JP2005233786A - Needle-like sample for local analysis, sample holder assembly, local analyzer and method for manufacturing needle-like sample for local analysis - Google Patents
Needle-like sample for local analysis, sample holder assembly, local analyzer and method for manufacturing needle-like sample for local analysis Download PDFInfo
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本発明は，電界イオン顕微鏡又はアトムプローブ電界イオン顕微鏡等の局所分析装置に好適な局所分析用針状試料に係り，特に，局所分析用針状試料，局所分析用針状試料を保持する試料ホルダ組立体，局所分析装置，及び局所分析用針状試料の作製方法に関する。 The present invention relates to a needle sample for local analysis suitable for a local analyzer such as a field ion microscope or an atom probe field ion microscope, and more particularly, a needle sample for local analysis, a sample holder for holding a needle sample for local analysis. The present invention relates to an assembly, a local analyzer, and a method for producing a needle sample for local analysis.
磁気記録の高密度化や電子デバイスの微細化の進展は，材料研究やプロセス技術の進歩に負うところが大きいが，進歩の原動力として分析技術も着実な進歩を続けている。特に，高密度化及び微細化に応じて，より微小な領域の構造や性質を調べる技術が要求されており，求められる空間分解能は，ミクロンレベルからナノメートルレベルないし原子レベルまで達しつつある。 Advances in materials recording and process technology greatly depend on the progress of high-density magnetic recording and miniaturization of electronic devices, but analytical technology continues to make steady progress as the driving force of progress. In particular, as the density and miniaturization increase, a technique for examining the structure and properties of smaller regions is required, and the required spatial resolution is reaching from the micron level to the nanometer level to the atomic level.
原子レベルでの局所分析技術として近年注目を集めているものに，電界イオン顕微鏡（ＦＩＭ）及びアトムプローブ電界イオン顕微鏡（アトムプローブ）がある。ＦＩＭ及びアトムプローブは，針状に整形した試料に数ｋＶから１０ｋＶオーダーの高電圧を印加し，先端に生じる高電界を利用して試料先端部分の構造を調べる技術である。ＦＩＭにおいては，まず真空チャンバー内に導入されたイメージングガスが試料先端近傍でイオン化する。イオン化した物質は，電界に導かれて試料に対向したマイクロチャネルプレートなどの検出器側に移動し，結像する。この結果，試料先端部分の構造が原子分解能で観察できる。一方，アトムプローブは，ＦＩＭの機能を拡張した分析装置で，高電界により試料先端部分の原子そのものを電界蒸発させ，電界蒸発により生じたイオンを質量分析することにより試料先端の物質が同定できる。電界蒸発は，試料の先端面から順次起こっていくため，試料先端からの原子の深さ方向分布を原子レベルの分解能で調べることができる。 Recently, field ion microscopes (FIM) and atom probe field ion microscopes (atom probes) are attracting attention as local analysis techniques at the atomic level. FIM and atom probe are techniques for applying a high voltage on the order of several kV to 10 kV to a sample shaped like a needle and examining the structure of the sample tip using a high electric field generated at the tip. In FIM, the imaging gas introduced into the vacuum chamber is first ionized in the vicinity of the sample tip. The ionized substance is guided to an electric field and moves to the detector side such as a microchannel plate facing the sample, and forms an image. As a result, the structure of the sample tip can be observed with atomic resolution. On the other hand, the atom probe is an analyzer that expands the function of the FIM, and the substance at the tip of the sample can be identified by subjecting the atom itself at the tip of the sample to field evaporation with a high electric field and mass analysis of ions generated by the field evaporation. Since field evaporation occurs sequentially from the tip surface of the sample, the depth distribution of atoms from the sample tip can be examined with atomic resolution.
近年，検出器部分の改良により，３次元アトムプローブ（トモグラフィックアトムプローブ又はポジションセンシティブアトムプローブ）と呼ばれる技術が登場している。３次元アトムプローブは，試料先端の原子の位置及び原子種を同時に測定できるため，試料先端の構造を原子分解能で３次元的に再構成できる点で他の局所分析装置にはない特長を有し，注目を集めている。以下，３次元アトムプローブを含むアトムプローブ及びＦＩＭを総称して「ＡＰＦＩＭ」と呼ぶ。 In recent years, a technique called a three-dimensional atom probe (tomographic atom probe or position sensitive atom probe) has appeared due to improvements in the detector portion. The 3D atom probe can measure the position and species of the atom at the tip of the sample at the same time, so it has a feature not available in other local analyzers in that the structure at the tip of the sample can be reconstructed three-dimensionally with atomic resolution. , Attracting attention. Hereinafter, the atom probe and the FIM including the three-dimensional atom probe are collectively referred to as “APFIM”.
ＡＰＦＩＭは高電界を利用するため，分析する試料には金属等の導電性の高い固体を用いる場合が多い。しかも，試料の形状は，一般的には，先端径１００ｎｍ前後若しくはそれ以下の針状にする必要がある。このため，従来は，ワイヤ形状をもつ均一な材料から電解研磨して針状の試料を作製するのが一般的である。薄膜や多層膜の分析にＡＰＦＩＭを採用するために，電解研磨で作った針の先端に所望の膜を成膜する手法が試みられた。しかし，薄膜や多層膜の分析として本来要求されるのは，実際に平板な基板または下地層の上に形成された膜そのものを分析することである。このため，ＡＰＦＩＭ分析用の針の先端に新たな薄膜を成膜する技術では，本来の目的を達成することができなかった。 Since APFIM uses a high electric field, a highly conductive solid such as a metal is often used as a sample to be analyzed. Moreover, the shape of the sample generally needs to be a needle shape with a tip diameter of around 100 nm or less. For this reason, conventionally, a needle-shaped sample is generally produced by electrolytic polishing from a uniform material having a wire shape. In order to employ APFIM for the analysis of thin films and multilayer films, an attempt was made to deposit a desired film on the tip of a needle made by electropolishing. However, what is originally required for the analysis of thin films and multilayer films is to analyze the film itself actually formed on the flat substrate or the underlayer. For this reason, the original purpose cannot be achieved by the technique of forming a new thin film on the tip of the needle for APFIM analysis.
一方，微細加工技術の進歩によって，試料作製上の制約を除去し，従来では不可能だった薄膜のＡＰＦＩＭによる分析例が報告され始めている。Ｄ．Ｊ．ラーソン（Larson）らは，リソグラフィ技術によって作った柱状構造体の上に所望の磁性積層膜を形成し，その後柱状構造体を折り取ったものを金属ワイヤの先端に接着し，磁性積層膜を含む先端部分を収束イオンビーム（ＦＩＢ）で加工することによってＡＰＦＩＭ分析用の針状試料を作製し，３次元アトムプローブで分析することに成功している。さらに，Ｄ．Ｊ．ラーソンらは，ダイヤモンドの微粒子をマスクとして用いることにより，０．５ｍｍ角に切断したＳｉ基板上の薄膜を加工して円錐状の構造を形成し，その先端部分の質量スペクトルを得ている。 On the other hand, with the progress of microfabrication technology, the sample production restrictions have been removed, and thin film APFIM analysis examples that have been impossible in the past have started to be reported. D. J. et al. Larson et al. Formed a desired magnetic layered film on a columnar structure made by lithography technology, and then bonded the folded structure of the columnar structure to the tip of the metal wire to include the magnetic layered film A needle-like sample for APFIM analysis was produced by processing the tip portion with a focused ion beam (FIB), and was successfully analyzed with a three-dimensional atom probe. In addition, D.C. J. et al. Larson et al. Processed a thin film on a Si substrate cut into 0.5 mm square by using diamond fine particles as a mask to form a conical structure, and obtained a mass spectrum at the tip.
また，平面状試料を直接ＦＩＢで加工して円錐状の構造を作り，それを折り取って金属ワイヤ先端に接着することで，針状試料を作製する技術も提案されている（例えば，特許文献１参照。）。平面状試料から円錐状の構造を作る手法を用いることにより，原理的には，平面状試料表面の所望の位置を含む針状試料が作製可能である。
上述したＡＰＦＩＭ測定用の試料作製方法は，従来になかったＡＰＦＩＭの適用可能性を示すものではあるが，いくつかの課題も有している。 The above-described sample preparation method for APFIM measurement shows applicability of APFIM, which has not been heretofore, but has some problems.
リソグラフィによって小さな柱状構造体を作り，柱状構造体の上に分析対象となる膜を成膜し被測定試料とする方法では，実際に基板の平面上に成膜した膜の構造と全く同一になる保証はない。また、成膜は柱状構造体の形成後であるため、基板上に形成された膜の所望の位置を分析する目的には使用することができない。即ち，磁気記録媒体や素子の開発等の分野にＡＰＦＩＭ分析を応用する場合に望まれるのは，記録媒体や素子として既に形成された膜の所望の位置の構造を調べることであるのに，柱状構造体を形成した後に成膜する方法では、本来の目的を達成することができない。 In a method in which a small columnar structure is formed by lithography and a film to be analyzed is formed on the columnar structure and used as a sample to be measured, the structure of the film actually formed on the plane of the substrate is exactly the same. There is no guarantee. Further, since the film formation is after the formation of the columnar structure, it cannot be used for the purpose of analyzing a desired position of the film formed on the substrate. That is, when applying APFIM analysis to the field of magnetic recording medium and element development, etc., it is desirable to investigate the structure of a desired position of a film already formed as a recording medium or element. In the method of forming a film after forming a structure, the original purpose cannot be achieved.
分析対象となる膜を成膜する柱状構造体は，一般に直径がμｍオーダーに整形される。柱状構造体を折り取って使用する場合は、極めて小さい棒状となるため取扱いが困難であり，歩留まりが低くなる。さらに，柱状構造体を折り取ってワイヤ先端に接着する方法では，折り取った端面の平坦性が保証されないため，柱状構造体をワイヤに接着するのが困難である。このため、接着時の再現性や歩留まりが低下する。さらに，結果として得られた針状試料の軸方向と，針状試料先端に存在する測定対象膜の法線方向とを再現性良く所望の角度に設定するのは困難である。この結果、膜の結晶方位を正しく把握することをも困難になり，分析技術としては問題である。 A columnar structure for forming a film to be analyzed is generally shaped to have a diameter on the order of μm. When the columnar structure is used after being broken, it is extremely small and is difficult to handle, resulting in a low yield. Further, in the method in which the columnar structure is broken and bonded to the wire tip, the flatness of the broken end surface is not guaranteed, and it is difficult to bond the columnar structure to the wire. For this reason, the reproducibility and yield at the time of adhesion | attachment fall. Furthermore, it is difficult to set the axial direction of the needle-like sample obtained as a result and the normal direction of the measurement target film existing at the tip of the needle-like sample at a desired angle with good reproducibility. As a result, it becomes difficult to correctly grasp the crystal orientation of the film, which is a problem as an analysis technique.
ダイヤモンドの微粒子をマスクとして薄膜上に円錐状の構造を用いる方法は，微粒子の配置が偶然に左右されるため，形成位置の制御が困難である。したがって，薄膜上の所望の位置を分析することは困難である。また，得られた針状試料の固定はワイヤ先端への接着であるため，リソグラフィによる方法と同様に，再現性や歩留まりが低く，出来上がった針状試料の先端方向とワイヤの軸方向との角度の制御も困難である。 The method of using a conical structure on a thin film with diamond fine particles as a mask is difficult to control the formation position because the arrangement of fine particles is affected by chance. Therefore, it is difficult to analyze a desired position on the thin film. In addition, since the obtained needle-like sample is fixed to the wire tip, the reproducibility and yield are low as in the lithography method, and the angle between the tip direction of the finished needle-like sample and the axial direction of the wire is low. It is also difficult to control.
一方，平面状試料を直接ＦＩＢで加工して円錐状の針状試料を作る方法は，実際の加工プロセスでは，所望の位置周辺の十分広い範囲に対して十分な深さでＦＩＢのみを用いて削り取らなければならないため，加工に時間がかかる。また，作製できる円錐状の部分は微小なため，取扱いが困難である。さらに，得られた円錐状の針状試料を平面状試料から折り取ってワイヤに接着する際の再現性や歩留まりが低く，更に針状部分の先端の向く方向の制御は困難である。 On the other hand, the method of making a conical needle sample by directly processing a flat sample with FIB is to use only FIB at a sufficient depth for a sufficiently wide range around the desired position in the actual processing process. Since it must be scraped off, processing takes time. In addition, the conical part that can be produced is very small and difficult to handle. Furthermore, the reproducibility and yield when the obtained conical needle-shaped sample is broken from the flat sample and bonded to the wire is low, and it is difficult to control the direction of the tip of the needle-shaped portion.
本発明は、上記した従来技術の欠点を除くためになされたものであって、その目的とするところは、薄膜状又は平面状の試料から所望の位置を抽出して作製することができ，試料作製時及び作製後の取扱いが容易で，ＡＰＦＩＭ導入時の試料の角度制御が容易且つ再現性が高い局所分析用針状試料，試料ホルダ組立体，局所分析装置，及び局所分析用針状試料の作製方法を提供することにある。 The present invention has been made to eliminate the above-mentioned drawbacks of the prior art, and the object of the present invention is to extract a desired position from a thin-film or planar sample, Easy to handle during and after fabrication, easy to control the angle of the sample when introducing APFIM, and highly reproducible needle sample for local analysis, sample holder assembly, local analyzer, and needle sample for local analysis It is to provide a manufacturing method.
上記目的を達成するために、本発明の第１の特徴は，（イ）第１主面及び第１主面に対向する第２主面を有する基板部と，（ロ）第１主面から突出した柱状部と，（ハ）柱状部の基板部に接続された側とは反対側の端部から柱状部が突出する方向に向かって錐体をなすように先鋭化された針状部とを備え，針状部の先端部に局所分析用の被測定領域を含む局所分析用針状試料であることを要旨とする。 In order to achieve the above object, the first feature of the present invention is that (a) a first main surface and a substrate portion having a second main surface opposite to the first main surface; and (b) from the first main surface. A protruding columnar part, and (c) a needle-shaped part sharpened so as to form a cone in a direction in which the columnar part protrudes from an end opposite to the side connected to the substrate part of the columnar part; And the needle-like sample for local analysis including the measurement region for local analysis at the tip of the needle-like part.
第２の特徴は，（イ）第１主面及び第１主面に対向する第２主面を有する基板部と，（ロ）第１主面から突出した柱状部と，（ハ）柱状部の基板部に接続された側とは反対側の端部から柱状部が突出する方向に向かって錐体をなすように先鋭化され，先鋭化された先端部に局所分析用の被測定領域を含む針状部と，（ニ）基板部の第２主面と接着するための平坦面を有する棒状の導電性ワイヤ部とを備える試料ホルダ組立体であることを要旨とする。 The second feature is (a) a first main surface and a substrate portion having a second main surface opposite to the first main surface, (b) a columnar portion protruding from the first main surface, and (c) a columnar portion. The region to be measured for local analysis is sharpened so as to form a cone from the end opposite to the side connected to the substrate part in the direction in which the columnar part protrudes. The gist of the invention is a sample holder assembly including a needle-like portion including a rod-like conductive wire portion having a flat surface for bonding to the second main surface of the substrate portion.
第３の特徴は，（イ）第１主面及び第１主面に対向する第２主面を有する基板部，第１主面から突出した柱状部，柱状部の基板部に接続された側とは反対側の端部から柱状部が突出する方向に向かって錐体をなすように先鋭化され，先鋭化された先端部に局所分析用の被測定領域を含む針状部，及び基板部の第２主面に接続され，基板部を保持する試料ホルダからなる試料ホルダ組立体を固定する固定部と，（ロ）固定部を介して針状部の被測定領域をイオン化するための電圧を供給する電圧供給部と、（ハ）柱状部の針状部の先端を通る中心軸上において被測定領域の先端に対向し、被測定領域を分析する分析部とを備える局所分析装置であることを要旨とする。 The third feature is (a) a substrate portion having a first principal surface and a second principal surface facing the first principal surface, a columnar portion protruding from the first principal surface, and a side connected to the substrate portion of the columnar portion. A needle-like part that is sharpened so as to form a cone in the direction in which the columnar part protrudes from the end opposite to the side, and includes a measurement region for local analysis at the sharpened tip part, and a substrate part And (b) a voltage for ionizing the measurement area of the needle-like portion via the fixing portion. The fixing portion is connected to the second main surface of the substrate and holds the sample holder assembly including the sample holder that holds the substrate portion. (C) a local analyzer comprising: an analysis unit that analyzes the region to be measured, facing the tip of the region to be measured on the central axis passing through the tip of the needle-like portion of the columnar part This is the gist.
第４の特徴は，（イ）被測定領域を含む構造体を切削し，第１主面及び第１主面に対向する第２主面を有する基板部及び基板部から突出した柱状部を形成するステップと，（ロ）柱状部の基板部に接続された側とは反対側の端部から柱状部が突出する方向に向かって錐体をなすように先鋭化し，先鋭化した先端部に被測定領域を含む針状部を形成するステップとを備える局所分析用針状試料の作製方法であることを要旨とする。 The fourth feature is (a) cutting a structure including a region to be measured to form a first main surface and a substrate portion having a second main surface opposite to the first main surface and a columnar portion protruding from the substrate portion. And (b) sharpening from the end of the columnar portion opposite to the side connected to the substrate portion to form a cone in the direction in which the columnar portion protrudes, and covering the sharpened tip portion The gist of the present invention is a method for producing a needle-like sample for local analysis comprising a step of forming a needle-like part including a measurement region.
本発明によれば、薄膜状又は平面状の試料から所望の位置を抽出して作製することができ，試料作製時及び作製後の取扱いが容易で，ＡＰＦＩＭ導入時の試料の角度制御が容易且つ再現性が高い局所分析用針状試料，試料ホルダ組立体，局所分析装置，及び局所分析用針状試料の作製方法を提供することができる。 According to the present invention, a desired position can be extracted from a thin-film or planar sample, and the sample can be easily handled during and after the fabrication, and the angle of the sample can be easily controlled when the APFIM is introduced. It is possible to provide a needle sample for local analysis, a sample holder assembly, a local analyzer, and a method for producing a needle sample for local analysis with high reproducibility.
次に、図面を参照して、本発明の実施の形態を説明する。以下の図面の記載において、同一又は類似の部分には同一又は類似の符号を付している。また、以下に示す実施の形態は、この発明の技術的思想を具体化するための装置や方法を例示するものであって、この発明の技術的思想は、構成部品の材質、形状、構造、配置等を下記のものに特定するものでない。この発明の技術的思想は、特許請求の範囲において、種々の変更を加えることができる。 Next, embodiments of the present invention will be described with reference to the drawings. In the following description of the drawings, the same or similar parts are denoted by the same or similar reference numerals. Further, the embodiments described below exemplify apparatuses and methods for embodying the technical idea of the present invention, and the technical idea of the present invention includes the material, shape, structure, The layout is not specified as follows. The technical idea of the present invention can be variously modified within the scope of the claims.
＜局所分析用針状試料構造＞
本発明の実施の形態に係る局所分析用針状試料１は，図１に示すように，第１主面及び第１主面に対向する第２主面を有する基板部２と，第１主面から突出した柱状部３と，柱状部３の基板部２に接続された側とは反対側の端部から，柱状部３が突出する方向に向かって錐体をなすように先鋭化され，先鋭化された先端部に局所分析用の被測定領域７４を含む針状部４とを備える。
<Needle sample structure for local analysis>
As shown in FIG. 1, a needle sample 1 for local analysis according to an embodiment of the present invention includes a first main surface and a substrate portion 2 having a second main surface opposite to the first main surface, and a first main surface. The columnar part 3 protruding from the surface and the end of the columnar part 3 opposite to the side connected to the substrate part 2 are sharpened so as to form a cone in the direction in which the columnar part 3 protrudes, A sharpened tip portion is provided with a needle-like portion 4 including a measurement region 74 for local analysis.
基板部２は，例えば，縦横５００μｍ四方，厚さ２００〜４００μｍの箱形である。基板部２の具体的な材料及び大きさは，分析対象の材料によってそれぞれ異なるが，例えば半導体基板上に形成した膜の構造等を分析する場合は，所望の半導体基板（例えばシリコン（Ｓｉ））を用いることが出来る。柱状部３は，基板部２と一体化しており，基板部２の第１主面の中央部から「第１の方向」に向かって縦横４０μｍ四方，高さ２００〜４００μｍに突出している。なお，「第１の方向」は，分析対象となる層の結晶方位等を考慮することにより，決定されるのが好ましい。即ち，図１に示すように，第１主面の伸延する方向に対して垂直方向を「第１の方向」としてもよいし，第１主面の伸延する方向に対して斜め方向を「第１の方向」としてもよい。 The substrate part 2 is, for example, a box shape having a length and width of 500 μm square and a thickness of 200 to 400 μm. The specific material and size of the substrate unit 2 vary depending on the material to be analyzed. For example, when analyzing the structure of a film formed on a semiconductor substrate, a desired semiconductor substrate (for example, silicon (Si)) Can be used. The columnar part 3 is integrated with the substrate part 2 and protrudes from the central part of the first main surface of the substrate part 2 in a 40 μm square and a height of 200 to 400 μm in the “first direction”. The “first direction” is preferably determined in consideration of the crystal orientation of the layer to be analyzed. That is, as shown in FIG. 1, the direction perpendicular to the direction in which the first main surface extends may be defined as the “first direction”, and the direction oblique to the direction in which the first main surface extends is defined as “first direction”. 1 direction ".
図２に示すように，柱状部３と基板部２との境界部分に，柱状部３から基板部２方向に向かってテーパー状に広がるテーパー部３ａを配置すれば，柱状部３の機械的強度が向上する。テーパー部３ａの配置する位置は特に限定しないが，例えば，第１主面から高さ２０μｍ付近に配置すれば，一定の目的を達成可能である。 As shown in FIG. 2, the mechanical strength of the columnar portion 3 can be obtained by arranging a tapered portion 3 a that extends in a tapered shape from the columnar portion 3 toward the substrate portion 2 at the boundary portion between the columnar portion 3 and the substrate portion 2. Will improve. The position at which the tapered portion 3a is disposed is not particularly limited. For example, if the tapered portion 3a is disposed at a height of about 20 μm from the first main surface, a certain purpose can be achieved.
針状部４は，図３に示すように，先端径Ｌが約９０ｎｍの針状の被測定領域７４を有する。先端径Ｌは，後述する局所分析装置５で発生させる電界強度により適宜変更可能であるが，一般的な局所分析装置においては，先端径Ｌが約２００ｎｍ以下のものが採用可能である。被測定領域７４には，導電性薄膜からなる第ｐ被測定膜７４ｐ，第ｑ被測定膜７４ｑ，第ｒ被測定膜７４ｒ，第ｓ被測定膜７４ｓ，第ｔ被測定膜７４ｔが順次積層された積層膜が含まれている。被測定領域７４を構成する第ｐ被測定膜７４ｐ，第ｑ被測定膜７４ｑ，第ｒ被測定膜７４ｒ，第ｓ被測定膜７４ｓ，第ｔ被測定膜７４ｔの具体的な材料及び大きさは分析対象の材料によって異なるが，例えば基板上に形成された磁気記録媒体や素子の結晶構造を測定したい場合は，Ｃｏ，Ｆｅ，Ｎｉ等の磁性体材料，銅（Ｃｕ）等の導電性材料等が用いられる。なお，図３に示す針状部４においては，第ｐ被測定膜７４ｐ，第ｒ被測定膜７４ｒ，第ｔ被測定膜７４ｔとしてコバルト鉄（ＣｏＦｅ）層が配置され，第ｑ被測定膜７４ｑ，第ｓ被測定膜７４ｓとしてＣｕ層が配置されている。第ｐ被測定膜７４ｐ，第ｑ被測定膜７４ｑ，第ｒ被測定膜７４ｒ，第ｓ被測定膜７４ｓ，第ｔ被測定膜７４ｔの厚さＴp，Ｔq，Ｔr，Ｔs，Ｔtは，それぞれ１〜５ｎｍ程度である。 As shown in FIG. 3, the needle-like portion 4 has a needle-like measurement region 74 having a tip diameter L of about 90 nm. The tip diameter L can be appropriately changed depending on the electric field intensity generated by the local analyzer 5 described later. However, in a general local analyzer, a tip having a tip diameter L of about 200 nm or less can be employed. In the measurement region 74, a p-th film to be measured 74p, a q-th film to be measured 74q, an r-th film to be measured 74r, an s-th film to be measured 74s, and a t-th film to be measured 74t are sequentially stacked. Laminated film is included. Specific materials and sizes of the p-th film to be measured 74p, the q-th film to be measured 74q, the r-th film to be measured 74r, the s-th film to be measured 74s, and the t-th film to be measured 74t constituting the measurement region 74 are as follows. For example, if you want to measure the crystal structure of a magnetic recording medium or element formed on a substrate, magnetic material such as Co, Fe, or Ni, conductive material such as copper (Cu), etc. Is used. In the needle-like portion 4 shown in FIG. 3, a cobalt iron (CoFe) layer is disposed as the p-th film to be measured 74p, the r-th film to be measured 74r, and the t-th film to be measured 74t, and the q-th film to be measured 74q. A Cu layer is disposed as the s-th film 74s to be measured. The thicknesses Tp, Tq, Tr, Ts, and Tt of the p-th film to be measured 74p, the q-th film to be measured 74q, the r-th film to be measured 74r, the s-th film to be measured 74s, and the t-th film to be measured 74t are 1 respectively. About 5 nm.
以下に示す局所分析装置の説明により更に明確となるが，実施の形態に係る局所分析用針状試料１によれば，先端に被測定領域７４を含む針状部４を有する柱状部３に一体化した基板部２を備える。このため，基板部２をピンセット等で挟むことにより，局所分析用針状試料１の作製時及び作製後の取扱いが容易になる。また，基板部２の第２主面は平坦であるため，後述する局所分析装置５内に固定するための導電性ワイヤ１１の先端に局所分析用針状試料１を固定するのが容易になるため，図１に示す局所分析用針状試料１によれば，分析の再現性が高くなると共に，局所分析用針状試料１の作製時又は分析装置導入時の歩留まりが向上する。また，図１に示す局所分析用針状試料１は，以下に述べるように，分析対象となる被測定領域７４として予め指定された所望の位置の周囲を選択的に切削することにより得られるので，平板状の試料から調べたい部分を選択的に抽出した局所分析用針状試料１が提供できる。 As will be further clarified by the following description of the local analyzer, according to the needle sample 1 for local analysis according to the embodiment, it is integrated with the columnar part 3 having the needle-like part 4 including the measurement region 74 at the tip. The substrate portion 2 is provided. For this reason, sandwiching the substrate part 2 with tweezers or the like facilitates handling during and after the production of the needle sample 1 for local analysis. Further, since the second main surface of the substrate unit 2 is flat, it is easy to fix the needle sample 1 for local analysis to the tip of the conductive wire 11 for fixing in the local analyzer 5 described later. Therefore, according to the needle sample 1 for local analysis shown in FIG. 1, the reproducibility of the analysis is improved and the yield at the time of producing the needle sample 1 for local analysis or introducing the analyzer is improved. Further, as will be described below, the needle sample 1 for local analysis shown in FIG. 1 can be obtained by selectively cutting around a desired position designated in advance as a measurement region 74 to be analyzed. The needle-like sample 1 for local analysis can be provided by selectively extracting the part to be examined from the flat sample.
＜局所分析用針状試料の第１の作製方法＞
次に，図４〜図８を用いて実施の形態に係る局所分析用針状試料１の第１の作製方法について説明する。なお，以下に述べる局所分析用針状試料１の作製方法は一例であり，この変形例を含めて，これ以外の種々の作製方法により実現可能であることは勿論である。
<First production method of needle-like sample for local analysis>
Next, the 1st preparation method of the needle-shaped sample 1 for local analysis which concerns on embodiment using FIG. 4 ~ FIG. 8 is demonstrated. The method for producing the needle sample 1 for local analysis described below is an example, and it is needless to say that it can be realized by various other production methods including this modification.
（イ）まず，表面にボロン（Ｂ）を１０20ｃｍ-3ドープした厚さ６００μｍのＳｉからなる基板７１を用意する。この基板７１を希フッ酸処理することにより表面の自然酸化膜を除去した後，直ちに成膜装置に導入し，タンタル（Ｔａ）からなる第１のシード層７２をスパッタ法により厚さ１０ｎｍ程度に堆積する。続いて，図４に示すように，第１のシード層７２の表面にＣｏＦｅからなる第２のシード層７３をスパッタ法により厚さ１５ｎｍ程度に堆積する。 (A) First, a substrate 71 made of Si having a thickness of 600 μm and boron (B) doped at 10 20 cm −3 on the surface is prepared. After removing the natural oxide film on the surface of the substrate 71 by dilute hydrofluoric acid treatment, the substrate 71 is immediately introduced into the film forming apparatus, and the first seed layer 72 made of tantalum (Ta) is formed to a thickness of about 10 nm by sputtering. accumulate. Subsequently, as shown in FIG. 4, a second seed layer 73 made of CoFe is deposited on the surface of the first seed layer 72 to a thickness of about 15 nm by sputtering.
（ロ）次に，図５に示すように，第２のシード層７３の表面にＣｕからなる第１被測定膜７４ａを堆積する。続いて，第１被測定膜７４ａの表面にＣｏＦｅからなる第２被測定膜７４ｂを堆積する。第２被測定膜７４ｂの表面にＣｕからなる第３被測定膜７４ｃを堆積し，第３被測定膜７４ｃの表面にＣｏＦｅからなる第４被測定膜７４ｄを堆積する。このように，Ｃｕ層とＣｏＦｅ層とを，それぞれ例えば１０層ずつ全部で２０層程度に積層し，被測定領域７４を形成する。そして，最上段の第ｔ被測定膜７４ｔの表面にニッケル鉄（ＮｉＦｅ）からなるキャップ層をスパッタ法により厚さ１５０ｎｍ程度に堆積し，成膜装置から取り出す。 (B) Next, as shown in FIG. 5, a first film to be measured 74 a made of Cu is deposited on the surface of the second seed layer 73. Subsequently, a second measured film 74b made of CoFe is deposited on the surface of the first measured film 74a. A third measured film 74c made of Cu is deposited on the surface of the second measured film 74b, and a fourth measured film 74d made of CoFe is deposited on the surface of the third measured film 74c. In this way, the Cu region and the CoFe layer are laminated in a total of about 20 layers, for example, 10 layers each to form the measurement region 74. Then, a cap layer made of nickel iron (NiFe) is deposited on the surface of the uppermost t-th film to be measured 74t by a sputtering method to a thickness of about 150 nm and taken out from the film forming apparatus.
（ハ）次に，図５に示すように、被測定領域７４が形成された側の面の基板７１を精密切削装置等により選択的に機械的に切削し，図６に示すように，第１のシード層７２Ａ，７２Ｂ，・・・・・，第２のシード層７３Ａ，７３Ｂ，・・・・・，被測定膜７４Ａ，７４Ｂ，・・・・・を先端に有する例えば高さ２００μｍ，４０μｍ角の四角柱構造７６Ａ，７６Ｂ，・・・・・，を複数個形成する。精密切削装置としては，ダイシングソー，マシンニングセンタ，フライス盤，超音波振動切削装置，噴射型切削装置，ワイヤリー，ダイアモンドブレード等が使用可能である。続いて，図７に示すように，四角柱構造７６Ａを中心として周囲５００μｍ四方を、精密切削装置等で機械的に切削し，縦横５００μｍ，厚さ４００μｍの基板部２Ａと基板部２Ａに一体化した四角柱状の柱状部３Ａを形成する。 (C) Next, as shown in FIG. 5, the substrate 71 on the surface on which the region to be measured 74 is formed is selectively mechanically cut by a precision cutting device or the like, and as shown in FIG. 1 seed layer 72A, 72B,..., Second seed layer 73A, 73B,..., Measured film 74A, 74B,. A plurality of 40 μm square structures 76A, 76B,... Are formed. As the precision cutting device, a dicing saw, a machining center, a milling machine, an ultrasonic vibration cutting device, a jet type cutting device, a wireless device, a diamond blade, or the like can be used. Subsequently, as shown in FIG. 7, the square 500 μm square is mechanically cut with a precision cutting device or the like around the square columnar structure 76A, and integrated into the substrate portion 2A and the substrate portion 2A having a length and width of 500 μm and a thickness of 400 μm. The square columnar portion 3A thus formed is formed.
（ニ）次に，図７に示す結果物をＦＩＢ装置に導入し，図８に示すように，「環状ミル」と呼ばれる方法により，柱状部３Ａの先端部分から柱状部３Ａが突出する方向に向かって錐体をなすように先鋭化する。「環状ミル」とは，ＦＩＢの加工機能の一つであり，円Ｘ，円Ｙの２つの同心円で挟まれた部分のみをＦＩＢにより切削する加工方法である。内側の円Ｙの径ｄを小さくしていくことにより，柱状部３Ａが突出する方向に向かって徐々に径を小さく制御しながら精密に切削していくことが可能である。また，ＦＩＢを用いることにより，被測定膜７４Ａの結晶方位に応じて最適な角度に制御しながら切削することができる。この結果，図１に示すような針状部４が形成できる。 (D) Next, the result shown in FIG. 7 is introduced into the FIB apparatus, and as shown in FIG. 8, in a direction in which the columnar portion 3A protrudes from the tip portion of the columnar portion 3A by a method called “annular mill”. Sharpen to make a cone. The “annular mill” is one of the processing functions of the FIB, and is a processing method in which only the portion sandwiched between two concentric circles X and Y is cut by the FIB. By reducing the diameter d of the inner circle Y, it is possible to cut precisely while controlling the diameter gradually in the direction in which the columnar portion 3A protrudes. Further, by using FIB, cutting can be performed while controlling to an optimum angle according to the crystal orientation of the film to be measured 74A. As a result, a needle-like portion 4 as shown in FIG. 1 can be formed.
本発明の実施の形態に係る局所分析用針状試料１の作製方法によれば，分析対象となる部分、例えば被測定膜７４Ａを含む被測定領域７４等が予め形成された基板７１の所望の位置の周囲を選択的に切削することにより，平板状の試料から調べたい部分を選択的に抽出した局所分析用針状試料１が作製できる。このため，記録媒体や素子が既に形成された平板状の試料から所望の領域を選択的に抽出し，抽出した膜等の微細構造を，ＡＰＦＩＭを用いて調べることができる。 According to the method for producing the needle sample 1 for local analysis according to the embodiment of the present invention, a desired portion of the substrate 71 on which a portion to be analyzed, for example, a measurement region 74 including a measurement film 74A is formed in advance. By selectively cutting around the position, the needle sample 1 for local analysis in which a portion to be examined from the flat sample is selectively extracted can be produced. For this reason, a desired region can be selectively extracted from a flat sample on which a recording medium or an element has already been formed, and the microstructure of the extracted film or the like can be examined using APFIM.
また，実施の形態に係る局所分析用針状試料１の作製方法では，被測定領域７４を先端に含む針状部４が接続された柱状の柱状部３に一体化するように平板状の基板部２を形成する。このため，基板部２をピンセット等で挟むことにより，局所分析用針状試料１の作製時及び作製後の取扱いが容易になる。基板部２から突出した柱状部３の突出する方向は，ＦＩＢにより切削方向を制御しながら精密に切削できるため，被測定膜７４の結晶方位等に合わせて局所分析用針状試料１を作製できる。この結果，局所分析用針状試料１の軸方向と局所分析用針状試料１の先端に存在する所望の被測定膜７４Ａの法線方向とを再現性良く所望の角度に調節でき，高い歩留まり且つ高い精度で測定可能な局所分析用針状試料１が作製できる。 Further, in the method for producing the needle sample 1 for local analysis according to the embodiment, a flat substrate so as to be integrated with the columnar column 3 to which the needle 4 including the region to be measured 74 is connected. Part 2 is formed. For this reason, sandwiching the substrate part 2 with tweezers or the like facilitates handling during and after the production of the needle sample 1 for local analysis. Since the protruding direction of the columnar part 3 protruding from the substrate part 2 can be precisely cut while controlling the cutting direction by FIB, the needle sample 1 for local analysis can be produced in accordance with the crystal orientation of the measured film 74 and the like. . As a result, the axial direction of the needle sample 1 for local analysis and the normal direction of the desired film 74A to be measured existing at the tip of the needle sample 1 for local analysis can be adjusted to a desired angle with high reproducibility and high yield. In addition, the needle sample 1 for local analysis that can be measured with high accuracy can be produced.
＜局所分析用針状試料の第２の作製方法＞
図９〜図１１を用いて、実施の形態に係る局所分析用針状試料１の第２の作製方法を説明する。なお、第２の作製方法では、平板状の基板７１から局所分析用針状試料１を作製する方法の一例を説明する。
<Second Preparation Method of Needle Sample for Local Analysis>
A second method for producing the needle sample 1 for local analysis according to the embodiment will be described with reference to FIGS. In the second manufacturing method, an example of a method for manufacturing the needle sample 1 for local analysis from the flat substrate 71 will be described.
図９に示すように，ボロン（Ｂ）を１０20ｃｍ-3ドープした厚さ６００μｍのＳｉからなる基板７１の表面に５ｍｍ程度の間隔をおいて，測定対象となる部分にレーザーマーカーにより印Ｍを付ける。印Ｍの付け方は任意であり，例えば，被測定領域が平板状試料の表面を含む場合には，選択した被測定領域を中心にした正方形の各頂点をなすように４つの印を付けるなど，測定領域を壊すことなく認識できる方法で付けることが望ましい。続いて，表面に印Ｍが付けられた側の基板７１を精密切削装置等により選択的に切削し，印Ｍを先端に有する高さ２００μｍ，４０μｍ角の四角柱構造７６を形成する。続いて，図１０に示すように，印Ｍを目印として周囲５００μｍ四方を精密切削装置で切削し，柱状部３に一体化した縦横５００μｍ，厚さ４００μｍの基板部２を形成する。 As shown in FIG. 9, the surface of the substrate 71 made of Si having a thickness of 600 μm doped with boron (B) at 10 20 cm −3 is spaced by about 5 mm, and a portion to be measured is marked with a laser marker. Add. The method of marking M is arbitrary. For example, when the measured area includes the surface of a flat sample, four marks are formed so as to form each vertex of a square centering on the selected measured area. It is desirable to attach the measurement area in such a way that it can be recognized without breaking it. Subsequently, the substrate 71 on the surface with the mark M on the surface is selectively cut by a precision cutting device or the like to form a rectangular column structure 76 having a mark M at the tip and a height of 200 μm and a 40 μm square. Subsequently, as shown in FIG. 10, a square 500 μm square is cut with a precision cutting device using the mark M as a mark to form a substrate portion 2 having a length and width of 500 μm and a thickness of 400 μm integrated with the columnar portion 3.
次に，図１０に示す結果物をＦＩＢ装置に導入し，図１１に示すように，柱状部３の先端を，環状ミルにより柱状部３の先端部分から柱状部３が突出する方向に向かって錐体をなすように先鋭化する。この結果，図１に示すような局所分析用針状試料１が形成できる。 Next, the result shown in FIG. 10 is introduced into the FIB apparatus, and as shown in FIG. 11, the tip of the columnar part 3 is moved in the direction in which the columnar part 3 protrudes from the tip part of the columnar part 3 by an annular mill. Sharpen to form a cone. As a result, a needle sample 1 for local analysis as shown in FIG. 1 can be formed.
実施の形態に係る局所分析用針状試料１の第２の作製方法によれば，平板状の基板７１の表面に印Ｍを付け，印Ｍを目印として，四角柱形状の柱状部３及び柱状部３に一体化した基板部２を形成する。このため，平板状の試料から調べたい部分を選択的に抽出して形成することができる。なお、基板７１に薄膜を成長させた後に印Ｍをつけ、印Ｍを目印として柱状部３及び基板部２を形成してもよいことは勿論である。また，得られた局所分析用針状試料１は，基板部２をピンセット等で挟むことにより取扱いが容易になる。このため，局所分析装置５の内部に局所分析用針状試料１を固定する際の再現性が高くなり，より再現性の高い測定を行うことができる。また，構造上の特徴から被測定領域が判別可能な場合は，印Ｍを付けなくても，構造上の特徴を利用して所望の領域を抽出した針状試料１を得ることができるのは勿論である。 According to the second method for producing the needle sample 1 for local analysis according to the embodiment, the mark M is marked on the surface of the flat substrate 71, and the square columnar column 3 and the columnar shape are marked with the mark M as a mark. The substrate part 2 integrated with the part 3 is formed. Therefore, it is possible to selectively extract and form a portion to be examined from a flat sample. Of course, after the thin film is grown on the substrate 71, the mark M may be applied, and the columnar portion 3 and the substrate portion 2 may be formed using the mark M as a mark. In addition, the obtained needle sample 1 for local analysis can be easily handled by sandwiching the substrate portion 2 with tweezers or the like. For this reason, the reproducibility at the time of fixing the needle-shaped sample 1 for local analysis inside the local analyzer 5 becomes high, and measurement with higher reproducibility can be performed. In addition, when the region to be measured can be discriminated from the structural feature, the needle-like sample 1 from which a desired region is extracted using the structural feature can be obtained without the mark M. Of course.
得られた局所分析用針状試料１をイオンミリング装置に導入し，アルゴン（Ａｒ）イオンによる表面クリーニングを行った後に透過型電子顕微鏡で観察した結果を図１２に示す。比較例として，ＦＩＢに導入した後，表面クリーニングを行わないで観察した結果を図１３に示す。図１２，１３中の白い部分がＦＩＢによる切削より形成されたアモルファス層４αを示し，図１２，１３中の黒い部分がアモルファス化しなかった部分を示している。図１３に示すように，表面クリーニングを行わなかった場合は，針状部４の周囲に厚さ２０ｎｍ以上のアモルファス層が観察される。一方，表面クリーニングを行った図１２に示す場合では，アモルファス層４αは認められるものの，厚さは５ｎｍ以下である。この結果から，局所分析用針状試料１を加工する際には，ＦＩＢに加えてイオンミリングによる表面クリーニングを行うことにより，より精度の高い分析が実現可能であることが分かる。 FIG. 12 shows the result of observation with a transmission electron microscope after introducing the obtained needle-like sample 1 for local analysis into an ion milling apparatus and performing surface cleaning with argon (Ar) ions. As a comparative example, FIG. 13 shows the result of observation without surface cleaning after introduction into FIB. The white portions in FIGS. 12 and 13 show the amorphous layer 4α formed by cutting with FIB, and the black portions in FIGS. 12 and 13 show portions that have not been amorphized. As shown in FIG. 13, when surface cleaning is not performed, an amorphous layer having a thickness of 20 nm or more is observed around the needle-like portion 4. On the other hand, in the case shown in FIG. 12 where surface cleaning is performed, the amorphous layer 4α is recognized, but the thickness is 5 nm or less. From this result, it is understood that when processing the needle sample 1 for local analysis, more accurate analysis can be realized by performing surface cleaning by ion milling in addition to FIB.
＜局所分析装置＞
実施の形態に係る局所分析用針状試料１の観察に適した局所分析装置５として，ＡＰＦＩＭの概要を図１４に示す。なお，図１４に示すＡＰＦＩＭは一例であり，各構成部品の材質、形状、構造、配置等は下記のものに限定するものはでない。本発明の実施の形態に係る局所分析装置５は，処理室（チャンバー）１００と，局所分析用針状試料１を処理室１００の内部に固定する固定部１０と，固定部１０を介して局所分析用針状試料１に接続され，局所分析用針状試料１の被測定膜７４に電圧を供給する電圧供給部２０と、被測定膜７４の先端を通る中心軸上において被測定膜７４の先端に対向し、被測定膜７４を分析する分析部６０とを備える。
<Local analyzer>
FIG. 14 shows an outline of APFIM as a local analyzer 5 suitable for observation of the needle sample 1 for local analysis according to the embodiment. The APFIM shown in FIG. 14 is an example, and the material, shape, structure, arrangement, etc. of each component are not limited to the following. A local analyzer 5 according to an embodiment of the present invention includes a processing chamber (chamber) 100, a fixing portion 10 for fixing the needle sample 1 for local analysis inside the processing chamber 100, and a local portion via the fixing portion 10. A voltage supply unit 20 that is connected to the analysis needle sample 1 and supplies a voltage to the measurement film 74 of the local analysis needle sample 1, and the measurement film 74 on the central axis that passes through the tip of the measurement film 74. An analysis unit 60 that faces the tip and analyzes the film to be measured 74 is provided.
処理室１００は，処理室１００内部を真空にするためのステンレス鋼（ＳＵＳ）等からなる金属製のチャンバーであり，フランジ５０の外側に真空ポンプが接続されている。水素（Ｈ2），ヘリウム（Ｈｅ），ネオン（Ｎｅ）等の結像ガスは，バルブ４５を介して処理室１００に接続されたガス供給部４０から処理室１００内に導入される。固定部１０に接続された電圧供給部２０は，局所分析用針状試料１の先端に１０9Ｖ／ｍ程度の負の電界，或いは５×１０10Ｖ／ｎｍ程度の正の電界を生じさせるための電圧を供給する。固定部１０は，局所分析用針状試料１を冷却するための冷却機３０が接続されている。 The processing chamber 100 is a metal chamber made of stainless steel (SUS) or the like for evacuating the processing chamber 100, and a vacuum pump is connected to the outside of the flange 50. An imaging gas such as hydrogen (H 2 ), helium (He), or neon (Ne) is introduced into the processing chamber 100 from a gas supply unit 40 connected to the processing chamber 100 via a valve 45. The voltage supply unit 20 connected to the fixed unit 10 generates a negative electric field of about 10 9 V / m or a positive electric field of about 5 × 10 10 V / nm at the tip of the needle sample 1 for local analysis. Supply voltage for. The fixing unit 10 is connected to a cooler 30 for cooling the needle sample 1 for local analysis.
固定部１０は，図１５に示すように，棒状の導電性ワイヤ１１及び導電性ワイヤ１１に接続された筒状の試料ホルダ１２を有する。導電性ワイヤ１１は，例えば長さ約１ｃｍ，直径約０．５ｍｍ程度のＣｕ，銀（Ａｇ），チタン（Ｔｉ）等からなるワイヤが使用可能であるが，ワイヤの材料や大きさは特に限定されない。試料ホルダ１２は，ＡＰＦＩＭの標準ホルダと互換性をもつように設計された既存の器具を用いることができる。図１５に示す固定部１０においては，ステンレス製の試料ホルダ１２の先端の中央に穴１２ａが設けられ，導電性ワイヤ１１の一方の先端を折り曲げて穴に差し込む等の固定方法により，試料ホルダ１２と導電性ワイヤ１１とが固定可能になっている。導電性ワイヤ１１の試料ホルダ１２に接続されない側の先端に，図１６に示すように，導電性エポキシ樹脂，銀ペースト等からなる導電性接着剤１３により局所分析用針状試料１を固定することで試料ホルダ組立体１０ａが形成できる。導電性接着剤を用いる代わりに，例えば，エポキシ樹脂等の絶縁性接着剤を用いて接着し，その後金属をコーティングするなどの方法で電気的接触を得てもよい。 As shown in FIG. 15, the fixing unit 10 includes a rod-shaped conductive wire 11 and a cylindrical sample holder 12 connected to the conductive wire 11. As the conductive wire 11, for example, a wire made of Cu, silver (Ag), titanium (Ti) or the like having a length of about 1 cm and a diameter of about 0.5 mm can be used, but the material and size of the wire are particularly limited. Not. The sample holder 12 can be an existing instrument designed to be compatible with the APFIM standard holder. In the fixing portion 10 shown in FIG. 15, a hole 12a is provided in the center of the tip of the stainless steel sample holder 12, and the sample holder 12 is fixed by a fixing method such as bending one end of the conductive wire 11 and inserting it into the hole. And the conductive wire 11 can be fixed. As shown in FIG. 16, the needle sample 1 for local analysis is fixed to the tip of the conductive wire 11 on the side not connected to the sample holder 12 with a conductive adhesive 13 made of conductive epoxy resin, silver paste or the like. Thus, the sample holder assembly 10a can be formed. Instead of using the conductive adhesive, for example, an electrical contact may be obtained by a method of bonding using an insulating adhesive such as an epoxy resin and then coating the metal.
分析部６０は，図１４に示すように，局所分析用針状試料１の中心軸が通る位置に対向し，且つ針状部４の先端部に直交する主面を有して配置されたマイクロチャネルプレート６１を備える。更に，分析部６０は，マイクロチャネルプレート６１の主面の伸延する方向と平行な主面を有してマイクロチャネルプレート６１に隣接して配置された蛍光板６２，マイクロチャネルプレート６１及び蛍光板６２の局所分析用針状試料１の中心軸と対向する位置に配置されたプローブホール６３を介して局所分析用針状試料１の先端に対向する検出器６４，及び局所分析用針状試料１の中心軸上に位置し，蛍光板６２を見通す観察窓６５を備える。 As shown in FIG. 14, the analysis unit 60 is a micro-array that has a main surface that is opposed to the position through which the central axis of the needle sample 1 for local analysis passes and that is orthogonal to the tip of the needle-like portion 4. A channel plate 61 is provided. Further, the analysis unit 60 has a main surface parallel to the extending direction of the main surface of the microchannel plate 61 and is disposed adjacent to the microchannel plate 61, the microchannel plate 61, and the local area of the fluorescent plate 62. A detector 64 facing the tip of the local analysis needle-like sample 1 through a probe hole 63 arranged at a position opposite to the central axis of the analysis needle-like sample 1, and the central axis of the local analysis needle-like sample 1 An observation window 65 is provided which is positioned above and allows the fluorescent screen 62 to be seen.
マイクロチャネルプレート６１は，針状部４の先端から放出される被測定膜７４のイオンの位置等を検出可能な二次元のイメージ増倍管である。蛍光板６２は，マイクロチャネルプレート６１により得られた像を検出する。観察窓６５は，蛍光板６２が検出した像を観察する窓である。検出器６４は，針状部４から放出されたイオンを質量分析する。検出器６４は出力装置７０に接続されている。なお，局所分析用針状試料と検出器６４の間には，主に質量分解能を向上させる目的で，イオン化した物質の飛行道程を変化させるリフレクトロンなどが設けられていても良い。 The microchannel plate 61 is a two-dimensional image intensifier capable of detecting the position of ions on the measurement target film 74 emitted from the tip of the needle-like portion 4. The fluorescent plate 62 detects an image obtained by the microchannel plate 61. The observation window 65 is a window for observing an image detected by the fluorescent screen 62. The detector 64 performs mass analysis on the ions emitted from the needle-like portion 4. The detector 64 is connected to the output device 70. Note that a reflectron or the like that changes the flight path of the ionized substance may be provided between the local analysis needle-like sample and the detector 64 mainly for the purpose of improving the mass resolution.
実施の形態に係る局所分析用針状試料１を用いた局所分析装置５によれば，固定部１０の導電性ワイヤ１１の先端に，基板部２を有する局所分析用針状試料１を固定する。局所分析用針状試料１は，基板部２をピンセットなどで挟むことにより取扱いが容易になる。このため，基板部２をもたない錐体の針状試料を固定する場合に比べ，導電性ワイヤ１１の先端に局所分析用針状試料１を固定するのが容易になる。 According to the local analysis device 5 using the local analysis needle sample 1 according to the embodiment, the local analysis needle sample 1 having the substrate portion 2 is fixed to the tip of the conductive wire 11 of the fixing portion 10. . The needle sample 1 for local analysis can be easily handled by sandwiching the substrate 2 with tweezers. For this reason, it becomes easier to fix the needle sample 1 for local analysis to the tip of the conductive wire 11 as compared to the case of fixing the cone needle sample without the substrate portion 2.
＜局所分析装置の測定方法＞
次に，実施の形態に係る局所分析装置５の測定方法について説明する。以下に示す局所分析装置５の測定方法は一例であり，測定条件，測定順序等は，下記のものに限定するものはでない。
<Measurement method of local analyzer>
Next, the measurement method of the local analyzer 5 according to the embodiment will be described. The measurement method of the local analyzer 5 shown below is an example, and the measurement conditions, measurement order, etc. are not limited to the following.
まず，図１５に示すように，導電性ワイヤ１１の一方の先端を折り曲げ，折り曲げた側の導電性ワイヤ１１の先端を試料ホルダ１２に設けられた穴１２ａに差し込んで固定する。続いて，図１に示す局所分析用針状試料１の基板部２をピンセットで挟み，肉眼で観察しながら，図１６に示すように，局所分析装置５の導電性ワイヤ１１の先端に固定する。続いて，導電性ワイヤ１１の先端に固定した局所分析用針状試料１を，図５に示す局所分析装置（ＡＰＦＩＭ）５に導入し，イメージングガスとしてＨ2とＮｅの混合ガスをガス供給部４０から供給し，冷却機３０で局所分析用針状試料１の先端を冷却しながら，電圧供給部２０により局所分析用針状試料１の先端に徐々に電圧を印加する。さらに，局所分析用針状試料１の先端の電界蒸発を助長するために電圧を上げ続け，針状部４の先端の被測定膜７４の構造を表す像を観察する。この過程で，局所分析用針状試料１の先端の軸の角度の調整は、得られる像を見ながら適宜行われる。 First, as shown in FIG. 15, one end of the conductive wire 11 is bent, and the end of the bent conductive wire 11 is inserted into a hole 12 a provided in the sample holder 12 and fixed. Subsequently, the substrate portion 2 of the local analysis needle-shaped sample 1 shown in FIG. 1 is sandwiched with tweezers and fixed to the tip of the conductive wire 11 of the local analysis device 5 as shown in FIG. 16 while observing with the naked eye. . Subsequently, the local analysis needle sample 1 fixed to the tip of the conductive wire 11 is introduced into the local analyzer (APFIM) 5 shown in FIG. 5, and a mixed gas of H 2 and Ne as an imaging gas is supplied to the gas supply unit. The voltage supply unit 20 gradually applies a voltage to the tip of the local analysis needle-shaped sample 1 while being supplied from 40 and cooling the tip of the local analysis needle-shaped sample 1 with the cooler 30. Further, the voltage is continuously raised to promote electric field evaporation at the tip of the local analysis needle-like sample 1, and an image representing the structure of the film to be measured 74 at the tip of the needle-like portion 4 is observed. In this process, the angle of the tip axis of the needle sample 1 for local analysis is adjusted as appropriate while looking at the obtained image.
続いて，局所分析装置５の導電性ワイヤ１１の先端に固定した局所分析用針状試料１の先端に存在する原子の質量分析を行うためのアトムプローブ分析を行う。ＦＩＭ観察の場合と同様に，冷却機３０で局所分析用針状試料１を冷却しながら，電圧供給部２０により局所分析用針状試料１の先端に徐々に電圧を印加し，更に，この電圧の２０％程度の大きさのパルス電圧を重畳する。局所分析用針状試料１の先端に高電界が加えられることにより，局所分析用針状試料１の先端の被測定領域７４の原子が電界蒸発を起こしてイオン化する。イオン化した原子は，プローブホールを通過して検出器６４に検出される。パルス電圧を加えた時間を基準にして，イオンの飛行時間を測定することによって質量分析が可能になる。 Subsequently, atom probe analysis for performing mass analysis of atoms present at the tip of the local analysis needle-like sample 1 fixed to the tip of the conductive wire 11 of the local analyzer 5 is performed. As in the case of FIM observation, while the local analysis needle sample 1 is cooled by the cooler 30, a voltage is gradually applied to the tip of the local analysis needle sample 1 by the voltage supply unit 20. A pulse voltage having a magnitude of about 20% is superimposed. When a high electric field is applied to the tip of the local analysis needle-like sample 1, atoms in the measurement region 74 at the tip of the local analysis needle-like sample 1 cause electric field evaporation to be ionized. The ionized atoms pass through the probe hole and are detected by the detector 64. Mass spectrometry can be performed by measuring the time of flight of ions with reference to the time when the pulse voltage is applied.
実施の形態に係る局所分析用針状試料１を用いた局所分析装置５によれば，取扱いが容易な局所分析用針状試料１を固定部１０に固定することにより，例えば１０個作った局所分析用針状試料１のすべてを失敗することなく固定できる。したがって，図１に示す局所分析用針状試料１を用いた局所分析装置５によれば，分析したい被測定膜７４の原子構造を高い歩留まりで，再現性良く分析できる。 According to the local analyzer 5 using the local analysis needle sample 1 according to the embodiment, by fixing the local analysis needle sample 1 that is easy to handle to the fixing portion 10, for example, 10 local samples are made. All of the analytical needle-like sample 1 can be fixed without failure. Therefore, according to the local analyzer 5 using the needle sample 1 for local analysis shown in FIG. 1, the atomic structure of the film 74 to be measured can be analyzed with high yield and high reproducibility.
図１に示す局所分析用針状試料１を用いて，図１４に示す局所分析装置５でＦＩＭ観察を行った結果を図１７に示す。図１７は，局所分析用針状試料１の先端の被測定膜７４に徐々に電圧を印加し，２ｋＶ付近から輝点が観察され始めた後も更に電圧を印加し続けた結果得られた像を示している。図１７に示す像から明らかなように，図３に示す針状部４の先端の被測定膜７４に形成された第ｔ被測定膜７４ｔ（ＣｏＦｅ層），第ｓ被測定膜７４ｓ（Ｃｕ層），・・・・・，第ｐ被測定膜７４ｐ（Ｃｕ層）に対応して，第ｔ被測定膜の像Ｉｔ，第ｓ被測定膜の像Ｉｓ，・・・・・，第ｐ被測定膜の像Ｉｐがそれぞれ同心円状のコントラストとして明瞭に映っているのが観察できる。
さらに，図１に示す局所分析用針状試料１に対し，図１４に示す局所分析装置５によりアトムプローブ分析を行った結果を図１８に示す。図１に示す局所分析用針状試料１の第ｔ被測定膜の膜厚Ｔｔ，第ｓ被測定膜の膜厚Ｔｓ，・・・・・，第ｐ被測定膜の膜厚Ｔｐの各膜厚にそれぞれ対応して測定される組成比が急峻に変化し，ＣｏＦｅ層とＣｕ層の交互積層構造が形成されていることが明瞭に確認できる。
FIG. 17 shows the result of FIM observation performed by the local analyzer 5 shown in FIG. 14 using the needle sample 1 for local analysis shown in FIG. FIG. 17 shows an image obtained as a result of applying a voltage gradually to the film 74 to be measured at the tip of the needle sample 1 for local analysis and further applying the voltage after the bright spot started to be observed from around 2 kV. Is shown. As apparent from the image shown in FIG. 17, the t-th measured film 74t (CoFe layer) and the s-th measured film 74s (Cu layer) formed on the measured film 74 at the tip of the needle-like portion 4 shown in FIG. ),... Corresponding to the p-th film 74p (Cu layer), the image It of the t-th film, the image Is of the s-th film,. It can be observed that the image Ip of the measurement film is clearly shown as a concentric contrast.
Further, FIG. 18 shows the result of atom probe analysis performed on the local analysis needle sample 1 shown in FIG. 1 by the local analysis device 5 shown in FIG. The film thickness Tt of the t-th film to be measured, the film thickness Ts of the s-th film to be measured,..., The film thickness Tp of the p-th film to be measured shown in FIG. It can be clearly confirmed that the composition ratios measured corresponding to the respective thicknesses change sharply, and an alternating laminated structure of CoFe layers and Cu layers is formed.
＜試料ホルダ組立体＞
図１６に示す導電性ワイヤ１１の代わりに，図１９に示すように，基板部２の第２主面と接着するための平坦面１１ａを先端に有する棒状の導電性ワイヤ１１Ａを用いれば、局所分析用針状試料１との固定を更に容易且つ確実に行うことができる試料ホルダ組立体１０ｂが得られる。図１９においては、基板部２の幅（図１９の紙面に向かって水平方向の長さ）か、基板部２の幅より大きい長さの平坦部分を確保した平坦面１１ａを先端部に有する棒状の導電性ワイヤ１１Ａが用いられている。図１９に示す導電性ワイヤ１１の平坦面１１ａは，例えば断面の直径が０．５ｍｍ程度のチタンワイヤの端面を機械的に研磨すればよい。導電性ワイヤ１１の平坦面１１ａには，加工方法によっては中心付近に小さな穴，或いは微小の凹凸が生じる場合もある。しかし，基板部２の第２主面の一部と接着し基板部２を固定できる程度の平坦な面、好ましくは基板部２の幅以上の大きさを確保した平坦な面、更に好ましくは基板部２の第２主面の占める面積以上の平坦な面が、導電性ワイヤ１１Ａに形成されていれば，一定の効果を奏する。
<Sample holder assembly>
In place of the conductive wire 11 shown in FIG. 16, if a rod-like conductive wire 11A having a flat surface 11a at the tip for bonding to the second main surface of the substrate portion 2 is used as shown in FIG. A sample holder assembly 10b that can be more easily and reliably fixed to the analysis needle-like sample 1 is obtained. In FIG. 19, a rod-like shape having a flat surface 11 a at the tip portion that secures a flat portion whose width is the width of the substrate portion 2 (the length in the horizontal direction toward the paper surface of FIG. 19) or longer than the width of the substrate portion 2. The conductive wire 11A is used. For the flat surface 11a of the conductive wire 11 shown in FIG. 19, for example, the end surface of a titanium wire having a cross-sectional diameter of about 0.5 mm may be mechanically polished. On the flat surface 11a of the conductive wire 11, a small hole or minute unevenness may occur near the center depending on the processing method. However, a flat surface that can be bonded to a part of the second main surface of the substrate portion 2 to fix the substrate portion 2, preferably a flat surface that secures a size larger than the width of the substrate portion 2, more preferably a substrate. If a flat surface equal to or larger than the area occupied by the second main surface of the portion 2 is formed on the conductive wire 11A, a certain effect is obtained.
図１９に示す試料ホルダ組立体１０ｂにおいて，導電性ワイヤ１１Ａに局所分析用針状試料１を固定する際は，局所分析用針状試料１の基板部２の第２主面が平坦面１１ａと対向するように，導電性接着剤１３を用いて導電性ワイヤ１１Ａと局所分析用針状試料１とを接着する。その後，導電性ワイヤ１１Ａに固定した局所分析用針状試料１を図１４に示す局所分析装置５の内部に固定する。この固定方法により，例えば図１６に示す導電性ワイヤ１１に局所分析用針状試料１を固定する場合に１０個のうちの９個が分析前に局所分析用針状試料１の角度を補正する必要があるのに比べ，図１９に示す導電性ワイヤ１１Ａを用いた場合では，１０個の局所分析用針状試料１のすべてが角度を補正する必要なく分析ができる。 In the sample holder assembly 10b shown in FIG. 19, when the local analysis needle sample 1 is fixed to the conductive wire 11A, the second main surface of the substrate portion 2 of the local analysis needle sample 1 is flat with the flat surface 11a. The conductive wire 11 </ b> A and the local analysis needle-like sample 1 are bonded using the conductive adhesive 13 so as to face each other. Thereafter, the needle sample 1 for local analysis fixed to the conductive wire 11A is fixed inside the local analyzer 5 shown in FIG. With this fixing method, for example, when the local analysis needle sample 1 is fixed to the conductive wire 11 shown in FIG. 16, nine of the ten samples correct the angle of the local analysis needle sample 1 before analysis. Compared to the necessity, when the conductive wire 11A shown in FIG. 19 is used, all of the ten local analysis needle-like samples 1 can be analyzed without the need for correcting the angle.
図２０に示すように，導電性ワイヤ１１Ｂの平坦面１１ａの周囲に突部１１ｂを配置し，図１２に示すように，基板部２が導電性ワイヤ１１Ｂの先端に一部埋設できるように導電性ワイヤ１１Ｂの先端を機械的切削により加工すれば，突部１１ｂが局所分析用針状試料１を固定する際のガイドの役割を果たす。このため，図２０に示す試料ホルダ組立体１０ｃによれば，局所分析装置５への固定が図１９に示す試料ホルダ組立体１０ｂを用いた場合より更に容易になる上，被測定膜７４の先端の角度の制御が簡単になる。 As shown in FIG. 20, the protrusion 11b is arranged around the flat surface 11a of the conductive wire 11B, and the substrate 2 is conductive so that it can be partially embedded in the tip of the conductive wire 11B as shown in FIG. If the tip of the conductive wire 11B is machined by mechanical cutting, the protrusion 11b serves as a guide when fixing the needle sample 1 for local analysis. Therefore, according to the sample holder assembly 10c shown in FIG. 20, the fixing to the local analyzer 5 becomes easier than in the case of using the sample holder assembly 10b shown in FIG. The control of the angle becomes easy.
例えば図２０に示す例においては，直径０．５ｍｍのチタンワイヤの中心部に，基板部２の大きさに合わせて設計した縦横０．３ｍｍ程度の四角形の溝を，精密切削装置等により形成する。平坦面１１ａは，図１０に示す導電性ワイヤ１１Ａと同様に，加工方法によっては小さな穴，或いは微小の凹凸が生じる場合もあるが，基板部２の第２主面の占める面積以上の平坦な面が全体として確保されればよい。また，図１２に示す導電性ワイヤ１１Ｂは，四角形の平坦面１１ａの四隅を平坦面１１ａに比べて深く切削することにより平坦面１１ａ表面に微小の凹凸が生じていても，本発明の効果を損ねるものではない。 For example, in the example shown in FIG. 20, a rectangular groove of about 0.3 mm in length and width designed to match the size of the substrate portion 2 is formed in the center of a 0.5 mm diameter titanium wire by a precision cutting device or the like. . Similar to the conductive wire 11A shown in FIG. 10, the flat surface 11a may have small holes or minute irregularities depending on the processing method. However, the flat surface 11a is flat more than the area occupied by the second main surface of the substrate portion 2. It is sufficient that the surface is secured as a whole. Further, the conductive wire 11B shown in FIG. 12 has the effect of the present invention even if minute irregularities are generated on the surface of the flat surface 11a by cutting the four corners of the rectangular flat surface 11a deeper than the flat surface 11a. It is not detrimental.
図２０に示す導電性ワイヤ１１Ｂに局所分析用針状試料１を固定する際は，図２１に示すように，局所分析用針状試料１の基板部２の第２主面が平坦面１１ａと対向するように，導電性接着剤１３を用いて導電性ワイヤ１１Ｂと局所分析用針状試料１とを接着する。その後，導電性ワイヤ１１Ｂに固定した局所分析用針状試料１を図１４に示す局所分析装置５内部に固定する。この固定方法によれば，図１９に示す導電性ワイヤ１１Ａを用いた場合と同様に局所分析用針状試料１の角度を補正する必要なく分析ができる。 When fixing the local analysis needle sample 1 to the conductive wire 11B shown in FIG. 20, as shown in FIG. 21, the second main surface of the substrate portion 2 of the local analysis needle sample 1 is a flat surface 11a. The conductive wire 11 </ b> B and the local analysis needle-like sample 1 are bonded using the conductive adhesive 13 so as to face each other. Thereafter, the local analysis needle-like sample 1 fixed to the conductive wire 11B is fixed inside the local analysis device 5 shown in FIG. According to this fixing method, analysis can be performed without the need to correct the angle of the needle sample 1 for local analysis, as in the case of using the conductive wire 11A shown in FIG.
さらに，導電性ワイヤ１１Ｂと局所分析用針状試料１との接着後の軸のズレを光学顕微鏡で観察すると，図１９に示す導電性ワイヤ１１Ａを用いた試料ホルダ組立体１０ｂでは，導電性ワイヤ１１Ａ端面の中心と局所分析用針状試料１の先端部との軸のズレが１０個中最大０．１５ｍｍ程度になる。一方，図２１に示す試料ホルダ組立体１０ｃでは，導電性ワイヤ１１Ｂ端面の中心と局所分析用針状試料１の先端部との軸のズレが，１０個中最大でも０．０８ｍｍ程度に抑えることができる。この結果から，図１１に示す導電性ワイヤ１１Ｂを用いた試料ホルダ組立体１０ｃによれば，局所分析用針状試料１を簡単に固定でき，局所分析用針状試料１の先端の向きと導電性ワイヤ１１Ｂの軸方向のズレを少なくできることが理解できる。したがって，再現性良く高い歩留まりで局所分析用針状試料１の被測定領域７４の分析ができる。 Further, when the deviation of the axis after bonding between the conductive wire 11B and the needle sample 1 for local analysis is observed with an optical microscope, the sample holder assembly 10b using the conductive wire 11A shown in FIG. The deviation of the axis between the center of the end face of 11A and the tip of the needle sample 1 for local analysis is about 0.15 mm at maximum. On the other hand, in the sample holder assembly 10c shown in FIG. 21, the axial misalignment between the center of the end surface of the conductive wire 11B and the tip of the needle sample 1 for local analysis is suppressed to about 0.08 mm at the maximum. Can do. From this result, according to the sample holder assembly 10c using the conductive wire 11B shown in FIG. 11, the needle sample 1 for local analysis can be easily fixed, the direction of the tip of the needle sample 1 for local analysis and the conductivity. It can be understood that the axial displacement of the conductive wire 11B can be reduced. Therefore, it is possible to analyze the measurement region 74 of the needle sample 1 for local analysis with high reproducibility and high yield.
（その他の実施の形態）
上記のように，本発明は実施の形態によって記載したが，この開示の一部をなす論述及び図面はこの発明を限定するものであると理解すべきではない。この開示から当業者には様々な代替実施の形態，実施例及び運用技術が明らかとなろう。
(Other embodiments)
As described above, the present invention has been described according to the embodiment. However, it should not be understood that the description and drawings constituting a part of this disclosure limit the present invention. From this disclosure, various alternative embodiments, examples, and operational techniques will be apparent to those skilled in the art.
上述した局所分析用針状試料１は，ＦＩＭ，アトムプローブ，三次元アトムプローブの他に，局所分析用針状試料１と同様な試料を測定することができる他の様々な局所分析装置に応用可能である。 The above-described needle sample 1 for local analysis is applied to various other local analyzers that can measure the same sample as the needle sample 1 for local analysis in addition to FIM, atom probe, and three-dimensional atom probe. Is possible.
局所分析用針状試料１の表面は，機械的な切削や研磨によって形成された凹凸や荒れが生じていても本発明の効果を損ねるものではない。また，柱状部３の形状を円柱状にする，柱状部３の高さを１５０μｍ，３００μｍにする，柱状部の縦横の幅を５０μｍ，３０μｍにする，或いは基板部２の大きさを３００μｍ四方にする等の変更を適宜加えても，実施の形態において説明した局所分析用針状試料１と同様の効果が得られることは勿論である。 Even if the surface of the needle sample 1 for local analysis has irregularities or roughness formed by mechanical cutting or polishing, the effect of the present invention is not impaired. Also, the shape of the columnar part 3 is made cylindrical, the height of the columnar part 3 is 150 μm and 300 μm, the vertical and horizontal widths of the columnar part are 50 μm and 30 μm, or the size of the substrate part 2 is 300 μm square. Needless to say, the same effects as those of the local analysis needle-like sample 1 described in the embodiment can be obtained even if appropriate changes are made.
上述した局所分析用針状試料１の作製方法においては，基板上に柱状部３を形成した後に基板部２の大きさを規定し，その後，柱状部３の先端を加工することによって針状部４を切削したが，加工手順は上述した方法に限定されない。また，上述した局所分析用針状試料１の作製方法では，針状部４を切削する際にＦＩＢを用いて切削したが，切削する手段はＦＩＢに限定されず，機械的な研磨，化学研磨，電解研磨又はそれらの組み合わせ等のどのような手段によっても上述した実施の形態に係る発明の奏する効果と同様の効果を得ることができる。 In the method for producing the needle sample 1 for local analysis described above, the size of the substrate part 2 is defined after the columnar part 3 is formed on the substrate, and then the tip of the columnar part 3 is processed to form the needle-like part. Although 4 was cut, the processing procedure is not limited to the method described above. Further, in the above-described method for producing the needle sample 1 for local analysis, the needle part 4 is cut using FIB when cutting, but the cutting means is not limited to FIB, and mechanical polishing and chemical polishing are performed. The effect similar to the effect of the invention according to the above-described embodiment can be obtained by any means such as electropolishing or a combination thereof.
このように，本発明はここでは記載していない様々な実施の形態等を含むことは勿論である。したがって，本発明の技術的範囲は上記の説明から妥当な特許請求の範囲に係る発明特定事項によってのみ定められるものである。 As described above, the present invention naturally includes various embodiments not described herein. Therefore, the technical scope of the present invention is defined only by the invention specifying matters according to the scope of claims reasonable from the above description.
１…局所分析用針状試料
２…基板部
３…柱状部
３ａ…テーパー部
４…針状部
４α…アモルファス層
５…局所分析装置
１０…固定部
１０ａ，１０ｂ，１０ｃ…試料ホルダ組立体
１１，１１Ａ，１１Ｂ…導電性ワイヤ
１１ａ…平坦面
１１ｂ…突部
１２…試料ホルダ
１３…導電性接着剤
２０…電圧供給部
３０…冷却器
４０…ガス供給部
４５…バルブ
５０…フランジ
６０…分析部
６１…マイクロチャネルプレート
６２…蛍光体
６３…プローブホール
６４…検出器
６５…観察窓
７０…出力装置
７１…基板
７２，７２Ａ，７２Ｂ…第１のシード層
７３，７３Ａ，７３Ｂ…第２のシード層
７４…被測定領域
７４Ａ，７４Ｂ…被測定膜
７４ａ…第１被測定膜
７４ｂ…第２被測定膜
７４ｃ…第３被測定膜
７４ｄ…第４被測定膜
７４ｐ…第ｐ被測定膜
７４ｑ…第ｑ被測定膜
７４ｒ…第ｒ被測定膜
７４ｓ…第ｓ被測定膜
７４ｔ…第ｔ被測定膜
７５…キャップ層
７６，７６Ａ，７６Ｂ…四角柱構造
DESCRIPTION OF SYMBOLS 1 ... Acicular sample for local analysis 2 ... Substrate part 3 ... Columnar part 3a ... Tapered part 4 ... Needle-like part 4 (alpha) ... Amorphous layer 5 ... Local analyzer 10 ... Fixed part 10a, 10b, 10c ... Sample holder assembly 11, DESCRIPTION OF SYMBOLS 11A, 11B ... Conductive wire 11a ... Flat surface 11b ... Projection 12 ... Sample holder 13 ... Conductive adhesive 20 ... Voltage supply part 30 ... Cooler 40 ... Gas supply part 45 ... Valve 50 ... Flange 60 ... Analysis part 61 ... microchannel plate 62 ... phosphor 63 ... probe hole 64 ... detector 65 ... observation window 70 ... output device 71 ... substrate 72, 72A, 72B ... first seed layer 73, 73A, 73B ... second seed layer 74 ... measurement region 74A, 74B ... measurement film 74a ... first measurement film 74b ... second measurement film 74c ... third measurement film 74d ... fourth measurement film 74p ... first p film to be measured 74q ... q-th film to be measured 74r ... r-th film to be measured 74s ... s-th film to be measured 74t ... t-th film to be measured 75 ... cap layer 76, 76A, 76B ... square pillar structure
Claims (7)
前記第１主面から突出した柱状部と，
前記柱状部の前記基板部に接続された側とは反対側の端部から前記柱状部が突出する方向に向かって錐体をなすように先鋭化された針状部
とを備え，前記針状部の先端部に局所分析用の被測定領域を含むことを特徴とする局所分析用針状試料。 A substrate portion having a first main surface and a second main surface opposite to the first main surface;
A columnar portion protruding from the first main surface;
A needle-like part sharpened so as to form a cone from the end of the columnar part opposite to the side connected to the substrate part in a direction in which the columnar part protrudes. A needle-like sample for local analysis, comprising a region to be measured for local analysis at the tip of the part.
前記第１主面から突出した柱状部と，
前記柱状部の前記基板部に接続された側とは反対側の端部から前記柱状部が突出する方向に向かって錐体をなすように先鋭化され，先鋭化された先端部に局所分析用の被測定領域を含む針状部と，
前記基板部の前記第２主面と接着するための平坦面を有する棒状の導電性ワイヤ部
とを備えることを特徴とする試料ホルダ組立体。 A substrate portion having a first main surface and a second main surface opposite to the first main surface;
A columnar portion protruding from the first main surface;
The columnar portion is sharpened so as to form a cone from the end opposite to the side connected to the substrate portion in the direction in which the columnar portion protrudes, and the sharpened tip is used for local analysis. A needle-shaped part including a region to be measured;
A sample holder assembly comprising: a rod-shaped conductive wire portion having a flat surface for bonding to the second main surface of the substrate portion.
前記固定部を介して前記針状部の前記被測定領域をイオン化するための電圧を供給する電圧供給部と、
前記柱状部の前記針状部の先端を通る中心軸上において前記被測定領域の先端に対向し、前記被測定領域を分析する分析部
とを備えることを特徴とする局所分析装置。 A substrate portion having a first principal surface and a second principal surface opposite to the first principal surface, a columnar portion protruding from the first principal surface, and a side of the columnar portion opposite to the side connected to the substrate portion A needle-like part which is sharpened so as to form a cone in a direction in which the columnar part protrudes from the end part, and includes a measurement region for local analysis at the sharpened tip part; and a second part of the substrate part A fixing part for fixing a sample holder assembly, which is connected to the main surface and comprises a sample holder for holding the substrate part;
A voltage supply unit for supplying a voltage for ionizing the measurement area of the needle-like part via the fixing part;
A local analysis apparatus comprising: an analysis unit configured to analyze the measurement region, facing the tip of the measurement region on a central axis passing through the tip of the needle-like portion of the columnar part.
前記柱状部の前記基板部に接続された側とは反対側の端部から前記柱状部が突出する方向に向かって錐体をなすように先鋭化し，先鋭化した先端部に前記被測定領域を含む針状部を形成するステップ
とを備えることを特徴とする局所分析用針状試料の作製方法。 Cutting a structure including a region to be measured to form a first main surface and a substrate portion having a second main surface facing the first main surface and a columnar portion protruding from the substrate portion;
The columnar part is sharpened so as to form a cone from the end opposite to the side connected to the substrate part in the direction in which the columnar part protrudes, and the measured region is formed at the sharpened tip part. And a step of forming a needle-shaped part including the needle-shaped sample for local analysis.
前記被測定領域に印を付けるステップと，
前記印の周辺に存在する前記被測定領域以外の領域を選択的に除去するステップ
を含むことを特徴とする請求項５に記載の局所分析用針状試料の作製方法。 The step of forming the columnar part includes:
Marking the measured area;
The method for producing a needle sample for local analysis according to claim 5, further comprising the step of selectively removing a region other than the region to be measured existing around the mark.
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