としてＡｌまたはＡｌ合金に代わりに、ＡｕやＡｇを使用して薄膜を形成することが提案されており、また、反射型ＳＴＮ液晶表示装置についても、薄膜材料として反射率の高いＡｇを使用することが提案されている。
【０００６】
しかしながら、Ａｕは高価であり、また、Ａｇは、Ａｌと比較して、耐食性、特に耐ハロゲン（Ｃｌ等）性、耐酸化性、耐硫化性に問題がある。例えば、Ａｇは、Ｃｌのようなハロゲン元素と反応すると、変色し反射率が低下し、また、硫黄や酸素と反応すると、Ａｇの硫化物や酸化物を生成して黒色化し反射率が低下する。
【０００７】
そのため、例えば、特開平７−３３６３号公報には、Ａｇに少量のＭｇを添加して合金化することにより、また、特開２０００−１０９９４３公報には、Ａｇに少量のＰｄを添加して合金化することにより、Ａｇの耐食性（耐ハロゲン性、耐酸化性、耐硫化性）を向上させることが提案されている。
【０００８】
しかしながら、これらのＡｇ合金化によっても、Ａｇの充分な耐食性が得られず、あるいは耐食性、特に耐ハロゲン（Ｃｌ等）性はある程度向上するものの、耐硫化性についてはＡｇとあまり変わらず充分な耐食性が得られない等の問題がある。
【０００９】
本発明の目的は、高い反射率を維持しながら、耐食性、特に、耐ハロゲン性、耐酸化性、耐硫化性が改善されたＡｇ合金からなる薄膜形成用のスパッタリングターゲット材を提供することである。
【００１０】
【課題を解決するための手段】
本発明者らは、上記の目的を達成すべく鋭意検討を重ねた結果、今回、Ａｇに、特定少量のＧｅ、Ｇａ、Ｓｂの少なくとも１種と、特定少量のＡｕ、Ｐｄ、Ｐｄの少なくとも１種を添加して合金化すると、これら両金属成分が相乗的に作用して、Ａｇがもつ高い反射率を維持しつつ、耐食性、特に、耐ハロゲン性、耐酸化性、耐硫化性が格段に向上したＡｇ合金が得られること、さらにＣｕを少量添加して合金化すると、耐食性、特に耐ハロゲン性、耐硫化性がより一層向上することを見出し、本発明を完成するに至った。
【００１１】
かくして、本発明は、Ａｇに、Ｇｅ、ＧａおよびＳｂから選ばれる少なくとも１種の金属成分（Ａ）０.１〜４.９mass％とＡｕ、ＰｄおよびＰｔから選ばれる少なくとも１種の金属成分（Ｂ）０.１〜４.９mass％を添加してなり、金属成分（Ａ）と金属成分（Ｂ）の合計添加量が０.２〜５mass％であるＡｇ合金より構成されていることを特徴とする高反射率を有する高耐食性薄膜形成用スパッタリングターゲット材を提供するものである。
【００１２】
本発明は、また、Ａｇに、Ｇｅ、ＧａおよびＳｂから選ばれる少なくとも１種の金属成分（Ａ）０.０５〜４.８５mass％とＡｕ、Ｐｄ及びＰｔから選ばれる少なくとも１種の金属成分（Ｂ）０.１〜４.９mass％とＣｕ ０.０５〜４.８５mass％を添加してなり、金属成分（Ａ）と金属成分（Ｂ）とＣｕの合計添加量が０.２〜５mass％であるＡｇ合金より構成されていることを特徴とする高反射率を有する高耐食性薄膜形成用スパッタリングターゲット材を提供するものである。
【００１３】
以下、本発明についてさらに詳細に説明する。
【００１４】
【発明の実施の形態】
本発明のスパッタリングターゲット材は、Ａｇをベースとし、これにＧｅ、ＧａおよびＳｂから選ばれる金属成分（Ａ）と、Ａｕ、ＰｄおよびＰｔから選ばれる金属成分（Ｂ）、さらに場合によりＣｕを添加し合金化してなるＡｇ合金からなるものである。
【００１５】
上記金属成分（Ａ）としては、Ｇｅ、ＧａおよびＳｂをそれぞれ単独で使用することができ、又は２種もしくは３種を併用してもよい。これら金属成分（Ａ）の添加量は、Ｃｕを添加しない場合には、合計で０.１〜４.９mass％、好ましくは０.３〜３mass％の範囲内、そしてＣｕを添加する場合には、合計で０.１〜４.８５mass％、好ましくは０.３〜３mass％の範囲内とすることができるが、特に、Ｇｅは０.１〜２mass％、Ｇａは０.１〜１.５mass％、そしてＳｂは０.１〜１.５mass％の範囲内で使用するのが好適である。
【００１６】
また、上記金属成分（Ｂ）は、Ａｕ、Ｐｄ、Ｐｔのそれぞれを単独で使用することができ、又は２種もしくは３種を併用してもよい。これら金属成分（Ｂ）の添加量は、Ｃｕを添加するしないにかかわらず、合計で０.１〜４.９mass％、好ましくは０.５〜３mass％の範囲内とすることができる。
【００１７】
Ａｇ合金中の金属成分（Ａ）と金属成分（Ｂ）の相対的比率は、特に制限されるものではなく、各金属成分の上記添加量範囲内で任意に変えることができるが、一般には、金属成分（Ａ）／金属成分（Ｂ）のmass比で１／２〜２／１、特に４／５〜５／４の範囲内が適当である。
【００１８】
さらに、Ａｇ合金中の金属成分（Ａ）と金属成分（Ｂ）の合計添加量は、Ｃｕを添加しない場合には、０.２〜５mass％、好ましくは１〜３mass％の範囲内とすることができる。
【００１９】
他方、必要に応じて添加されるＣｕは、金属成分（Ａ）と金属成分（Ｂ）の合計に対して０.０５〜４.８５mass％、好ましくは０.５〜３mass％の範囲内で使用することができる。その際のＡｇ合金中の上記金属成分（Ａ）と金属成分（Ｂ）とＣｕの合計添加量は０.２〜５mass％、好ましくは０.５〜３mass％の範囲内とすることができ、また、Ａｇ合金中の金属成分（Ａ）と金属成分（Ｂ）とＣｕの相対的比率は、特に制限されるものではなく、各金属成分の上記添加量範囲内で任意に変えることができるが、一般には、金属成分（Ａ）及び金属成分（Ｂ）は、金属成分（Ａ）／金属成分（Ｂ）のmass比で、１／２〜２／１、特に４／５〜５／４の範囲内が適当であり、Ｃｕは、Ｃｕ／金属成分（Ａ）＋（Ｂ）のmass比で、１／５〜３／２、特に１／２〜１／１の範囲内が適当である。
【００２０】
Ａｇ合金は、例えば、Ａｇに、上記の金属成分（Ａ）及び金属成分（Ｂ）ならびに場合によりさらにＣｕを上記の量で添加し、ガス炉、高周波溶解炉などの適当な金属溶解炉内で約１０００〜約１０５０℃の温度で溶融することにより製造することができる。溶解時の雰囲気は空気中で十分であるが、必要に応じ、不活性ガス雰囲気又は真空を使用してもよい。
【００２１】
原料として使用されるＡｇ、金属成分（Ａ）（Ｇｅ、Ｇａ、Ｓｂ）及び金属成分（Ｂ）（Ａｕ、Ｐｄ、Ｐｔ）ならびにＣｕは、粒状、板状、塊状等の形態で市販されているものを使用することができるが、通常、純度が９９.９％以上、特に９９.９５％以上のものが好適である。
【００２２】
かくして、Ａｇ中に、金属成分（Ａ）及び金属成分（Ｂ）をそれぞれ前記の割合で含有するＡｇ合金が得られる。このＡｇ合金から構成されるスパッタリングターゲット材は、Ａｇが本来もつ高い反射率を維持しており、しかも、耐ハロゲン（特にＣｌ）性、耐酸化性、耐硫化性などの耐食性が、従来のＡｇ−Ｍｇ合金やＡｇ−Ｐｄ合金に比べて、はるかに向上している。
【００２３】
したがって、本発明の上記Ａｇ合金から構成されるスパッタリングターゲット材は、高反射率が要求されるＣＤ−ＲやＤＶＤに代表される光ディスク媒体の反射膜用として、また、反射型ＳＴＮ液晶表示装置や有機ＥＬ表示装置などの光反射性薄膜用として有利に使用することができる。
【００２４】
本発明のＡｇ合金から構成されるスパッタリングターゲット材からの反射膜の形成は、それ自体既知のスパッタリング法、例えば、高周波（ＲＦ）スパッタリング法、直流（ＤＣ）スパッタリング法、マグネトロンスパッタリング法等により行なうことができる。
【００２５】
以下、本発明を実施例によりさらに具体的に説明する。
【００２６】
【実施例】
実施例１〜５及び比較例１〜７
Ａｇに、下記表１に示す量の金属成分（Ａ）（Ｇｅ、Ｇａ、Ｓｂ）、金属成分（Ｂ）（Ａｕ、Ｐｄ、Ｐｔ）及び場合によりＣｕを加え、ガス炉内で約１０５０℃の温度に加熱して溶融した後、鋳型で鋳造し、加工してスパッタリングターゲット材を作製した。
【００２７】
【表１】
このスパッタリングターゲット材を用い、ＲＦスパッタリング法により、ガラス基板上に厚さが約２００ｎｍの薄膜を形成させた。
【００２９】
得られた薄膜が付着したガラス基板を大気中に暴露して耐酸化性を試験した。また、薄膜が付着した別のガラス基板をそれぞれ１０％食塩（ＮａＣｌ）水溶液中及び０.０１％硫化ナトリウム（Ｎａ2Ｓ）水溶液中に浸漬して耐ハロゲン（塩素）性及び耐硫化性を試験した。各試験において、所定時間後の薄膜の状態を目視で評価した。結果を下記表２に示す。
【００３０】
【表２】
また、得られた作製直後の薄膜の５００〜７００ｎｍの波長域における光の反射率（垂直入射光）を測定したところ、実施例１〜５の薄膜の反射率はいずれも９０％以上であった。一方、比較例２の薄膜の反射率は８０〜９０％であり、反射率が低かった。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a sputtering target material for forming a thin film having improved corrosion resistance, particularly halogen resistance, oxidation resistance, and sulfidation resistance while maintaining a high reflectance, and a thin film formed using this sputtering target material.
[0002]
[Prior art and problems]
Reflective films used in optical recording media such as CD (Compact Disc) and DVD (Digital Versatile Disc), display devices such as reflective STN (Super Twist Nematic) liquid crystal display devices, organic EL (Electro luminescence) display devices In general, Al or an Al alloy is used for the light-reflective conductive film used in the above.
[0003]
The light-reflective thin film used for applications such as the above-mentioned optical recording media, liquid crystal display devices, and organic EL display devices is generally produced by producing a sputtering target material having desired properties and using the sputtering target material. It is manufactured by forming a film by an RF (high frequency) sputtering method or a DC (direct current) sputtering method.
[0004]
The thin film made of Al or Al alloy produced by the above method has a certain degree of reflectivity, low electrical resistance, and forms a passive film on the surface layer, so that it has stable corrosion resistance even in the air. However, the reflectance of a thin film made of Al or an Al alloy is, for example, about 80% in the case of light having a wavelength of 700 nm, and is not sufficiently satisfactory for applications requiring high reflectance.
[0005]
Therefore, a thin film having a high reflectance is required. For example, an optical disk medium represented by CD-R or DVD is formed by using Au or Ag as a sputtering target material instead of Al or Al alloy. It is also proposed to use Ag having a high reflectivity as a thin film material for the reflective STN liquid crystal display device.
[0006]
However, Au is expensive, and Ag has problems in corrosion resistance, particularly halogen resistance (such as Cl), oxidation resistance, and sulfidation resistance, as compared with Al. For example, when Ag reacts with a halogen element such as Cl, the color changes and the reflectance decreases, and when it reacts with sulfur or oxygen, Ag sulfide or oxide is generated and blackened to reduce the reflectance. .
[0007]
Therefore, for example, in JP-A-7-3363, a small amount of Mg is added to alloy with Ag, and in JP-A 2000-109943, an alloy with a small amount of Pd added to Ag. It has been proposed to improve the corrosion resistance (halogen resistance, oxidation resistance, sulfidation resistance) of Ag.
[0008]
However, even though these Ag alloys are used, sufficient corrosion resistance of Ag cannot be obtained, or although corrosion resistance, particularly halogen resistance (Cl, etc.) is improved to some extent, sulfidation resistance is not much different from Ag and sufficient corrosion resistance is obtained. There is a problem that cannot be obtained.
[0009]
An object of the present invention is to provide a sputtering target material for forming a thin film made of an Ag alloy having improved corrosion resistance, in particular, halogen resistance, oxidation resistance, and sulfidation resistance while maintaining high reflectance. .
[0010]
[Means for Solving the Problems]
As a result of intensive studies to achieve the above-mentioned object, the present inventors have determined that at least one of a specific small amount of Ge, Ga, Sb and a specific small amount of Au, Pd, Pd is included in Ag. When seeded and alloyed, these two metal components act synergistically to maintain the high reflectivity of Ag, while having excellent corrosion resistance, particularly halogen resistance, oxidation resistance, and sulfidation resistance. It has been found that an improved Ag alloy can be obtained, and further, when a small amount of Cu is added to form an alloy, corrosion resistance, particularly halogen resistance and sulfidation resistance are further improved, and the present invention has been completed.
[0011]
Thus, in the present invention, at least one metal component (A) selected from Ge, Ga, and Sb (0.1) to 4.9 mass% and at least one metal component (selected from Au, Pd, and Pt) are added to Ag. B) 0.1 to 4.9 mass% is added, and the total added amount of the metal component (A) and the metal component (B) is 0.2 to 5 mass%, and is composed of an Ag alloy. A sputtering target material for forming a highly corrosion-resistant thin film having a high reflectance is provided.
[0012]
In the present invention, at least one metal component selected from Ge, Ga and Sb (A) of 0.05 to 4.85 mass% and at least one metal component selected from Au, Pd and Pt ( B) 0.1 to 4.9 mass% and Cu 0.05 to 4.85 mass% are added, and the total amount of addition of metal component (A), metal component (B) and Cu is 0.2 to 5 mass%. The present invention provides a sputtering target material for forming a highly corrosion-resistant thin film having a high reflectivity, characterized in that it is made of an Ag alloy that is:
[0013]
Hereinafter, the present invention will be described in more detail.
[0014]
DETAILED DESCRIPTION OF THE INVENTION
The sputtering target material of the present invention is based on Ag, to which is added a metal component (A) selected from Ge, Ga and Sb, a metal component (B) selected from Au, Pd and Pt, and optionally Cu. It is made of an Ag alloy formed by alloying.
[0015]
As said metal component (A), Ge, Ga, and Sb can each be used individually, or 2 or 3 types may be used together. The addition amount of these metal components (A) is 0.1 to 4.9 mass% in total when Cu is not added, preferably 0.3 to 3 mass%, and when Cu is added. In total, it can be in the range of 0.1 to 4.85 mass%, preferably 0.3 to 3 mass%. In particular, Ge is 0.1 to 2 mass%, and Ga is 0.1 to 1.5 mass. % And Sb are preferably used within the range of 0.1 to 1.5 mass%.
[0016]
In addition, as the metal component (B), each of Au, Pd, and Pt can be used alone, or two or three of them can be used in combination. The addition amount of these metal components (B) can be within a range of 0.1 to 4.9 mass%, preferably 0.5 to 3 mass%, regardless of whether Cu is added.
[0017]
The relative ratio between the metal component (A) and the metal component (B) in the Ag alloy is not particularly limited, and can be arbitrarily changed within the above-described addition amount range of each metal component. The mass ratio of metal component (A) / metal component (B) is suitably in the range of 1/2 to 2/1, particularly 4/5 to 5/4.
[0018]
Furthermore, the total addition amount of the metal component (A) and the metal component (B) in the Ag alloy should be within a range of 0.2 to 5 mass%, preferably 1 to 3 mass%, when Cu is not added. Can do.
[0019]
On the other hand, Cu added as necessary is used in the range of 0.05 to 4.85 mass%, preferably 0.5 to 3 mass% with respect to the total of the metal component (A) and the metal component (B). can do. The total addition amount of the metal component (A), metal component (B) and Cu in the Ag alloy at that time can be in the range of 0.2 to 5 mass%, preferably 0.5 to 3 mass%. Moreover, the relative ratio of the metal component (A), the metal component (B), and Cu in the Ag alloy is not particularly limited and can be arbitrarily changed within the above-described addition amount range of each metal component. In general, the metal component (A) and the metal component (B) have a mass ratio of metal component (A) / metal component (B) of 1/2 to 2/1, particularly 4/5 to 5/4. The range is appropriate, and Cu is a mass ratio of Cu / metal component (A) + (B), and is preferably in the range of 1/5 to 3/2, particularly 1/2 to 1/1.
[0020]
In the case of Ag alloy, for example, the above-mentioned metal component (A) and metal component (B) and optionally Cu are further added to Ag in the above-mentioned amount, and in an appropriate metal melting furnace such as a gas furnace or a high-frequency melting furnace. It can be produced by melting at a temperature of about 1000 to about 1050 ° C. The atmosphere at the time of dissolution is sufficient in air, but an inert gas atmosphere or a vacuum may be used if necessary.
[0021]
Ag, metal components (A) (Ge, Ga, Sb) and metal components (B) (Au, Pd, Pt) and Cu used as raw materials are commercially available in the form of particles, plates, lumps, etc. Although those having a purity of 99.9% or more, particularly 99.95% or more are suitable.
[0022]
Thus, an Ag alloy containing the metal component (A) and the metal component (B) in the aforementioned proportions in Ag is obtained. The sputtering target material composed of this Ag alloy maintains the high reflectivity inherent in Ag, and further has corrosion resistance such as halogen resistance (particularly Cl) resistance, oxidation resistance, and sulfidation resistance. -Compared to Mg alloy and Ag-Pd alloy, it is much improved.
[0023]
Therefore, the sputtering target material composed of the above-described Ag alloy of the present invention is used for a reflective film of an optical disk medium represented by CD-R or DVD that requires high reflectivity, a reflective STN liquid crystal display device, It can be advantageously used for a light reflective thin film such as an organic EL display device.
[0024]
The reflective film is formed from the sputtering target material composed of the Ag alloy of the present invention by a sputtering method known per se, for example, a radio frequency (RF) sputtering method, a direct current (DC) sputtering method, a magnetron sputtering method, or the like. Can do.
[0025]
Hereinafter, the present invention will be described more specifically with reference to examples.
[0026]
【Example】
Examples 1-5 and Comparative Examples 1-7
Ag is added with metal components (A) (Ge, Ga, Sb), metal components (B) (Au, Pd, Pt) and optionally Cu in the amounts shown in Table 1 below. After being heated and melted at a temperature, it was cast in a mold and processed to produce a sputtering target material.
[0027]
[Table 1]
Using this sputtering target material, a thin film having a thickness of about 200 nm was formed on a glass substrate by RF sputtering.
[0029]
The glass substrate to which the obtained thin film was attached was exposed to the atmosphere and tested for oxidation resistance. In addition, another glass substrate to which the thin film was attached was immersed in a 10% sodium chloride (NaCl) aqueous solution and a 0.01% sodium sulfide (Na 2 S) aqueous solution to test the halogen (chlorine) resistance and sulfidation resistance. did. In each test, the state of the thin film after a predetermined time was visually evaluated. The results are shown in Table 2 below.
[0030]
[Table 2]
Moreover, when the reflectance (perpendicular incident light) of the light in the 500-700 nm wavelength range of the obtained thin film immediately after preparation was measured, all the reflectance of the thin film of Examples 1-5 was 90% or more. . On the other hand, the reflectance of the thin film of Comparative Example 2 was 80 to 90%, and the reflectance was low.
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| WO2003100112A1 (en) * | 2002-05-28 | 2003-12-04 | Ishifuku Metal Industry Co., Ltd. | Sputtering target material |
| US7514037B2 (en) | 2002-08-08 | 2009-04-07 | Kobe Steel, Ltd. | AG base alloy thin film and sputtering target for forming AG base alloy thin film |
| CN100446101C (en) * | 2003-03-13 | 2008-12-24 | 三菱麻铁里亚尔株式会社 | Silver alloy sputterig target for forming reflective layer of optical recording medium |
| CN100443609C (en) * | 2003-09-26 | 2008-12-17 | 古屋金属株式会社 | Silver alloy, sputtering target material thereof, and thin film thereof |
| KR20060089214A (en) * | 2003-09-26 | 2006-08-08 | 가부시키가이샤 후루야긴조쿠 | Silver alloy, sputtering target material thereof, and thin film thereof |
| EP1736558A4 (en) | 2003-12-10 | 2009-06-17 | Tanaka Precious Metal Ind | Silver alloy for reflective film |
| WO2005056851A1 (en) * | 2003-12-10 | 2005-06-23 | Tanaka Kikinzoku Kogyo K.K. | Silver alloy excelling in performance of reflectance maintenance |
| JP4540687B2 (en) * | 2007-04-13 | 2010-09-08 | 株式会社ソニー・ディスクアンドデジタルソリューションズ | Read-only optical information recording medium |
| JP5628662B2 (en) * | 2010-12-29 | 2014-11-19 | 石福金属興業株式会社 | Reflective film made of Ag-based alloy |
| JP2013077547A (en) * | 2011-09-15 | 2013-04-25 | Mitsubishi Materials Corp | Conductive film and manufacturing method thereof, and silver alloy sputtering target for conductive film formation and manufacturing method thereof |
| JP5159963B1 (en) * | 2012-01-13 | 2013-03-13 | 三菱マテリアル株式会社 | Silver alloy sputtering target for forming conductive film and method for producing the same |
| JP6326242B2 (en) * | 2014-02-17 | 2018-05-16 | 京セラ株式会社 | Silver alloy and ornaments for ornaments |
| JP6600035B2 (en) * | 2018-04-16 | 2019-10-30 | 京セラ株式会社 | Ring, necklace chain and pendant head |
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| JP4007702B2 (en) * | 1998-10-05 | 2007-11-14 | 株式会社フルヤ金属 | Sputtering target material for forming a thin film, a thin film formed using the same, and an optical recording medium |
| JP3365762B2 (en) * | 2000-04-28 | 2003-01-14 | 株式会社神戸製鋼所 | Reflective layer or translucent reflective layer for optical information recording medium, optical information recording medium, and sputtering target for optical information recording medium |
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