JP5285149B2 - ZnO−Ga2O3系スパッタリングターゲット用焼結体及びその製造方法 - Google Patents
ZnO−Ga2O3系スパッタリングターゲット用焼結体及びその製造方法 Download PDFInfo
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- JP5285149B2 JP5285149B2 JP2011511309A JP2011511309A JP5285149B2 JP 5285149 B2 JP5285149 B2 JP 5285149B2 JP 2011511309 A JP2011511309 A JP 2011511309A JP 2011511309 A JP2011511309 A JP 2011511309A JP 5285149 B2 JP5285149 B2 JP 5285149B2
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- 238000005477 sputtering target Methods 0.000 title claims description 23
- 238000004519 manufacturing process Methods 0.000 title claims description 21
- 229910007674 ZnO—Ga2O3 Inorganic materials 0.000 title 1
- 238000005245 sintering Methods 0.000 claims description 75
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 56
- 239000001301 oxygen Substances 0.000 claims description 56
- 229910052760 oxygen Inorganic materials 0.000 claims description 56
- 239000000843 powder Substances 0.000 claims description 27
- 239000002245 particle Substances 0.000 claims description 26
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 claims description 17
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 claims description 17
- 239000011812 mixed powder Substances 0.000 claims description 17
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 15
- 229910001195 gallium oxide Inorganic materials 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 15
- 238000009826 distribution Methods 0.000 claims description 12
- 238000000465 moulding Methods 0.000 claims description 5
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 2
- 229910001882 dioxygen Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 description 26
- 238000004544 sputter deposition Methods 0.000 description 19
- 238000011156 evaluation Methods 0.000 description 13
- 238000012360 testing method Methods 0.000 description 11
- 239000002994 raw material Substances 0.000 description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000012545 processing Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 206010021143 Hypoxia Diseases 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000009694 cold isostatic pressing Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Description
これにより、ノジュールやフレークの発生を抑制できるGZOスパッタリングターゲットを提供することができる。また、抵抗率が2×10−3Ω・cm以下と非常に小さいため、低抵抗のGZO薄膜を成膜することが可能となる。
原料粉末としては、酸化亜鉛(ZnO)粉末と、酸化ガリウム(Ga2O3)粉末とが用いられる。酸化亜鉛粉末の平均粒径は1μm以下であり、酸化ガリウム粉末の平均粒径は1.5μm以下であるが、粒径はこれらに限られない。混合工程ST1では、これら原料粉末の混合粉末が作製される。
次に、得られた混合粉末を所定形状に成形する工程が行われる(ST2)。混合粉末の成形は、冷間プレス、冷間静水圧プレス(CIP)などの冷間成形法を用いることができる。成形圧力は特に限定されず、例えば1トン/cm2以上である。形状も特に限定されず、板状、ブロック状など適宜の形状に成形される。
続いて、得られた成形体を焼結する工程が行われる(ST3)。焼結工程において、成形体は、焼結炉の中に設置された容器の中に収容され、当該容器の内部で焼結される。図2は、焼結炉の概略構成を示す断面図である。
焼結体S2の作製後、所望のターゲットサイズに機械加工される(ST4)。加工形状は、典型的には矩形状あるいは円形状であるが、勿論これに限られない。
酸化亜鉛(ZnO)粉末および酸化ガリウム(Ga2O3)粉末を原料粉末とし、それぞれを重量比99.4:0.6の割合で混合した。酸化亜鉛粉末の平均粒径は0.1μm、酸化ガリウム粉末の平均粒径は1.3μmとした。これらの原料粉末を樹脂製ポットに入れ、湿式ボールミル混合法を用いて混合粉末を作製した。ここで、ボールミルのボールにはジルコニアボールを、バインダーにはポリアクリルアミド系(2重量%)を用い、混合時間は24時間とした。混合後、スラリーを取り出し、乾燥、造粒した。
焼結保持時間を4時間としたほかは、実施例1と同様の条件で焼結体を作製した。得られた焼結体の抵抗率は1.24×10−3Ω・cm、相対密度は99.8%、平均粒径は33μmであった。当該焼結体でターゲットを作製し、実施例1と同様なスパッタ試験を行った。評価結果を図4に示す。
焼結保持時間を2時間としたほかは、実施例1と同様の条件で焼結体を作製した。得られた焼結体の抵抗率は1.39×10−3Ω・cm、相対密度は99.6%、平均粒径は34μmであった。当該焼結体でターゲットを作製し、実施例1と同様なスパッタ試験を行った。評価結果を図4に示す。
焼結温度を1300℃としたほかは、実施例1と同様の条件で焼結体を作製した。得られた焼結体の抵抗率は1.84×10−3Ω・cm、相対密度は99.4%、平均粒径は13μmであった。当該焼結体でターゲットを作製し、実施例1と同様なスパッタ試験を行った。評価結果を図4に示す。
酸素導入量を10L/分としたほかは、実施例1と同様の条件で焼結体を作製した。得られた焼結体の抵抗率は1.14×10−3Ω・cm、相対密度は99.8%、平均粒径は35μmであった。当該焼結体でターゲットを作製し、実施例1と同様なスパッタ試験を行った。評価結果を図4に示す。
酸素導入量を5L/分としたほかは、実施例1と同様の条件で焼結体を作製した。得られた焼結体の抵抗率は1.07×10−3Ω・cm、相対密度は99.9%、平均粒径は38μmであった。当該焼結体でターゲットを作製し、実施例1と同様なスパッタ試験を行った。評価結果を図4に示す。
酸素導入量を1L/分としたほかは、実施例1と同様の条件で焼結体を作製した。得られた焼結体の抵抗率は0.96×10−3Ω・cm、相対密度は99.7%、平均粒径は30μmであった。当該焼結体でターゲットを作製し、実施例1と同様なスパッタ試験を行った。評価結果を図4に示す。
焼結温度を1500℃、保持時間を2時間としたほかは、実施例1と同様の条件で焼結体を作製した。得られた焼結体の抵抗率は1.32×10−3Ω・cm、相対密度は98.4%、平均粒径は50μmであった。当該焼結体でターゲットを作製し、実施例1と同様なスパッタ試験を行った。評価結果を図4に示す。
焼結温度を1550℃、保持時間を2時間としたほかは、実施例1と同様の条件で焼結体を作製した。得られた焼結体の抵抗率は1.28×10−3Ω・cm、相対密度は97.8%、平均粒径は72μmであった。当該焼結体でターゲットを作製し、実施例1と同様なスパッタ試験を行った。評価結果を図4に示す。
焼結温度を1200℃、酸素導入量を10L/分、保持時間を16時間としたほかは、実施例1と同様の条件で焼結体を作製した。得られた焼結体の抵抗率は1.9×10−3Ω・cm、相対密度は99.5%、平均粒径は5μmであった。当該焼結体でターゲットを作製し、実施例1と同様なスパッタ試験を行った。評価結果を図4に示す。
図2及び図3に示した気密性の容器を使用せず、焼結温度を1400℃、酸素導入量を30L/分としたほかは、実施例1と同様の条件で焼結体を作製した。得られた焼結体の抵抗率は2.03×10−3Ω・cm、相対密度は99.2%、平均粒径は60μmであった。当該焼結体でターゲットを作製し、実施例1と同様なスパッタ試験を行った。評価結果を図4に示す。
ZnO:Ga2O3の重量比を95:5にし、焼結温度1500℃としたほかは、実施例1と同様の条件で焼結体を作製した。得られた焼結体の抵抗率は数MΩ・cm、相対密度は81.6%、平均粒径は2μmであった。当該焼結体でターゲットを作製し、実施例1と同様なスパッタ試験を行った。評価結果を図4に示す。
11…炉本体
12…ヒータ
20…容器
31…配管
S1…成形体
S2…焼結体
Claims (5)
- 酸化亜鉛粉末と酸化ガリウム粉末との混合粉末を成形し、
第1の孔及び第2の孔を有し、焼結炉内に設置される容器の中に前記混合粉末の成形体を収容し、
前記第1の孔を通じて前記容器の内部に導入された酸素を前記第2の孔に排気して、前記容器内を酸素ガス雰囲気に維持しながら前記成形体を1200℃以上1500℃以下の焼結温度に昇温させ、
前記容器の内部に酸素が導入された状態で前記焼結温度を保持し、
前記容器の内部への酸素の導入が停止された状態で炉内を降温させて焼結体を還元する
ZnO−Ga2O3系スパッタリングターゲット用焼結体の製造方法。 - 請求項1に記載のZnO−Ga2O3系スパッタリングターゲット用焼結体の製造方法であって、
前記容器の内部に導入される酸素の流量は、20L/分以下である
ZnO−Ga2O3系スパッタリングターゲット用焼結体の製造方法。 - 請求項1に記載のZnO−Ga2O3系スパッタリングターゲット用焼結体の製造方法であって、
前記酸化ガリウム粉末の混合比は、2重量%以下である
ZnO−Ga2O3系スパッタリングターゲット用焼結体の製造方法。 - 請求項1に記載のZnO−Ga2O3系スパッタリングターゲット用焼結体の製造方法であって、
前記容器は前記焼結炉内に複数設置されており、前記複数の容器の各々に収容された前記成形体を同時に焼結する
ZnO−Ga2O3系スパッタリングターゲット用焼結体の製造方法。 - 酸化亜鉛粉末と酸化ガリウム粉末との混合粉末の焼結体からなり、
98%以上の相対密度と、
50μm以下の平均粒子径と、
2×10−3Ω・cm以下の抵抗率とを有し、
前記焼結体の面内方向及び深さ方向における抵抗率の分布がそれぞれ20%以下である
ZnO−Ga2O3系スパッタリングターゲット用焼結体。
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JPH0625838A (ja) * | 1992-07-10 | 1994-02-01 | Asahi Glass Co Ltd | スパッタリングターゲット |
JPH10297962A (ja) * | 1997-04-28 | 1998-11-10 | Sumitomo Metal Mining Co Ltd | スパッタリングターゲット用ZnO−Ga2O3系焼結体およびその製造方法 |
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