JP2019513903A - HiPIMSを用いて成長欠陥を低減させたTiCN - Google Patents
HiPIMSを用いて成長欠陥を低減させたTiCN Download PDFInfo
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- 230000009643 growth defect Effects 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 82
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000007789 gas Substances 0.000 claims abstract description 62
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 57
- 238000000151 deposition Methods 0.000 claims abstract description 24
- 238000000576 coating method Methods 0.000 claims abstract description 19
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 239000011248 coating agent Substances 0.000 claims abstract description 18
- 230000008021 deposition Effects 0.000 claims abstract description 18
- 238000004544 sputter deposition Methods 0.000 claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001873 dinitrogen Inorganic materials 0.000 claims abstract description 8
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 7
- 239000010439 graphite Substances 0.000 claims abstract description 7
- 229910052786 argon Inorganic materials 0.000 claims abstract description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 18
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 6
- 229910052756 noble gas Inorganic materials 0.000 claims description 3
- 239000010410 layer Substances 0.000 description 97
- 239000010936 titanium Substances 0.000 description 32
- 239000000523 sample Substances 0.000 description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 13
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical group [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 7
- 239000013074 reference sample Substances 0.000 description 7
- 239000013077 target material Substances 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 6
- 238000001208 nuclear magnetic resonance pulse sequence Methods 0.000 description 5
- 238000005546 reactive sputtering Methods 0.000 description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 231100000572 poisoning Toxicity 0.000 description 4
- 230000000607 poisoning effect Effects 0.000 description 4
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 230000001419 dependent effect Effects 0.000 description 3
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 229910052774 Proactinium Inorganic materials 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 150000001247 metal acetylides Chemical class 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 230000002123 temporal effect Effects 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
- C23C14/0057—Reactive sputtering using reactive gases other than O2, H2O, N2, NH3 or CH4
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
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- C—CHEMISTRY; METALLURGY
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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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- 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
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- 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
- C23C14/0664—Carbonitrides
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- 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
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- 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
- C23C14/3435—Applying energy to the substrate during sputtering
- C23C14/345—Applying energy to the substrate during sputtering using substrate bias
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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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C23C14/3485—Sputtering using pulsed power to the target
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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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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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
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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
- H01J37/3411—Constructional aspects of the reactor
- H01J37/3414—Targets
- H01J37/3426—Material
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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
- H01J37/3464—Operating strategies
- H01J37/3467—Pulsed operation, e.g. HIPIMS
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Abstract
Description
反応性スパッタリングまたはHiPIMSプロセスを用いた被覆では、しばしば金属ターゲットを噴霧材料源として用い、この際に少なくとも1つの反応性ガスを、作動ガスに追加して採用する。本発明の枠内では、「噴霧する」の概念と「スパッタリング」の概念とは同一であると理解される。ターゲットとは、本発明の枠内では、この方法を行う際に材料が削り取られるスパッタリング源の構成部分を称する。
本発明の課題は、成長欠陥がより小さく、しかし同時に可能な限り層硬度の損失がなくまたは層の内部応力が上昇しないTiCN層を生産することができる方法を提供することである。
本発明の課題は、請求項1に記載の方法を提供することにより解決される。
反応性雰囲気は、追加的に第2反応性ガスとして炭素含有ガス好ましくはCH4を含み、この炭素含有ガスを、TiCN層を生成するための炭素源として用い、TiCN層の析出時には、双極性のバイアス電圧を被覆されるべき基板上にかけ、
または
TiCN層を生成するための炭素源として、少なくとも1つの炭素含有ターゲット例えば黒鉛ターゲットを用い、このターゲットを、反応性ガスとして窒素ガスのみを有する反応性雰囲気を有する被覆チャンバ中で、HiPIMS方法を用いてスパッタし、この際、Ti含有ターゲットは好ましくは第1電力給電機器または第1電力給電ユニットを用いてパルス電力で作動し、かつ黒鉛含有ターゲットは、好ましくは第2電力給電機器または第2電力給電ユニットを用いてパルス電力で作動する。
発明者が見出した点は、驚くべきことに、HiPIMSプロセスの際に双極性のバイアス電圧を用いると、反応性HiPIMSプロセスを用いて、非常に高い硬度を有するTiCNからなる硬質材料層を、非常に滑らかな層表面とともに同時に、さらに内部応力を比較的低くして製造することが可能であるとの点である。また、驚くべきことに、反応性HiPIMSプロセスを用いて、このHiPIMSプロセスにおいて窒素のみを反応性ガスとして用い、TiCNの生産用の炭素を炭素含有ターゲットから準備する場合に、非常に高い硬度とともに同時に、非常に滑らかな層表面を有するTiCNからなる硬質材料層を製造することが可能であることも発明者は見出した。
第1実施例にしたがって一例として示した全てのTiCN層を、接着層として薄いTiN層を備えて製造した。まず、このTiN接着層を、被覆されるべき表面上に析出し、この際、以下のパラメータを用いた。すなわち、パルス電力Ppulseは60kWで、ターゲットにおける平均電力Pavは9.0kWで、tpulseが25ミリ秒、全圧ptotが0.81Paであり、N2部分圧が0.01Paであり、Ar部分圧が0.4Paであり、一定のバイアス電圧が−80Vであり、被覆温度が450℃であった。
第2実施例により一例として示された全てのTiCN層は、接着層として薄いTiN層を備えて生成された。まず、TiN接着層を、被覆されるべき表面上に析出し、この際、以下のパラメータを用いた。すなわち、パルス電力Ppulse、は60kW、ターゲットにおける平均電力Pavは9.0kW、tpulseが25ミリ秒、全圧ptotが0.81Paであり、N2部分圧が0.01Paであり、Ar部分圧が0.4Paであり、一定のバイアス電圧が−80Vであり、被覆温度が450℃であった
反応性雰囲気は、追加的に第2反応性ガスとして炭素含有ガスを含み、この炭素含有ガスを、TiCN層を生成するための炭素源として用い、TiCN層の析出時には、双極性のバイアス電圧を被覆されるべき基板上にかけ、
または
TiCN層を生成するための炭素源として、少なくとも1つの炭素含有ターゲットを用い、このターゲットを、HiPIMS方法を用いて、反応性ガスとして窒素ガスのみを有する反応性雰囲気を有する被覆チャンバ中でスパッタする方法である。
Claims (9)
- HiPIMSを用いて、少なくとも1つのTiCN層を備えた被覆部を、被覆されるべき基板の表面に塗布する方法であって、前記少なくとも1つのTiCN層を析出するために、前記TiCN層を生成するためのTi源として、Ti含有ターゲットを少なくとも1つ用い、前記Ti含有ターゲットを、被覆チャンバ中の反応性雰囲気中でHiPIMS方法を用いてスパッタし、前記反応性雰囲気は、少なくとも1つの希ガス好ましくはアルゴンを含み、少なくとも窒素ガスを反応性ガスとして含む、方法において、
前記少なくとも1つのTiCN層を析出する間に、成長欠陥を低減させるために、
前記反応性雰囲気は、追加的に第2反応性ガスとして炭素含有ガスを含み、前記炭素含有ガスを、TiCN層を生成するための炭素源として用い、前記TiCN層の析出時には、双極性のバイアス電圧を前記被覆されるべき基板上にかけ、
または
前記TiCN層を生成するための炭素源として、少なくとも1つの炭素含有ターゲットを用い、前記ターゲットを、反応性ガスとして窒素ガスのみを有する反応性雰囲気を有する前記被覆チャンバ中で、HiPIMS方法を用いてスパッタすることを特徴とする、方法。 - 炭素源として炭素含有ガスを用い、前記炭素含有ガスはCH4を含み、またはCH4からなる、請求項1に記載の方法。
- 炭素源として炭素含有ガスを用い、前記炭素含有ガスはC2H4を含み、またはC2H4からなる、請求項1に記載の方法。
- 炭素源として少なくとも1つの炭素含有ターゲットを用い、1つまたは複数のTi含有ターゲットは第1電力給電機器または第1電力給電ユニットを用いてパルス電力で作動し、かつ1つまたは複数の炭素含有ターゲットは、第2電力給電機器または第2電力給電ユニットを用いてパルス電力で作動する、請求項1に記載の方法。
- 少なくとも1つのTi含有ターゲットは、Tiからなる金属ターゲットである、請求項4に記載の方法。
- 少なくとも1つのTi含有ターゲットは、TiCからなるセラミック製のターゲットである、請求項4に記載の方法。
- 少なくとも1つの炭素含有ターゲットは黒鉛からなる、請求項4〜6のいずれか1項に記載の方法。
- 前記少なくとも1つの炭素含有ターゲットは複合材料からなる、請求項4〜6のいずれか1項に記載の方法。
- 前記ターゲットは、少なくとも1つの金属と炭化物とを含む複合材料からなる、請求項8に記載の方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US201662326098P | 2016-04-22 | 2016-04-22 | |
US62/326,098 | 2016-04-22 | ||
PCT/EP2017/000500 WO2017182124A1 (de) | 2016-04-22 | 2017-04-21 | Ticn mit reduzierten wachstumsdefekten mittels hipims |
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JP2019513903A true JP2019513903A (ja) | 2019-05-30 |
JP7179291B2 JP7179291B2 (ja) | 2022-11-29 |
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KR102626873B1 (ko) * | 2021-11-17 | 2024-01-17 | 이계영 | HiPIMS를 이용한 전극 증착 방법 |
CN115928009A (zh) * | 2022-06-23 | 2023-04-07 | 广东华升纳米科技股份有限公司 | TiCN涂层及其制备方法 |
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US20190136363A1 (en) | 2019-05-09 |
US11542587B2 (en) | 2023-01-03 |
CN109154061A (zh) | 2019-01-04 |
KR102335906B1 (ko) | 2021-12-09 |
CA3021704C (en) | 2023-11-14 |
RU2018140962A (ru) | 2020-05-22 |
RU2018140962A3 (ja) | 2020-06-12 |
US20230135238A1 (en) | 2023-05-04 |
JP7179291B2 (ja) | 2022-11-29 |
CN109154061B (zh) | 2021-07-13 |
WO2017182124A1 (de) | 2017-10-26 |
CA3021704A1 (en) | 2017-10-26 |
IL262524B (en) | 2021-12-01 |
RU2742325C2 (ru) | 2021-02-04 |
ES2828090T3 (es) | 2021-05-25 |
EP3445890A1 (de) | 2019-02-27 |
IL262524A (en) | 2018-12-31 |
KR20190002538A (ko) | 2019-01-08 |
MY189225A (en) | 2022-01-31 |
EP3445890B1 (de) | 2020-07-29 |
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