JP4465711B2 - GaSb phase change recording film for producing phase change recording medium excellent in storage stability of recording mark and sputtering target for forming this recording film - Google Patents
GaSb phase change recording film for producing phase change recording medium excellent in storage stability of recording mark and sputtering target for forming this recording film Download PDFInfo
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- JP4465711B2 JP4465711B2 JP2004290940A JP2004290940A JP4465711B2 JP 4465711 B2 JP4465711 B2 JP 4465711B2 JP 2004290940 A JP2004290940 A JP 2004290940A JP 2004290940 A JP2004290940 A JP 2004290940A JP 4465711 B2 JP4465711 B2 JP 4465711B2
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- 229910005542 GaSb Inorganic materials 0.000 title claims description 26
- 238000003860 storage Methods 0.000 title claims description 17
- 238000005477 sputtering target Methods 0.000 title claims description 6
- 239000000203 mixture Substances 0.000 claims description 14
- 229910052738 indium Inorganic materials 0.000 claims description 11
- 229910052797 bismuth Inorganic materials 0.000 claims description 9
- 229910052787 antimony Inorganic materials 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 239000000956 alloy Substances 0.000 description 8
- 229910045601 alloy Inorganic materials 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 230000005496 eutectics Effects 0.000 description 5
- 238000004544 sputter deposition Methods 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 238000005219 brazing Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
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Description
この発明は、記録マークの保存安定性に優れた各種相変化型記録媒体に使用されるＧａＳｂ系相変化型記録膜およびそのＧａＳｂ系相変化型記録膜を形成するための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 GaSb phase change recording film used for various phase change recording media excellent in storage stability of recording marks and a sputtering target for forming the GaSb phase change recording film. .
一般に、光ビーム照射による非晶質相と結晶相との可逆的な相変化を利用して情報の記録、再生および消去を行う記録媒体において用いられる記録膜は、Ｇａ−Ｓｂ二元共晶系相変化型記録膜が用いられており、その中でもＧａ１２Ｓｂ８８共晶組成を有するＧａ−Ｓｂ二元系相変化型記録膜は、結晶化速度が大きく高速記録に好適であるところから広く知られている。このＧａ１２Ｓｂ８８共晶組成を有するＧａ−Ｓｂ二元系相変化型記録膜は、融点：５８８．０℃、結晶化温度：２０４．９℃を有し、このＧａ１２Ｓｂ８８共晶組成を有するＧａ−Ｓｂ二元系相変化型記録膜は、該膜と同一の成分組成を有する焼結合金からなるターゲットを用いてスパッタリングすることにより作製されることも知られている（例えば、非特許文献１参照）。 In general, a recording film used in a recording medium for recording, reproducing, and erasing information using a reversible phase change between an amorphous phase and a crystalline phase caused by light beam irradiation is a Ga-Sb binary eutectic system. Phase change recording films are used. Among them, a Ga—Sb binary phase change recording film having a Ga 12 Sb 88 eutectic composition is widely known because it has a high crystallization speed and is suitable for high-speed recording. It has been. The Ga—Sb binary phase change recording film having this Ga 12 Sb 88 eutectic composition has a melting point: 588.0 ° C. and a crystallization temperature: 204.9 ° C., and this Ga 12 Sb 88 eutectic composition It is also known that a Ga—Sb binary phase-change recording film having the following characteristics is produced by sputtering using a target made of a sintered alloy having the same component composition as the film (for example, non- Patent Document 1).
しかし、前記従来のＧａ１２Ｓｂ８８の共晶組成を有するＧａ−Ｓｂ二元系相変化型記録膜を形成した相変化型記録媒体は、Ｇａ−Ｓｂ二元系相変化型記録膜を非晶質化して保存された記録マークを有する相変化型記録媒体を高温雰囲気に長時間放置しておくとＧａ−Ｓｂ二元系相変化型記録膜が結晶化し、そのために記録マークの保存安定性が悪いという問題点があった。 However, the conventional phase change recording medium on which the Ga—Sb binary phase change recording film having the eutectic composition of Ga 12 Sb 88 is formed has a non-crystalline Ga—Sb binary phase change recording film. When a phase change type recording medium having a record mark which has been qualitatively stored is left in a high temperature atmosphere for a long time, the Ga-Sb binary phase change type recording film is crystallized, so that the storage stability of the record mark is improved. There was a problem of being bad.
そこで、本発明者らは、記録マークの保存安定性に一層優れた相変化型記録媒体を得るべく研究を行なった。その結果、
（イ）通常のＧａ−Ｓｂ二元系相変化型記録膜にＴｅを０．２〜２０％未満（以下、％は原子％を示す）を含有せしめたＧａＳｂ系相変化型記録膜に、さらにＩｎおよびＢｉの内の１種または２種を合計で０．２〜２０％未満含有せしめたＧａＳｂ系相変化型記録膜を形成した相変化型記録媒体は、さらに一層高温雰囲気に長時間放置しておいても優れた記録マークの保存安定性を有している、
（ロ）前記（イ）記載の記録マークの保存安定性に優れた相変化型記録媒体に形成するＧａＳｂ系相変化型記録膜は、このＧａＳｂ系相変化型記録膜と同一の成分組成を有する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る、という研究結果が得られたのである。
Therefore, the present inventors have studied to obtain a phase change type recording medium having further excellent recording mark storage stability. as a result,
(B) conventional GaSb binary phase-change recording film than from 0.2 to 20% of Te (hereinafter,% represents the atomic%) in the GaSb-based phase-change recording film for the additional inclusion of further A phase change type recording medium on which a GaSb phase change type recording film containing one or two of In and Bi in total less than 0.2 to 20% is formed is left in an even higher temperature atmosphere for a long time. It has excellent storage stability for recording marks.
(B) The GaSb phase change recording film formed on the phase change recording medium excellent in storage stability of the recording mark described in (a) has the same component composition as the GaSb phase change recording film. The research result that it was obtained by sputtering using a target 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）Ｇａ：５〜２０％未満を含有し、さらにＴｅを０．２〜２０％未満を含有し、さらにＩｎおよびＢｉの内の１種または２種を合計で０．２〜２０％未満を含有し、残部がＳｂおよび不可避不純物からなる組成を有する記録マークの保存安定性に優れた相変化型記録媒体を形成するためのＧａＳｂ系相変化型記録膜、
（２）Ｇａ：５〜２０％未満を含有し、さらにＴｅを０．２〜２０％未満を含有し、さらにＩｎおよびＢｉの内の１種または２種を合計で０．２〜２０％未満を含有し、残部がＳｂおよび不可避不純物からなる組成を有する前記（１）記載のＧａＳｂ系相変化型記録膜を形成する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 present invention has been made based on such research results,
(1) Ga: contains 5 to less than 20%, further contains Te to less than 0.2 to 20%, and further includes one or two of In and Bi in total less than 0.2 to 20% A GaSb phase change recording film for forming a phase change recording medium excellent in storage stability of a recording mark having a composition comprising Sb and inevitable impurities in the balance,
(2) Ga: contains 5 to less than 20%, further contains Te to less than 0.2 to 20%, and further includes one or two of In and Bi in total less than 0.2 to 20% A sputtering target for forming the GaSb-based phase change recording film according to the above (1), which has a composition comprising Sb and inevitable impurities.
この発明の記録マークの保存安定性に優れた相変化型記録媒体に形成されるＧａＳｂ系相変化型記録膜の成分組成を前述のごとく限定した理由を説明する。
（ａ） Ｇａ
この発明の記録マークの保存安定性に優れたＧａＳｂ系相変化型記録膜に含まれるＧａを５〜２０％未満に限定したのは、Ｇａの含有量が５％未満では結晶化温度が低くなり過ぎてマーク形成ができなくなるので好ましくなく、一方、Ｇａ：２０以上であると、結晶化温度が高くなり過ぎて結晶化が困難になるので好ましくないという理由によるものである。
The reason why the component composition of the GaSb phase change recording film formed on the phase change recording medium excellent in storage stability of the recording mark of the present invention is limited as described above will be described.
(A) Ga
The reason why the GaSb phase change type recording film excellent in storage stability of the recording mark of the present invention is limited to 5 to less than 20% is that the crystallization temperature is lowered when the Ga content is less than 5%. This is not preferable because marks cannot be formed too much. On the other hand, Ga: 20 or more is not preferable because the crystallization temperature becomes too high and crystallization becomes difficult.
（ｂ） Ｔｅ
この成分は、記録マークの保存安定性に優れた相変化型記録媒体を作製するためのＧａＳｂ系相変化型記録膜に添加する成分であるが、この成分を０．２％未満添加しても記録マークを安定させる効果が薄いので好ましくなく、一方、２０％以上を含有させると融点が高くなるためにアモルファス化がし難くなるので好ましくない。したがって、この発明のＧａＳｂ系相変化型記録膜に含まれるＴｅを０．２〜２０％未満に定めた。この発明のＧａＳｂ系相変化型記録膜に含まれるＴｅの含有量の一層好ましい範囲は３〜１５％である。
(B) Te
This component is a component added to GaSb-based phase-change recording film for producing a phase change type recording medium having excellent storage stability of the recording mark, even if the components were added in less than 0.2% Since the effect of stabilizing the recording mark is thin, it is not preferable. On the other hand, the content of 20% or more is not preferable because the melting point becomes high and it becomes difficult to make it amorphous. Therefore, Te contained in the GaSb phase change recording film of the present invention is set to 0.2 to less than 20%. A more preferable range of the content of Te contained in the GaSb phase change recording film of the present invention is 3 to 15%.
（ｃ） Ｉｎ、Ｂｉ
これら成分は、記録マークの保存安定性に優れた相変化型記録媒体を作製するためのＧａＳｂ系相変化型記録膜に必要に応じて添加する成分であるが、これら成分を０．２％未満添加しても一層の記録マークを安定させる効果が得られず、一方、２０％以上を含有させると融点が低くなりすぎるため、記録膜が変質し易くなるので好ましくない。したがって、この発明の相変化型記録媒体に形成するＧａＳｂ系相変化型記録膜に含まれるＩｎおよびＢｉのうちの１種または２種の合計を０．２〜２０％未満に定めた。この発明のＧａＳｂ系相変化型記録膜に含まれるＩｎおよびＢｉの含有量の一層好ましい範囲は３〜１５％である。
(C) In, Bi
These components are components added as needed to a GaSb phase change recording film for producing a phase change recording medium excellent in storage stability of recording marks. However, these components are less than 0.2%. Even if it is added, the effect of stabilizing the recording mark of one layer cannot be obtained. On the other hand, if 20% or more is contained, the melting point becomes too low and the recording film is easily deteriorated, which is not preferable. Thus, defining the sum of one or two of In and Bi contained in the GaSb-based phase-change recording film formed on the phase change type recording medium of the present invention to less than 0.2 to 20%. A more preferable range of the contents of In and Bi contained in the GaSb-based phase change recording film of the present invention is 3 to 15%.
この発明のＧａＳｂ系相変化型記録膜は、この発明のＧａＳｂ系相変化型記録膜の成分組成と同じ成分組成を有する合金をＡｒガス雰囲気中で溶解した後、鉄製モールドに出湯して合金インゴットを作製し、これらを不活性ガス雰囲気中で粉砕して合金粉末を作製し、この合金粉末を真空ホットプレスすることによりスパッタリングターゲットを作製し、かかる条件で作製したスパッタリングターゲットを通常のスパッタリング装置に装入し、通常の条件でスパッタすることにより形成することができる。
前記真空ホットプレスは、圧力：１４６〜１５５ＭＰａ、温度：３７０〜４３０℃、１〜２時間保持の条件で行なわれ、その後、モールドの温度が２７０〜３００℃まで下がった時点で冷却速度：１〜３℃／ｍｉｎ．で常温まで冷却することにより行われることが一層好ましい。
The GaSb-based phase change recording film of the present invention is obtained by dissolving an alloy having the same component composition as that of the GaSb-based phase change recording film of the present invention in an Ar gas atmosphere, and then pouring the molten iron into an iron mold. These are pulverized in an inert gas atmosphere to produce an alloy powder, a sputtering target is produced by vacuum hot pressing the alloy powder, and the sputtering target produced under such conditions is put into a normal sputtering apparatus. It can be formed by charging and sputtering under normal conditions.
The vacuum hot press is performed under the conditions of pressure: 146 to 155 MPa, temperature: 370 to 430 ° C., holding for 1 to 2 hours, and then cooling rate: 1 to 1 when the temperature of the mold is lowered to 270 to 300 ° C. 3 ° C./min. More preferably, it is carried out by cooling to room temperature.
この発明のＧａＳｂ系相変化型記録膜を形成した相変化型記録媒体は、高温雰囲気に長時間放置しておいても記録マークの保存安定性に優れており、新しい光メモリー産業の発展に大いに貢献し得るものである。 The phase change type recording medium on which the GaSb phase change type recording film of the present invention is formed has excellent storage stability of recording marks even when left in a high temperature atmosphere for a long time, and greatly contributes to the development of a new optical memory industry. It can contribute.
Ｇａ、Ｓｂ、Ｔｅ、ＩｎおよびＢｉをＡｒガス雰囲気中で溶解し鋳造して合金インゴットを作製し、この合金インゴットをＡｒ雰囲気中で粉砕することにより、いずれも粒径：２５０μｍ以下の合金粉末を作製した。
これら合金粉末を温度：４００℃、圧力：１４６ＭＰａで真空ホットプレスすることによりホットプレス体を作製し、これらホットプレス体を超硬バイトを使用し、旋盤回転数：２００ｒｐｍの条件で研削加工することにより直径：７６．２ｍｍ、厚さ：３ｍｍの寸法を有する円盤状の表１に示される成分組成を有する本発明ターゲット１〜５、比較ターゲット１〜４および従来ターゲット１を作製した。
Ga, Sb, Te, In, and Bi are melted and cast in an Ar gas atmosphere to produce an alloy ingot, and the alloy ingot is pulverized in an Ar atmosphere, so that any alloy powder having a particle size of 250 μm or less is obtained. Produced.
These alloy powders are hot-pressed by vacuum hot pressing at a temperature of 400 ° C. and a pressure of 146 MPa, and these hot-pressed bodies are ground using a cemented carbide tool at a lathe speed of 200 rpm. The present invention targets 1 to 5 , comparative targets 1 to 4 and the conventional target 1 having the component composition shown in Table 1 having a disk shape having a diameter of 76.2 mm and a thickness of 3 mm were prepared.
さらに、ガラス基板を用意した。次に、表１に示される本発明ターゲット１〜５、比較ターゲット１〜４および従来ターゲット１をそれぞれ銅製の冷却用バッキングプレートに純度：９９．９９９重量％のインジウムろう材にてハンダ付けした。 Furthermore, a glass substrate was prepared. Next, the present invention targets 1 to 5 , comparative targets 1 to 4 and the conventional target 1 shown in Table 1 were each soldered to a copper cooling backing plate with an indium brazing material having a purity of 99.999% by weight.
これら銅製の冷却用バッキングプレートに純度：９９．９９９重量％のインジウムろう材にてハンダ付けした各種ターゲットを直流マグネトロンスパッタリング装置に装入し、ガラス基板を各種ターゲットと距離を８０ｍｍとなるようにセットした後、到達真空度：２×１０−３Ｐａ以下になるまで真空引きを行い、その後、全圧：５×１０−１ＰａになるまでＡｒガスを供給し、
・ 基板温度：室温、
・投入電力：ＤＣ１００Ｗ、
の条件でスパッタリングを行い、ガラス基板の表面に、表２に示される厚さ：３０ｎｍを有するいずれもアモルファス相である本発明ＧａＳｂ系相変化型記録膜１〜５、比較ＧａＳｂ系相変化型記録膜１〜４および従来ＧａＳｂ系相変化型記録膜１を形成した。
Various targets soldered with an indium brazing material having a purity of 99.999% by weight to these copper cooling backing plates are loaded into a DC magnetron sputtering apparatus, and the glass substrate is set so that the distance between the various targets is 80 mm. After that, vacuuming is performed until the ultimate degree of vacuum is 2 × 10 −3 Pa or less, and then Ar gas is supplied until the total pressure is 5 × 10 −1 Pa.
・ Substrate temperature: room temperature
-Input power: DC100W
Sputtering is carried out under the following conditions: on the surface of the glass substrate, the present invention GaSb-based phase change recording films 1 to 5 having a thickness of 30 nm shown in Table 2 are all amorphous phases, and comparative GaSb-based phase change recording. Films 1 to 4 and a conventional GaSb phase change recording film 1 were formed.
このようにしてガラス基板の上に、記録膜（膜厚：３０ｎｍ）を成膜することにより表３に示される本発明サンプル記録媒体１〜５、比較サンプル記録媒体１〜４および従来サンプル記録媒体１を作製し、これら本発明サンプル記録媒体１〜５、比較サンプル記録媒体１〜４および従来サンプル記録媒体１を温度：１３０℃に保持された高温炉に表３に示される時間装入したのち取出し、絶対反射率測定装置（日本分光株式会社製）にて反射率を測定し、その値を表３に示すことにより記録マークの保存安定性を評価した。この場合、サンプル記録媒体を高温の雰囲気に長時間保持することによりアモルファスの記録膜は結晶化するところから、反射率が高くなるほど記録マークの保存安定性は悪いと評価される。 By forming a recording film (film thickness: 30 nm) on the glass substrate in this way, the present invention sample recording media 1 to 5 , comparative sample recording media 1 to 4 and conventional sample recording media shown in Table 3 1 was prepared, and the sample recording media 1 to 5 of the present invention, the comparative sample recording media 1 to 4 and the conventional sample recording media 1 were loaded into a high temperature furnace maintained at 130 ° C. for the time shown in Table 3. The reflectance was measured with an absolute reflectance measuring device (manufactured by JASCO Corporation), and the storage stability of the recording mark was evaluated by showing the value in Table 3 . In this case, since the amorphous recording film is crystallized by holding the sample recording medium in a high temperature atmosphere for a long time, it is evaluated that the storage stability of the recording mark is worse as the reflectance is higher.
表３に示される結果から、サンプル記録媒体作製直後（０時間）の本発明サンプル記録媒体１〜５、比較サンプル記録媒体１〜４および従来サンプル記録媒体１の反射率はほぼ同じ値を示すが、９６０時間高温の雰囲気に保持された本発明サンプル記録媒体１〜５は従来サンプル記録媒体１に比べて反射率が格段に小さいところから、記録マークの保存安定性が格段に優れていることがわかる。しかし、この発明の範囲から外れた成分組成を有する比較サンプル記録媒体１〜４は何らかの好ましくない特性が現れることが分かる。 From the results shown in Table 3 , the reflectances of the inventive sample recording media 1 to 5 , the comparative sample recording media 1 to 4, and the conventional sample recording media 1 immediately after the sample recording medium production (0 hour) show substantially the same values. The sample recording media 1 to 5 of the present invention held in a high-temperature atmosphere for 960 hours have a remarkably low reflectance compared to the conventional sample recording medium 1, and thus the storage stability of the recording mark is remarkably excellent. Recognize. However, it can be seen that comparative sample recording media 1 to 4 having a component composition outside the scope of the present invention exhibit some undesirable characteristics.
Claims (3)
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| JP2004290940A JP4465711B2 (en) | 2004-10-04 | 2004-10-04 | GaSb phase change recording film for producing phase change recording medium excellent in storage stability of recording mark and sputtering target for forming this recording film |
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