JP2000329664A - Observation method of transmission electron microscope and holding jig - Google Patents
Observation method of transmission electron microscope and holding jigInfo
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- JP2000329664A JP2000329664A JP11136754A JP13675499A JP2000329664A JP 2000329664 A JP2000329664 A JP 2000329664A JP 11136754 A JP11136754 A JP 11136754A JP 13675499 A JP13675499 A JP 13675499A JP 2000329664 A JP2000329664 A JP 2000329664A
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】この発明は、透過型電子顕微
鏡（以下、「ＴＥＭ」という）によって磁性材料を観察
する方法および保持治具に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for observing a magnetic material with a transmission electron microscope (hereinafter, referred to as "TEM") and a holding jig.
【０００２】[0002]
【従来の技術】透過型電子顕微鏡（ＴＥＭ）によって試
料観察を行う場合、試料対象材料を薄片化することが必
要である。そのため対象材料によっては、試料作製が困
難となる。例えば、めっき鋼板のめっき被膜−鋼板界面
の断面方向からの観察を行う場合、電解研摩法およびイ
オンミリング法等では、めっき被膜のみが選択的に研摩
されてしまう問題がある。また、ミクロトーム法では、
試料を切削するために、試料の変形、破壊および疵等に
より本来の構造を保てない等の問題が生じる。2. Description of the Related Art When observing a sample with a transmission electron microscope (TEM), it is necessary to thin the material to be sampled. Therefore, depending on the target material, it is difficult to prepare a sample. For example, when observing the plating film of a plated steel sheet from the cross-sectional direction of the interface between the plating film and the steel sheet, there is a problem that only the plating film is selectively polished in the electrolytic polishing method and the ion milling method. In the microtome method,
Since the sample is cut, there arises a problem that the original structure cannot be maintained due to deformation, destruction, and flaws of the sample.
【０００３】これに対し、収束イオンビーム（Ｆｏｃｕ
ｓｅｄ Ｉｏｎ Ｂｅａｍ）法（以下、「ＦＩＢ」とい
う）では、以上のような問題を生じることなく、所望の
箇所を高精度で加工可能であり、１００ｎｍ程の厚さの
薄片ならば困難なく作製が可能である。従って、近年、
ＦＩＢは、ＴＥＭ試料作製に盛んに使われるようになっ
ている。On the other hand, a focused ion beam (Focu)
In the sed ion beam (hereinafter, referred to as "FIB") method, a desired portion can be processed with high accuracy without causing the above-described problems, and a thin piece having a thickness of about 100 nm can be manufactured without difficulty. It is possible. Therefore, in recent years,
FIB has been actively used for TEM sample preparation.
【０００４】一般にＦＩＢにより作製するＴＥＭ試料
は、ＴＥＭの試料ホルダに装着可能なように、図３に示
すような試料保持リングを備える試料保持用の治具に装
着される。リングの材質は主にＣｕであるが、試料中に
Ｃｕが存在する場合等、分析の障害となる場合には、他
の材質（Ｔｉ、Ａｕ等）が用いられる。図３に示す従来
の保持治具においては、円弧状のリング５の径５ａは約
３ｍｍ、リング幅５ｂは約０．５ｍｍに設定されてい
る。In general, a TEM sample manufactured by FIB is mounted on a sample holding jig provided with a sample holding ring as shown in FIG. 3 so as to be mountable on a TEM sample holder. The material of the ring is mainly Cu, but in the case where Cu is present in the sample or other obstacles to the analysis, other materials (Ti, Au, etc.) are used. In the conventional holding jig shown in FIG. 3, the diameter 5a of the arc-shaped ring 5 is set to about 3 mm, and the ring width 5b is set to about 0.5 mm.
【０００５】試料ホルダの構成上、円弧状のリング５の
中心部近傍に観察領域６を位置させる必要が有るため、
試料（対象材料）４は、図４に示すように、例えば、
２．０ｍｍ（横幅）×０．５ｍｍ×５０μｍ＝０．０５
ｍｍ3（体積）の大きさに前加工されて、図５に示すよ
うにリング５に接着される。図４において、４ａは試料
の横幅を示す。[0005] Because of the structure of the sample holder, it is necessary to position the observation area 6 near the center of the circular ring 5.
The sample (target material) 4 is, for example, as shown in FIG.
2.0 mm (width) × 0.5 mm × 50 μm = 0.05
It is pre-processed to a size of mm 3 (volume) and adhered to the ring 5 as shown in FIG. In FIG. 4, 4a indicates the width of the sample.
【０００６】[0006]
【発明が解決しようとする課題】しかしながら、前加工
試料４が鉄鋼材料等のような磁性材料の場合には、上記
のように体積が０．０５ｍｍ3もあると、リング中心部
のみならずその周辺にも試料が位置し、透過型電子顕微
鏡の磁界レンズの磁界が乱され、ＴＥＭ観察が困難にな
る問題がある。However, when the pre-processed sample 4 is a magnetic material such as a steel material, if the volume is as large as 0.05 mm 3 as described above, not only the center of the ring but also There is also a problem that the sample is located in the periphery, and the magnetic field of the magnetic lens of the transmission electron microscope is disturbed, making TEM observation difficult.
【０００７】従って、この発明の目的は、観察試料が磁
性材料の場合においても、磁界レンズの磁界が乱れるこ
となくＴＥＭ観察を実施することができる透過型電子顕
微鏡の観察方法、および、当該試料を安定して保持する
ことができる保持治具を提供することにある。Accordingly, an object of the present invention is to provide a transmission electron microscope observation method capable of performing a TEM observation without disturbing the magnetic field of a magnetic lens even when an observation sample is a magnetic material, and a method for observing the sample. An object of the present invention is to provide a holding jig that can stably hold.
【０００８】[0008]
【課題を解決するための手段】我々は、上記課題を解決
するために鋭意研究を重ねた。その結果、観察領域以外
の部分が多く残存することが、レンズの磁界撹乱の要因
であること、即ち、試料の体積をできるだけ減少し観察
領域以外の箇所を減らすことにより、磁界の乱れを減少
することができることを知見した。この発明は、上記の
知見に基づいてなされたものである。Means for Solving the Problems We have made intensive studies to solve the above problems. As a result, the fact that many parts other than the observation area remain is the cause of the magnetic field disturbance of the lens, that is, the magnetic field disturbance is reduced by reducing the volume of the sample as much as possible and reducing the parts other than the observation area. I realized that I can do it. The present invention has been made based on the above findings.
【０００９】請求項１記載の発明は、透過型電子顕微鏡
の観察方法において、前記観察される磁性材料は予めそ
の体積が０.０２５ｍｍ3以下になるように加工され、し
かる後、収束イオンビーム法により観察領域を薄片化加
工されることに特徴を有する透過型電子顕微鏡の磁界レ
ンズの磁界の乱れの少ない透過型電子顕微鏡の観察方法
である。According to a first aspect of the present invention, in the observation method of the transmission electron microscope, the magnetic material to be observed is processed beforehand so that its volume becomes 0.025 mm 3 or less, and thereafter, the focused ion beam method is used. This is a method for observing a transmission electron microscope, which is characterized in that the observation area is thinned by the method, wherein the magnetic field of the magnetic lens of the transmission electron microscope is less disturbed.
【００１０】請求項２記載の発明は、磁性材料を保持す
るための試料保持リングを備える透過型電子顕微鏡の試
料保持治具において、前記試料保持リングは、横幅２ｍ
ｍ以下の磁性材料をリング中心部近傍に保持可能なリン
グ幅を有することに特徴を有する透過型電子顕微鏡の保
持治具である。According to a second aspect of the present invention, in a sample holding jig of a transmission electron microscope having a sample holding ring for holding a magnetic material, the sample holding ring has a width of 2 m.
A holding jig for a transmission electron microscope characterized by having a ring width capable of holding a magnetic material of m or less in the vicinity of the center of the ring.
【００１１】ＦＩＢによって磁性材料（試料）の体積を
０．０２５ｍｍ3以下に加工することにより、ＴＥＭの
観察領域以外の部分の面積が減少しレンズの磁界の乱れ
を防止することができる。By processing the volume of the magnetic material (sample) to 0.025 mm 3 or less by the FIB, the area of the portion other than the observation region of the TEM can be reduced, and the magnetic field of the lens can be prevented from being disturbed.
【００１２】体積を０．０２５ｍｍ3以下とすると、試
料の横幅は２ｍｍ以下と小さくなる。従来、透過型電子
顕微鏡の試料保持治具が備える試料保持リングは、その
径が約３ｍｍ、リング幅は約０.５ｍｍが一般的なの
で、このようにリング幅が小さい従来のリングでは、横
幅が２ｍｍ以下の試料を中心部近傍に保持することはで
きない。従来の保持治具は、保持リングの中心部近傍が
空域となっているからである（図５参照）。請求項２に
記載のリング幅を有する試料保持治具によれば、横幅２
ｍｍ以下の試料をリングの中心部近傍に保持可能であ
る。When the volume is 0.025 mm 3 or less, the lateral width of the sample becomes as small as 2 mm or less. Conventionally, a sample holding ring provided in a sample holding jig of a transmission electron microscope generally has a diameter of about 3 mm and a ring width of about 0.5 mm. Samples of 2 mm or less cannot be held near the center. This is because, in the conventional holding jig, the vicinity of the center of the holding ring is an air space (see FIG. 5). According to the sample holding jig having the ring width described in claim 2, the width 2
mm or less can be held near the center of the ring.
【００１３】[0013]
【発明の実施の形態】次に、この発明の実施の形態を図
面を参照しながら説明する。Next, an embodiment of the present invention will be described with reference to the drawings.
【００１４】図１は、この発明の実施の形態に係る試料
保持治具である。図１に示すように、保持治具は円弧状
のリング２を備えている。リング２の径２ａは３ｍｍで
従来のリング５（図３参照）と同じであるが、そのリン
グ幅２ｂは１ｍｍとなっている。このように、リング２
は、横幅２ｍｍまたはそれ以下の試料１を円弧の中心部
近傍に保持するのに十分なリング幅２ｂを有しており、
リング２の中心部近傍に試料（磁性材料）１を保持でき
るようになっている。FIG. 1 shows a sample holding jig according to an embodiment of the present invention. As shown in FIG. 1, the holding jig includes an arc-shaped ring 2. The diameter 2a of the ring 2 is 3 mm, which is the same as that of the conventional ring 5 (see FIG. 3), but the ring width 2b is 1 mm. Thus, ring 2
Has a ring width 2b sufficient to hold the sample 1 having a width of 2 mm or less near the center of the arc,
The sample (magnetic material) 1 can be held near the center of the ring 2.
【００１５】図１に示す加工試料（磁性材料）１は、Ｆ
ＩＢによって｛１．０ｍｍ（横幅）×０．５ｍｍ×５０
μ＝０．０２５ｍｍ3（体積）｝の大きさに加工されて
いる。これは、図４に示す大きさ｛２．０ｍｍ（横幅）
×０．５ｍｍ×５０μｍ＝０．０５ｍｍ3（体積）｝の
従来の加工試料４の半分の大きさである。また、試料１
の体積は０．０２５ｍｍ3未満でもよい。A processed sample (magnetic material) 1 shown in FIG.
1.0mm (width) x 0.5mm x 50 by IB
μ = 0.025 mm 3 (volume)｝. This is the size shown in FIG. 4 ｛2.0 mm (width)
× 0.5 mm × 50 μm = 0.05 mm 3 (volume)｝, which is half the size of the conventional processed sample 4. Sample 1
May be less than 0.025 mm 3 .
【００１６】本実施の形態では、試料１の体積が従来の
試料４の半分以下となっている上に、ＴＥＭの電子線入
射方向から見て、より等方的な試料形状（図１参照）に
なっているので、ＴＥＭの磁界レンズの乱れを抑えるこ
とができる。例えば、従来の治具５を用いた試料４の大
きさでは（図３〜５参照）、試料４の傾斜角度０°か
ら、分析のために２０°傾斜させたとき、電子ビームは
軸から大きく外れてしまい再度の大幅な軸調整が必要に
なり、ときには、ビームを軸の中心に戻すために電子銃
のシフトが必要な場合がある。本発明では、電子ビーム
は移動するものの、像観察用の蛍光板内にビームが留ま
っており、再度の軸調整も最小限で可能である。更に、
分析であれば再度の軸調整は必要ない。In the present embodiment, the volume of the sample 1 is less than half of that of the conventional sample 4, and the sample is more isotropic when viewed from the electron beam incident direction of the TEM (see FIG. 1). , The disturbance of the magnetic lens of the TEM can be suppressed. For example, in the case of the size of the sample 4 using the conventional jig 5 (see FIGS. 3 to 5), when the sample 4 is tilted by 20 ° for analysis from the tilt angle of 0 °, the electron beam becomes large from the axis. It may deviate and require a major axis adjustment again, and sometimes the electron gun needs to be shifted to return the beam to the center of the axis. In the present invention, although the electron beam moves, the beam stays in the fluorescent plate for image observation, and the axial adjustment again can be minimized. Furthermore,
There is no need to adjust the axis again for analysis.
【００１７】図２は、この発明の実施の形態に係る他の
保持治具である。図２に示すように、リング３の径３ａ
は３ｍｍである。ほぼ直径方向に設けられた直線状の切
り欠き３ｂの中心部近傍に試料を保持することにより、
試料１をリング３の円弧の中心部近傍に保持することが
できる。図２に示すリング３を備える保持治具によって
も図１の保持治具と同等の効果を得ることができる。FIG. 2 shows another holding jig according to the embodiment of the present invention. As shown in FIG. 2, the diameter 3a of the ring 3
Is 3 mm. By holding the sample near the center of the linear notch 3b provided substantially in the diameter direction,
The sample 1 can be held near the center of the arc of the ring 3. The same effect as the holding jig of FIG. 1 can be obtained by the holding jig provided with the ring 3 shown in FIG.
【００１８】[0018]
【実施例】次に、この発明の実施例を説明する。Next, an embodiment of the present invention will be described.
【００１９】｛２．０ｍｍ（横幅）×０．５ｍｍ×５０
μｍ＝０．０５ｍｍ3（体積）｝の、従来の大きさの磁
性材料の供試体１を調製した。次いで、供試体１を従来
の保持治具（図３参照）に接着し、ＴＥＭ観察実験に供
した。$ 2.0 mm (width) x 0.5 mm x 50
A specimen 1 of a magnetic material having a conventional size of μm = 0.05 mm 3 (volume)｝ was prepared. Next, the specimen 1 was adhered to a conventional holding jig (see FIG. 3) and subjected to a TEM observation experiment.
【００２０】また、供試体１と同じ大きさの磁性材料の
試料を本発明保持治具（図１参照）に接着し、ＦＩＢに
よって下記に示す大きさの供試体２〜５に加工した。そ
して、それぞれＴＥＭ観察に供した。供試体２〜５の大
きさは下記の通りであった。Further, a sample of a magnetic material having the same size as the sample 1 was adhered to the holding jig of the present invention (see FIG. 1), and processed into samples 2 to 5 having the following sizes by FIB. Then, each was subjected to TEM observation. The sizes of the test specimens 2 to 5 were as follows.
【００２１】供試体２：｛１．６（横幅）ｍｍ×０．５
ｍｍ×５０μｍ＝０．０４ｍｍ3（体積）｝ 供試体３：｛１．４（横幅）ｍｍ×０．５ｍｍ×５０μ
ｍ＝０．０３５ｍｍ3（体積）｝ 供試体４：｛１．２（横幅）ｍｍ×０．５ｍｍ×５０μ
ｍ＝０．０３０ｍｍ3（体積）｝ 供試体５：｛１．０（横幅）ｍｍ×０．５ｍｍ×５０μ
ｍ＝０．０２５ｍｍ3（体積）｝ ＴＥＭ観察は、試料傾斜角度０°のときに、電子ビーム
の光軸調整を行い、次いで、２０°傾斜して以下の項目
（１）〜（３）について比較を行った。 （１）倍率５万倍で、蛍光板上でのビームのずれ（蛍光
板中心部からのビームのずれ量）。 （２）ビームの非点補正量｛従来の大きさの試料（供試
体１）を用いたときに必要な補正量を１とした｝。 （３）像の非点補正量｛従来の大きさの試料（供試体
１）を用いたときに必要な補正量を１とした｝。Specimen 2: $ 1.6 (width) mm x 0.5
mm × 50 μm = 0.04 mm 3 (volume)} Specimen 3: {1.4 (width) mm × 0.5 mm × 50 μm
m = 0.035mm 3 (volume)｝ Specimen 4: 1.2 (width) mm × 0.5mm × 50μ
m = 0.030 mm 3 (volume)｝ Specimen 5: ｛1.0 (width) mm × 0.5 mm × 50 μ
m = 0.025 mm 3 (volume)｝ In the TEM observation, when the sample tilt angle is 0 °, the optical axis of the electron beam is adjusted, and then the sample is tilted by 20 ° and the following items (1) to (3) are performed. A comparison was made. (1) Deflection of the beam on the phosphor plate at a magnification of 50,000 times (amount of displacement of the beam from the center of the phosphor plate). (2) Astigmatism correction amount of beam {The correction amount required when using a sample of the conventional size (specimen 1) was set to 1}. (3) Astigmatism correction amount of image {The correction amount required when using a sample of the conventional size (specimen 1) was set to 1}.
【００２２】その結果を表１に示す。The results are shown in Table 1.
【００２３】[0023]
【表１】 表１に示すように、本発明例である供試体５では、蛍光
板上でのビームの移動量、ビームおよび像の非点補正量
が、比較例（供試体１〜４）よりも大幅に減少している
ことが分かる。以上より、本発明によれば、ＴＥＭ観察
およびＴＥＭ−ＥＤＸ（エネルギー分散型蛍光Ｘ線）分
析の効率が大幅に向上することが分かる。[Table 1] As shown in Table 1, in the specimen 5 of the present invention, the amount of movement of the beam on the phosphor plate and the amount of astigmatism correction of the beam and the image were significantly reduced as compared with the comparative examples (the specimens 1 to 4). You can see that it is doing. From the above, it can be seen that according to the present invention, the efficiency of TEM observation and TEM-EDX (energy dispersive X-ray fluorescence) analysis is significantly improved.
【００２４】[0024]
【発明の効果】以上説明したように、この発明によれ
ば、従来の前加工法で作製した試料よりも体積の小さい
試料を用いることによって、ＴＥＭの磁界レンズに与え
る影響を減少させることができ、ＴＥＭの軸調整が容易
となり、良好な像および分析結果を得ることができ、Ｔ
ＥＭ観察およびＴＥＭ−ＥＤＸ（エネルギー分散型蛍光
Ｘ線）分析の効率が大幅に向上し、かくして有用な効果
がもたらされる。As described above, according to the present invention, the influence on the magnetic lens of the TEM can be reduced by using a sample having a smaller volume than a sample manufactured by the conventional pre-processing method. , Axis adjustment of the TEM becomes easy, and good images and analysis results can be obtained.
The efficiency of EM observation and TEM-EDX (energy dispersive X-ray fluorescence) analysis is greatly improved, and thus a useful effect is provided.
【図１】この発明の実施の形態に係る保持治具および試
料の装着状態を示す斜視図である。FIG. 1 is a perspective view showing a holding jig and a mounted state of a sample according to an embodiment of the present invention.
【図２】この発明の実施の形態に係る他の保持治具を示
す説明図である。FIG. 2 is an explanatory diagram showing another holding jig according to the embodiment of the present invention.
【図３】従来のＦＩＢで加工するＴＥＭ観察用試料の保
持治具を示す説明図である。FIG. 3 is an explanatory view showing a conventional jig for holding a TEM observation sample processed by FIB.
【図４】従来のＴＥＭ観察用試料を示す斜視図である。FIG. 4 is a perspective view showing a conventional TEM observation sample.
【図５】従来の保持治具および試料の装着状態を示す斜
視図である。FIG. 5 is a perspective view showing a mounting state of a conventional holding jig and a sample.
１ 試料 ２ リング ２ａ リング径 ２ｂ リング幅 ３ リング ３ａ リング径 ３ｂ 切り欠き ４ 従来の試料 ４ａ 横幅 ５ リング ５ａ リング径 ５ｂ リング幅 ６ 観察領域 1 Sample 2 Ring 2a Ring diameter 2b Ring width 3 Ring 3a Ring diameter 3b Notch 4 Conventional sample 4a Width 5 Ring 5a Ring diameter 5b Ring width 6 Observation area
Claims (2)
前記観察される磁性材料は予めその体積が０.０２５ｍ
ｍ3以下になるように加工され、しかる後、収束イオン
ビーム法により観察領域を薄片化加工されることを特徴
とする透過型電子顕微鏡の磁界レンズの磁界の乱れの少
ない透過型電子顕微鏡の観察方法。1. A method for observing a transmission electron microscope, comprising:
The observed magnetic material has a volume of 0.025 m in advance.
m 3 is processed so as to become less, thereafter, observation of the focused ion beam method by transmission electron microscopy less transmission electron microscope of field disturbances in magnetic lens of the observation area, characterized in that it is processed sliced Method.
グを備える透過型電子顕微鏡の試料保持治具において、
前記試料保持リングは、横幅が２ｍｍ以下の磁性材料を
リング中心部近傍に保持可能なリング幅を有することを
特徴とする透過型電子顕微鏡の保持治具。2. A sample holding jig of a transmission electron microscope having a sample holding ring for holding a magnetic material,
A holding jig for a transmission electron microscope, wherein the sample holding ring has a ring width capable of holding a magnetic material having a width of 2 mm or less near a center of the ring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11136754A JP2000329664A (en) | 1999-05-18 | 1999-05-18 | Observation method of transmission electron microscope and holding jig |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11136754A JP2000329664A (en) | 1999-05-18 | 1999-05-18 | Observation method of transmission electron microscope and holding jig |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2000329664A true JP2000329664A (en) | 2000-11-30 |
Family
ID=15182728
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11136754A Pending JP2000329664A (en) | 1999-05-18 | 1999-05-18 | Observation method of transmission electron microscope and holding jig |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2000329664A (en) |
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