JP2001098362A - Sputtering target material for forming optical recording medium protective layer exhibiting excellent cracking resistance under high output sputtering condition - Google Patents
Sputtering target material for forming optical recording medium protective layer exhibiting excellent cracking resistance under high output sputtering conditionInfo
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- JP2001098362A JP2001098362A JP27352099A JP27352099A JP2001098362A JP 2001098362 A JP2001098362 A JP 2001098362A JP 27352099 A JP27352099 A JP 27352099A JP 27352099 A JP27352099 A JP 27352099A JP 2001098362 A JP2001098362 A JP 2001098362A
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- Japan
- Prior art keywords
- target material
- protective layer
- recording medium
- optical recording
- sputtering
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- Compositions Of Oxide Ceramics (AREA)
- Physical Vapour Deposition (AREA)
- Optical Record Carriers And Manufacture Thereof (AREA)
- Manufacturing Optical Record Carriers (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】この発明は、半導体レーザー
などの光ビームを用いて、情報の記録や再生、さらに消
去を行う光ディスクなどの光記録媒体の構成層である保
護層をスパッタリング法にて形成するのに用いられるス
パッタリングターゲット材（以下、ターゲット材と云
う）に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for forming a protective layer, which is a constituent layer of an optical recording medium such as an optical disk, on which information is recorded, reproduced, and erased by using a light beam such as a semiconductor laser by a sputtering method. The present invention relates to a sputtering target material (hereinafter, referred to as a target material) used for the sputtering.
【０００２】[0002]
【従来の技術】一般に、上記の光ディスクなどの光記録
媒体が、基本的に例えばポリカーボネイトの基板と、こ
れの表面にいずれもスパッタリング法により形成された
下部保護層、記録層、上部保護層、および反射層の構成
層からなることが知られている。また、上記の光記録媒
体が、例えば図１に概略縦断面図で示される高周波マグ
ネトロンスパッタリング装置を用い、まず、内部を循環
する冷却水によって冷却されたバッキングプレートに所
定の組成をもったターゲット材を取り付け、装置内を真
空排気装置にて排気した後、Ａｒガスを導入して所定の
スッパッタガス圧に保持し、この状態でマッチングボッ
クスを介して設置された高周波電源にてターゲット材に
高周波電力を印加し、これによってターゲット材と、こ
れに対向し、かつ所定の間隔を設けて配置した、例えば
ポリカーボネイトの基板との間にプラズマを発生させ、
このプラズマ中のＡｒイオンをターゲット材の表面に衝
突させてスパッタし、スパッタ粒子を基板表面にそれぞ
れ構成層として蒸着することにより製造されている。さ
らに、上記の光記録媒体の構成層である保護層（下部保
護層および上部保護層）の形成に、例えば特開平６−６
５７２５号公報に記載される通り、重量％で（以下、％
は重量％を示す）、酸化けい素（以下、ＳｉＯ2で示
す）：３〜２５％、硫化亜鉛（以下、ＺｎＳで示す）：
残り、の配合組成を有する混合粉末のホットプレス焼結
体で構成されたターゲット材が用いられていることも知
られている。2. Description of the Related Art Generally, an optical recording medium such as the above-mentioned optical disk is basically composed of, for example, a polycarbonate substrate, and a lower protective layer, a recording layer, an upper protective layer, and a lower protective layer all formed on the surface of the substrate by a sputtering method. It is known that the reflective layer comprises a constituent layer. In addition, the above-mentioned optical recording medium uses, for example, a high-frequency magnetron sputtering apparatus shown in a schematic longitudinal sectional view in FIG. 1, and firstly a target material having a predetermined composition is formed on a backing plate cooled by cooling water circulating inside. After the inside of the apparatus is evacuated by a vacuum evacuation apparatus, Ar gas is introduced and maintained at a predetermined sputter gas pressure, and in this state, high-frequency power is applied to the target material by a high-frequency power supply installed through a matching box. Applied, thereby generating a plasma between the target material and the substrate, for example, a polycarbonate substrate opposed to the target material and arranged at a predetermined interval,
It is manufactured by causing Ar ions in the plasma to collide with the surface of the target material to perform sputtering, and depositing sputtered particles as constituent layers on the substrate surface. Further, the formation of the protective layers (the lower protective layer and the upper protective layer), which are the constituent layers of the above-mentioned optical recording medium, is described in, for example, JP-A-6-6 / 1994.
As described in Japanese Patent No. 5725, in weight% (hereinafter,%
Represents weight%), silicon oxide (hereinafter, represented by SiO 2 ): 3 to 25%, zinc sulfide (hereinafter, represented by ZnS):
It is also known that a target material composed of a hot press sintered body of a mixed powder having the remaining composition is used.
【０００３】[0003]
【発明が解決しようとする課題】一方、近年の上記の光
ディスクなどの光記録媒体の生産性の向上に対する要求
は強く、これに伴い、構成層の成膜速度も高速化の傾向
にあり、しかし高速成膜を行うためにはターゲット材に
印加する電力を高くして高出力スパッタ条件とする必要
があるが、特に上記の従来ターゲット材を用いて保護層
を形成するに際して、これの高速成膜を行う目的でスパ
ッタ条件を高出力スパッタ条件とすると、ターゲット材
に割れが発生し易くなり、比較的短時間で使用寿命に至
るのが現状である。On the other hand, there is a strong demand for improvement in productivity of optical recording media such as the above-mentioned optical discs in recent years, and accordingly, the film forming speed of the constituent layers tends to be increased. In order to perform high-speed film formation, it is necessary to increase the power applied to the target material to achieve high-output sputtering conditions. In particular, when forming the protective layer using the above-described conventional target material, the high-speed film formation is performed. If the sputtering conditions are set to the high-power sputtering conditions for the purpose of performing the above, cracks are likely to occur in the target material, and the service life is currently reached in a relatively short time.
【０００４】[0004]
【課題を解決するための手段】そこで、本発明者らは,
上述の観点から、上記の光記録媒体保護層形成用の従来
ターゲット材に着目し、これの耐割損性向上を図るべく
研究を行った結果、上記の従来ターゲット材におけるＳ
ｉＯ2粉末およびＺｎＳ粉末に加えて所定割合の酸化チ
タン（以下、ＴｉＯ2で示す）粉末を配合し、混合して
なる混合粉末のホットプレス焼結体を光記録媒体保護層
形成用ターゲット材として用いると、ホットプレス時に
前記ＴｉＯ2粉末が前記ＳｉＯ2粉末およびＺｎＳ粉末の
間にあって、これら両粉末のいずれにも強固に密着し、
この結果として粉末相互間の密着性が著しく向上するよ
うになり、したがって高速成膜を行うために高出力スパ
ッタ条件としても前記ターゲット材における粉末相互間
の密着性向上効果による耐割損性向上効果によってこれ
の割れが著しく抑制されるようになり、長期に亘っての
実用を可能とするばかりでなく、前記ＴｉＯ2粉末は光
記録媒体保護層の特性評価基準となる光屈折率および光
透過率にほとんど影響を及ぼすことがない、すなわち前
記ＴｉＯ2粉末を配合しても上記従来ターゲット材を用
いて形成した光記録媒体保護層の示す光屈折率および光
透過率と同等の光屈折率と光透過率を示すという研究結
果を得たのである。Means for Solving the Problems Therefore, the present inventors have proposed:
From the above viewpoint, the present inventors focused on the conventional target material for forming the protective layer of the optical recording medium described above, and conducted research to improve the breakage resistance.
A hot press sintered body of a mixed powder obtained by mixing and mixing a predetermined ratio of titanium oxide (hereinafter, referred to as TiO 2 ) powder in addition to the TiO 2 powder and the ZnS powder as a target material for forming a protective layer of an optical recording medium When used, the TiO 2 powder is located between the SiO 2 powder and the ZnS powder during hot pressing, and firmly adheres to both of these powders.
As a result, the adhesion between the powders is remarkably improved. Therefore, even if the target material is subjected to high-power sputtering conditions for performing high-speed film formation, the effect of improving the splitting resistance between the powders in the target material is improved. This significantly suppresses the cracking, and not only enables practical use for a long period of time, but also makes the TiO 2 powder have a light refractive index and a light transmittance which are used as a criterion for evaluating the characteristics of the optical recording medium protective layer. In other words, even if the TiO 2 powder is blended, the light refractive index and light transmittance are equivalent to the light refractive index and light transmittance of the optical recording medium protective layer formed using the conventional target material. The research results show that it shows transmittance.
【０００５】この発明は、上記の研究結果に基づいてな
されたものであって、ＳｉＯ2：３〜２５％、ＴｉＯ2：
５〜３５％、ＺｎＳ：残り、の配合組成を有する混合粉
末のホットプレス焼結体で構成してなる、高出力スパッ
タ条件ですぐれた耐割損性を発揮する光記録媒体保護層
形成用ターゲット材に特徴を有するものである。The present invention has been made based on the results of the above-mentioned research, and is based on SiO 2 : 3 to 25% and TiO 2 :
5 to 35%, ZnS: The target for forming an optical recording medium protective layer, which is made of a hot-press sintered body of a mixed powder having the remaining composition and exhibits excellent cracking resistance under high output sputtering conditions. The material has characteristics.
【０００６】この発明の光記録媒体保護層形成用ターゲ
ット材を構成するホットプレス焼結体の配合組成を上記
の通りに限定した理由を説明する。 （ａ）ＳｉＯ2 ＺｎＳは、光記録媒体保護層に要求される高い光屈折率
と光透過率、さらに耐熱性を具備することから、光記録
媒体保護層の主要成分として用いられている。反面Ｚｎ
Ｓ単独で例えば光ディスクの保護層を形成した場合、内
部応力の高い保護層となってしまい、この状態で前記光
ディスクに記録のためのレーザー照射を行うと、前記レ
ーザー照射に伴う急熱・急冷によって前記保護層に割れ
が発生し易いものとなる。そこで、光記録媒体保護層で
はＺｎＳにＳｉＯ2を配合して、保護層中の残留内部応
力を低減するようにしたものである。したがって、ホッ
トプレス焼結体におけるＳｉＯ2の配合割合が３％未満
では、前記保護層における内部応力の発生を抑制する作
用が不充分であり、一方その配合割合が２５％を超える
と、ＺｎＳによってもたらされる上記の特性に低下傾向
が現れるようになることから、その配合割合を３〜２５
％、望ましくは１０〜１５％と定めた。The reason why the composition of the hot press sintered body constituting the target material for forming the protective layer of the optical recording medium of the present invention is limited as described above will be described. (A) SiO 2 ZnS is used as a main component of an optical recording medium protective layer because it has a high optical refractive index and light transmittance required for the optical recording medium protective layer and further has heat resistance. On the other hand, Zn
For example, when a protective layer of an optical disk is formed by S alone, it becomes a protective layer having a high internal stress, and when laser irradiation for recording is performed on the optical disk in this state, rapid heating and quenching accompanying the laser irradiation cause Cracking is likely to occur in the protective layer. Therefore, in the optical recording medium protection layer, ZnS is mixed with SiO 2 to reduce the residual internal stress in the protection layer. Therefore, if the content of SiO 2 in the hot-pressed sintered body is less than 3%, the effect of suppressing the generation of internal stress in the protective layer is insufficient. Since the above-mentioned properties to be provided tend to decrease, the mixing ratio is 3 to 25.
%, Preferably 10 to 15%.
【０００７】（ｂ）ＴｉＯ2 上記の通り、所定割合に配合されたＳｉＯ2粉末とＺｎ
Ｓ粉末の混合粉末からのホットプレス焼結体は、前記Ｓ
ｉＯ2粉末とＺｎＳ粉末の相互間の密着性が不充分であ
るために、これに高出力スパッタが負荷されると、割れ
が発生し易くなることから、高速成膜に適用することが
できないものである。これに対して、前記ＳｉＯ2粉末
とＺｎＳ粉末に加えて所定割合のＴｉＯ2粉末を配合し
てなる混合粉末のホットプレス焼結体においては、前記
ＴｉＯ2粉末が前記ＳｉＯ2粉末およびＺｎＳ粉末の間に
あって、これら両粉末のいずれにも強固に密着すること
から、全体として粉末相互間の密着性の高いものとな
り、この結果ターゲット材としての適用に際して、高速
成膜を行うために前記ターゲット材に高出力スパッタを
負荷しても、割れの発生が著しく抑制されるようにな
る。したがってこの粉末相互間の密着性向上効果による
耐割損性向上効果を十分に発揮させるためには、その配
合割合が５％未満では不充分で、５％以上の配合が必要
であり、一方その配合割合が３５％を越えると、例えば
光ディスクの保護層とした場合に、レーザー光の吸収が
大きくなるなどの光学特性の劣化が避けられなくなるこ
とから、その配合割合を５〜３５％、望ましくは２０〜
３０％と定めた。(B) TiO 2 As described above, SiO 2 powder and Zn mixed in a predetermined ratio
The hot-pressed sintered body from the mixed powder of S powder
Inadequate adhesion between the iO 2 powder and ZnS powder, and when high-power sputtering is applied to this, cracks are likely to occur. It is. On the other hand, in a hot-press sintered body of a mixed powder obtained by mixing a predetermined ratio of TiO 2 powder in addition to the SiO 2 powder and the ZnS powder, the TiO 2 powder is formed of the SiO 2 powder and the ZnS powder. In between, the powder adheres firmly to both of these powders, resulting in high adhesion between the powders as a whole. As a result, when applied as a target material, the powder is applied to the target material in order to perform high-speed film formation. Even if high-power sputtering is applied, the occurrence of cracks is significantly suppressed. Therefore, in order to sufficiently exhibit the effect of improving the breakage resistance due to the effect of improving the adhesion between the powders, if the compounding ratio is less than 5%, it is insufficient, and the compounding ratio of 5% or more is necessary. If the compounding ratio exceeds 35%, for example, when it is used as a protective layer of an optical disc, deterioration of optical characteristics such as an increase in absorption of laser light is unavoidable. Therefore, the compounding ratio is 5 to 35%, desirably. 20 ~
It was determined to be 30%.
【０００８】[0008]
【発明の実施の態様】つぎに、この発明の光記録媒体保
護層形成用ターゲット材を実施例により具体的に説明す
る。原料粉末として、平均粒径：５μｍを有する純度：
９９．９９９％以上のＺｎＳ粉末、同５μｍを有する純
度：９９．９９％以上のＳｉＯ2粉末、および同１μｍ
を有する純度：９９．９％以上のＴｉＯ2粉末を用意
し、これら原料粉末を表１に示される配合組成に配合
し、ボールミルで２時間混合した後、この混合粉末を黒
鉛型に充填した状態で、ホットプレス装置に装入し、雰
囲気：１×１０-2Ｔｏｒｒの真空雰囲気、温度：１１５
０℃、圧力：２００ｋｇｆ／ｃｍ2、保持時間：５時間
の条件で焼結してホットプレス焼結体とすることによ
り、いずれも直径：３０ｍｍ×厚さ：０．５ｍｍの寸法
をもった本発明ターゲット材１〜１０および従来ターゲ
ット材１〜５をそれぞれ製造した。Next, the target material for forming an optical recording medium protective layer of the present invention will be described in detail with reference to examples. Purity having an average particle size of 5 μm as a raw material powder:
99.999% or more ZnS powder, purity of 5 μm or more Purity: 99.99% or more SiO 2 powder and 1 μm or more
Purity: 99.9% or more of TiO 2 powder is prepared, and these raw material powders are blended in the blending composition shown in Table 1, mixed in a ball mill for 2 hours, and then filled in a graphite mold. Then, it was charged into a hot press apparatus, and the atmosphere was a vacuum atmosphere of 1 × 10 −2 Torr, and the temperature was 115.
By sintering under the conditions of 0 ° C., pressure: 200 kgf / cm 2 , and holding time: 5 hours to obtain a hot-pressed sintered body, a book having a size of 30 mm in diameter × 0.5 mm in thickness is obtained. Inventive target materials 1 to 10 and conventional target materials 1 to 5 were produced, respectively.
【０００９】ついで、まず、この結果得られた本発明タ
ーゲット材１〜１５を構成するホットプレス焼結体のＴ
ｉＯ2およびＴｉＮについて、光記録媒体保護層の特性
評価基準となる光屈折率および光透過率に及ぼす影響を
調べた。すなわち、上記の本発明ターゲット材１〜１５
および従来ターゲット材１〜５のそれぞれを、無酸素銅
製の水冷バッキングプレートにハンダ付けした状態で、
図１に示される構造をもった高周波マグネトロンスパッ
タリング装置に装着し、まず装置内を真空排気装置にて
１×１０-6Ｔｏｒｒの真空雰囲気とした後、Ａｒガスを
導入して装置内雰囲気を１．５×１０-3Ｔｏｒｒのスパ
ッタガス圧とし、引き続いて高周波電源よりマッチング
ボックスを介してターゲット材に５００Ｗ（平均電力密
度：４．１ｗ／ｃｍ２）のスパッタ電力を印加して、前
記ターゲット材と対向し、かつ５ｃｍの間隔を設けて平
行配置した直径：３ｃｍ×厚さ：０．５ｍｍのガラスか
らなる基板と前記ターゲット材間にプラズマを発生さ
せ、プラズマ中のＡｒイオンを前記ターゲット材の表面
に衝突させて前記ターゲット材をスパッタし、スパッタ
粒子を前記基板表面に蒸着することにより厚さ：９０ｎ
ｍの光記録媒体保護層を形成した。この結果形成された
光記録媒体保護層の光屈折率および光透過率を評価する
目的で、波長：７８０ｎｍのレーザーを用い、屈折率お
よび消衰係数を測定した。この測定結果を表１に示し
た。Next, first, the T of the hot-pressed sintered body constituting the target materials 1 to 15 of the present invention obtained as a result is obtained.
The effects of iO 2 and TiN on the light refractive index and light transmittance, which are the criteria for evaluating the characteristics of the optical recording medium protective layer, were examined. That is, the target materials 1 to 15 of the present invention described above.
And, in a state where each of the conventional target materials 1 to 5 is soldered to a water-cooled backing plate made of oxygen-free copper,
Attached to the high-frequency magnetron sputtering apparatus having the structure shown in FIG. 1, after a vacuum atmosphere of 1 × 10 -6 Torr by a vacuum exhaust device is first in the apparatus, while introducing Ar gas apparatus Atmosphere The sputtering gas pressure was set to 0.5 × 10 −3 Torr, and subsequently, a sputtering power of 500 W (average power density: 4.1 w / cm 2) was applied to the target material from a high-frequency power supply via a matching box, and the sputtering was performed. Plasma is generated between a substrate made of glass having a diameter of 3 cm and a thickness of 0.5 mm, which are opposed to each other and are arranged in parallel with an interval of 5 cm, and the target material, and Ar ions in the plasma are subjected to the surface of the target material. The target material is sputtered by collision with the substrate, and sputtered particles are vapor-deposited on the substrate surface to obtain a thickness of 90 n.
m of the optical recording medium protective layer was formed. For the purpose of evaluating the light refractive index and light transmittance of the optical recording medium protective layer formed as a result, the refractive index and the extinction coefficient were measured using a laser having a wavelength of 780 nm. The measurement results are shown in Table 1.
【００１０】ついで、上記の各種ターゲット材の耐割損
性を評価する目的で、ターゲット材へのスパッタ電力の
印加条件を、上記の５００Ｗから１００Ｗづつ上げて行
き、この間上昇スパッタ電力毎に１分間保持する条件と
する以外は、上記の光記録媒体保護層形成条件と同一の
条件でスパッタを行い、前記ーゲット材に割れが発生し
た時点の印加スパッタ電力（割れ発生臨界スパッタ電
力）を測定した。この測定結果を表１に示した。Next, in order to evaluate the cracking resistance of the various target materials, the conditions for applying the sputtering power to the target material are increased by 100 W from the above-mentioned 500 W, and during this period, the sputter power is increased for one minute. Sputtering was performed under the same conditions as the above-described optical recording medium protective layer forming conditions except that the conditions were maintained, and the applied sputter power (critical cracking sputter power) at the time when the target material cracked was measured. The measurement results are shown in Table 1.
【００１１】[0011]
【表１】 [Table 1]
【００１２】[0012]
【発明の効果】表１に示される結果から、ＴｉＯ2粉末
を配合したホットプレス焼結体からなる本発明ターゲッ
ト材１〜１５と、ＴｉＯ2粉末の配合がないホットプレ
ス焼結体からなる従来ターゲット材１〜５との比較か
ら、５〜３５％の割合でＴｉＯ2粉末を配合することに
よって耐割損性が著しく向上し、しかもこのＴｉＯ2粉
末の配合によっても光記録媒体保護層の屈折率の低下お
よび消衰係数の上昇がほとんど見られないことが明らか
である。上述のように、この発明のターゲット材は、高
出力スパッタの負荷によっても割れの発生が抑制され、
すぐれた耐割損性を示すことから、従来光記録媒体保護
層と同等の特性を具備した保護層の高速生膜を可能と
し、生産性の向上に寄与するものである。From the results shown in Table 1 according to the present invention, the present invention target material 15 consisting of hot-pressed sintered body containing a combination of TiO 2 powder, conventionally made of hot-pressed sintered body is not the formulation of TiO 2 powder From the comparison with the target materials 1 to 5, the addition of TiO 2 powder at a ratio of 5 to 35% significantly improves the breakage resistance, and the addition of this TiO 2 powder also allows the optical recording medium protective layer to be refracted. It is clear that there is little decrease in the rate and no increase in the extinction coefficient. As described above, in the target material of the present invention, the generation of cracks is suppressed even by the load of high-power sputtering,
Since it shows excellent breakage resistance, it enables a high-speed film formation of a protective layer having the same characteristics as the conventional optical recording medium protective layer, and contributes to an improvement in productivity.
【図１】高周波マグネトロンスパッタリング装置を例示
する概略縦断面図である。FIG. 1 is a schematic longitudinal sectional view illustrating a high-frequency magnetron sputtering apparatus.
フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｇ１１Ｂ 7/24 ５３４ Ｇ１１Ｂ 7/26 ５３１ 7/26 ５３１ Ｃ０４Ｂ 35/00 Ｐ Ｆターム(参考） 4G030 AA16 AA37 AA56 BA01 GA09 GA29 4K029 AA09 AA24 BA17 BA18 BA35 BA43 BA46 BA48 BA51 BB02 BC08 BD12 CA05 DC05 DC09 DC39 5D029 LA14 LA15 LA17 LC06 5D121 AA04 EE14 Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat II (reference) G11B 7/24 534 G11B 7/26 531 7/26 531 C04B 35/00 PF term (reference) 4G030 AA16 AA37 AA56 BA01 GA09 GA29 4K029 AA09 AA24 BA17 BA18 BA35 BA43 BA46 BA48 BA51 BB02 BC08 BD12 CA05 DC05 DC09 DC39 5D029 LA14 LA15 LA17 LC06 5D121 AA04 EE14
Claims (1)
成したことを特徴とする、高出力スパッタ条件ですぐれ
た耐割損性を発揮する光記録媒体保護層形成用スパッタ
リングターゲット材。1. A hot-press sintered body of a mixed powder having a composition of, by weight, silicon oxide: 3 to 25%, titanium oxide: 5 to 35%, zinc sulfide: balance, A sputtering target material for forming an optical recording medium protective layer which exhibits excellent crack resistance under high output sputtering conditions.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27352099A JP3915110B2 (en) | 1999-09-28 | 1999-09-28 | Sputtering target material for forming an optical recording medium protective layer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27352099A JP3915110B2 (en) | 1999-09-28 | 1999-09-28 | Sputtering target material for forming an optical recording medium protective layer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2001098362A true JP2001098362A (en) | 2001-04-10 |
| JP3915110B2 JP3915110B2 (en) | 2007-05-16 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP27352099A Expired - Fee Related JP3915110B2 (en) | 1999-09-28 | 1999-09-28 | Sputtering target material for forming an optical recording medium protective layer |
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| Country | Link |
|---|---|
| JP (1) | JP3915110B2 (en) |
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1999
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|---|---|
| JP3915110B2 (en) | 2007-05-16 |
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