JPWO2019202753A1 - 酸化物焼結体、スパッタリングターゲットおよび酸化物薄膜の製造方法 - Google Patents
酸化物焼結体、スパッタリングターゲットおよび酸化物薄膜の製造方法 Download PDFInfo
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- 238000005477 sputtering target Methods 0.000 title claims description 67
- 238000004544 sputter deposition Methods 0.000 title claims description 27
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 239000010409 thin film Substances 0.000 title claims description 11
- 239000011701 zinc Substances 0.000 claims abstract description 50
- 239000013078 crystal Substances 0.000 claims abstract description 35
- 229910052738 indium Inorganic materials 0.000 claims abstract description 11
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 8
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 7
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000002441 X-ray diffraction Methods 0.000 claims description 14
- 238000005452 bending Methods 0.000 claims description 10
- 230000003746 surface roughness Effects 0.000 claims description 7
- 239000010408 film Substances 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims 1
- 239000000843 powder Substances 0.000 description 31
- 239000002245 particle Substances 0.000 description 25
- 238000000034 method Methods 0.000 description 21
- 239000002994 raw material Substances 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 18
- 239000011812 mixed powder Substances 0.000 description 15
- 230000002159 abnormal effect Effects 0.000 description 12
- 239000002002 slurry Substances 0.000 description 12
- 238000005259 measurement Methods 0.000 description 11
- 238000010304 firing Methods 0.000 description 10
- 239000002612 dispersion medium Substances 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 7
- 238000009826 distribution Methods 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000006259 organic additive Substances 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 238000009694 cold isostatic pressing Methods 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 5
- 238000007580 dry-mixing Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004299 exfoliation Methods 0.000 description 2
- 238000003702 image correction Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000007569 slipcasting Methods 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NAWXUBYGYWOOIX-SFHVURJKSA-N (2s)-2-[[4-[2-(2,4-diaminoquinazolin-6-yl)ethyl]benzoyl]amino]-4-methylidenepentanedioic acid Chemical compound C1=CC2=NC(N)=NC(N)=C2C=C1CCC1=CC=C(C(=O)N[C@@H](CC(=C)C(O)=O)C(O)=O)C=C1 NAWXUBYGYWOOIX-SFHVURJKSA-N 0.000 description 1
- 238000007088 Archimedes method Methods 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000006061 abrasive grain Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910001651 emery Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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Abstract
Description
0.01≦In/(In+Ga+Zn)<0.20 ・・(1)
0.10≦Ga/(In+Ga+Zn)≦0.49 ・・(2)
0.50≦Zn/(In+Ga+Zn)≦0.89 ・・(3)
0.01≦In/(In+Ga+Zn)<0.20 ・・(1)
0.10≦Ga/(In+Ga+Zn)≦0.49 ・・(2)
0.50≦Zn/(In+Ga+Zn)≦0.89 ・・(3)
0.05≦In/(In+Ga+Zn)≦0.15 ・・(4)
0.15≦Ga/(In+Ga+Zn)≦0.45 ・・(5)
0.50≦Zn/(In+Ga+Zn)≦0.80 ・・(6)
各元素の原子比が、以下の式(7)〜(9)を満たすことがより好ましい。
0.05≦In/(In+Ga+Zn)≦0.15 ・・(7)
0.20≦Ga/(In+Ga+Zn)≦0.40 ・・(8)
0.50≦Zn/(In+Ga+Zn)≦0.70 ・・(9)
A.24.5°〜26.0°
B.31.0°〜32.5°
C.32.5°〜33.2°
D.33.2°〜34.0°
E.34.5°〜35.7°
F.35.7°〜37.0°
G.38.0°〜39.2°
H.39.2°〜40.5°
I.43.0°〜45.0°
J.46.5°〜48.5°
K.55.5°〜57.8°
L.57.8°〜59.5°
M.59.5°〜61.5°
N.65.5°〜68.0°
O.68.0°〜69.0°
P.69.0°〜70.0°
実施形態の酸化物スパッタリングターゲットは、たとえば以下に示すような方法により製造することができる。まず、原料粉末を混合する。原料粉末としては、通常In2O3粉末、Ga2O3粉末およびZnO粉末である。
ここで説明するスリップキャスト法では、混合粉末と有機添加物とを含有するスラリーを、分散媒を用いて調製し、かかるスラリーを型に流し込んで分散媒を除去することにより成形を行う。ここで用いることができる有機添加物は、公知のバインダーや分散剤などである。
ここで説明するCIP法では、混合粉末と有機添加物とを含有するスラリーを、分散媒を用いて調製し、かかるスラリーを噴霧乾燥して得られた乾燥粉末を型に充填して加圧成形を行う。ここで用いることができる有機添加物は、公知のバインダーや分散剤などである。
平均粒径が0.6μmであるIn2O3粉末と、平均粒径が1.5μmであるGa2O3粉末と、平均粒径が0.8μmであるZnO粉末とを株式会社アーステクニカ製のハイスピードミキサで乾式混合して、混合粉末を調製した。
実施例1と同様な方法を用いて、スパッタリングターゲットを得た。なお、実施例2〜3では、混合粉末の調製の際、すべての原料粉末に含まれる金属元素の原子比が、表1に記載の原子比となるように各原料粉末を配合した。
比較例1〜3では、混合粉末の調製の際、すべての原料粉末に含まれる金属元素の原子比がIn/(In+Ga+Zn)=0.1、Ga/(In+Ga+Zn)=0.3、Zn/(In+Ga+Zn)=0.6となるように各原料粉末を配合した。なお、焼成温度は表1に記載の温度となる様にし、また比較例2では乾式混合を行わなかった。それ以外は実施例1と同様な方法を用いて、スパッタリングターゲットを得た。
ρ={(C1/100)/ρ1+(C2/100)/ρ2+(C3/100)/ρ3}−1 ・・(10)
・C1:酸化物焼結体の製造に用いたIn2O3粉末の質量%
・ρ1:In2O3の密度(7.18g/cm3)
・C2:酸化物焼結体の製造に用いたGa2O3粉末の質量%
・ρ2:Ga2O3の密度(5.95g/cm3)
・C3:酸化物焼結体の製造に用いたZnO粉末の質量%
・ρ3:ZnOの密度(5.60g/cm3)
・装置:SmartLab(株式会社リガク製、登録商標)
・線源:CuKα線
・管電圧:40kV
・管電流:30mA
・スキャン速度:5deg/min
・ステップ:0.02deg
・スキャン範囲:2θ=20度〜70度
A.24.5°〜26.0°
B.31.0°〜32.5°
C.32.5°〜33.2°
D.33.2°〜34.0°
E.34.5°〜35.7°
F.35.7°〜37.0°
G.38.0°〜39.2°
H.39.2°〜40.5°
I.43.0°〜45.0°
J.46.5°〜48.5°
K.55.5°〜57.8°
L.57.8°〜59.5°
M.59.5°〜61.5°
N.65.5°〜68.0°
O.68.0°〜69.0°
P.69.0°〜70.0°
ΔE*=((ΔL)2+(Δa)2+(Δb)2)1/2 ・・(11)
(アーキング評価)
A:非常に少ない。
B:多い。
C:非常に多い。
Claims (11)
- インジウム、ガリウムおよび亜鉛を、以下の式(1)〜(3)を満たす比率で含む酸化物焼結体であって、
単相の結晶相で構成され、
前記結晶相の平均粒径が15.0μm以下である酸化物焼結体。
0.01≦In/(In+Ga+Zn)<0.20 ・・(1)
0.10≦Ga/(In+Ga+Zn)≦0.49 ・・(2)
0.50≦Zn/(In+Ga+Zn)≦0.89 ・・(3) - インジウム、ガリウムおよび亜鉛を、以下の式(4)〜(6)を満たす比率で含む請求項1に記載の酸化物焼結体。
0.05≦In/(In+Ga+Zn)≦0.15 ・・(4)
0.15≦Ga/(In+Ga+Zn)≦0.45 ・・(5)
0.50≦Zn/(In+Ga+Zn)≦0.80 ・・(6) - インジウム、ガリウムおよび亜鉛を、以下の式(7)〜(9)を満たす比率で含む請求項1または2に記載の酸化物焼結体。
0.05≦In/(In+Ga+Zn)≦0.15 ・・(7)
0.20≦Ga/(In+Ga+Zn)≦0.40 ・・(8)
0.50≦Zn/(In+Ga+Zn)≦0.70 ・・(9) - 前記結晶相は、X線回折測定(CuKα線)により得られるチャートにおいて、以下のA〜Pの領域に回折ピークが観測される請求項1〜3のいずれか一つに記載の酸化物焼結体。
A.24.5°〜26.0°
B.31.0°〜32.5°
C.32.5°〜33.2°
D.33.2°〜34.0°
E.34.5°〜35.7°
F.35.7°〜37.0°
G.38.0°〜39.2°
H.39.2°〜40.5°
I.43.0°〜45.0°
J.46.5°〜48.5°
K.55.5°〜57.8°
L.57.8°〜59.5°
M.59.5°〜61.5°
N.65.5°〜68.0°
O.68.0°〜69.0°
P.69.0°〜70.0° - 相対密度が97.0%以上である
請求項1〜4のいずれか一つに記載の酸化物焼結体。 - 抗折強度が40MPa以上である
請求項1〜5のいずれか一つに記載の酸化物焼結体。 - 比抵抗が40mΩcm以下である
請求項1〜6のいずれか一つに記載の酸化物焼結体。 - 請求項1〜7のいずれか一つに記載の酸化物焼結体からなるスパッタリングターゲット。
- 表面粗さの最大高さRyが15.0μm以下である
請求項8に記載のスパッタリングターゲット。 - 色差ΔE*が10以下である
請求項8または9に記載のスパッタリングターゲット。 - 請求項8〜10のいずれか一つに記載のスパッタリングターゲットをスパッタリングして成膜する、酸化物薄膜の製造方法。
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