JP5522648B2 - Joint protection structure of the diamond surface and the metal strip - Google Patents

Joint protection structure of the diamond surface and the metal strip Download PDF

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JP5522648B2
JP5522648B2 JP2008094925A JP2008094925A JP5522648B2 JP 5522648 B2 JP5522648 B2 JP 5522648B2 JP 2008094925 A JP2008094925 A JP 2008094925A JP 2008094925 A JP2008094925 A JP 2008094925A JP 5522648 B2 JP5522648 B2 JP 5522648B2
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diamond
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bonding
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JP2009252775A (en )
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和寛 池田
仁 梅澤
真一 鹿田
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独立行政法人産業技術総合研究所
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本発明は、ダイヤモンドと金属片との密着性、高温安定性、薬品耐性に関するものであり、応用例としては、工具、電極、電子デバイスがあげられる。 The present invention, adhesion between the diamond and the metal piece, high temperature stability, relates chemical resistance, as the application example, a tool, the electrode, the electronic device and the like. とくに、ボンディングの機械強度、高温での金属片の剥離、強酸・強アルカリ中において、ダイヤモンドと金属片による構造を強固に保持することが要求される状況に適する。 In particular, the mechanical strength of the bonding, peeling of the metal pieces at high temperatures, in strong acid-strong in alkali, suitable conditions it is required to firmly hold the structure by diamond and the metal piece.

ダイヤモンドは、高温あるいは極限環境下でも利用できる材料として知られ、センサや電極としての応用が広範囲にわたって開発されている。 Diamond is known as a material which can be used even under high-temperature or extreme environment, application as a sensor or an electrode has been developed extensively. ところが、ダイヤモンドと金属片とを同時に利用するような構造を要する場面においては、金属片とダイヤモンドの界面の強度、金属片自身の高温ないし薬品中での脆弱性により、極限環境での利用には制限がある。 However, in situations requiring such a structure as to utilize the diamond and the metal piece at the same time, the strength of the interface between the metal piece and the diamond, the vulnerability in a hot or chemical metal pieces themselves, for use in extreme environments is There is a limit.

この問題を解決すべく本発明では、Ru被膜によるダイヤモンド上の金属片、例えば電極、素子をRu被膜により保護することで、高温あるいは強反応性化学物質中においても金属片とダイヤモンド表面との接合を保持したまま、機能を発揮する構造を提供する。 In the present invention to solve this problem, a metal piece on the diamond by Ru film, for example, an electrode, an element to protect the Ru film, the bonding between the high temperature or strongly reactive chemical metal piece and the diamond surface even during while holding the, to provide a structure that serves the function.

上記目的を達成するために本発明は、ダイヤモンド表面と金属片との接合を接合の面積より大きな面積のRu被膜によって保護することで、高強度、高温、耐薬品性のある信頼性の高い構造を見出すに至った。 To accomplish the above object, to protect the Ru film of larger area than the bonded bonding between the diamond surface and the metal piece, high strength, high temperature, high reliability with a chemical structure I came to find.
すなわち、本発明は、ダイヤモンド表面と金属片との接合を、金属片とダイヤモンド表面の非結合面に、当該金属片を覆いつくす当該金属片より面積の大きいRu被膜を設けることにより保護したダイヤモンド表面と金属片との接合保護構造である。 That is, the present invention, the bonding between the diamond surface and the metal piece, metal pieces and the non-binding surface of the diamond surface, protected diamond surface by providing a large Ru coating area than the metal piece completely covering the metal strip and a joint protection structure of a metal strip.
また本発明では、ダイヤモンドを電気伝導性とすることができる。 In the present invention, it is possible to electrically conductive diamond.
さらに本発明では、金属片と、電気伝導性ダイヤモンドとがオーム性の電気伝導界面を持たせることができる。 Further, in the present invention, it is possible to provide a metal piece, and an electrical conductivity diamond ohmic electrical conduction interfaces.
また本発明では、電気伝導性ダイヤモンドをダイヤモンド半導体とすることができる。 In the present invention, the electrically conductive diamond may be diamond semiconductor.
さらに本発明では、ダイヤモンドを絶縁性とすることができる。 Further, in the present invention, diamond can be insulating.
また本発明では、Ru被膜として、Ruそのもの(純度99.9以上)を適用することができる。 In the present invention, as Ru coating, it can be applied Ru itself (99.9 or higher).
さらに本発明では、オーミック電極を形成する金属がTi/Ptの積層構造である請求項3に記載したダイヤモンド表面と金属片との接合保護構造。 Further, in the present invention, bonding protective structure of the diamond surface and the metal pieces as claimed in claim 3 metal forming the ohmic electrode is a laminated structure of Ti / Pt.
また本発明では、Ru被膜上にさらに異なる金属被膜を設置したダイヤモンド表面と金属片との接合保護構造とすることができる。 Also in the present invention can be a bonded protective structure further different metal coating installation diamond surface and the metal strip on Ru coating.
さらに本発明では、Ru被膜上に設置される金属被膜をTi, Pt, Au, Ni, Moから選ばれる金属とすることができる。 Further, in the present invention may be a metal selected metal coating is placed on the Ru film Ti, Pt, Au, Ni, from Mo.
また本発明では、金属片が電極であり、ダイヤモンドをダイヤモンド半導体とすることができる。 In the present invention, a metal piece electrode, it is possible to diamond and diamond semiconductor.

本発明により、Ru被膜により覆われた金属片は良好に保護され、例えばダイヤモンド表面上の電極のボンディング強度を向上させるだけでなく、高温長期信頼性、HFのような強酸中でも、ダイヤモンド表面上の電極の構造保持を行うことが出来た。 The present invention, metal strips covered with Ru film are better protected, for example, not only improves the bonding strength of the electrode on the diamond surface, high temperature long-term reliability, even in a strong acid such as HF, on the diamond surface We were able to perform the structure holding the electrodes.

本発明は、ダイヤモンド表面と金属片との接合を接合の面積より大きな面積のRu被膜によって保護する構造であり、ダイヤモンドが電気伝導性の場合も絶縁性の場合も同様の効果が得られる。 The present invention is a structure for protecting the Ru film of larger area than the bonded bonding between the diamond surface and the metal piece, diamond even if the electrical conductivity is obtained a similar effect in the case of insulation. また、金属片と、伝導性ダイヤモンドとがオーム性の電気伝導界面を持つ素子構造である場合、伝導性ダイヤモンドが半導体である電子素子が含まれる。 Further, a metal piece, a conductive diamond be a device structure with ohmic electrical conduction interfaces include electronic elements conductivity diamond is a semiconductor. また、ダイヤモンドが絶縁性であるとき、ダイヤモンド表面上に設置した金属片をRu被膜により被覆した構造も含まれる。 Further, when the diamond is insulative, also contain metal pieces was placed onto the diamond surface is coated with Ru film structure. そのうえ、金属片がRuそのものである構造にも適用できる。 Moreover, the metal strip can also be applied to the structure is intended that Ru. 電極としては、オーミック電極を形成する金属がTi/Ptの積層構造である上記半導体ダイヤモンド上の電極への適用も含まれる。 As the electrode, a metal forming an ohmic electrode also includes application to the semiconducting diamond electrode on a stacked structure of Ti / Pt. この構造の適用には、Ru被膜上にさらに異なる金属を設置した構造も同様である。 The application of this structure, the same applies to the structure in which established a further different metal on Ru coating. そのため、Ru被膜上に設置される金属がTi, Pt, Au, Ni, Moである構造も含まれる。 Therefore, the metal to be placed on the Ru film is Ti, Pt, Au, Ni, also includes structure which is Mo. すなわち、このような構造が電極の役割をする場合、半導体デバイスの機能を持つ構造を適用することが出来る。 That is, if such a structure is the role of the electrodes can be applied a structure having the function of semiconductor devices.
本発明において、特に強酸中に曝す場合、設置後のRu被膜には焼鈍として、200℃〜800℃の範囲で加熱を行うことが望ましい。 In the present invention, especially when exposed to during a strong acid, as annealing the Ru film after installation, it is preferable to perform heating in the range of 200 ° C. to 800 ° C..
さらに本発明では、Ru被膜の面積が被覆を要する金属の面積よりも大きな事が望ましい。 Further, in the present invention, large it is desirable than the area of ​​the metal area of ​​the Ru film requires coating.
本発明でダイヤモンド表面上に設置するRu被膜の設置方法は、どのような方法でも良いが例としてイオンビームスパッタ法、パルスレーザー堆積法、RFスパッタ法によって作製される。 Installation of Ru film is placed on the diamond surface in the present invention may be in any way an ion beam sputtering method as an example, pulsed laser deposition, made by RF sputtering. 厚さは特に規定しない。 The thickness is not particularly defined.
形状は、どのようなものでも良いが、実施例では100μm間隔で島状に点在するφ30μmの電極を配置した。 Shape, what may be one, but arranged electrodes φ30μm scattered like islands in 100μm intervals in the embodiment.

本発明においては、ダイヤモンドとは、天然のもの、人工のものを問わない。 In the present invention, a diamond, a naturally occurring, regardless of the man-made.
また、ダイヤモンドはどのような結晶系のもの、どのような終端構造のものであっても良い。 Further, diamond of any such crystal systems may be of any termination structures.

本発明では、ダイヤモンド表面と金属片でオーミック伝導を形成する場合、オーミック電極の作成についても、周知の材料と周知方法を用いてどのような手順で行っても良い。 In the present invention, when forming an ohmic conductive diamond surface and the metal piece, for the creation of an ohmic electrode, it may be performed in any procedure using known methods and known materials.

さらに本発明においては、天然、人工を問わず、ダイヤモンドならどのタイプのものでも良く、表面の結晶構造は(001)、(111)、(110)などが挙げられる。 Further, in the present invention, natural, whether artificial, may be of any if the diamond type crystal structure of the surface (001), (111), and the like (110).

さらに本発明におけるダイヤモンド表面は、炭素終端ダイヤモンド、水素終端ダイヤモンド、酸素終端ダイヤモンドなどが挙げられる。 Diamond surface in still present invention, the carbon-terminated diamond, hydrogen terminated diamond, such as oxygen-terminated diamond like. また、単層から2〜3層であれば、シリコン化合物のような極薄中間層が入っても良い。 Further, if two or three layers of a single layer, ultrathin intermediate layer may contain such as silicon compound.

アニールを行わなくても良い密着性を示すが、Ru被膜の設置後、真空・あるいは不活性ガス雰囲気中400℃以上でアニールすることで、より高い強度を持たせることが出来る。 It represents an adhesion even without annealing, but after the installation of the Ru film, by annealing in a vacuum-or inert gas atmosphere 400 ° C. or higher, can have a higher strength.
本発明について実施例を用いてさらに詳しく説明するが、本発明はこれら実施例に限定されるものではない。 The present invention will be described in more detail with reference to examples for, the present invention is not limited to these examples.

ダイヤモンド上に、電子線描画装置を利用し、円形φ30μmのパターンを用意し、そこへ真空蒸着気によりTiを30nm蒸着し、リフトオフ工程を経ることでTiの金属片を1600個用意した。 On the diamond, using an electron beam lithography system, to prepare a pattern of circular Fai30myuemu, the Ti and 30nm deposited by vacuum deposition gas thereto, and the metal pieces of Ti by passing through a lift-off process was 1600 prepared. 次に、ダイヤモンド上に、電子線描画装置を利用し、円形φ20μmのパターンを用意し、そこへ真空蒸着気によりRuを20nm蒸着し、リフトオフ工程を経ることでTiの金属片を1600個用意した。 Then, on the diamond, using an electron beam lithography system, to prepare a pattern of circular [phi] 20 [mu] m, the Ru was 20nm deposited by vacuum deposition gas thereto, and the metal pieces of Ti by passing through a lift-off process was 1600 prepared . そのパターンと正確に中心が一致、重なり合うように、Ruの円形パターンφ30μmを描画し、RFスパッタ法によりRuを200nm成膜した。 The pattern exactly centered match, so overlapping, it draws a circular pattern φ30μm of Ru, was 200nm deposited Ru by RF sputtering. 次にリフトオフ工程で不要な部分を取り除いた後、アセトンの入っているビーカーに入れ、超音波洗浄機を行い、次に別のテフロン(登録商標)製の容器に入れたHF液中に曝露した。 Then after removing unnecessary portions by a lift-off process, put in a beaker containing the acetone, subjected to ultrasonic cleaning machine, and then exposed to another Teflon HF solution that takes into (registered trademark) container .

(比較例) (Comparative Example)
ダイヤモンド上に、一般にダイヤモンドとの密着性が良いとされるTiで構成するφ30μmの電極をRFスパッタ法により設置し、アセトンの入っているビーカーに入れ、超音波洗浄機を行い、次に別のテフロン(登録商標)製の容器に入れたHF液中に曝露した。 On the diamond, generally the φ30μm of electrodes made of Ti adhesion is good and the diamond is placed by a RF sputtering method, placed in a beaker containing the acetone, subjected to ultrasonic cleaning machine, then the other Teflon exposed to HF solution that takes into (registered trademark) container.

実施例1で得られたものは、図1に示すように、超音波、HFに対して、良い機械的、化学的耐性を示した。 Those obtained in Example 1, as shown in FIG. 1, ultrasonic, against HF, showed good mechanical, chemical resistant.

ダイヤモンド上に、一般にダイヤモンドとの密着性が良いTiで構成するφ20μmの電極に加えて、密着性は良くないが、電子デバイス用途として用いられることの多いAuで構成するφ20μmの電極をそれぞれ電子線描画とRFスパッタ法を用いることで、厚さ30nmで1600個ずつ設置し、それらの上に、φ30μmのRu(99.9%)で構成するφ30μmの電極をRFスパッタ法により、厚さ200 nm設置し、アセトンの入っているビーカーに入れ、超音波洗浄機で洗浄した。 On the diamond, generally in addition to the electrodes of φ20μm constituted by having good adhesion Ti of the diamond, but adhesion is not good, respectively electron beam electrodes φ20μm be configured in which are often used as an electronic device applications Au by using the drawing and RF sputtering, established by 1600 with a thickness of 30 nm, on them, the electrodes of φ30μm constituted by Ru (99.9%) of φ30μm by RF sputtering, installed thickness 200 nm , placed in a beaker containing the acetone and washed by an ultrasonic cleaner. また、テフロン(登録商標)製ビーカーに入れ、HF液中に曝露した。 Furthermore, placed in a Teflon beaker, it was exposed in the HF solution.

(比較例) (Comparative Example)
ダイヤモンド上に、一般にダイヤモンドとの密着性が良いTiに加えて、密着性は良くないが、電子デバイス用途として用いられることの多いAuで構成するφ30μmの電極をRFスパッタ法により厚さ200nmで設置し、アセトンの入っているビーカーに入れ、超音波洗浄機で洗浄した。 Placed on the diamond, generally in addition to Ti having good adhesion to the diamond, but adhesion is not good, the electrodes of φ30μm be configured in many Au it is used as an electronic device applications a thickness of 200nm by an RF sputtering method was placed in a beaker containing the acetone and washed by an ultrasonic cleaner.

本発明はダイヤモンド表面と金属片との接合の機械的強度が強くすることができ、接合は強酸耐性があるため、ダイヤモンド工具の接着、MEMS装置、表面デバイス、バルク半導体デバイス、電極として、さまざまな構造、耐久性を持たせることができ、ダイヤモンドの化学的安定性を利用する高信頼性PHセンサや、電気分解用電極、分子認識デバイス、パワーデバイス、Ruや多種金属のもつ触媒機能等を組み合わせた複合機能性デバイスへの応用、また、それらの高温度動作を可能とすることができ、産業上の利用可能性が高い。 Since the present invention can be the mechanical strength of the bond between the diamond surface and the metal strip is stronger, bonding is strong resistance, adhesion of the diamond tool, MEMS device, the surface device, the bulk semiconductor devices, as electrode, a variety of structure, it is possible to have a durability, combinations and reliability PH sensor utilizing the chemical stability of diamond, electrolysis electrodes, molecular recognition devices, power devices, a catalytic function, etc. with the Ru and wide metal composite functional application to a device, also, it is possible to enable their high temperature operation, has high industrial applicability.

ショットキー電極周囲に不活化のための保護絶縁膜を設けた構造 Structure in which a protective insulating film for inactivation around the Schottky electrode それぞれの金属片より大きな面積のRu被膜で被覆した後の耐久性試験。 Durability test was coated with Ru film of a larger area than each of the metal pieces. 各種環境下におけるダイヤモンド表面上の金属残存率(%) Metal remaining ratio on the diamond surface under different environments (%)

Claims (5)

  1. ダイヤモンド表面と金属片との接合を、金属片とダイヤモンド表面の非結合面に、当該金属片を覆いつくす当該金属片より面積の大きいRu被膜を設けることにより保護したダイヤモンド表面と金属片との接合保護構造であって、前記ダイヤモンドが電気伝導性であり、前記金属片と前記電気伝導性のダイヤモンドとがオーム性の電気伝導界面を持つことを特徴とする接合保護構造。 The bonding between the diamond surface and the metal strip, the non-binding surface of the metal piece and the diamond surface, the bonding of the protective diamond surface and the metal strip by providing a large Ru coating area than the metal piece completely covering the metal strip a protective structure, said diamond is electrically conductive, bonding protective structure and said metal piece and the electrical conductivity of the diamond is characterized by having the ohmic electrical conduction interfaces.
  2. 前記電気伝導性ダイヤモンドがダイヤモンド半導体である請求項1に記載された接合保護構造。 It has been bonded protective structure according to claim 1 wherein the electrically conductive diamond is a diamond semiconductor.
  3. オーミック電極を形成する前記金属片がTi/Ptの積層構造であることを特徴とする請求項1又は2に記載された接合保護構造。 It has been bonded protective structure according to claim 1 or 2, wherein the metal strip is characterized in that it is a laminated structure of Ti / Pt which forms an ohmic electrode.
  4. 前記Ru被膜上にさらに異なる金属被膜を設置したことを特徴とする請求項1乃至のいずれか1項に記載された接合保護構造。 It has been bonded protective structure according to any one of claims 1 to 3, characterized in that it has established a further different metal coating on the Ru film.
  5. 前記Ru被膜上に設置される前記金属被膜がTi,Pt,Au,Ni,Moから選ばれる金属であることを特徴とする請求項に記載された接合保護構造。 Bonding protective structure according to claim 4, wherein the metal coating is placed on the Ru film is a metal selected Ti, Pt, Au, Ni, from Mo.
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