JPH036218B2 - - Google Patents
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- Publication number
- JPH036218B2 JPH036218B2 JP24183184A JP24183184A JPH036218B2 JP H036218 B2 JPH036218 B2 JP H036218B2 JP 24183184 A JP24183184 A JP 24183184A JP 24183184 A JP24183184 A JP 24183184A JP H036218 B2 JPH036218 B2 JP H036218B2
- Authority
- JP
- Japan
- Prior art keywords
- target material
- composite target
- sintered composite
- weight
- 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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- 239000013077 target material Substances 0.000 claims description 62
- 239000002131 composite material Substances 0.000 claims description 48
- 238000009792 diffusion process Methods 0.000 claims description 24
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 22
- 150000002910 rare earth metals Chemical class 0.000 claims description 22
- 229910045601 alloy Inorganic materials 0.000 claims description 21
- 239000000956 alloy Substances 0.000 claims description 21
- 229910052723 transition metal Inorganic materials 0.000 claims description 19
- 150000003624 transition metals Chemical class 0.000 claims description 19
- 239000002923 metal particle Substances 0.000 claims description 12
- 239000012535 impurity Substances 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 5
- 229910052691 Erbium Inorganic materials 0.000 claims description 5
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 5
- 229910052689 Holmium Inorganic materials 0.000 claims description 5
- 229910052775 Thulium Inorganic materials 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 229910052771 Terbium Inorganic materials 0.000 claims description 4
- 239000000843 powder Substances 0.000 description 33
- 239000002245 particle Substances 0.000 description 32
- 238000004544 sputter deposition Methods 0.000 description 32
- 239000000203 mixture Substances 0.000 description 25
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 13
- 229910052760 oxygen Inorganic materials 0.000 description 13
- 239000001301 oxygen Substances 0.000 description 13
- 230000035939 shock Effects 0.000 description 12
- 239000012071 phase Substances 0.000 description 10
- 238000001755 magnetron sputter deposition Methods 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000010409 thin film Substances 0.000 description 6
- 239000010408 film Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 5
- 229910001117 Tb alloy Inorganic materials 0.000 description 4
- 230000005415 magnetization Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910001279 Dy alloy Inorganic materials 0.000 description 3
- 229910017061 Fe Co Inorganic materials 0.000 description 3
- 229910000640 Fe alloy Inorganic materials 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 229910000765 intermetallic Inorganic materials 0.000 description 3
- -1 iron group metals Chemical class 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 229910001106 Ho alloy Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000005242 forging Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- 229910000767 Tm alloy Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
Description
〔産業上の利用分野〕
この発明は、光磁気記録材料として最近注目さ
れている希土類金属と遷移金属（鉄族金属）とか
らなる薄膜をスパツタリングにより製造する際に
用いられる焼結複合ターゲツト材に関する。
〔従来の技術〕
光磁気記録用の薄膜をスパツタリングにより製
造するための従来の希土類金属と遷移金属（鉄族
金属）とを構成成分とするターゲツト材として
は、
(1)２種の金属を真空もしくは不活性雰囲気中で
アーク熔解して作つた酸素含有量が0.5〜3.0重量
％である合金ターゲツト材（組成は希土類金属が
30〜50重量％、遷移金属が70〜50重量％）、及び
(2)遷移金属板上に希土類金属のチツプを置いた複
合ターゲツト材あるいは希土類金属板上に遷移金
属チツプを置いた同様ターゲツト材がある。
〔発明が解決しようとする問題点〕
しかしながら、上記の(1)の合金ターゲツト材に
は、
(a) 靭性がない（抵抗力：２Kg／mm2以下）ため割
れ易く、取り扱いが難しい。
(b) 耐熱衝撃性がないため、スパツタリング中の
熱衝撃により割れることが多い。
(c) ターゲツト材中の酸素含有量が0.5〜3.0重量
％と高いために、この合金ターゲツト材を用い
てスパツタリングにより得られた薄膜は、光磁
気記録のために必要な垂直磁化膜となりにく
い。
(d) ターゲツト材の大きさはアーク熔解炉の大き
さに依存するが、現在の所、せいぜい直径が60
mmのものまでしか得られない。
(e) このターゲツト材を用いた例えばマグネトロ
ンスパツタリング（スパツタリング条件はAr
分圧：１×10-2torr、出力：0.5A、145V、プ
リスパツタリング時間：30分、基板はスライド
ガラス、基板とターゲツト間の距離：70mm、バ
イアス電圧：0V、基板回転：10rpm）のとき
のスパツタリング速度は1000〜2000Å／min.
と遅い。
以上、(a)〜(e)の問題点がある。
そして、上記の(2)の複合ターゲツト材には、
(a) 回転や反転することができないし、チツプを
均一な分布状態として使用することが困難であ
る。
(b) 板内に磁力線が入り易く、板表面に出にく
い。
又、板表面上のチツプの存在により磁界が均
一でなくなる。
(c) このターゲツト材を用した例えばマグネトロ
ンスパツタリング（スパツタリング条件は(1)の
合金ターゲツト材の(e)の条件と同じ）のときの
スパツタリング速度は1000〜2000Å／min.と
遅い。
以上、(a)〜(c)の問題点がある。
したがつて、この発明の目的は、靭性、耐熱衝
撃性共に大きく、取り扱い中やスパツタリングの
熱衝撃により割れることもなく、回転や反転する
こともでき、しかも、酸素含有量が少なくて光磁
気記録に好適な垂直磁化膜を早いスパツタリング
速度で形成することができるターゲツト材を提供
することである。
〔問題点を解決するための手段〕
本発明者らは、先に、次のような複合ターゲツ
ト材の製造方法を出願した（特願昭59−219227
号）。即ち、
希土類金属の１種以上であつて、かつその形状
が粉末、小粒及びチツプのうちの１種以上と、遷
移金属の１種以上の粉末との混合物を真空中、あ
るいは不活性雰囲気中で混合物中に存在する金属
成分系の共融点未満の温度で熱間成形することを
特徴とする製造方法である。
この製造方法により初めて得られた、希土類金
属粒子と遷移金属粒子との界面に反応拡散相が存
在する組織を有する焼結複合ターゲツト材が前記
目的を達成することを本発明者らは種々検討の結
果見い出した。
この発明は、上記知見に基いて発明されたもの
であり、
Tb、Gd、Dy、Ho、Tm及びEr並びにそれら
の合金からなる群より選ばれた希土類金属粒子と
反応拡散相を構成する希土類金属の１種以上：30
〜50％、
Fe、Co及びNi並びにそれらの合金からなる群
より選ばれた遷移金属粒子と反応拡散相を構成す
る遷移金属の１種以上と不可避不純物：残りから
なる組成（以上、重量％）、及び、
希土類金属粒子と遷移金属粒子との界面に反応
拡散相が存在する組織を有することを特徴とする
焼結複合ターゲツト材である。
以下、この発明の構成を説明する。
(i) 組成成分と不可避不純物
この発明の焼結複合ターゲツト材は、希土類
金属の１種以上と遷移金属の１種以上と不可避
不純物からなる組成を有するものである。
この発明の焼結複合ターゲツト材の組成成分
である希土類金属は、Tb、Gd、Dy、Ho、
Tm及びEr並びにそれらの合金からなる群より
１種以上が選ばれる。それらの合金とは、Tb、
Gd、Dy、Ho、Tm及びErのうちの２種以上か
らなる合金を意味する。
又、この発明の焼結複合ターゲツト材の組成
成分である遷移金属は、Fe、Co及びNi並びに
それらの合金からなる群より１種以上が選ばれ
る。それらの合金とは、Fe、Co及びNiのうち
の２種以上からなる合金を意味する。
そして、不可避不純物としては、元素周期律
表の3a族元素、Si、Ca、Al、Ｃ、Ｐ、Ｓ、
Ta、Mn酸素等が挙げられる。
(ii) 組 成
この発明の焼結複合ターゲツトは、(i)項で述
べた希土類金属、すなわちTb、Gd、Dy、Ho、
Tm、及びEr、並びにそれらの合金からなる群
より選ばれた希土類金属の１種以上と、Fe、
Co及びNi、並びにそれらの合金からなる群よ
り選ばれた遷移金属の１種以上とで構成された
光磁気記録用薄膜をスパツタリングにより形成
するのに用いられるものであり、前記希土類金
属の１種以上：30〜50重量％を含有し、残りが
前記遷移金属の１種以上と不可避不純物からな
る組成を有するが、前記希土類金属が30重量％
未満でも50重量％を超えても、この焼結複合タ
ーゲツト材を用いてスパツタリングにより得ら
れる膜の磁化特性は垂直とはならずにすべて面
内磁化特性を有し、さらに保磁力も小さくな
り、実用上使用できない特性であるから、希土
類金属の含有量を30〜50重量％と定めた。
次に、不可避不純物は、原料等の製法上、元
素周期律表の3a族、Si、Ca及びAlがそれぞれ
0.1重量％以下、Ｃ、Ｐ及びＳがそれぞれ0.1重
量％以下、Ta及びMnがそれぞれ0.3重量％以
下含んでいる。
(iii) 酸素含有量
この発明の焼結複合ターゲツト材中に不可避
不純物として含まれる酸素の量は、従来の合金
ターゲツト材と比較して、大巾に低減されてお
り、0.3重量％以下である。したがつて、この
発明の焼結複合ターゲツト材を用いてスパツタ
リングにより得られた膜は光磁気記録に必要な
垂直磁化特性を示すのである。
(iv) 組 織
この発明の焼結複合ターゲツト材は、第３図
の顕微鏡写真にも示されるように、希土類金属
粒子と遷移金属粒子との界面に反応拡散相が存
在する組織を有する。反応拡散相は上記第３図
の顕微鏡写真に示すように層を形成する場合も
あり、又、層を形成しないで例えば分散（点
在）状態で存在する場合もある。接合強度の面
からは、反応拡散相（希土類金属と遷移金属と
の固相拡散及び反応により生じた相）は層状で
存在するのが好ましい。
この反応拡散相の含有割合（但し、空隙を除
いた含有割合）は、0.2〜80容量％が望ましい。
その含有割合が0.2容量％未満では、粒子同志
の結合力が弱くなり、取り扱い及び加工中に破
損し易くなるため、取り扱いや加工が困難乃至
不可能となり、一方、80容量％を超えると、靭
性が低下し、取り扱い中に簡単に砕けたり、ス
パツタリング中の熱衝撃などにより表面に微小
クラツクが入つたり割れたりするようになるか
らである。より望ましくは、反応拡散相の含有
割合は１〜50容量％である。
〔実施例〕
以下、実施例により、この発明の焼結複合ター
ゲツト材を詳しく説明する。
実施例 １
平均粒径が100μｍのTb粉末（純度：99.9％）
とFe粉末（純度99.99％）とを用意し、Tb粉末：
49重量％、Fe粉末：51重量％の配合割合で配合
し、ボールミルを用いて30分間トルエン中で混合
し、その後、取り出し乾燥し、内径が127mmのホ
ツトプレスモールド内に160ｇ充填し、昇温速度
800℃／hr.で昇温し、800℃に達したら、真空度
10-3torr、加圧圧力400Kg／cm2及び保持時間15分
の条件でホツトプレスを行ない、加熱終了後炉冷
し、取り出した後表面を研摩し、配合組成と実質
的に同じ組成を有し、かつ第１図のａ及びｂに示
す組織、即ち、Tb粒子とFe粒子との界面に平均
層厚1μｍのTb2Feなどの金属間化合物からなる反
応拡散層が存在し、しかもTb粒子とFe粒子と反
応拡散層とがそれぞれ44容量％、48容量％、及び
８容量％である組織を有し、直径が127mmで厚さ
1.5mmの焼結複合ターゲツト材を得た。この焼結
複合ターゲツト材の酸素含有量は0.1重量％であ
る。反応拡散層が金属間化合物からなつているこ
とは、XMAライン分析で確認した。
この焼結複合ターゲツト材の抗折力は13Kg／mm2
であり、耐熱衝撃性も良好であつた。
マグネトロンスパツタリング（スパツタリング
条件は(1)の合金ターゲツト材の問題点(e)の条件と
同じ）に、この焼結複合ターゲツト材を用いたと
きのスパツタリング速度は5000Å／min.であつ
た。
実施例 ２
平均粒径が20μｍのFe粉末（純度：99.99％）と
Co粉末（純度：99.99％）とTb粉末（純度：99.9
％）とGd粉末（純度：99.9％）とを用意し、Fe
粉末：39.4重量％、Co粉末：36.4重量％、Tb粉
末：12.5重量％、Gd粉末：11.7重量％の配合割合
で配合し、以下、ホツトプレスモールド内径を
203mm、充填量を770ｇ及びホツトプレス温度を
600℃とすることを除いて、実施例１と同様に行
ない、配合組成と実質的に同じ組成を有し、かつ
Tb粒子やGd粒子とFe粒子やCo粒子との界面に
層厚が１〜5μｍの範囲である反応拡散層が存在
し、しかも、Tb粒子、Gd粒子、Fe粒子、Co粒
子及び反応拡散層がそれぞれ23容量％、12容量
％、32容量％、28容量％及び５容量％である組織
を有し、直径が203mmで厚さ３mmの焼結複合ター
ゲツト材を得た。この焼結複合ターゲツト材の酸
素含有量は0.2重量％である。
この焼結複合ターゲツト材の抗折力は12Kg／mm2
であり、耐熱衝撃性も良好であつた。実施例１と
同じスパツタリング条件のマグネトロンスパツタ
リングに用いたときのスパツタリング速度は6200
Å／min.であつた。
実施例 ３
平均幅0.2mm×平均厚0.05mm×平均長さ２mmの
Tb片（純度：99.9％）とFe−５重量％Co合金片
を用意し、Tb片：49重量％、Fe合金片：51重量
％の配合割合で配合し、以下、充填量を170ｇ及
びホツトプレス温度を600℃とすることを除いて、
実施例１と同様に行ない、配合組成と実質的に同
じ組成を有し、かつ第２図に示す組織、即ち、片
状のTb粒子と片状のFe合金粒子との界面に反応
拡散層が存在し、Tb粒子、Fe合金粒子及び反応
拡散層がそれぞれ21容量％、55容量％及び24容量
％である組織を有し、直径が127mmで厚さ２mmの
焼結複合ターゲツト材を得た。この焼結複合ター
ゲツト材の酸素含有量は0.01重量％である。
この焼結複合ターゲツト材の抗折力は17Kg／mm2
であり、耐熱衝撃性も良好であつた。実施例１と
同じスパツタリング条件のマグネトロンスパツタ
リングに用いたときのスパツタリング速度は4700
Å／min.であつた。
実施例 ４
平均粒径100μｍのCo粉末（純度：99.99％）に
平均層厚1μｍでFeをメツキする。この結果得ら
れた粉末の組成は、Co：97重量％、Fe：３重量
％からなる。
別に、平均粒径100μｍのTb−20重量％Ho合金
粉末をも用意し、FeメツキCo粉末：58.4重量％、
Tb合金粉末：41.6重量％の配合割合で配合し、
以下、充填量を310ｇ及びホツトプレス温度を600
℃とすることを除いて、実施例１と同様に行な
い、配合組成と実質的に同じ組成を有し、反応拡
散層がFeメツキ層とTb合金粒子との界面に存在
し、Tb合金粒子とFe層とCo粒子と反応拡散層が
それぞれ44容量％、2.8容量％、53容量％及び0.2
容量％である組織を有し、直径が127mmで厚さ３
mmの焼結複合ターゲツト材を得た。この焼結複合
ターゲツト材の酸素含有量は0.18重量％である。
この焼結複合ターゲツト材の抗折力は９Kg／mm2
であり、耐熱衝撃性も良好であつた。実施例１と
同じスパツタリング条件のマグネトロンスパツタ
リングに用いたときのスパツタリング速度は4500
Å／min.であつた。
実施例 ５
平均粉径10μｍのTb−５重量％Tm合金粉末、
平均粒径10μｍのDy−５重量％Ho合金粉末及び
平均粒径200μｍのFeシヨツト（純度：99.99％）
を用意し、Tb合金粉末：20重量％、Dy合金粉
末：23重量％及びFeシヨツト：57重量％の配合
組成で配合し、以下、ホツトプレスモールド内径
を203mm、充填量を750ｇ及びホツトプレス温度を
600℃とすることを除いて、実施例１と同様に行
ない、配合組成と実質的に同じ組成を有し、かつ
第３図に示す組織、即ち、反応拡散層がTb合金
粒子やDy合金粒子とFe粒子との界面に存在し、
Tb合金粒子：Dy合金粒子：Fe粒子：反応拡散層
＝17容量％：17容量％：17容量％：17容量％：49
容量％の組織を有し、直径が203mmで厚さ４mmの
焼結複合ターゲツト材を得た。この焼結複合ター
ゲツト材の酸素含有量は0.24重量％である。
この焼結複合ターゲツト材の抗折力は10Kg／mm2
であり、耐熱衝撃性も良好であつた。実施例１と
同じスパツタリング条件のマグネトロンスパツタ
リングに用いたときのスパツタリング速度は5800
Å／min.であつた。
実施例 ６
原料粉末として、いずれも100μｍの平均粒径
を有するTb粉末（純度：99.9％）、Fe−Co合金
粉末（Co：25原子％含有）、およびFe粉末（純
度：99.99％）を用意し、これら原料粉末を、
Tb：48.5重量％、Fe−Co合金：27.64重量％、
Fe：23.86重量％の割合に配合し、高純度Arガス
雰囲気中で20分間乾式混合し、この混合粉末：
270ｇを、1.2mm厚のステンレス鋼板で成形され、
真空引きパイプを側面に有し、かつ内径：125mm
×深さ：４mm、すなわち外形：127.4mm×厚さ：
6.4mmの寸法を有する缶体の中に充填し、前記真
空引きパイプを通して、前記缶体内を１×
10-6torrの真空度まで真空引きし、真空封入を行
なつた後、この缶体に対して、２段圧延機を用
い、加熱温度：600℃、圧下率：７％の条件での
熱間圧延を繰り返し10回施して、その厚さを４mm
とし、ついで昇温速度：700℃／hr、加熱温度：
680℃、保持時間：10時間の条件で加熱し、冷却
した後、外側の缶材を旋盤にて除去することによ
つて、焼結複合ターゲツト材を製造した。
この結果得られた焼結複合ターゲツト材の金属
顕微鏡による組織（倍率：200倍）を第４図に示
したが、図示されるように、Tb粒子（黒い部分）
とFeまたはFe−Co合金粒子（白い部分）との界
面に金属間化合物からなる反応拡散層が形成され
ていることが明らかである。
また、この焼結複合ターゲツト材は、抗折力：
13Kg／mm2を示し、かつ実施例１におけると同一の
条件でのマグネトロンスパツタリングでは、4800
Å／minのスパツタリング速度を示した。
実施例 ７
原料粉末として、いずれも平均粒径が80μｍの
Tb粉末（純度：99.9％）およびFe粉末（純度：
99.99％）を用い、これら原料粉末を、Tb：48.68
重量％、Fe：51.32重量％の割合に配合し、かつ
熱間圧延に代つて、200ton鍛造機を用い、700℃
の温度で熱間鍛造を行ない、さらに加熱条件を、
昇温速度：700℃／hr、加熱温度：780℃、保持時
間：４時間とする以外は実施例７におけると同一
の条件で焼結複合ターゲツト材を製造した。
この結果得られた焼結複合ターゲツト材の金属
顕微鏡による組織（倍率：200倍）を第５図に示
したが、同様に、Tb粒子とFe粒子との界面には
反応拡散層が存在することが示されている。
また、この焼結複合ターゲツト材は、抗折力：
８Kg／mm2を示し、かつ実施例１におけると同一の
条件で、5200Å／minのスパツタリング速度を示
した。
実施例 ８
実施例１において、第１表に示す配合組成の配
合物を用いる他は、ほぼ同様にして、配合組成と
実質的に同じ組成であつて第１表記載の酸素含有
量を有し、かつ、希土類金属粒子と遷移金属粒子
との界面に第１表に示す含有量の反応拡散相が存
在する組織を有する焼結複合ターゲツト材（直径
127mm、厚さ５mm）を得た。
これらの焼結複合ターゲツト材の抗折力及び実
施例１と同じ条件でのマグネトロンスパツタリン
グにおけるスパツタリング速度を測定し、その結
果を第１表に示した。
〔発明の総括的効果〕
実施例１〜７及び第１表からわかるように、こ
の発明の焼結複合ターゲツト材は、抗折力が約７
〜20Kg／mm2と靭性が大きく、耐熱衝撃性も良好な
ので、取り扱い中やスパツタリングの熱衝撃によ
り割れることがない。そして、一体的に形成され
た物であり靭性も大きいので、回転や反転するこ
ともできるものである。又、この発明の焼結複合
ターゲツト材の酸素含有量は、0.3重量％以下で
あるので、この発明の焼結複合ターゲツト材を用
いてスパツタリングすれば、光磁気記録に好適な
垂直磁化膜を簡単に製造することができる。しか
も、その際に、スパツタリング速度が4000〜7000
Å／min.と、従来のターゲツト材に比べて２〜
７倍も大きいので、1/2〜1/7の短時間で所望の膜
厚の薄膜を製造することができるものであり、し
たがつて、この発明の焼結複合ターゲツト材は、
スパツタリング法の欠点であつた小さ
[Industrial Application Field] This invention relates to a sintered composite target material used in the production of thin films made of rare earth metals and transition metals (iron group metals) by sputtering, which have recently attracted attention as magneto-optical recording materials. . [Prior art] Conventional target materials containing rare earth metals and transition metals (iron group metals) for producing thin films for magneto-optical recording by sputtering include: (1) two types of metals are heated in a vacuum; Or an alloy target material with an oxygen content of 0.5 to 3.0% by weight (composition is rare earth metal) made by arc melting in an inert atmosphere.
30-50% by weight, transition metals 70-50% by weight), and
(2) There is a composite target material in which a rare earth metal chip is placed on a transition metal plate, or a similar target material in which a transition metal chip is placed on a rare earth metal plate. [Problems to be Solved by the Invention] However, the alloy target material in (1) above (a) has no toughness (resistance: 2 Kg/mm 2 or less), so it is easily broken and difficult to handle. (b) Because it has no thermal shock resistance, it often cracks due to thermal shock during sputtering. (c) Since the oxygen content in the target material is as high as 0.5 to 3.0% by weight, thin films obtained by sputtering using this alloy target material are difficult to form perpendicularly magnetized films necessary for magneto-optical recording. (d) The size of the target material depends on the size of the arc melting furnace, but at present it is at most 60 mm in diameter.
You can only get up to mm. (e) For example, magnetron sputtering using this target material (sputtering conditions are Ar
Partial pressure: 1×10 -2 torr, Output: 0.5A, 145V, Pre-sputtering time: 30 minutes, Substrate is slide glass, Distance between substrate and target: 70mm, Bias voltage: 0V, Substrate rotation: 10rpm) The sputtering speed is 1000-2000Å/min.
And slow. Above, there are problems (a) to (e). The composite target material mentioned in (2) above has the following problems: (a) It cannot be rotated or reversed, and it is difficult to use the target material in a uniformly distributed state. (b) Magnetic lines of force easily enter the board and are difficult to come out on the board surface. Also, the presence of chips on the plate surface makes the magnetic field non-uniform. (c) When using this target material, for example, in magnetron sputtering (the sputtering conditions are the same as those in (e) for the alloy target material in (1)), the sputtering speed is as slow as 1000 to 2000 Å/min. Above, there are problems (a) to (c). Therefore, the object of the present invention is to have high toughness and thermal shock resistance, not to break due to thermal shock during handling or sputtering, to be able to be rotated or turned over, and to have a low oxygen content for magneto-optical recording. It is an object of the present invention to provide a target material capable of forming a perpendicularly magnetized film suitable for use at a high sputtering speed. [Means for solving the problem] The present inventors previously filed an application for the following method for manufacturing a composite target material (Japanese Patent Application No. 219-227-1982).
issue). That is, a mixture of one or more types of rare earth metals, which are in the form of powders, small particles, and chips, and one or more types of transition metal powders is prepared in a vacuum or in an inert atmosphere. This manufacturing method is characterized by hot forming at a temperature below the eutectic point of the metal components present in the mixture. The present inventors conducted various studies to find that the sintered composite target material, which was obtained for the first time by this manufacturing method and has a structure in which a reaction-diffusion phase exists at the interface between rare earth metal particles and transition metal particles, achieves the above object. I found the result. This invention was invented based on the above knowledge, and includes rare earth metal particles selected from the group consisting of Tb, Gd, Dy, Ho, Tm, Er, and alloys thereof, and a rare earth metal constituting a reaction diffusion phase. One or more types: 30
~50%, transition metal particles selected from the group consisting of Fe, Co, Ni, and alloys thereof, one or more transition metals constituting the reaction diffusion phase, and unavoidable impurities: a composition consisting of the remainder (wt%) and a sintered composite target material characterized by having a structure in which a reaction-diffusion phase exists at the interface between rare earth metal particles and transition metal particles. The configuration of this invention will be explained below. (i) Composition Components and Unavoidable Impurities The sintered composite target material of the present invention has a composition consisting of one or more rare earth metals, one or more transition metals, and unavoidable impurities. The rare earth metals that are the compositional components of the sintered composite target material of this invention include Tb, Gd, Dy, Ho,
One or more types are selected from the group consisting of Tm, Er, and alloys thereof. These alloys are Tb,
It means an alloy consisting of two or more of Gd, Dy, Ho, Tm and Er. Further, as the transition metal that is a compositional component of the sintered composite target material of the present invention, one or more types are selected from the group consisting of Fe, Co, Ni, and alloys thereof. These alloys mean alloys consisting of two or more of Fe, Co, and Ni. Unavoidable impurities include Group 3a elements of the periodic table of elements, Si, Ca, Al, C, P, S,
Examples include Ta, Mn oxygen, etc. (ii) Composition The sintered composite target of this invention contains the rare earth metals mentioned in section (i), namely Tb, Gd, Dy, Ho,
one or more rare earth metals selected from the group consisting of Tm, Er, and alloys thereof, Fe,
It is used to form by sputtering a magneto-optical recording thin film composed of one or more transition metals selected from the group consisting of Co, Ni, and alloys thereof, and one of the rare earth metals. or more: Contains 30 to 50% by weight, with the remainder consisting of one or more of the transition metals and unavoidable impurities, but the rare earth metal contains 30% by weight
Even if it is less than 50% by weight or more than 50% by weight, the magnetization characteristics of the film obtained by sputtering using this sintered composite target material will not be perpendicular but will have in-plane magnetization characteristics, and the coercive force will also be small. Since the characteristics make it impossible for practical use, the rare earth metal content was set at 30 to 50% by weight. Next, due to the manufacturing method of raw materials, unavoidable impurities include Group 3a of the periodic table of elements, Si, Ca, and Al, respectively.
C, P and S each contain 0.1% by weight or less, and Ta and Mn each contain 0.3% by weight or less. (iii) Oxygen content The amount of oxygen contained as an unavoidable impurity in the sintered composite target material of the present invention is significantly reduced compared to conventional alloy target materials, and is 0.3% by weight or less. . Therefore, a film obtained by sputtering using the sintered composite target material of the present invention exhibits perpendicular magnetization characteristics necessary for magneto-optical recording. (iv) Structure The sintered composite target material of the present invention has a structure in which a reaction-diffusion phase exists at the interface between rare earth metal particles and transition metal particles, as shown in the micrograph of FIG. The reaction-diffusion phase may form a layer as shown in the micrograph of FIG. 3, or may exist in a dispersed (dotted) state without forming a layer. From the viewpoint of bonding strength, it is preferable that the reaction-diffusion phase (the phase produced by solid phase diffusion and reaction between the rare earth metal and the transition metal) exists in a layered form. The content ratio of this reaction-diffusion phase (however, the content ratio excluding voids) is preferably 0.2 to 80% by volume.
If the content is less than 0.2% by volume, the bonding force between the particles will be weak and they will be easily damaged during handling and processing, making handling and processing difficult or impossible.On the other hand, if the content exceeds 80% by volume, the toughness The reason for this is that the surface of the material decreases, and it becomes easily broken during handling, or that minute cracks or cracks form on the surface due to thermal shock during sputtering. More preferably, the content of the reaction-diffusion phase is 1 to 50% by volume. [Example] Hereinafter, the sintered composite target material of the present invention will be explained in detail with reference to Examples. Example 1 Tb powder with an average particle size of 100 μm (purity: 99.9%)
and Fe powder (purity 99.99%) and Tb powder:
49% by weight, Fe powder: 51% by weight, mixed in toluene for 30 minutes using a ball mill, then taken out and dried, filled with 160g in a hot press mold with an inner diameter of 127mm, and heated. speed
Raise the temperature at 800℃/hr. When it reaches 800℃, reduce the vacuum level.
Hot pressing was carried out under the conditions of 10 -3 torr, pressurization pressure of 400 Kg/cm 2 and holding time for 15 minutes, and after heating, the product was cooled in the furnace, and after being taken out, the surface was polished to have a composition substantially the same as the blended composition. , and the structure shown in Figure 1 a and b, that is, a reaction diffusion layer consisting of an intermetallic compound such as Tb 2 Fe with an average layer thickness of 1 μm exists at the interface between the Tb particles and the Fe particles, and It has a structure in which the Fe particles and the reaction diffusion layer are 44% by volume, 48% by volume, and 8% by volume, respectively, and the diameter is 127 mm and the thickness is
A 1.5 mm sintered composite target material was obtained. The oxygen content of this sintered composite target material is 0.1% by weight. It was confirmed by XMA line analysis that the reaction diffusion layer was composed of intermetallic compounds. The transverse rupture strength of this sintered composite target material is 13Kg/mm 2
The thermal shock resistance was also good. When this sintered composite target material was used for magnetron sputtering (the sputtering conditions were the same as those for problem (e) of the alloy target material in (1)), the sputtering rate was 5000 Å/min. Example 2 Fe powder with an average particle size of 20 μm (purity: 99.99%)
Co powder (purity: 99.99%) and Tb powder (purity: 99.9)
%) and Gd powder (purity: 99.9%), and
Powder: 39.4% by weight, Co powder: 36.4% by weight, Tb powder: 12.5% by weight, Gd powder: 11.7% by weight.
203mm, filling amount 770g and hot press temperature
It was carried out in the same manner as in Example 1 except that the temperature was 600°C, and the mixture had substantially the same composition as the blended composition, and
A reaction-diffusion layer with a layer thickness of 1 to 5 μm exists at the interface between Tb particles, Gd particles, Fe particles, and Co particles. Sintered composite target materials with a diameter of 203 mm and a thickness of 3 mm were obtained, each having a structure of 23% by volume, 12% by volume, 32% by volume, 28% by volume, and 5% by volume, respectively. The oxygen content of this sintered composite target material is 0.2% by weight. The transverse rupture strength of this sintered composite target material is 12Kg/mm 2
The thermal shock resistance was also good. When used for magnetron sputtering under the same sputtering conditions as in Example 1, the sputtering speed was 6200.
It was Å/min. Example 3 Average width 0.2mm x average thickness 0.05mm x average length 2mm
Prepare Tb pieces (purity: 99.9%) and Fe-5wt% Co alloy pieces, and mix them at a blending ratio of Tb pieces: 49wt% and Fe alloy pieces: 51wt%. Except that the temperature is 600℃,
The process was carried out in the same manner as in Example 1, and the composition was substantially the same as the blended composition, and the structure shown in FIG. 2 was obtained, that is, a reaction diffusion layer was formed at the interface between flaky Tb particles and flaky Fe alloy particles. A sintered composite target material having a diameter of 127 mm and a thickness of 2 mm was obtained, having a structure in which Tb particles, Fe alloy particles, and reaction diffusion layers were present at 21% by volume, 55% by volume, and 24% by volume, respectively. The oxygen content of this sintered composite target material is 0.01% by weight. The transverse rupture strength of this sintered composite target material is 17Kg/mm 2
The thermal shock resistance was also good. The sputtering speed when used for magnetron sputtering under the same sputtering conditions as in Example 1 was 4700.
It was Å/min. Example 4 Co powder (purity: 99.99%) with an average particle size of 100 μm is plated with Fe to an average layer thickness of 1 μm. The composition of the resulting powder was 97% by weight of Co and 3% by weight of Fe. Separately, Tb-20 wt% Ho alloy powder with an average particle size of 100 μm was prepared, Fe-metsuki Co powder: 58.4 wt%,
Tb alloy powder: Blend at a blending ratio of 41.6% by weight,
Below, the filling amount is 310g and the hot press temperature is 600g.
The process was carried out in the same manner as in Example 1, except that the temperature was set at Fe layer, Co particles and reaction diffusion layer are respectively 44 volume%, 2.8 volume%, 53 volume% and 0.2 volume%
It has a structure with a volume of %, a diameter of 127 mm and a thickness of 3
A sintered composite target material of mm was obtained. The oxygen content of this sintered composite target material is 0.18% by weight. The transverse rupture strength of this sintered composite target material is 9Kg/mm 2
The thermal shock resistance was also good. When used for magnetron sputtering under the same sputtering conditions as in Example 1, the sputtering speed was 4500.
It was Å/min. Example 5 Tb-5 wt% Tm alloy powder with an average powder diameter of 10 μm,
Dy-5wt% Ho alloy powder with an average particle size of 10 μm and Fe shot with an average particle size of 200 μm (purity: 99.99%)
were prepared and mixed with a composition of Tb alloy powder: 20% by weight, Dy alloy powder: 23% by weight, and Fe shot: 57% by weight, and the hot press mold inner diameter was 203 mm, the filling amount was 750 g, and the hot press temperature was set as follows.
The process was carried out in the same manner as in Example 1 except that the temperature was 600°C, and the composition was substantially the same as that of the blended composition, and the structure shown in Fig. 3, that is, the reaction diffusion layer was Tb alloy particles or Dy alloy particles. exists at the interface between and Fe particles,
Tb alloy particles: Dy alloy particles: Fe particles: Reaction diffusion layer = 17 volume%: 17 volume%: 17 volume%: 17 volume%: 49
A sintered composite target material having a structure of % by volume, a diameter of 203 mm and a thickness of 4 mm was obtained. The oxygen content of this sintered composite target material is 0.24% by weight. The transverse rupture strength of this sintered composite target material is 10Kg/mm 2
The thermal shock resistance was also good. When used for magnetron sputtering under the same sputtering conditions as in Example 1, the sputtering speed was 5800.
It was Å/min. Example 6 As raw material powders, Tb powder (purity: 99.9%), Fe-Co alloy powder (Co: 25 at% content), and Fe powder (purity: 99.99%) were prepared, all of which had an average particle size of 100 μm. Then, these raw material powders are
Tb: 48.5% by weight, Fe-Co alloy: 27.64% by weight,
Fe: 23.86% by weight, dry mixed in high purity Ar gas atmosphere for 20 minutes, this mixed powder:
270g is molded from a 1.2mm thick stainless steel plate,
Has a vacuum pipe on the side and inner diameter: 125mm
× Depth: 4mm, i.e. External size: 127.4mm × Thickness:
Fill a can with dimensions of 6.4 mm, pass through the vacuum pipe, and vacuum the inside of the can 1×.
After evacuation to a vacuum level of 10 -6 torr and vacuum sealing, the can was heated using a two-high rolling mill at a heating temperature of 600°C and a rolling reduction of 7%. Repeat rolling 10 times to reduce the thickness to 4mm.
Then, heating rate: 700℃/hr, heating temperature:
A sintered composite target material was produced by heating at 680° C. for a holding time of 10 hours, cooling, and then removing the outer can stock using a lathe. The structure of the resulting sintered composite target material as seen under a metallurgical microscope (magnification: 200x) is shown in Figure 4. As shown, Tb particles (black areas)
It is clear that a reaction diffusion layer consisting of an intermetallic compound is formed at the interface between the Fe or Fe-Co alloy particles (white part). Additionally, this sintered composite target material has transverse rupture strength:
13Kg/mm 2 and magnetron sputtering under the same conditions as in Example 1, 4800
The sputtering speed was Å/min. Example 7 As the raw material powder, the average particle size was 80 μm.
Tb powder (purity: 99.9%) and Fe powder (purity:
99.99%) and these raw powders, Tb: 48.68
Weight%, Fe: 51.32% by weight, and instead of hot rolling, a 200ton forging machine was used and the temperature was 700°C.
Hot forging is carried out at a temperature of
A sintered composite target material was produced under the same conditions as in Example 7 except that the temperature increase rate was 700°C/hr, the heating temperature was 780°C, and the holding time was 4 hours. Figure 5 shows the structure of the resulting sintered composite target material as seen with a metallurgical microscope (magnification: 200x), and similarly, a reaction diffusion layer exists at the interface between Tb particles and Fe particles. It is shown. Additionally, this sintered composite target material has transverse rupture strength:
8 Kg/mm 2 , and under the same conditions as in Example 1, a sputtering rate of 5200 Å/min. Example 8 In almost the same manner as in Example 1, except that a formulation having the formulation shown in Table 1 was used, a mixture having substantially the same composition as the formulation and having the oxygen content listed in Table 1 was used. and a sintered composite target material (with diameter
127 mm, thickness 5 mm) was obtained. The transverse rupture strength of these sintered composite target materials and the sputtering speed in magnetron sputtering under the same conditions as in Example 1 were measured, and the results are shown in Table 1. [Overall Effects of the Invention] As can be seen from Examples 1 to 7 and Table 1, the sintered composite target material of the present invention has a transverse rupture strength of approximately 7.
It has high toughness of ~20Kg/mm 2 and good thermal shock resistance, so it will not break due to thermal shock during handling or sputtering. Furthermore, since it is integrally formed and has great toughness, it can also be rotated and reversed. Furthermore, since the oxygen content of the sintered composite target material of this invention is 0.3% by weight or less, by sputtering using the sintered composite target material of this invention, a perpendicular magnetization film suitable for magneto-optical recording can be easily produced. can be manufactured. Moreover, at that time, the sputtering speed is 4000 to 7000.
Å/min. compared to conventional target materials.
Since it is 7 times larger, a thin film with a desired thickness can be produced in a short time of 1/2 to 1/7. Therefore, the sintered composite target material of the present invention is
The shortcoming of the sputtering method was the small size.
【表】【table】
【表】
な薄膜形成速度を大巾に改良することができるも
のである。その原因は明らかではないが、１つに
は、この発明の焼結複合ターゲツト材はもれ磁束
が広く、かつ大きいためとも考えられる。[Table] It is possible to greatly improve the thin film formation speed. The reason for this is not clear, but it is thought that one reason is that the sintered composite target material of the present invention has a wide and large leakage magnetic flux.
第１図のａは、この発明の焼結複合ターゲツト
材の金属組織を示す顕微鏡写真、第１図のｂは、
第１図のａの顕微鏡写真を説明するための一部拡
大模式図、第２図は、この発明の別の焼結複合タ
ーゲツト材の金属組織を示す顕微鏡写真、第３
図、第４図、および第５図は、それぞれこの発明
の更に別の焼結複合ターゲツト材の金属組織を示
す顕微鏡写真である。
Fig. 1a is a micrograph showing the metal structure of the sintered composite target material of the present invention, and Fig. 1b is a photomicrograph showing the metal structure of the sintered composite target material of this invention.
FIG. 1 is a partially enlarged schematic diagram for explaining the micrograph of a in FIG. 1, FIG.
4 and 5 are micrographs showing the metallographic structure of yet another sintered composite target material of the present invention.
Claims (1)
れらの合金からなる群より選ばれた希土類金属粒
子と反応拡散相を構成する希土類金属の１種以
上：30〜50％、 Fe、Co及びNi、並びにそれらの合金からなる
群より選ばれた遷移金属粒子と反応拡散相を構成
する遷移金属の１種以上と不可避不純物：残り、 からなる組成（以上、重量％）、及び、 希土類金属粒子と遷移金属粒子との界面に反応
拡散相が存在する組織、 を有することを特徴とする焼結複合ターゲツト
材。[Claims] 1. One or more rare earth metals constituting the reaction diffusion phase with rare earth metal particles selected from the group consisting of Tb, Gd, Dy, Ho, Tm, Er, and alloys thereof: 30 to 50 %, transition metal particles selected from the group consisting of Fe, Co, Ni, and alloys thereof, one or more transition metals constituting the reaction-diffusion phase, and unavoidable impurities: the remainder (in weight %) 1. A sintered composite target material comprising: , and a structure in which a reaction-diffusion phase exists at the interface between rare earth metal particles and transition metal particles.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24183184A JPS61119648A (en) | 1984-11-16 | 1984-11-16 | Sintered composite target material |
| US06/787,529 US4620872A (en) | 1984-10-18 | 1985-10-15 | Composite target material and process for producing the same |
| DE19853537191 DE3537191A1 (en) | 1984-10-18 | 1985-10-18 | COMPOSITE TARGET MATERIAL AND METHOD FOR THE PRODUCTION THEREOF |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24183184A JPS61119648A (en) | 1984-11-16 | 1984-11-16 | Sintered composite target material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61119648A JPS61119648A (en) | 1986-06-06 |
| JPH036218B2 true JPH036218B2 (en) | 1991-01-29 |
Family
ID=17080143
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24183184A Granted JPS61119648A (en) | 1984-10-18 | 1984-11-16 | Sintered composite target material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61119648A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20150037500A (en) * | 2013-09-30 | 2015-04-08 | 가부시키가이샤 스크린 홀딩스 | Structure for electronic device, plasma cvd apparatus and film forming method |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62256962A (en) * | 1986-04-30 | 1987-11-09 | Mitsubishi Metal Corp | Sputtering target material for forming photomagnetic decording medium |
| JPH0768612B2 (en) * | 1987-04-20 | 1995-07-26 | 日立金属株式会社 | Alloy powder for rare earth metal-iron group metal target, rare earth metal-iron group metal target, and methods for producing the same |
| JPS63274764A (en) * | 1987-04-30 | 1988-11-11 | Sumitomo Metal Mining Co Ltd | Alloy target for magneto-optical recording |
| JP2744991B2 (en) * | 1987-11-27 | 1998-04-28 | 松下電器産業株式会社 | Sputtering target |
| JP2988021B2 (en) * | 1991-06-12 | 1999-12-06 | 三菱マテリアル株式会社 | High strength target material for forming magneto-optical recording thin films with low magnetic permeability |
-
1984
- 1984-11-16 JP JP24183184A patent/JPS61119648A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20150037500A (en) * | 2013-09-30 | 2015-04-08 | 가부시키가이샤 스크린 홀딩스 | Structure for electronic device, plasma cvd apparatus and film forming method |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61119648A (en) | 1986-06-06 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |