JP7087229B2 - コーティング源 - Google Patents
コーティング源 Download PDFInfo
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- JP7087229B2 JP7087229B2 JP2017538609A JP2017538609A JP7087229B2 JP 7087229 B2 JP7087229 B2 JP 7087229B2 JP 2017538609 A JP2017538609 A JP 2017538609A JP 2017538609 A JP2017538609 A JP 2017538609A JP 7087229 B2 JP7087229 B2 JP 7087229B2
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- 239000011248 coating agent Substances 0.000 title claims description 40
- 238000000576 coating method Methods 0.000 title claims description 40
- 239000000843 powder Substances 0.000 claims description 43
- 239000000203 mixture Substances 0.000 claims description 37
- 230000000087 stabilizing effect Effects 0.000 claims description 35
- 229910052751 metal Inorganic materials 0.000 claims description 31
- 239000002184 metal Substances 0.000 claims description 31
- 239000000463 material Substances 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 25
- 239000010936 titanium Substances 0.000 claims description 16
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 15
- 229910052719 titanium Inorganic materials 0.000 claims description 13
- 238000000280 densification Methods 0.000 claims description 12
- 238000005240 physical vapour deposition Methods 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 4
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 3
- 239000007769 metal material Substances 0.000 claims description 2
- 150000003609 titanium compounds Chemical class 0.000 claims 2
- 239000013078 crystal Substances 0.000 claims 1
- 239000012071 phase Substances 0.000 description 53
- 230000008569 process Effects 0.000 description 18
- 239000002245 particle Substances 0.000 description 13
- 239000011159 matrix material Substances 0.000 description 5
- 230000007704 transition Effects 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 238000005476 soldering Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 238000002490 spark plasma sintering Methods 0.000 description 3
- 238000005477 sputtering target Methods 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000005304 joining Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical group [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical group [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- AUNXOLCRDMKODF-UHFFFAOYSA-N [Si]([O-])([O-])([O-])O[Si]([O-])([O-])[O-].[Ti+4].[Si]([O-])([O-])([O-])O[Si]([O-])([O-])[O-].[Si]([O-])([O-])([O-])O[Si]([O-])([O-])[O-].[Si]([O-])([O-])([O-])O[Si]([O-])([O-])[O-].[Ti+4].[Ti+4].[Ti+4].[Ti+4].[Ti+4] Chemical compound [Si]([O-])([O-])([O-])O[Si]([O-])([O-])[O-].[Ti+4].[Si]([O-])([O-])([O-])O[Si]([O-])([O-])[O-].[Si]([O-])([O-])([O-])O[Si]([O-])([O-])[O-].[Si]([O-])([O-])([O-])O[Si]([O-])([O-])[O-].[Ti+4].[Ti+4].[Ti+4].[Ti+4].[Ti+4] AUNXOLCRDMKODF-UHFFFAOYSA-N 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000002826 coolant Substances 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
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical group [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 239000004482 other powder Substances 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical group [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
- H01J37/3488—Constructional details of particle beam apparatus not otherwise provided for, e.g. arrangement, mounting, housing, environment; special provisions for cleaning or maintenance of the apparatus
- H01J37/3491—Manufacturing of targets
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- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
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- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
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- C22C1/04—Making non-ferrous alloys by powder metallurgy
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- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0078—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only silicides
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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
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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
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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
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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
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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
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- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Plasma & Fusion (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Composite Materials (AREA)
- Dispersion Chemistry (AREA)
- Physical Vapour Deposition (AREA)
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Description
-2つの粉末混合物がそれぞれ加圧され別個の中間圧縮体を生成し、次いで熱時高密度化される。
-1つの粉末混合物のみが加圧されて中間圧縮体を生成し、これが、次いで、第二の粉末混合物と共に熱時高密度化される。
-第一及び第二の粉末混合物が加圧されて中間圧縮体を生成し、次いで、(所望により他の粉末混合物と共に)熱時高密度化される。
-ターゲット層と機械的安定化層との間の明確に画定された界面を避けることができる。これにより、従来技術に関して述べた界面の不利が生じない。本発明のプロセスの結果、界面は全く存在せず、代わりに、2以上の相からなる複合体の追加の相の粒子の濃度が機械的安定化層からターゲット層の方向に増加していく空間的に延長された接合帯域が、明確な界面を形成することなく、存在する。
-始めに述べたはんだ付け(特許文献3)に関して、コーティング源の低融点はんだ材料による熱的な弱体化はない。従って、本発明によって製造されたコーティング源は、PVD操作において、より高い電力で使用することができる。
-本発明のプロセスは、ターゲット層に、特許文献4のプロセスが使用できないような脆弱な材料を使用することを可能にする。
-チタン、鉄、ニッケル、銅のような純金属
-上述の純金属の合金
-上述の純金属又は上述の合金に基づく複合体
である。
チタンからなる安定化相を有するチタン-シリコン含有コーティング源を製造するために、下記の手順を採用した。
-チタン(Ti)粉末及び二珪化チタン(TiS2)粉末を混合して第一の粉末混合物としてチタン-シリコン(TiSi)前駆体を得る。
-加圧冶具(ここでは、グラファイト-SPS冶具)に第二の粉末混合物としての純チタン粉末を充填する。
-先に半分充填した冶具にTiSi前駆体を充填する。
-900~1,400℃の温度範囲でSPSにより二層集合体を高密度化する。
-切削加工により最終の機械加工をしてターゲットを得る。
-脆弱なTiSiターゲット層と機械的安定化層としてのチタンからなる延性のバッキングプレートとの2層構造
-ターゲット層を形成する複合体の熱膨張係数と安定化層の熱膨張係数との比は、0.5から2.0、好ましくは0.75から1.33の範囲内にある。
-ターゲット層から安定化相への遷移は、接合帯域を構成するが拡散結合又ははんだ付けの場合のようには界面を形成せず、連続的である。
ターゲット層2の第一の相としての金属相Mに埋め込まれた少なくとも2相からなる複合体の追加の相Pが明確に見られる。金属相Mは、ここでは、マトリクスを形成する。示された例では、ターゲット層2の相Mは、安定化層3に対応する。言い換えれば、機械的安定化層3は、ターゲット層2の相Mを形成するのと同じ材料でできている。
この例の追加の相Pは、珪化チタンであり、金属相Mで形成されたチタンマトリクス中に埋め込まれている。
結晶粒界は、結晶粒界エッチングにより、可視化されている。従って、ここでは、個々の粒子の形状及び方向を見ることが可能である。
ここで、サイズバーから認識できるが、図1のそれとは異なるサイズスケールに留意されたい。
図2a及び図2bの像は、図2bにおいてはTiSi粒子の結晶粒界(追加の相Pに対応する)が、明確に認識できるように、黒太線で輪郭を付けられている点で、異なっている。その他の点では、図2bは図2aに対応している。
金属組織学的研磨断面の方向は、頁の右手の余白の矢印で明確にされている。参照記号2の矢印は、ターゲット層2が延在する方向を示す。参照記号3の矢印は、安定化層3が延在する方向を示す。
個々のTiSi粒子(相P)は、金属相Mに埋め込まれている。参照記号の線は、例示のために、相P又は金属相Mの個々の粒子に向けられていることに言及しておく。当然、相P及び金属相Mは、多くの粒子で構成されている。いまの材料系では、相Pのやや丸みを帯びた粒子が、その形状により、金属相Mの角張った粒子から容易に区別できる。
安定化層3の微細構造がターゲット層2の金属相Mの中に連続的に入り込んでいるのが分かる。安定化層3及びターゲット層2の金属相Mの中の個々のTi粒子が、その粒子の内部の特徴的な双晶形成により認識できる。接合帯域において、追加の相P(ここでは、TiSi粒子)の粒子の濃度が、安定化層3の材料からターゲット層2の方向に向かって、増加しているのが分かる。
その組成がターゲット層2に対応する第一の粉末混合物6及びその組成が機械的安定化層3に対応する第2の粉末混合物7が加工冶具5内に層状に存在する。高密度化は、矢印で示されたように軸方向に実施される。
2 ターゲット層
3 安定化層
31 口金状突起
4 接合帯域
5 加圧冶具
51 上部パンチ
52 下部パンチ
53 加熱装置
6 第一の粉末混合物
7 第二の粉末混合物
M 金属相
P 追加の相
Claims (15)
- 物理蒸着のためのコーティング源(1)の製造方法であって、
前記コーティング源(1)が、少なくとも
金属相(M)の結晶粒界を有する複数の粒と1以上の追加の相(P)の結晶粒界を有する複数の粒とを含有する2以上の相からなる複合体からなるターゲット層(2)と、
前記ターゲット層(2)の一側面で前記ターゲット層(2)に接合した機械的安定化層(3)と、を有し、
前記2以上の相からなる複合体に対応する組成を有する第一の粉末混合物(6)及び前記機械的安定化層(3)に対応する組成を有する第二の粉末混合物(7)は、前記第一の粉末混合物(6)及び前記第二の粉末混合物(7)が、加圧治具中で、粉末が焼結されて固体が形成されるような温度で軸方向に圧縮される熱時加圧により、重畳層として熱時高密度化され、
前記ターゲット層(2)及び前記機械的安定化層(3)が、前記機械的安定化層(3)の金属相が前記ターゲット層(2)の前記金属相(M)に入りこむことで、前記追加の相(P)の前記結晶粒界を有する複数の粒の数が前記機械的安定化層(3)から前記ターゲット層(2)の方向に増加していく接合帯域(4)を介して、互いに接合していること
を特徴とする製造方法。 - 高密度化の間に、前記重畳層に電流が供給され又は前記重畳層が誘導加熱される請求項1に記載の製造方法。
- 前記第一又は第二の粉末混合物(6,7)が予備的にのみ高密度化された中間圧縮体の形状で使用され、最終的な高密度化及び接合が熱時高密度化によって行なわれる請求項1又は2に記載の製造方法。
- チタン又はチタン合金が前記2以上の相からなる複合体の金属相(M)として用いられる請求項1~3のいずれか1項に記載の製造方法。
- 前記2以上の相からなる複合体の金属相(M)の材料及び前記機械的安定化層(3)の材料が少なくとも80原子% 同じ金属からなる請求項1~4のいずれか1項に記載の製造方法。
- 前記追加の相(P)が、前記2以上の相からなる複合体に基づいて、25体積%を超える比率で用いられる請求項1~5のいずれか1項に記載の製造方法。
- チタン以外の元素又はチタン化合物が前記追加の相(P)として用いられる請求項1~6のいずれか1項に記載の製造方法。
- 前記第一及び第二の粉末混合物(6,7)が、互いにその全面を相接して、互いにその上下に配置されている請求項1~7のいずれか1項に記載の製造方法。
- 物理蒸着のためのコーティング源(1)であって、
金属相(M)の結晶粒界を有する複数の粒と1以上の追加の相(P)の結晶粒界を有する複数の粒とを含有する2以上の相からなる複合体からなり、前記金属相(M)及び存在する前記追加の相(P)の全てが1,000℃を超える融点を有するターゲット層(2)と、
前記ターゲット層(2)の一側面上で前記ターゲット層(2)に接合している機械的安定化層(3)と、を有し、、
前記ターゲット層(2)及び前記機械的安定化層(3)が、前記機械的安定化層(3)の金属相が前記ターゲット層(2)の前記金属相(M)に入りこむことで、前記2以上の相からなる複合体の前記追加の相(P)の前記結晶粒界を有する複数の粒の数が前記機械的安定化層(3)から前記ターゲット層(2)の方向に増加していく接合帯域(4)を介して、互いに接合していることを特徴とするコーティング源。 - 前記2以上の相からなる複合体の前記金属相(M)がチタン又はチタン合金を含有してなる請求項9に記載のコーティング源(1)。
- 前記2以上の相からなる複合体の前記金属相(M)の材料及び前記機械的安定化層(3)の材料が少なくとも80原子%同じ金属からなる請求項9又は10に記載のコーティング源(1)。
- 前記追加の相(P)が、前記2以上の相からなる複合体に基づいて、25体積%を超える比率で存在する請求項9~11のいずれか1項に記載のコーティング源(1)。
- 前記追加の相(P)がチタン以外の元素又はチタン化合物からなる請求項9~12のいずれか1項に記載のコーティング源(1)。
- 前記機械的安定化層(3)が前記ターゲット層(2)の金属相(M)を形成するのと同じ金属材料からなり、前記2以上の相からなる複合体の前記追加の相(P)の複数の粒を少なくとも本質的に含有しない請求項9~13のいずれか1項に記載のコーティング源。
- 前記機械的安定化層(3)自体が2以上の相からなる複合体からなる請求項9~13のいずれか1項に記載のコーティング源。
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