JP6392776B2 - スパッタリングターゲット - Google Patents
スパッタリングターゲット Download PDFInfo
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- JP6392776B2 JP6392776B2 JP2015546588A JP2015546588A JP6392776B2 JP 6392776 B2 JP6392776 B2 JP 6392776B2 JP 2015546588 A JP2015546588 A JP 2015546588A JP 2015546588 A JP2015546588 A JP 2015546588A JP 6392776 B2 JP6392776 B2 JP 6392776B2
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- 238000005477 sputtering target Methods 0.000 title claims description 73
- 239000000843 powder Substances 0.000 claims description 83
- 239000002994 raw material Substances 0.000 claims description 41
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 21
- 238000004519 manufacturing process Methods 0.000 claims description 17
- 238000004090 dissolution Methods 0.000 claims description 16
- 229910052733 gallium Inorganic materials 0.000 claims description 13
- 229910052725 zinc Inorganic materials 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims 1
- 238000007654 immersion Methods 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 45
- 239000011812 mixed powder Substances 0.000 description 37
- 238000000034 method Methods 0.000 description 29
- 239000002002 slurry Substances 0.000 description 26
- 238000002156 mixing Methods 0.000 description 24
- 239000010408 film Substances 0.000 description 21
- 238000004544 sputter deposition Methods 0.000 description 19
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 17
- 229910003437 indium oxide Inorganic materials 0.000 description 17
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 17
- 229910001195 gallium oxide Inorganic materials 0.000 description 16
- 239000011230 binding agent Substances 0.000 description 14
- 239000011787 zinc oxide Substances 0.000 description 14
- 229910052738 indium Inorganic materials 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 239000011701 zinc Substances 0.000 description 12
- 150000001875 compounds Chemical class 0.000 description 10
- 239000002612 dispersion medium Substances 0.000 description 10
- 239000006259 organic additive Substances 0.000 description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 239000002270 dispersing agent Substances 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000010304 firing Methods 0.000 description 6
- 229920005646 polycarboxylate Polymers 0.000 description 6
- 238000001694 spray drying Methods 0.000 description 6
- 239000000470 constituent Substances 0.000 description 5
- 238000007569 slipcasting Methods 0.000 description 5
- 239000000839 emulsion Substances 0.000 description 4
- 229910052602 gypsum Inorganic materials 0.000 description 4
- 239000010440 gypsum Substances 0.000 description 4
- 239000013077 target material Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000002159 abnormal effect Effects 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 238000007580 dry-mixing Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 229910007541 Zn O Inorganic materials 0.000 description 1
- 239000006061 abrasive grain Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 239000003232 water-soluble binding agent Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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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
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- 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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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
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- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
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- C04B2235/81—Materials characterised by the absence of phases other than the main phase, i.e. single phase materials
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- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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Description
<スパッタリングターゲットの製造方法>
本発明のスパッタリングターゲットは、たとえば、該ターゲットの製造に必要な複数の原料粉末である酸化インジウム(In2O3)粉末、酸化ガリウム(Ga2O3)粉末、酸化亜鉛(ZnO)粉末、IGZO粉末を混合し、得られた混合原料を成形して成形体を作製し、該成形体を焼成して製造することができる。
工程1では、原料粉末から成形体を作製する。
スリップキャスト方法では、前記混合粉末および有機添加物を含有するスラリーを調製し、このスラリーを型に流し込み、次いで排水して成形する。
スラリーを噴霧乾燥する方法では、前記混合粉末および有機添加物を含有するスラリーを調製し、この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する。
工程2では、工程1で得られた成形体を焼成し、焼成体を作製する。焼成炉には特に制限はなく、セラミックスターゲット材の製造に従来使用されている焼成炉を使用することができる。
工程3では、工程2で得られた焼成体を切削加工し、スパッタリングターゲットを作製する。加工は、平面研削盤等を用いて行う。加工後の表面粗度Raは、砥石の砥粒の大きさを選定することにより制御することができる。
1.相対密度
スパッタリングターゲットの相対密度はアルキメデス法に基づき測定した。具体的には、スパッタリングターゲットの空中重量を体積(スパッタリングターゲットの水中重量/計測温度における水比重)で除し、下記式(X)に基づく理論密度ρ文字(g/cm3)に対する百分率の値を相対密度(単位:%)とした。
2.溶解残渣
スパッタリングターゲットを3cm角以下に破砕した試料4kgを、80℃の28質量%塩酸10kgに、温度を80℃に保持し、撹拌しながら24時間浸漬した。24時間浸漬した時点で試料の溶解は進行していないことを確認した。得られた残渣含有液をろ過して、溶解残渣を回収し、100℃で24時間乾燥して、その質量を測定した。浸漬した試料の質量に対する溶解残渣の質量の比率(溶解残渣の質量比(%))を求めた。
3.原料粉末のメジアン径(D50)
原料粉末のメジアン径(D50)は日機装株式会社製レーザー回折・散乱式粒度分布測定装置(HRA9320-X100)を用いて測定した。溶媒は水を使用し、測定物質の屈折率2.20で測定した。
4.ノジュール量
スパッタリングターゲットをCu製の基材に、低融点半田としてインジウムを使用して接合し、下記条件でスパッタを行った。
装置:DCマグネトロンスパッタ装置、排気系クライオポンプ、ロータリーポンプ
到達真空度:3×10-4Pa
スパッタ圧力:0.4Pa
酸素分圧:4×10-2Pa
スパッタ後のターゲットの表面を写真撮影し、画像解析により、ターゲット表面の面積に対するターゲット表面におけるノジュールの面積の比率(%)をノジュール量とした。また、このノジュール量を面積比率の少ない方から下記のA〜Dの判定基準で評価した。
B:3%以上6%未満
C:6%以上9%未満
D:9%以上
ノジュール量が少ないほど好適なスパッタリング膜が形成出来ていると評価できる。AまたはB判定となったターゲットはノジュール量が少なく、生成された膜の大面積での均一性、膜質、導電率、透光性等の膜特性が良好となる。従って、AまたはB判定となったターゲットであれば従来よりも歩留り良く、効率的に酸化物半導体膜を得ることができるといえる。
[実施例1]
メジアン径(D50)が0.8μmである酸化亜鉛粉末と、メジアン径(D50)が0.6μmである酸化インジウム粉末と、メジアン径(D50)が2μmである酸化ガリウム粉末とをポット中でジルコニアボールによりボールミル乾式混合して、混合粉末を調製した。混合粉末における酸化インジウム粉末の含有量は44.2質量%、酸化亜鉛粉末の含有量は25.9質量%、酸化ガリウム粉末の含有量は29.9質量%であった。この配合比により、実質的に溶解残渣以外の部分の組成がInGaZnO4である単相構造のスパッタリングターゲットが得られる。
[実施例2]
実施例1と同様に乾式混合して混合粉末を調製した。
[実施例3]
実施例2と同様にして乾燥粉末を得た。
[実施例4]
メジアン径(D50)が3.2μmである酸化亜鉛粉末と、メジアン径(D50)が2.5μmである酸化インジウム粉末と、メジアン径(D50)が4.5μmである酸化ガリウム粉末とをポット中でジルコニアボールによりボールミル乾式混合して、混合粉末を調製した。混合粉末における酸化インジウム粉末の含有量は44.2質量%、酸化亜鉛粉末の含有量は25.9質量%、酸化ガリウム粉末の含有量は29.9質量%であった。この配合比により、実質的に溶解残渣以外の部分の組成がInGaZnO4である単相構造のスパッタリングターゲットが得られる。
[比較例1]
実施例1と同様に乾式混合して混合粉末を調製した。
[比較例2]
メジアン径(D50)が7.2μmである酸化亜鉛粉末と、メジアン径(D50)が8.5μmである酸化インジウム粉末と、メジアン径(D50)が7.5μmである酸化ガリウム粉末とをポット中でジルコニアボールによりボールミル乾式混合して、混合粉末を調製した。混合粉末における酸化インジウム粉末の含有量は44.2質量%、酸化亜鉛粉末の含有量は25.9質量%、酸化ガリウム粉末の含有量は29.9質量%であった。
[比較例3]
メジアン径(D50)が0.8μmである酸化亜鉛粉末と、メジアン径(D50)が0.6μmである酸化インジウム粉末と、メジアン径(D50)が4.5μmである酸化ガリウム粉末とをポット中でジルコニアボールによりボールミル乾式混合して、混合粉末を調製した。混合粉末における酸化インジウム粉末の含有量は44.2質量%、酸化亜鉛粉末の含有量は25.9質量%、酸化ガリウム粉末の含有量は29.9質量%であった。
Claims (5)
- In、GaおよびZnの酸化物からなるスパッタリングターゲットであって、80℃の28質量%塩酸に、該塩酸に対し40質量%の量の前記スパッタリングターゲットを24時間浸漬したときに得られる溶解残渣であるGa 2 ZnO 4 およびInGaO 3 の、前記浸漬したスパッタリングターゲットに対する質量比が0.5質量%以下であり、
相対密度が99.7%以上であるスパッタリングターゲット。 - 前記溶解残渣以外の部分が単相構造である請求項1に記載のスパッタリングターゲット。
- 前記溶解残渣以外の部分の組成がInGaZnO4である請求項1または2に記載のスパッタリングターゲット。
- 請求項1に記載のスパッタリングターゲットの製造原料である複数の原料粉末の混合を湿式で行い、得られた混合原料を成形して成形体を作製し、該成形体を焼成する、請求項1〜3のいずれかに記載のスパッタリングターゲットの製造方法。
- 前記複数の原料粉末のメジアン径(D50)が5μm以下であり、さらに前記各原料粉末相互のメジアン径(D50)の差が2μm以下である請求項4に記載のスパッタリングターゲットの製造方法。
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