JP7174203B2 - Transmission electron microscope (TEM) with photoelectron microscope (PEEM) capability - Google Patents
Transmission electron microscope (TEM) with photoelectron microscope (PEEM) capability Download PDFInfo
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Description
本発明は、バルク(塊状)材料の表面に光を当て、放出された光電子の拡大像を作る装置であるPEEMの機能を、TEMの付属装置として用いる方法に関する。 The present invention relates to a method of using the capabilities of a PEEM, a device that illuminates the surface of a bulk material and produces a magnified image of the emitted photoelectrons, as an adjunct to a TEM.
PEEMの空間分解能は一般に低く、数10nmに留まっている。(非特許文献1) The spatial resolution of PEEM is generally low, remaining at several tens of nm. (Non-Patent Document 1)
そのため出願人らはPEEMの空間分解能向上のため、対物レンズの収差低減、検出信号量の増大、収差の補正について特許を出願した。(特許文献1) Therefore, the applicants filed a patent application for reduction of objective lens aberration, increase in detected signal amount, and correction of aberration in order to improve the spatial resolution of PEEM. (Patent Document 1)
レンズの収差補正が施されている最上級のTEMにおいては、原子分解能に達しているが、試料は薄膜に限定され、バルク材料は観察できない。(非特許文献2) A top-class TEM with lens aberration correction has reached atomic resolution, but samples are limited to thin films, and bulk materials cannot be observed. (Non-Patent Document 2)
そのためバルク試料を観察できるSEM(走査型電子顕微鏡)機能を内蔵したSTEM(走査透過型電子顕微鏡)が開発されたが、3~5nmの触媒粒子の報告に留まり、原子分解能は得られない。(非特許文献3図6) Therefore, a STEM (scanning transmission electron microscope) with a built-in SEM (scanning electron microscope) function that can observe bulk samples has been developed, but only reports of catalyst particles of 3 to 5 nm are available, and atomic resolution cannot be obtained. (Non-Patent
特許文献1に開示されるPEEMにおいては、高分解を性能発現させるには振動、騒音、室温など設置環境に対する対策を個別に施さなければならない。 In the PEEM disclosed in Patent Literature 1, in order to exhibit high resolution performance, it is necessary to individually take measures against the installation environment such as vibration, noise, and room temperature.
前述の通りTEMは上記の設置環境対策が施されており、薄膜材料の原子分解能を有しているが、バルク材料については附属のSEMの入射電子線がバルク材料の内部で拡散されるため、原子分解能は得られない。 As mentioned above, the TEM has the above installation environment measures, and has the atomic resolution of thin film materials. Atomic resolution cannot be obtained.
SEMの代わりにPEEMをTEMに附属させる。そのためには、 A PEEM is attached to the TEM instead of the SEM. for that purpose,
TEMにPEEM機能を内蔵させるためには、試料1に光2を当てなければならない。 In order to integrate the PEEM function into the TEM, the sample 1 must be exposed to the
TEMの試料1はアース電位であるため、試料1に光2を当てても発生する光電子はエネルギーが低く、レンズ系の作用を施されるに必要な加速電圧を得られないため、試料は高電位3に配されなければならない。 Since the sample 1 of the TEM is at ground potential, even if the sample 1 is exposed to the
試料に光を当てるため、PEEMの光源6はTEMのカメラ室5に設置する。カメラ室を装備していない場合は、付属装置挿入用のフランジ7や、レンズの絞り8を利用する。 The PEEM light source 6 is placed in the TEM camera chamber 5 to illuminate the sample. When the camera room is not equipped, the flange 7 for inserting the accessory device and the diaphragm 8 of the lens are used.
PEEMに用いる試料ホルダ 図2は薄膜とバルクの両方を保持できる構造 図3であって、1KV以上の高電圧3を印加する機構を有し、高電圧による非軸対称な電場分布の発生を防ぐため、試料の両端の箇所は絶縁性の材質4で構成する。 A sample holder used for PEEM Figure 2 shows a structure that can hold both a thin film and a bulk. Therefore, both ends of the sample are made of an insulating material 4 .
PEEMを専用機でなく図1bに示すようにTEMの付属装置として構成することにより、設置環境に対する原子分解能対策を施したTEMにてPEEMでも原子分解能発現を可能にする。 By constructing the PEEM not as a dedicated device but as an accessory device of the TEM as shown in FIG. 1b, it is possible to achieve atomic resolution even in the PEEM with a TEM that has taken atomic resolution measures for the installation environment.
これにより装置一台で薄膜試料とバルク試料の原子分解能観察を可能にする。 This enables atomic resolution observation of thin film samples and bulk samples with a single device.
試料ホルダ 図2を用いることにより、試料1を交換することなくTEM像とPEEM像を切換えて、または同時に観察できることから、試料交換による視野のずれや、試料の変質を防ぐことができる。 2. By using the sample holder FIG. 2, the TEM image and the PEEM image can be switched or simultaneously observed without exchanging the sample 1, so it is possible to prevent the shift of the field of view and the deterioration of the sample due to the sample exchange.
図1において、TEMの機能を保持したまま、PEEMとしても使用できることにより、設置環境対策を施したTEMの鏡筒をそのまま使用することで原子分解能観察を容易にする。 In FIG. 1, the TEM can be used as a PEEM while maintaining the TEM function, so that the atomic resolution observation can be facilitated by using the TEM lens barrel that has taken measures for the installation environment as it is.
試料1は材質4により試料ホルダ図2のホルダ部より絶縁され高電位に配することができ、試料より放出する光電子がレンズ作用を受けるに必要な加速電圧を得ることができる。 The sample 1 can be insulated from the holder portion of the sample holder shown in FIG. 2 by the material 4 and placed at a high potential, so that the photoelectrons emitted from the sample can obtain the acceleration voltage necessary for receiving the lens action.
試料1にはカメラ室5内の光源部6またはフランジ7またはレンズの絞り8より光2を照射することにより光電子9を放出させ、PEEMとしての機能を発現する。 When the sample 1 is irradiated with the
図4aにおいて光2を当てることにより試料1から放出された光電子9は、対物レンズ10で焦点合わせと初段の拡大を行い、結像レンズ11,12,13で拡大され、蛍光板14で可視像に変換され観察し、カメラ室5で撮影される。 Photoelectrons 9 emitted from the sample 1 by applying
TEMの場合は図4bのように電子線16は試料の薄膜部20を透過して対物レンズ10で焦点合わせと初段の拡大を行い、結像レンズ11,12,13で拡大され、蛍光板14で可視像に変換され観察し、カメラ室5で撮影される。 In the case of the TEM, as shown in FIG. 4b, an
試料は図3aのように同一試料をエッチングして薄膜部とバルク部を形成させて試料移動させてそれぞれを観察するか、図3bのように、PEEMの場合はバルク試料23を、TEMの場合は薄膜試料22を載せて同じく試料移動させて観察する。 As shown in FIG. 3a, the same sample is etched to form a thin film portion and a bulk portion, and the sample is moved to observe each. Alternatively, as shown in FIG. is observed by placing a thin film sample 22 and moving the sample in the same manner.
1.試料
2.光
3.高電圧部
4.絶縁材質
5.カメラ室
6.光源部
7.鏡筒フランジ
8.レンズ絞り
9.光電子
10.対物レンズ
11.結像レンズ1
12.結像レンズ2
13.結像レンズ3
14.蛍光板
15.電子銃部
16.電子線
17.集束レンズ1
18.集束レンズ2
19.集束レンズ3
20.薄膜部
21.バルク部
22.薄膜試料
23.バルク試料
24.加速電圧部1.
12.
13.
14. fluorescent plate 15 .
18.
19. Converging
20.
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Citations (2)
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JP2000040483A (en) | 1998-07-23 | 2000-02-08 | Hitachi Ltd | Sample heating holder for electron microscope and sample observing method |
JP2006331979A (en) | 2005-05-30 | 2006-12-07 | Jeol Ltd | Test piece holder of electron microscope |
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JPH0374039A (en) * | 1989-08-11 | 1991-03-28 | Jeol Ltd | Transmission electron microscope equipped with photoelectronic microscope |
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JP2000040483A (en) | 1998-07-23 | 2000-02-08 | Hitachi Ltd | Sample heating holder for electron microscope and sample observing method |
JP2006331979A (en) | 2005-05-30 | 2006-12-07 | Jeol Ltd | Test piece holder of electron microscope |
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