JP2001325911A - Sample platform and scanning electron microscope equipped with the sample platform - Google Patents
Sample platform and scanning electron microscope equipped with the sample platformInfo
- Publication number
- JP2001325911A JP2001325911A JP2000144573A JP2000144573A JP2001325911A JP 2001325911 A JP2001325911 A JP 2001325911A JP 2000144573 A JP2000144573 A JP 2000144573A JP 2000144573 A JP2000144573 A JP 2000144573A JP 2001325911 A JP2001325911 A JP 2001325911A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- fine particles
- sample stage
- electron microscope
- sample platform
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000010419 fine particle Substances 0.000 claims abstract description 39
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000000725 suspension Substances 0.000 claims description 16
- 238000010894 electron beam technology Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims 1
- 230000001678 irradiating effect Effects 0.000 claims 1
- 239000000758 substrate Substances 0.000 claims 1
- 239000002002 slurry Substances 0.000 abstract 2
- 239000002245 particle Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
Description
【0001】[0001]
【発明の属する技術分野】本発明は、走査電子顕微鏡に
おいて液体に懸濁している微粒子を観察するための試料
作成に関し、微粒子を分散させる作用を有することを特
徴とする試料台の発明およびその試料作製手法に関す
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to the preparation of a sample for observing fine particles suspended in a liquid with a scanning electron microscope, and relates to an invention of a sample stage having an action of dispersing fine particles and a sample thereof. It relates to a manufacturing method.
【0002】[0002]
【従来の技術】走査電子顕微鏡において、微粒子を解析
するための試料作製法の一つに、微粒子を液体に懸濁
し、試料台表面に懸濁液を滴下し乾燥させる手法があ
る。この手法は液体と反応しない微粒子に対して広く使
用でき、試料作製が比較的容易であるという利点があ
る。一方、懸濁液が乾燥する際に表面張力により微粒子
が凝集し、一般に最適な分散条件を得るためには段階的
な濃度変換が必要であり、最適な条件を得るために、多
大な時間を費やすという問題がある。2. Description of the Related Art In a scanning electron microscope, as one of sample preparation methods for analyzing fine particles, there is a method in which fine particles are suspended in a liquid, the suspension is dropped on the surface of a sample table, and dried. This technique has the advantage that it can be widely used for fine particles that do not react with a liquid, and that sample preparation is relatively easy. On the other hand, when the suspension is dried, the fine particles agglomerate due to surface tension.In general, stepwise concentration conversion is required to obtain optimal dispersion conditions, and a great deal of time is required to obtain optimal conditions. There is a problem of spending.
【0003】[0003]
【発明が解決しようとする課題】本発明の目的は、液体
に懸濁している微粒子を試料台に固定する段階におい
て、微粒子を分散させる作用を有する試料台およびその
試料作製法を提供することである。SUMMARY OF THE INVENTION An object of the present invention is to provide a sample stage having an action of dispersing fine particles at the stage of fixing fine particles suspended in a liquid to the sample stage, and a method of preparing the sample. is there.
【0004】[0004]
【課題を解決するための手段】本発明においては、走査
電子顕微鏡の試料台において、液体に懸濁している微粒
子の形状解析を行う際、懸濁液を滴下する位置の表面に
凹凸形状を設けることにより、試料台表面へ滴下した懸
濁液が溝方向へと移動するため、それに合わせて微粒子
が移動し、溝部分にて捕集される。これにより個々の微
粒子が溝部分に分散した状態のまま固定される効果があ
る。According to the present invention, when a shape analysis of fine particles suspended in a liquid is performed on a sample stage of a scanning electron microscope, an irregular shape is formed on a surface at a position where the suspension is dropped. As a result, the suspension dropped on the surface of the sample stage moves in the groove direction, so that the fine particles move accordingly, and are collected in the groove portion. Thereby, there is an effect that the individual fine particles are fixed in a state of being dispersed in the groove portion.
【0005】[0005]
【発明の実施の形態】以下に、本発明の実施の形態を詳
細に説明する。図1に、本発明が適用された表面に凹凸
形状を有する試料台の概略図を示す。断面図Bに示され
るように表面に溝が形成されている。なお溝の形状およ
びサイズは懸濁に用いる液体の種類や粒子のサイズに合
わせて作製されるものとする。図2に試料台表面におけ
る凹凸形状の例を示す。図2Aのように表面形状を鋸状
にすることにより固定可能な粒子径の範囲を広くできる
ため、粒子径が未知の微粒子に対しても対応できる。ま
た、図2Bのように凹凸のピッチを連続的に変えた試料
台を用いることにより、粒子径の異なる2種類以上の粒
子試料を含む懸濁液から、それぞれの粒子を選別して固
定することも可能である。また、図2Cのように0.2
4μm のピッチ径を持つ標準マイクロスケール(JQ
A認証)を試料台として用いることにより、その上に固
定した微粒子の高精度寸法測定を行うことも可能であ
る。Embodiments of the present invention will be described below in detail. FIG. 1 is a schematic view of a sample stage to which the present invention is applied, the sample stage having an uneven surface. As shown in the sectional view B, a groove is formed on the surface. The shape and size of the groove are to be prepared according to the type of liquid used for suspension and the size of particles. FIG. 2 shows an example of the uneven shape on the surface of the sample table. By making the surface shape serrated as shown in FIG. 2A, the range of the particle size that can be fixed can be widened, so that it is possible to cope with fine particles whose particle size is unknown. Further, by using a sample stage in which the pitch of the concavities and convexities is continuously changed as shown in FIG. 2B, each particle is selected and fixed from a suspension containing two or more types of particle samples having different particle sizes. Is also possible. Also, as shown in FIG.
Standard micro-scale with a pitch diameter of 4 μm (JQ
A certification) can be used as a sample stage to perform high-precision dimensional measurement of fine particles fixed thereon.
【0006】図3に本発明が適用された試料台を配受す
る走査電子顕微鏡の概略図を示す。走査電子顕微鏡では
電子銃(2)より発生した電子線(3)を収束レンズ
(4)により収束し、試料ステージ(5)上の試料台
(6)に固定された試料上に照射する。その際偏向コイ
ル(7)により電子線を走査し、試料より発生した信号
(8)を検出器(9)により捕集しCRT上に表示す
る。FIG. 3 is a schematic diagram of a scanning electron microscope for receiving a sample stage to which the present invention is applied. In the scanning electron microscope, an electron beam (3) generated from an electron gun (2) is converged by a converging lens (4) and is irradiated onto a sample fixed on a sample stage (6) on a sample stage (5). At that time, an electron beam is scanned by a deflection coil (7), a signal (8) generated from the sample is collected by a detector (9), and displayed on a CRT.
【0007】図4に凹凸形状を有する試料台に微粒子試
料を固定した状態の概略図を示す。微粒子試料(10)
は凹凸形状を有する試料台の溝部分において固定され
る。FIG. 4 is a schematic view showing a state in which a fine particle sample is fixed on a sample stage having an uneven shape. Fine particle sample (10)
Is fixed in a groove portion of a sample stage having an uneven shape.
【0008】図5に微粒子を含む懸濁液を凹凸形状を有
する試料台に滴下した際の液体および微粒子の挙動につ
いての概略図を示す。液体に懸濁した状態の微粒子は凹
凸形状を有する試料台上に滴下されると、懸濁液(1
1)は溝部分へと流れ込み、その流れにあわせて微粒子
も試料台の溝方向へと移動し、溝部分にて固定される。FIG. 5 is a schematic view showing the behavior of the liquid and the fine particles when the suspension containing the fine particles is dropped on the sample stage having the uneven shape. When the fine particles suspended in the liquid are dropped on a sample stage having an uneven shape, the suspension (1) is formed.
1) flows into the groove portion, and the fine particles also move in the groove direction of the sample table in accordance with the flow, and are fixed in the groove portion.
【0009】図6に実際に同一試料を表面が平坦な試料
台と、凹凸のある試料台に固定した際の観察例を示す。
図6Aのように従来の表面が平坦な試料台上に滴下した
場合では、微粒子の凝集,積層が生じている。図6Bの
ように表面に凹凸形状を有する試料台上に滴下した場合
では、微粒子が凝集,積層することなく分散している。FIG. 6 shows an observation example when the same sample is actually fixed to a sample table having a flat surface and a sample table having irregularities.
As shown in FIG. 6A, when the conventional surface is dropped on a flat sample stage, aggregation and lamination of fine particles occur. As shown in FIG. 6B, when dropped on a sample stage having an uneven surface, fine particles are dispersed without aggregation and lamination.
【0010】図7に今回の発明の実施フローを示す。微
粒子は液体に懸濁し適当な濃度に調製し(101)、表
面に凹凸形状を有する試料台上に滴下される(10
2)。滴下後、試料を乾燥させて微粒子を試料台上に固
定する(103)。固定が完了した試料は観察装置へ挿
入され、粒子観察(104)および分散状態の確認が行
われる(105)。微粒子が分散している場合には引き
続き微粒子の形状解析を行う。もし微粒子が凝集してい
たり、微粒子を発見できない時には、懸濁液濃度が極端
に高い、あるいは低い事が原因として考えられるため、
ステップ101に戻り、再度懸濁液の調製を行い、固定
操作を繰り返す。FIG. 7 shows a flow chart for implementing the present invention. The fine particles are suspended in a liquid, adjusted to an appropriate concentration (101), and dropped on a sample table having an uneven surface (10).
2). After the dropping, the sample is dried to fix the fine particles on the sample stage (103). The fixed sample is inserted into an observation device, and the observation of particles (104) and the confirmation of the dispersion state are performed (105). When the fine particles are dispersed, the shape analysis of the fine particles is continuously performed. If the particles are agglomerated or cannot be found, it may be because the suspension concentration is extremely high or low.
Returning to step 101, the suspension is prepared again, and the fixing operation is repeated.
【0011】[0011]
【発明の効果】この発明によれば、液体に懸濁している
微粒子を試料台へ固定する段階において、微粒子が凝集
してしまう問題を解消でき、微粒子を分散させた状態の
まま固定が可能な試料台および試料固定手法を提供でき
る。また、従来は平均3桁の濃度範囲において微粒子懸
濁液を調製し最適条件を検討する必要があったが、本発
明により濃度を変えた懸濁液を調製することなく分散さ
せることが可能であることから、溶液の調製から微粒子
を固定した試料台の作成までの時間が短縮(約1/3)
できる。According to the present invention, at the stage of fixing the fine particles suspended in the liquid to the sample stage, the problem that the fine particles are aggregated can be solved, and the fine particles can be fixed in a dispersed state. A sample stage and a sample fixing method can be provided. Conventionally, it has been necessary to prepare a fine particle suspension in an average concentration range of three digits and to examine the optimum conditions. However, the present invention can disperse the suspension without preparing a suspension having a different concentration. Because of this, the time from the preparation of the solution to the preparation of the sample stage on which the fine particles are fixed is reduced (about 1/3)
it can.
【図1】本発明に基づく溝のある試料の概略図である。FIG. 1 is a schematic view of a grooved sample according to the present invention.
【図2】表面に溝のある試料台の溝の断面形状例を示す
図である。FIG. 2 is a diagram illustrating an example of a cross-sectional shape of a groove of a sample stage having a groove on a surface.
【図3】試料台を配受する走査電子顕微鏡の概略図であ
る。FIG. 3 is a schematic diagram of a scanning electron microscope for receiving and receiving a sample stage.
【図4】図1に微粒子試料を固定した状態を示す図であ
る。FIG. 4 is a view showing a state in which a fine particle sample is fixed in FIG.
【図5】微粒子を含む溶液を溝試料台に滴下した際の微
粒子の挙動について示した図である。FIG. 5 is a diagram showing behavior of the fine particles when a solution containing the fine particles is dropped on a groove sample table.
【図6】実際の試料観察例である。FIG. 6 is an actual sample observation example.
【図7】本発明の実施フローを示す図である。FIG. 7 is a diagram showing an implementation flow of the present invention.
1…溝のある試料台、2…電子銃、3…電子線、4…収
束レンズ、5…試料ステージ、6…試料台、7…偏向コ
イル、8…試料から発生した信号、9…検出器、10…
微粒子試料、11…微粒子を含む懸濁液。DESCRIPTION OF SYMBOLS 1 ... Sample table with a groove, 2 ... Electron gun, 3 ... Electron beam, 4 ... Convergent lens, 5 ... Sample stage, 6 ... Sample table, 7 ... Deflection coil, 8 ... Signal generated from sample, 9 ... Detector , 10 ...
Fine particle sample, 11: suspension containing fine particles.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 山田 満彦 茨城県ひたちなか市大字市毛1040番地 株 式会社日立サイエンスシステムズ内 (72)発明者 多持 隆一郎 茨城県ひたちなか市大字市毛1040番地 株 式会社日立サイエンスシステムズ内 (72)発明者 鈴木 猛夫 茨城県ひたちなか市大字市毛1040番地 株 式会社日立サイエンスシステムズ内 (72)発明者 熊田 隆雄 茨城県ひたちなか市大字市毛882番地 株 式会社日立製作所計測器グループ内 (72)発明者 腰原 俊介 茨城県ひたちなか市大字市毛1040番地 株 式会社日立サイエンスシステムズ内 Fターム(参考) 2G001 AA03 BA07 CA03 GA06 HA13 MA04 QA01 QA10 RA03 RA10 RA20 SA12 SA30 5C001 AA01 BB07 CC04 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Mitsuhiko Yamada 1040 Ichimo Ichiki, Hitachinaka City, Ibaraki Prefecture Inside Hitachi Science Systems Co., Ltd. Within Hitachi Science Systems (72) Inventor Takeo Suzuki 1040, Oji-shi, Oita, Hitachinaka City, Ibaraki Prefecture Inside Hitachi Science Systems Co., Ltd. Within the Group (72) Inventor Shunsuke Koshihara 1040 Ichimo, Hitachinaka-shi, Ibaraki F-term within Hitachi Science Systems, Ltd. (Reference) 2G001 AA03 BA07 CA03 GA06 HA13 MA04 QA01 QA10 RA03 RA10 RA20 SA12 SA30 5C001 AA01 BB07 CC04
Claims (4)
し照射させる手段と、電子線を試料上に走査するための
偏向手段と、試料台を配受するステージと、試料表面か
ら発生した信号を検出する検出器を備える走査電子顕微
鏡に設けられる試料台において、前記試料台は試料貼付
位置に凹凸形状を有することを特徴とする試料台。An electron gun for generating an electron beam, means for converging and irradiating the electron beam, deflecting means for scanning the electron beam on a sample, a stage for receiving and receiving a sample stage, A sample stage provided in a scanning electron microscope having a detector for detecting a generated signal, wherein the sample stage has an uneven shape at a position where a sample is stuck.
マイクロスケール(JQA認証)の少なくとも一部であ
ることを特徴とする試料台。2. The sample stage according to claim 1, wherein the uneven shape is at least a part of a standard micro-scale (JQA certification).
含むことを特徴とする走査電子顕微鏡。3. A scanning electron microscope according to claim 1, wherein said sample stage is included.
であって、凹凸形状を有した基板を搭載し、そこへ懸濁
液を滴下し、乾燥後、走査電子顕微鏡内に挿入し、走査
電子顕微鏡による観察を行うことを特徴とする微粒子解
析方法。4. A method for analyzing fine particles suspended in a liquid, comprising mounting a substrate having an uneven shape, dripping the suspension there, drying, and inserting the suspension into a scanning electron microscope. A method for analyzing fine particles, comprising observing with a scanning electron microscope.
Priority Applications (1)
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JP2000144573A JP3746186B2 (en) | 2000-05-12 | 2000-05-12 | Sample stage and scanning electron microscope equipped with the sample stage |
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JP2000144573A JP3746186B2 (en) | 2000-05-12 | 2000-05-12 | Sample stage and scanning electron microscope equipped with the sample stage |
Publications (2)
Publication Number | Publication Date |
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JP2001325911A true JP2001325911A (en) | 2001-11-22 |
JP3746186B2 JP3746186B2 (en) | 2006-02-15 |
Family
ID=18651216
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2015159870A1 (en) * | 2014-04-18 | 2015-10-22 | 株式会社堀場製作所 | Sample dispersion device and sample dispersion method |
JP2016119300A (en) * | 2014-12-22 | 2016-06-30 | エフ・イ−・アイ・カンパニー | Fiducial-mark-based correlative microscopy |
CN108663387A (en) * | 2018-05-16 | 2018-10-16 | 国家纳米科学中心 | A kind of method that wet etching prepares nano particle TEM sample |
WO2019150524A1 (en) * | 2018-02-01 | 2019-08-08 | 株式会社日立ハイテクノロジーズ | Particle measurement device and method |
-
2000
- 2000-05-12 JP JP2000144573A patent/JP3746186B2/en not_active Expired - Fee Related
Cited By (8)
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---|---|---|---|---|
WO2015159870A1 (en) * | 2014-04-18 | 2015-10-22 | 株式会社堀場製作所 | Sample dispersion device and sample dispersion method |
JPWO2015159870A1 (en) * | 2014-04-18 | 2017-04-13 | 株式会社堀場製作所 | Sample dispersion apparatus and sample dispersion method |
GB2548652A (en) * | 2014-04-18 | 2017-09-27 | Horiba Ltd | Sample dispersion device and sample dispersion method |
US9869615B2 (en) | 2014-04-18 | 2018-01-16 | Horiba, Ltd. | Sample dispersion device and sample dispersion method |
JP2016119300A (en) * | 2014-12-22 | 2016-06-30 | エフ・イ−・アイ・カンパニー | Fiducial-mark-based correlative microscopy |
WO2019150524A1 (en) * | 2018-02-01 | 2019-08-08 | 株式会社日立ハイテクノロジーズ | Particle measurement device and method |
US11143606B2 (en) | 2018-02-01 | 2021-10-12 | Hitachi High-Tech Corporation | Particle measuring device and particle measuring method |
CN108663387A (en) * | 2018-05-16 | 2018-10-16 | 国家纳米科学中心 | A kind of method that wet etching prepares nano particle TEM sample |
Also Published As
Publication number | Publication date |
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JP3746186B2 (en) | 2006-02-15 |
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