JP6634371B2 - MgO系セラミックス膜、半導体製造装置用部材及びMgO系セラミックス膜の製法 - Google Patents
MgO系セラミックス膜、半導体製造装置用部材及びMgO系セラミックス膜の製法 Download PDFInfo
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- JP6634371B2 JP6634371B2 JP2016531233A JP2016531233A JP6634371B2 JP 6634371 B2 JP6634371 B2 JP 6634371B2 JP 2016531233 A JP2016531233 A JP 2016531233A JP 2016531233 A JP2016531233 A JP 2016531233A JP 6634371 B2 JP6634371 B2 JP 6634371B2
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- 239000000919 ceramic Substances 0.000 title claims description 39
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 239000004065 semiconductor Substances 0.000 title claims description 12
- 238000007751 thermal spraying Methods 0.000 claims description 46
- 229910020068 MgAl Inorganic materials 0.000 claims description 26
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 25
- 239000000463 material Substances 0.000 claims description 25
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 20
- 238000005259 measurement Methods 0.000 claims description 19
- 239000013078 crystal Substances 0.000 claims description 16
- 239000000758 substrate Substances 0.000 claims description 11
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- 238000005260 corrosion Methods 0.000 description 31
- 230000007797 corrosion Effects 0.000 description 31
- 239000002994 raw material Substances 0.000 description 29
- 238000000034 method Methods 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 239000002245 particle Substances 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- 238000005530 etching Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- SXAMGRAIZSSWIH-UHFFFAOYSA-N 2-[3-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,2,4-oxadiazol-5-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NOC(=N1)CC(=O)N1CC2=C(CC1)NN=N2 SXAMGRAIZSSWIH-UHFFFAOYSA-N 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 230000004580 weight loss Effects 0.000 description 6
- WZFUQSJFWNHZHM-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 WZFUQSJFWNHZHM-UHFFFAOYSA-N 0.000 description 5
- 239000008187 granular material Substances 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- 238000005507 spraying Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- ZRPAUEVGEGEPFQ-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]pyrazol-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C=1C=NN(C=1)CC(=O)N1CC2=C(CC1)NN=N2 ZRPAUEVGEGEPFQ-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000004453 electron probe microanalysis Methods 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 239000006104 solid solution Substances 0.000 description 3
- 229910052596 spinel Inorganic materials 0.000 description 3
- 239000011029 spinel Substances 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 239000000126 substance 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
- 239000004677 Nylon Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- UAMZXLIURMNTHD-UHFFFAOYSA-N dialuminum;magnesium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Mg+2].[Al+3].[Al+3] UAMZXLIURMNTHD-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 210000003739 neck Anatomy 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- YJLUBHOZZTYQIP-UHFFFAOYSA-N 2-[5-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NN=C(O1)CC(=O)N1CC2=C(CC1)NN=N2 YJLUBHOZZTYQIP-UHFFFAOYSA-N 0.000 description 1
- 238000007088 Archimedes method Methods 0.000 description 1
- 238000012935 Averaging Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
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- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/3065—Plasma etching; Reactive-ion etching
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
- C23C4/11—Oxides
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- 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
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
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- C23C4/129—Flame spraying
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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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
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- H01L21/48—Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
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- H01L2924/0543—13th Group
- H01L2924/05432—Al2O3
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Description
(溶射用原料の作製)
実験例1〜7の溶射用原料は、以下の方法で作製した。まず、MgO原料(純度99.9質量%以上、粒度(D50)3μm以下)、Al2O3原料(純度99.9質量%以上、粒度(D50)1μm以下)を表1に示す質量%となるように秤量し、粉末30質量%、水70質量%、また粉末に対し1質量%の分散剤(ユケン工業製セランダー)となるように水と分散剤を加えた。玉石を直径20mmの鉄芯入ナイロンボールとして、ナイロン製のポットでこれらを湿式混合した。混合後したスラリーを、スプレードライヤーを用いて噴霧し、顆粒を作製した。このような顆粒を「SD顆粒」と称する。その後、大気雰囲気1600℃で熱処理した。得られた熱処理粉末を目開き75μmの篩で振動篩を行い、篩下に得られた原料を溶射用原料とした。
1)XRD測定
X線回折装置により結晶相を同定した。測定条件はCuKα、40kV、40mA、2θ=10−70°とし、封入管式X線回折装置(ブルカー・エイエックスエス製 D8 ADVANCE)を使用した。測定のステップ幅は0.02°とし、ピークトップの回折角を特定するためNIST製Si標準試料粉末(SRM640C)を添加し、ピーク位置を補正した。その結果を表1に示す。
2)粒度分布
得られた溶射用原料の粉末について粒度分布を求めた。測定は日機装製MicrotracMT3300EX IIで行い、累積粒径で10%(D10)と90%(D90)を求めた。その結果を表1に示す。
3)SEM観察
得られた溶射用原料についてSEM観察を行った。
実験例2の溶射用原料のXRD測定結果を図1に示す。図1から、結晶相はMgOとMgAl2O4からなることがわかった。図示はしていないが、実験例1,3〜8についても同様であった。SEM観察を行ったところ、実験例1〜7については元のMgO及びAl2O3原料よりも一次粒径が大きくなりつつ、粒子同士のネックがつながっており、熱処理によりMgOとAl2O3が反応してMgOとMgAl2O4を生成しつつ、一部焼結が進んでMgOとMgAl2O4の接触が良好になったことが確認された。一方、実験例8においてはMgOとMgAl2O4の粒成長は見られず、粒子同士のネックがつながっている様子は見られなかった。
(溶射膜の作製)
溶射用基板としてRa>1μmのアルミニウム基板を用意した。実験例1〜9で得られた溶射用原料を大気雰囲気で表2に示す条件にて溶射用基板にプラズマ溶射を実施した。
1)XRD測定
X線回折装置により結晶相を同定した。得られた溶射膜を基板より剥がし、乳鉢にて粉砕して粉末状とした。測定条件はCuKα、40kV、40mA、2θ=10−70°とし、封入管式X線回折装置(ブルカー・エイエックスエス製 D8 ADVANCE)を使用した。測定のステップ幅は0.02°とし、ピークトップの回折角を特定するためNIST製Si標準試料粉末(SRM640C)を添加し、ピーク位置補正した。ICDD78−0430で示されるMgO(111)面、(200)面、(220)面付近にそれぞれ回折ピークが検出されることを確認したあと、各溶射膜のMgO(200)面の回折角のピークトップの位置を求めた。また、市販のソフトウェアMDI社製JADE7のピークサーチ機能から各ピーク高さを求めた。JADE7のピークサーチ条件は、フィルタタイプについては可変、放物線フィルタ、ピーク位置決定についてはピークトップ、しきい値と範囲については、しきい値σ=3.0、ピーク強度%カットオフ=0.1、BG決定の範囲=1.0、BG平均化のポイント数=7とし、Kα2ピークを消去ON、現存のピークリストを消去ONとした。各溶射膜の結晶相、MgO(200)面の回折角のピークトップ位置、回折ピーク(A)〜(C)の高さを表2に示す。なお、回折ピーク(A)〜(C)については後述する。
2)成分分析
得られた溶射膜を基板より剥がし、乳鉢にて粉末にし、化学分析を行った。試料を溶解させたあと、Mg及びAlをキレート滴定法にて定量した。結果を表2に示す。
3)耐食性試験
得られた溶射膜の表面を鏡面研磨し、一部マスクをしてICPプラズマ耐食試験装置を用いて下記条件の耐食試験を行った。段差計により測定したマスク面と暴露面との段差を試験時間で割ることにより各材料のエッチングレートを算出した。結果を表2に示す。
ICP:800W、バイアス:450W、導入ガス:NF3/O2/Ar=75/35/140sccm 0.05Torr、暴露時間:5h、試料温度:室温
4)吸水性試験
実験例1−1〜7−1について、溶射膜を基板から剥がし30℃95%湿度環境下で4日間保管した後、TG−DTAにて大気500℃まで加熱して重量減を求めた。結果を表2に示す。MgOについては溶射膜が得られなかったことから、市販のMgO粉末をプレス成形し、1600℃で熱処理した後、厚み約200μmにしたものを溶射膜と仮定して同様の方法で重量減を求めた。得られた重量減を溶射膜(MgOについては焼結体の膜面)の片側の面積で換算した。値を表2に示す。
5)構成元素
実験例1−1〜7−1の溶射膜断面を真空脱泡しながらエポキシ樹脂中に埋めこみエポキシ樹脂を固化させた後に鏡面研磨を行い、EPMAを用いて構成元素の検出及び同定を行った。
6)気孔率
溶射膜を樹脂(エポキシ樹脂)に包埋することにより溶射膜の気孔を樹脂で埋めた後、溶射膜の断面を切り出して研磨し、その後SEM(走査型電子顕微鏡)にて溶射膜断面のSEM画像を取得した。SEM画像は、倍率500倍、712×532ピクセルの画像とした。得られた画像は、画像解析ソフト(Media Cybernetics社製 Image−Pro Plus 7.0J)を用いて、まず16ビットグレイスケールに変換した後(乗算でスケーリング)、2値化処理を行い、膜の気孔率を算出した。2値化する際のしきい値は、判別分析法として大津の2値化を用いて設定した。
実験例1−1〜8−1の溶射膜をXRD測定したところ、MgO(200)面を含め、ICDD78−0430で示されるMgO付近に回折ピークが検出されること、またマグネシウムアルミニウム酸化物(MgAl2O4)が検出されることを確認した。
Claims (7)
- MgOにAlNではなくAlが固溶しており、CuKα線を用いたときのXRD測定においてMgO(200)面の回折ピークが2θ=42.92°よりも高角側にシフトしており、結晶相としてMgOとMgAl2O4を含む、MgO系セラミックス膜。
- 前記XRD測定において、前記MgO(200)面の回折ピークと、該MgO(200)面の回折ピークよりも高角側でMgAl 2 O 4 (400)面の回折ピークとの間に見られる新たな回折ピーク、又はショルダーとを有している、
請求項1に記載のMgO系セラミックス膜。 - MgとAlを酸化物換算した際のMgOとAl2O3の質量比MgO/Al2O3が2.33より大きい、
請求項1又は2に記載のMgO系セラミックス膜。 - 気孔率が20%以下である、
請求項1〜3のいずれか1項に記載のMgO系セラミックス膜。 - 溶射膜である、
請求項1〜4のいずれか1項に記載のMgO系セラミックス膜。 - 請求項1〜5のいずれか1項に記載のMgO系セラミックス膜で表面が覆われた、半導体製造装置用部材。
- 溶射用原料としてMgOとAl2O3を顆粒状にした後1200℃以上で熱処理したものを作製し、該溶射用原料を所定の基板に溶射することにより請求項5に記載のMgO系セラミックス膜を製造する、
MgO系セラミックス膜の製法。
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