TWI421362B - Bi-Ge-O sintered body sputtering target and its manufacturing method and optical recording medium - Google Patents

Bi-Ge-O sintered body sputtering target and its manufacturing method and optical recording medium Download PDF

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TWI421362B
TWI421362B TW099137404A TW99137404A TWI421362B TW I421362 B TWI421362 B TW I421362B TW 099137404 A TW099137404 A TW 099137404A TW 99137404 A TW99137404 A TW 99137404A TW I421362 B TWI421362 B TW I421362B
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sintered body
geo
powder
sputtering target
target
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TW201129710A (en
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Atsushi Nara
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Jx Nippon Mining & Metals Corp
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Description

Bi-Ge-O系燒結體濺鍍靶及其製造方法及光記錄媒體
本發明係關於一種Bi-Ge-O系燒結體濺鍍靶及該靶之製造方法以及光記錄媒體，特別是關於耐熱衝擊性優異，可於高功率下濺鍍故而可期待生產效率之大幅度改善，且於濺鍍時不會產生靶之破裂，粒子之產生較少，可穩定地製作高品質之薄膜，且可獲得不會產生記錄位元之誤碼之光記錄媒體的Bi-Ge-O系燒結體濺鍍靶及該靶之製造方法以及光記錄媒體。
單寫多讀型(WORM，Write Once Read Many)光記錄媒體係利用藍色波長區域(350～500 nm)之雷射光亦可進行高密度之記錄的光記錄媒體，特別係具有高記錄感度且具有多層記錄層之光記錄媒體。
光碟為了因應高密度化之要求，正利用多層化來實現高密度化。於使用藍色LD之光碟中亦同樣正在進行高密度記錄用光記錄媒體之開發。
為實現可高密度多層記錄之單寫多讀型光記錄媒體，具有穩定之組成、構造之材料自不必言，亦需要透光特性優異之膜，此種材料多為氧化物，一般熔點較高，因而較多使用濺鍍法作為成膜法。
因此，為獲得此種膜而需要適當之濺鍍靶。然而，由於構成靶之化合物之形態、構造等亦會對濺鍍特性造成影響，因此當使構成靶之化合物為適於所需要之膜之特性時，是否可穩定地進行良好之濺鍍便成為問題。
於使用濺鍍法於基板形成光記錄媒體用薄膜之情形時，有時會因靶材料造成粒子之產生變多，而使品質降低。特別是高記錄密度媒體方面，粒子等造成之記錄位元之誤碼便成為深刻之問題。由此，產生成為不合格品而良率降低之問題。
先前，提出之光記錄媒體，提出有多種材料。例如專利文獻1中記載有一種光記錄媒體，其係於基板上至少形成記錄層者，且記錄層之構成元素之主成分為Bi及O(氧)，並且含有B，進而含有選自Ge、Li、Sn、Cu、Fe、Pd、Zn、Mg、Nd、Mn、Ni中之至少一種元素X。
又，專利文獻2中記載有一種單寫多讀型光記錄媒體，其特徵在於：記錄層含有Bi、M(M為Mg、Al、Cr、Mn、Co、Fe、Cu、Zn、Li、Si、Ge、Zr、Ti、Hf、Sn、Mo、V、Nb、Y、Ta中之至少一種元素)及氧，記錄資訊之記錄標記部包含該記錄層所含有之元素之結晶及/或該等元素之氧化物之結晶。
此外，亦提出有專利文獻3～專利文獻8。於該等之中，考慮有由鉍(Bi)、鍺(Ge)、氧(O)所構成之光記錄媒體之組合，又，亦記載有藉由燒結體靶之濺鍍而將該等光記錄媒體成膜。然而，該Bi-Ge-O系燒結體濺鍍靶，存在如下之問題：熱衝擊較弱，因於高功率濺鍍時產生破裂、龜裂之情形較多，由此產生粒子，損害記錄膜等之品質。
專利文獻1：日本特開2008-210492號公報
專利文獻2：日本特開2006-116948號公報
專利文獻3：日本特開2003-48375號公報
專利文獻4：日本特開2005-161831號公報
專利文獻5：日本特開2005-108396號公報
專利文獻6：日本特開2007-169779號公報
專利文獻7：日本特開2008-273167號公報
專利文獻8：日本第4271063號公報
本發明之課題係關於一種Bi-Ge-O系燒結體濺鍍靶及該靶之製造方法以及光記錄媒體，特別是提供一種耐熱衝擊性優異，可於高功率下濺鍍故而可期待生產效率之大幅度改善，且於濺鍍時不會產生靶之破裂，粒子之產生較少，可穩定地製作高品質之薄膜，且可獲得不會產生記錄位元之誤碼之光記錄媒體的Bi-Ge-O系燒結體濺鍍靶及該靶之製造方法以及光記錄媒體。
為解決上述課題，本發明者等人進行了銳意研究，結果獲得如下之知識見解：藉由使分散系之Bi12 GeO20 粒子微粒子化，從而各粒子之加熱、冷卻時之熱膨脹、熱收縮量減少，耐熱衝擊性提高。
根據該知識見解，本發明提供：
1)一種Bi-Ge-O系燒結體濺鍍靶，其係由鉍(Bi)、鍺(Ge)、氧(O)所構成者，其特徵在於：Bi與Ge之原子數比為0.57<(Bi/(Bi+Ge))<0.75，由Bi12 GeO20 、Bi4 Ge3 O12 之2相構成結晶相；
2)如上述1)之Bi-Ge-O系燒結體濺鍍靶，其中，Bi12 GeO20 與Bi4 Ge3 O12 之莫耳比為(Bi12 GeO20 /Bi4 Ge3 O12 )<0.56；
3)如上述1)或2)之Bi-Ge-O系燒結體濺鍍靶，其中，靶燒結體中之Bi12 GeO20 之最大粒徑為3 μm以下；
4)如上述1)至3)中任一項之燒結體濺鍍靶，其中，對靶施加200℃、30分鐘之加熱後，藉由水中急冷施以熱衝擊之情形時的該熱衝擊前後之平均彎曲強度降低率為50%以下；
5)一種光記錄媒體，其係使用上述1)至4)中任一項之靶進行濺鍍而成膜。
又，本發明提供：
6)一種Bi-Ge-O系燒結體濺鍍靶之製造方法，其特徵在於：將混合GeO2 粉14.3 mol%及Bi2 O3 粉85.7 mol%後進行固相反應所獲得之Bi12 GeO20 粉、與混合GeO2 粉60.0 mol%及Bi2 O3 粉40.0 mol%後進行固相反應所獲得之Bi4 Ge3 O12 粉末作為起始原料，並進行熱壓，藉此製作燒結體；
7)如上述6)之Bi-Ge-O系燒結體濺鍍靶之製造方法，其中，將Bi12 GeO20 粉及Bi4 Ge3 O12 粉末作為起始原料，以Bi與Ge之原子數比成為0.57<(Bi/(Bi+Ge))<0.75之方式混合後，於600～840℃、加壓力0～400 kg/cm2 下熱壓，藉此製作燒結體；
8)如上述6)或7)之Bi-Ge-O系燒結體濺鍍靶之製造方法，其中，使用經微粉碎成平均粒徑1 μm以下之Bi12 GeO20 粉。
本發明之Bi-Ge-O系燒結體濺鍍靶具有如下之優異效果：耐熱衝擊性特別優異，可/於高功率下濺鍍故而可期待生產效率之大幅度改善，且於濺鍍時不會產生靶之破裂，粒子之產生較少，可穩定地製作高品質之薄膜，且可獲得不會產生記錄位元之誤碼之光記錄媒體。
本發明之Bi-Ge-O系燒結體濺鍍靶係由鉍(Bi)、鍺(Ge)、氧(O)所構成，其特徵在於：Bi與Ge之原子數比為0.57<(Bi/(Bi+Ge))<0.75，由Bi12 GeO20 、Bi4 Ge3 O12 之2相構成結晶相。利用該組成之記錄膜為可利用多層化達成高密度記錄之較佳組成，可穩定地進行良好之濺鍍成膜。
一般於將氧化鉍(Bi2 O3 )與氧化鍺(GeO2 )之粉末作為起始原料，將其燒結來製作該組成靶之情形時，會成為Bi12 GeO20 與Bi4 Ge3 O12 之2相共存組成。
然而，由於Bi12 GeO20 與Bi4 Ge3 O12 之熱膨脹係數差較大，因此產生熱衝擊極弱，高功率下之濺鍍成膜時會產生破裂之問題。此外，Bi12 GeO20 之熱膨脹係數為1.39×10-5 ，Bi4 Ge3 O12 之熱膨脹係數為6.00×10-6 。
另一方面，於該組成範圍內，Bi4 Ge3 O12 會成為母材，Bi12 GeO20 粒子會成為分散系。此時明瞭到藉由使分散系之Bi12 GeO20 粒子微粒子化，從而各粒子之加熱、冷卻時之熱膨脹、熱收縮量會減少，耐熱衝擊性會提高。
又明瞭到若將Bi2 O3 及GeO2 作為起始原料，於Bi12 GeO20 與Bi4 Ge3 O12 共存之狀態下進行微粉碎，則Bi4 Ge3 O12 會選擇性地微粉碎，而分散系之Bi12 GeO20 難以粉碎。
因此，藉由將Bi12 GeO20 及Bi4 Ge3 O12 作為起始原料，預先微粉碎Bi12 GeO20 ，而實現了耐熱衝擊性之提高。
其結果可獲得如下之較大優點：靶之耐熱衝擊性提高，因此可於高功率下成膜，可使生產效率上升。
又，可獲得如下之效果：由破裂或龜裂所引起之粒子之產生顯著減少，可製作穩定之高品質之薄膜，並且可製造不會產生記錄位元之誤碼且能夠達成高記錄密度之光記錄媒體。
將Bi12 GeO20 與Bi4 Ge3 O12 之莫耳比設為(Bi12 GeO20 /Bi4 Ge3 O12 )<0.56在提高耐熱衝擊性方面有效。
進而，於使靶燒結體中之Bi12 GeO20 之粒徑微細化之情形時，更有效的是將最大粒徑設為3 μm以下、較佳為1 μm以下。對上述靶施加200℃、30分鐘之加熱後，藉由水中急冷施以熱衝擊之情形時的該熱衝擊前後之平均彎曲強度降低率可達到50%以下。
於先前製品之Bi12 GeO20 與Bi4 Ge3 O12 之2相共存組成的靶之情形時，上述熱衝擊前後之平均彎曲強度降低率超過80%，相對於此而具有較大之改善效果。由此，不但抑制由熱衝擊所引起靶之破裂，而且可直接地評價靶之特性。
本發明包括使用上述靶進行濺鍍而成膜之光記錄媒體。
當製造Bi-Ge-O系燒結體濺鍍靶時，將GeO2 粉14.3 mol%及Bi2 O3 粉85.7 mol%混合後進行固相反應所獲得之Bi12 GeO20 粉，與將GeO2 粉60.0 mol%及Bi2 O3 粉40.0 mol%混合後進行固相反應所獲得之Bi4 Ge3 O12 粉末作為起始原料，將該等進行混合並熱壓，藉此可製作燒結體。
進而，當製造本申請案發明之Bi-Ge-O系燒結體濺鍍靶時，特別有效的是：將Bi12 GeO20 粉及Bi4 Ge3 O12 粉末作為起始原料，以Bi與Ge之原子數比成為0.57<(Bi/(Bi+Ge))<0.75之方式混合後，於600～840℃、加壓力0～400 kg/cm2 下熱壓，藉此製作燒結體。
於此情形時，亦有效的是使用將平均粒徑微粉碎為1 μm以下之Bi12 GeO20 粉。
該燒結條件為可獲得均勻組成之靶之較佳條件。雖亦可於偏離上述範圍之燒結條件下製造靶，但由於靶品質之再現性較差，故較理想的是將燒結條件設為上述之範圍。又，將上述原料階段之Bi與Ge之原子數比即0.57<(Bi/(Bi+Ge))<0.75直接反映於靶中，可獲得該組成比之靶。
實施例
以下，根據實施例及比較例進行說明。再者，本實施例僅為一例，並不受到該例任何限制。即，本發明僅受到申請專利範圍限制，且包括本發明所包含之實施例以外之各種變形。
(實施例1)
將純度3 N(99.9%)之氧化鉍與氧化鍺之粉末作為起始原料，預先準備Bi12 GeO20 粉及Bi4 Ge3 O12 粉末，分別將該等以Bi與Ge之原子數比成為0.67之方式調合Bi12 GeO20 粉16.67 mol%與Bi4 Ge3 O12 粉83.33 mol%後，加以混合，進而將混合後之粉末填充於碳製模具，於溫度700℃、壓力250 kg/cm2 之條件下進行熱壓。
將熱壓後之燒結體精加工製成靶。靶之相對密度為96%(100%密度時為7.15 g/cm3 )。
藉由X射線繞射測定確認該燒結體為Bi12 GeO20 、Bi4 Ge3 O12 之2相構造。
繼而，將該燒結體之掃描式電子顯微鏡觀察照片示於圖1。藉此確認到：Bi4 Ge3 O12 為母材(照片之灰色部分)、Bi12 GeO20 為分散系(照片之白色部分)。又，確認Bi12 GeO20 之最大粒徑為3 μm以下、平均粒徑為1 μm以下。
繼而，對該靶施加200℃、30分鐘之加熱後，藉由水中急冷施以熱衝擊。其後，藉由JIS標準1601實施彎曲試驗(自靶中之任意部位5處，選取寬度為4±0.1 mm、高度為3±0.1 mm、長度為40～50 mm之試驗片進行測定，求出5處之測定結果之平均值)，測定該熱衝擊前後之平均彎曲強度比(強度之降低率)。將該測定結果同樣示於表1。因測定部位不同而產生稍許偏差，但任一者均未滿50%，強度之降低率較少。
繼而，使用該靶，於玻璃基板上以1 kW預濺鍍約1小時後，以2 kW濺鍍10 s，停止5 s，並反覆進行10,000次，該濺鍍循環之作業後，打開腔室目視觀察靶之異常，完全未發現靶有破裂或龜裂之產生。又，濺鍍中之粒子之產生亦較少。
其結果，本申請案發明之實施例係具有如下優異效果的良好之靶：不會產生靶之破裂，可提高生產效率且可穩定地製作高品質之薄膜，能夠獲得不會產生記錄位元之誤碼之光記錄媒體。
(比較例1)
將純度3 N(99.9%)之氧化鉍與氧化鍺之粉末作為起始原料，分別將該等以Bi與Ge之原子數比成為0.67之方式調合GeO2 粉50.0 mol%、Bi2 O3 粉50.0 mol%後，加以混合，進而將混合後之粉末填充於碳製模具，於溫度730℃、壓力250 kg/cm2 之條件下進行熱壓。
將熱壓後之燒結體精加工製成靶。靶之相對密度為103%(100%密度時為7.44 g/cm3 )。
經由該燒結體之X射線繞射測定確認到靶之結晶相為Bi12 GeO20 、Bi4 Ge3 O12 之2相構造。
繼而，將該燒結體之掃描式電子顯微鏡觀察照片示於圖2。藉此確認：Bi4 Ge3 O12 為母材(照片之灰色部分)、Bi12 GeO20 為分散系(照片之白色部分)。又，確認到Bi12 GeO20 之最大粒徑為8 μm以下、平均粒徑為4 μm以下。
繼而，對該靶施加200℃、30分鐘之加熱後，藉由水中急冷施以熱衝擊。其後，藉由JIS1601實施平均彎曲強度試驗。將該熱衝擊前後之平均彎曲強度比(強度之降低率)之測定結果同樣示於表1。其結果，平均彎曲強度之降低率為82.1%。
繼而，使用該靶，於玻璃基板上以1 kW預濺鍍約1小時後，以2 kW濺鍍10 s，停止5 s，並反覆進行10次，該濺鍍循環之作業後，打開腔室目視觀察靶之異常，結果靶產生了破裂。又，與實施例相比，粒子之產生顯著增加。認為其原因係濺鍍中之靶之破裂。
[產業上之可利用性]
根據本發明之Bi-Ge-O系燒結體濺鍍靶及該靶之製造方法，具有如下之優異效果：耐熱衝擊性特別優異，可於高功率下濺鍍故而可期待生產效率之大幅度改善，且於濺鍍時不會產生靶之破裂，粒子之產生較少，可穩定地製作高品質之薄膜，且可獲得不會產生記錄位元之誤碼之光記錄媒體。並且可提供一種能夠提高光記錄媒體之成膜之生產效率，且適於製造光記錄媒體之靶。
圖1係表示實施例1中所獲得之燒結體之掃描式電子顯微鏡觀察結果之照片。
圖2係表示比較例1中所獲得之燒結體之掃描式電子顯微鏡觀察結果之照片。

Claims (9)

  1. 一種Bi-Ge-O系燒結體濺鍍靶，其係由鉍(Bi)、鍺(Ge)、氧(O)所構成者，其特徵在於：Bi與Ge之原子數比為0.57<(Bi/(Bi+Ge))<0.75，由Bi12 GeO20 、Bi4 Ge3 O12 之2相構成結晶相。
  2. 如申請專利範圍第1項之Bi-Ge-O系燒結體濺鍍靶，其中，Bi12 GeO20 與Bi4 Ge3 O12 之莫耳比為(Bi12 GeO20 /Bi4 Ge3 O12 )<0.56。
  3. 如申請專利範圍第1項或第2項之Bi-Ge-O系燒結體濺鍍靶，其中，靶燒結體中之Bi12 GeO20 之最大粒徑為3μm以下。
  4. 如申請專利範圍第1項或第2項之Bi-Ge-O系燒結體濺鍍靶，其中，對靶施加200℃、30分鐘之加熱後，藉由水中急冷施以熱衝擊時的該熱衝擊前後之平均彎曲強度降低率為50%以下。
  5. 如申請專利範圍第3項之Bi-Ge-O系燒結體濺鍍靶，其中，對靶施加200℃、30分鐘之加熱後，藉由水中急冷施以熱衝擊時的該熱衝擊前後之平均彎曲強度降低率為50%以下。
  6. 一種光記錄媒體，其係使用申請專利範圍第1項至第5項中任一項之靶進行濺鍍而成膜。
  7. 一種Bi-Ge-O系燒結體濺鍍靶之製造方法，其特徵在於：將混合GeO2 粉14.3mol%及Bi2 O3 粉85.7mol%後進行 固相反應所獲得之Bi12 GeO20 粉、與混合GeO2 粉60.0mol%及Bi2 O3 粉40.0mol%後進行固相反應所獲得之Bi4 Ge3 O12 粉末作為起始原料，並進行熱壓，藉此製作燒結體。
  8. 如申請專利範圍第7項之Bi-Ge-O系燒結體濺鍍靶之製造方法，其中，將Bi12 GeO20 粉及Bi4 Ge3 O12 粉末作為起始原料，以Bi與Ge之原子數比成為0.57<(Bi/(Bi+Ge))<0.75之方式混合之後，於600~840℃、加壓力0~400kg/cm2 下熱壓，藉此製作燒結體。
  9. 如申請專利範圍第7項或第8項之Bi-Ge-O系燒結體濺鍍靶之製造方法，其中，使用經微粉碎成平均粒徑1μm以下之Bi12 GeO20 粉。
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