JP2020098762A - Transfer jig, sample piece preparation method, and sample piece analysis method - Google Patents
Transfer jig, sample piece preparation method, and sample piece analysis method Download PDFInfo
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本発明は、搬送用治具、試料片作製方法および試料片分析方法に属する。 The present invention relates to a carrying jig, a sample piece manufacturing method, and a sample piece analysis method.
特許文献１の［請求項１］［請求項６］等には、金属含有粒子を樹脂でコーティングしたものから、観察対象となる箇所（すなわち金属含有粒子を含む箇所）を試料片として摘出することが記載されている。この摘出には集束イオンビーム（以降、ＦＩＢとも称する。）が用いられる。この加工をＦＩＢ加工とも称する。摘出した試料片を薄片化したうえで電子顕微鏡による観察が行われる。 In [Claim 1] and [Claim 6] of Patent Document 1, a part to be observed (that is, a part including metal-containing particles) is extracted as a sample piece from a metal-containing particle coated with a resin. Is listed. A focused ion beam (hereinafter also referred to as FIB) is used for this extraction. This processing is also called FIB processing. The extracted sample piece is thinned and then observed with an electron microscope.
ＦＩＢ加工に関し、特許文献２も知られている。特許文献２では、グリッドサポート３０２に固定されたＴＥＭ（透過型電子顕微鏡用）グリッド１００と呼ばれる保持部材に対し、薄片化された試料片２００を保持させ、その状態の試料片に対しＴＥＭを用いた分析を行っている（例えば特許文献２の図２、図３）。 Patent document 2 is also known regarding FIB processing. In Patent Document 2, a holding member called a TEM (for transmission electron microscope) grid 100 fixed to a grid support 302 holds a thinned sample piece 200, and the TEM is used for the sample piece in that state. Analysis is performed (for example, FIGS. 2 and 3 of Patent Document 2).
ＦＩＢ装置内にて薄片化された試料片を得るためには、ＦＩＢ装置内にバルク試料（単に試料とも称する。）を搬送しなければならない。従来だと試料搬送後、特許文献２に示すＴＥＭグリッドと呼ばれる保持部材をＦＩＢ装置内に搬送していた。つまり、ＦＩＢ装置内を予め真空にしていた場合、試料搬送時および保持部材搬送時の２回、ＦＩＢ装置内の真空を破る必要がある。 In order to obtain a thinned sample piece in the FIB apparatus, a bulk sample (also simply referred to as a sample) must be transferred into the FIB apparatus. Conventionally, a holding member called a TEM grid shown in Patent Document 2 was carried into the FIB apparatus after the sample was carried. That is, when the inside of the FIB device is evacuated in advance, it is necessary to break the vacuum in the FIB device twice during the sample transfer and the holding member transfer.
上記のように真空を破る機会が複数回存在することにより試料の変質が生じ得ることが、本発明者の鋭意研究によって明らかとなった。試料が変質してしまうと、試料の本来の状態（例えば元素拡散状況等）を正確に分析できなくなる。 As described above, the inventors of the present invention have clarified that alteration of the sample may occur due to the presence of multiple opportunities to break the vacuum. When the sample is altered, the original state of the sample (for example, element diffusion state) cannot be accurately analyzed.
本発明の課題は、真空を破ることに伴う試料の変質を抑制することである。 An object of the present invention is to suppress alteration of the sample due to breaking the vacuum.
この知見に基づき本発明者は、一つの搬送用治具に対し、試料と、ＦＩＢ装置内にて試料から摘出された試料片を保持する保持部材とを固定する、という手法を想到した。この手法ならば、ＦＩＢ装置内を予め真空にしていた場合、試料搬送時にのみＦＩＢ装置内の真空を破ることになり、試料の変質のおそれを抑制できる。 Based on this finding, the present inventor has conceived a method of fixing a sample and a holding member for holding a sample piece extracted from the sample in the FIB device to one carrying jig. According to this method, when the inside of the FIB device is evacuated in advance, the vacuum inside the FIB device is broken only when the sample is transported, and the risk of deterioration of the sample can be suppressed.
上記の知見に基づいて成された本発明の態様は、以下の通りである。
本発明の第１の態様は、
試料を集束イオンビーム（ＦＩＢ）装置内へと搬送する搬送用治具であって、
前記試料を前記搬送用治具に固定する第１固定部材と、
前記ＦＩＢ装置内にて前記試料から摘出された試料片を保持する保持部材を前記搬送用治具に固定する第２固定部材と、
を備えた、搬送用治具である。
Aspects of the present invention made based on the above findings are as follows.
The first aspect of the present invention is
A transport jig for transporting a sample into a focused ion beam (FIB) device,
A first fixing member for fixing the sample to the carrying jig;
A second fixing member for fixing the holding member, which holds the sample piece extracted from the sample in the FIB device, to the transport jig;
It is a jig for transportation provided with.
本発明の第２の態様は、第１の態様に記載の態様において、
前記第１固定部材は押え部材である。
A second aspect of the present invention is the aspect described in the first aspect,
The first fixing member is a pressing member.
本発明の第３の態様は、
第１または第２の態様に記載の搬送用治具における前記第１固定部材にて前記試料を固定する第１固定工程と、
前記第２固定部材にて前記保持部材を固定する第２固定工程と、
前記第１固定工程および前記第２固定工程後、前記搬送用治具を前記ＦＩＢ装置内に搬送する搬送工程と、
前記ＦＩＢ装置内にて前記試料から前記試料片を摘出する摘出工程と、
前記摘出工程の雰囲気のまま前記ＦＩＢ装置内にて前記保持部材に対し前記試料片を保持させる保持工程と、
を有する、試料片作製方法である。
A third aspect of the present invention is
A first fixing step of fixing the sample with the first fixing member in the carrying jig according to the first or second aspect;
A second fixing step of fixing the holding member with the second fixing member;
A carrying step of carrying the carrying jig into the FIB device after the first fixing step and the second fixing step;
An extracting step of extracting the sample piece from the sample in the FIB apparatus,
A holding step of holding the sample piece with respect to the holding member in the FIB device in the atmosphere of the extracting step;
Is a method for preparing a sample piece.
本発明の第４の態様は、
第１の態様に記載の試料片作製方法にて作製された前記試料片を分析する分析工程を有する、試料片分析方法である。
A fourth aspect of the present invention is
It is a sample piece analysis method having an analysis step of analyzing the sample piece produced by the sample piece production method according to the first aspect.
本発明によれば、真空を破ることに伴う試料の変質を抑制する技術を提供できる。 According to the present invention, it is possible to provide a technique for suppressing the alteration of the sample due to breaking the vacuum.
以下、本発明の実施の形態について、以下に説明する。 Hereinafter, embodiments of the present invention will be described below.
＜搬送用治具＞
図１は、本実施形態に係る搬送用治具１をＺ１からＺ２に向かう方向で見た時の概略平面図である。
図２は、本実施形態に係る搬送用治具１をＹ２からＹ１に向かう方向で見た時の概略側面図である。
図３は、本実施形態に係るグリッドＧをＸ２からＸ１に向かう方向で見た時の概略正面拡大図である。
なお、本明細書においては天地方向の天の方向を上方（Ｚ１方向）、地の方向を下方（Ｚ２方向）とする。また、水平方向においてグリッドＧが設けられた側をＸ２方向、その反対方向であって固定されたバルク試料Ｓが設けられた側をＸ１方向とする。水平方向においてＸ１−Ｘ２に垂直な方向であって図１の上方をＹ１方向、その反対方向をＹ２方向とする。
<Transfer jig>
FIG. 1 is a schematic plan view of the carrying jig 1 according to the present embodiment as viewed in the direction from Z1 to Z2.
FIG. 2 is a schematic side view of the carrying jig 1 according to the present embodiment as viewed in the direction from Y2 to Y1.
FIG. 3 is a schematic front enlarged view of the grid G according to the present embodiment as viewed in the direction from X2 to X1.
In addition, in the present specification, the upward direction is the upward direction (Z1 direction), and the downward direction is the downward direction (Z2 direction). Further, the side on which the grid G is provided in the horizontal direction is the X2 direction, and the side opposite to that, on which the fixed bulk sample S is provided, is the X1 direction. In the horizontal direction, a direction perpendicular to X1-X2, the upper side of FIG. 1 is the Y1 direction, and the opposite direction is the Y2 direction.
本実施形態に係る搬送用治具１は、試料Ｓを集束イオンビーム（ＦＩＢ）装置内へと搬送する機能を奏する。搬送対象となる試料Ｓには特に限定は無い。例えば形状および材質については特に限定は無い。但し、本発明の目的は試料Ｓの変質の抑制である。そのため、試料Ｓが大気雰囲気下では比較的変質しやすい材質の場合、本実施形態を適用することにより試料Ｓの変質を抑制でき、本発明の効果が顕著になる。本実施形態ではシート状の試料Ｓを例示する。 The carrying jig 1 according to the present embodiment has a function of carrying the sample S into the focused ion beam (FIB) apparatus. The sample S to be transported is not particularly limited. For example, the shape and material are not particularly limited. However, the purpose of the present invention is to suppress the alteration of the sample S. Therefore, when the sample S is a material that is relatively easily deteriorated in the atmosphere, the deterioration of the sample S can be suppressed by applying the present embodiment, and the effect of the present invention becomes remarkable. In this embodiment, a sheet-shaped sample S is exemplified.
本実施形態に係る搬送用治具１は、主に以下の構成を備える。
・試料Ｓを搬送用治具１に機械的に固定する第１固定部材（本実施形態だと爪３）
・ＦＩＢ装置内にて試料Ｓから摘出された試料片ＳＰを保持する保持部材を搬送用治具１に固定する第２固定部材（本実施形態だとクリップ４）
The carrying jig 1 according to the present embodiment mainly has the following configuration.
First fixing member for mechanically fixing the sample S to the transfer jig 1 (the claw 3 in this embodiment)
- second fixing member in FIB apparatus to fix the holding member for holding the specimen S P which has been removed from the sample S in the transport jig 1 (the clip 4 that it present embodiment)
本実施形態に係る搬送用治具１の一具体例としては、以下のものを挙げる。
まず、金属製の土台２を用意する。
The following is given as a specific example of the carrying jig 1 according to the present embodiment.
First, the metal base 2 is prepared.
土台２のＸ１方向側には爪３が設けられている。この爪３に（バルク）試料Ｓを挟み込み、機械的に固定する。この爪３が本実施形態における第１固定部材の一例に該当する。 A claw 3 is provided on the side of the base 2 in the X1 direction. The (bulk) sample S is sandwiched between the claws 3 and mechanically fixed. The claw 3 corresponds to an example of the first fixing member in the present embodiment.
第１固定部材に関しては、試料Ｓを搬送用治具１に固定可能なもので、導電性があればその態様に限定は無い。例えば、第１固定部材については、試料Ｓを固定する押え部材のうち上記爪３以外のものを採用しても構わない。 Regarding the first fixing member, the sample S can be fixed to the jig 1 for transportation, and there is no limitation on the mode as long as it has conductivity. For example, as the first fixing member, a holding member for fixing the sample S other than the claw 3 may be adopted.
土台２のＸ２方向側にはクリップ４が設けられている。このクリップ４にグリッドＧ（すなわち保持部材）を挟み込み、固定する。このクリップ４が本実施形態における第２固定部材の一例に該当する。 A clip 4 is provided on the side of the base 2 in the X2 direction. The grid G (that is, the holding member) is sandwiched in the clip 4 and fixed. The clip 4 corresponds to an example of the second fixing member in this embodiment.
第２固定部材に関しても、ＦＩＢ装置内にて試料Ｓから摘出された試料片ＳＰを保持する保持部材を搬送用治具１に固定可能なもので、導電性があれば、上記各構成の態様に限定は無い。例えば、第２固定部材については、グリッドＧを固定する押え部材のうち上記クリップ４以外のものを採用しても構わない。 Also with respect to the second fixing member, with a holding member for holding the specimen S P which has been removed from the sample S in the FIB apparatus capable fixed to the transport jig 1, if conductivity, the above-mentioned respective structures There is no limitation on the mode. For example, as the second fixing member, a holding member that fixes the grid G other than the clip 4 may be used.
また、各部材の素材に関しても、電気伝導性があり、分析対象となる試料Ｓの変質に影響を及ぼすおそれがないまたは少ないものであれば限定は無いが、試料冷却あるいは試料加熱を加味する場合は熱伝導性が高いものが好ましい。特に第２固定部材が固定するのはグリッドＧ（保持部材）であるため導電性さえあれば素材に限定は無く、クリップ４の押さえつけのような機械的な固定に限定されない。 Also, the material of each member is not limited as long as it has electrical conductivity and does not affect or has little influence on the alteration of the sample S to be analyzed, but in the case of adding sample cooling or sample heating Is preferably high in thermal conductivity. In particular, since the second fixing member fixes the grid G (holding member), the material is not limited as long as it has conductivity, and is not limited to mechanical fixing such as pressing the clip 4.
なお、本実施形態の第１固定部材による「機械的な固定」とは、導電ペーストのような液体固化による固定ではなく、また導電テープのような粘弾性物質を用いた粘着による固定ではなく、挟み込みや引っ掛け等の物理的係合による固定を指す。 The "mechanical fixing" by the first fixing member of the present embodiment does not mean fixing by solidifying liquid such as conductive paste, and fixing by adhesion using a viscoelastic substance such as conductive tape, It refers to fixing by physical engagement such as pinching or hooking.
先に述べたように、導電ペーストを使用すると、試料Ｓの変質をもたらすおそれがある。また、導電性物質により構成され且つ粘弾性物質が設けられた導電テープの場合も不具合が生じることが本発明者の鋭意研究により明らかとなっている。 As described above, the use of the conductive paste may cause deterioration of the sample S. Further, it has been clarified by the inventor of the present invention that problems also occur in the case of a conductive tape which is made of a conductive substance and is provided with a viscoelastic substance.
具体的に言うと、導電テープを用いる場合、ＦＩＢ加工の際のイオンビームによる加熱およびその加熱に対向して行われるＦＩＢ装置のステージでの冷却による温度変化により、導電テープに設けられた粘弾性物質が固化する等して、導電テープ自体が収縮／膨張する。このような固化、収縮が起こると、ＦＩＢ加工中に試料Ｓ位置が変動してしまい、適切に試料片ＳＰを摘出するのが困難となるという知見が得られた。 Specifically, when a conductive tape is used, the viscoelasticity provided on the conductive tape is affected by the temperature change due to the heating by the ion beam at the time of FIB processing and the cooling at the stage of the FIB device performed opposite to the heating. The conductive tape itself contracts/expands as the substance solidifies. Such solidification, the shrinkage occurs, the sample S position fluctuates, suitably is finding that it becomes difficult to remove the specimen S P obtained during FIB processing.
そのため、本実施形態では、導電ペーストでも導電テープでもない、機械的な固定を行うべく、第１固定部材を搬送用治具１に備えさせている。 Therefore, in the present embodiment, the transport jig 1 is provided with the first fixing member for mechanical fixing, which is neither the conductive paste nor the conductive tape.
＜試料片作製方法＞
以下、本実施形態に係る搬送用治具１を用いて試料片ＳＰを作製する方法について述べる。
<Sample piece manufacturing method>
Hereinafter, methods for making the specimen S P using the transfer jig 1 of the present embodiment.
まず、本実施形態に係る搬送用治具１における第１固定部材にて試料Ｓを機械的に固定する（第１固定工程）。 First, the sample S is mechanically fixed by the first fixing member of the carrying jig 1 according to the present embodiment (first fixing step).
次に、第２固定部材にて銅（Ｃｕ）製のグリッドＧ（保持部材）を固定する（第２固定工程）。 Next, the grid G (holding member) made of copper (Cu) is fixed by the second fixing member (second fixing step).
保持部材の態様に限定は無い。本実施形態においては、例えば図３に示すように、特許文献２に記載のグリッドＧ、すなわちメッシュ（網目）の目部分を両断したもの（すなわち２つの凸部に挟まれた凹部（メッシュの目の一部）が複数存在するグリッド）の一部を使用する。 There is no limitation on the form of the holding member. In the present embodiment, for example, as shown in FIG. 3, the grid G described in Patent Document 2, that is, the mesh (mesh) mesh is divided into two parts (that is, a concave portion sandwiched between two convex portions (mesh mesh). Part of) and multiple grids) are used.
なお、第１固定工程および第２固定工程はグローブボックス内で大気非暴露下（例えばＡｒ雰囲気下）で行うのが、試料Ｓの変質を更に抑制可能となるため、好ましい。また、第１固定工程の前においてシート状の試料Ｓを準備する工程も、同じくグローブボックス内で大気非暴露下で行うのが好ましい。 The first fixing step and the second fixing step are preferably performed in the glove box under non-exposure to the atmosphere (for example, in an Ar atmosphere) because the deterioration of the sample S can be further suppressed. Further, the step of preparing the sheet-like sample S before the first fixing step is also preferably performed in the glove box without being exposed to the atmosphere.
第１固定工程および第２固定工程後、搬送用治具１は、容器内を所定の雰囲気下（Ａｒ雰囲気下すなわち大気非暴露下）に維持できる移送容器内に封入する。その状態で移送容器ごと、搬送用治具１をＦＩＢ装置内に搬送する（第１搬送工程）。 After the first fixing step and the second fixing step, the carrying jig 1 is sealed in a transfer container capable of maintaining the inside of the container under a predetermined atmosphere (Ar atmosphere, that is, not exposed to the atmosphere). In that state, the transfer jig 1 is transferred into the FIB apparatus together with the transfer container (first transfer step).
搬送工程に前後して、ＦＩＢ装置内は真空引きする。また、移送容器内も、ＦＩＢ装置に取り付けた段階で真空引きする。そして、ＦＩＢ装置内に搬送用治具１を配置し、搬送用器具の第１固定部材にて機械的に固定された試料Ｓから試料片ＳＰを摘出する（摘出工程）。摘出工程としては、公知のＦＩＢ加工を適用すればよく、例えば特許文献１および特許文献２に記載の手法を適用すればよい。 Before and after the carrying step, the inside of the FIB device is evacuated. Further, the inside of the transfer container is also evacuated when it is attached to the FIB device. Then, the carrying jig 1 is arranged in the FIB device, and the sample piece SP is extracted from the sample S mechanically fixed by the first fixing member of the carrying instrument (extracting step). As the extraction step, known FIB processing may be applied, for example, the methods described in Patent Document 1 and Patent Document 2 may be applied.
そして、摘出工程の雰囲気のままＦＩＢ装置内にて保持部材に対し試料片ＳＰを保持させる（保持工程）。この保持は、特許文献２に記載のように、グリッドＧ（保持部材）の凸部分の先端に試料片ＳＰを付着させることにより行ってもよい。保持の態様に限定は無い。本工程は、既存のＦＩＢ装置に搭載された機能にて実施可能である。 Then, the sample piece SP is held by the holding member in the FIB device in the atmosphere of the extraction step (holding step). This retention, as described in Patent Document 2 may be performed by attaching the specimen S P to the tip of the convex portion of the grid G (holding member). There is no limitation on the mode of holding. This step can be performed by the function installed in the existing FIB device.
＜試料片分析方法＞
以下、上記の試料片作製方法にて作製された試料片ＳＰを分析する分析工程を有する、試料片分析方法について説明する。
<Sample piece analysis method>
Hereinafter, having analysis step of analyzing a specimen S P which has been prepared in the above sample piece preparation method will be described specimen analyzing method.
分析工程は試料片ＳＰに対する分析であれば特に限定は無い。例えば、ＦＩＢ装置内での試料片ＳＰの表面観察（ＳＩＭ観察）でもよいし、ＳＥＭが付属した装置である場合はＳＥＭ観察でもよい。 Analyzing step is not particularly limited as long as analysis of specimens S P. For example, it may be the surface observation of the specimen S P output in the FIB device (SIM observation), if a device that SEM was included may be a SEM observation.
その一方、別の装置を用いた分析を行ってもよい。この別の装置としては特に限定は無いが、例えばＴＥＭ（透過型電子顕微鏡）装置を使用してもよい。ＴＥＭ装置を使用する場合、試料片Ｓｐを薄片化しておく必要がある。この薄片化の具体的な方法としては、特許文献１の［００４９］−［００５０］に記載の手法を採用してもよい。 On the other hand, analysis using another device may be performed. The other device is not particularly limited, but for example, a TEM (transmission electron microscope) device may be used. When the TEM device is used, it is necessary to thin the sample piece Sp. As a specific method of thinning, the method described in [0049]-[0050] of Patent Document 1 may be adopted.
このＴＥＭ装置を使用して分析を行う場合、先ほど挙げた移送容器を再度使用する。具体例を挙げると、移送容器内を所定の雰囲気下（例えばＡｒ雰囲気下すなわち大気非暴露下）とし、大気非暴露環境のグローブボックス内へと移送容器ごと搬送用治具１を搬送する（第２搬送工程）。そして、ＴＥＭ装置用のホルダーに、保持部材ごと試料片ＳＰを設置する。その後、ＴＥＭ装置用ホルダーを移送容器内に封入する。その状態で移送容器ごと、ＴＥＭ装置用ホルダーをＴＥＭ装置内に搬送する（第３搬送工程）。その際、移送容器内の雰囲気は大気非暴露下（例えばＡｒ雰囲気）とする。そして、ＴＥＭ装置内にＴＥＭ装置用ホルダーを設置し、分析を行う。 When the analysis is performed using this TEM device, the transfer container mentioned above is used again. As a specific example, the inside of the transfer container is under a predetermined atmosphere (for example, under an Ar atmosphere, that is, under non-exposed atmosphere), and the transfer jig 1 is transferred together with the transfer container into the glove box in the non-exposed atmosphere ( 2 transportation process). Then, the sample piece SP is set together with the holding member in the holder for the TEM device. Then, the holder for the TEM device is enclosed in the transfer container. In this state, the TEM device holder is transferred into the TEM device together with the transfer container (third transfer step). At that time, the atmosphere in the transfer container is not exposed to the atmosphere (for example, Ar atmosphere). Then, a holder for the TEM device is installed in the TEM device and analysis is performed.
＜本実施形態がもたらす効果＞
本実施形態に係る搬送用治具１によれば、試料Ｓと、ＦＩＢ装置内にて試料Ｓから摘出された試料片ＳＰを保持する保持部材とを固定可能となる。そのため、ＦＩＢ装置内を予め真空にしていた場合、試料Ｓ搬送時にのみＦＩＢ装置内の真空を破ることになり、試料Ｓの変質のおそれを抑制できる。
しかも、一つの搬送用治具１に対し、試料Ｓと保持部材とを固定するとともに、導電ペーストではなく、機械的に搬送用治具１へと試料Ｓを固定することにより、試料Ｓに対して影響を与えることを抑制可能となる。
その結果、ＦＩＢ加工に伴う一連の作業中の試料Ｓの変質を抑制可能となる。
<Effects of this embodiment>
According to the transport jig 1 according to this embodiment, the sample S, can be fixed and a holding member for holding the specimen S P which has been removed from the sample S in the FIB apparatus. Therefore, if the inside of the FIB device is evacuated in advance, the vacuum inside the FIB device is broken only when the sample S is transported, and the risk of alteration of the sample S can be suppressed.
Moreover, by fixing the sample S and the holding member to one carrying jig 1, and mechanically fixing the sample S to the carrying jig 1 instead of the conductive paste, Can be suppressed.
As a result, it is possible to suppress alteration of the sample S during a series of operations associated with FIB processing.
本実施形態に係る試料片作製方法によれば、本実施形態に係る搬送用治具１を使用しているため、真空を破ることに伴う試料Ｓの変質を抑制可能となる。また、本実施形態に係る試料片分析方法でも同様に、本実施形態に係る搬送用治具１を使用しているため、真空を破ることに伴う試料Ｓの変質を抑制可能となる。 According to the sample piece manufacturing method of the present embodiment, since the carrying jig 1 of the present embodiment is used, it is possible to suppress the deterioration of the sample S due to breaking the vacuum. Further, also in the sample piece analysis method according to the present embodiment, similarly, since the transport jig 1 according to the present embodiment is used, it is possible to suppress the deterioration of the sample S due to breaking the vacuum.
＜変形例＞
なお、本発明の技術的範囲は上述した実施の形態に限定されるものではなく、発明の構成要件やその組み合わせによって得られる特定の効果を導き出せる範囲において、種々の変更や改良を加えた形態も含む。
<Modification>
Note that the technical scope of the present invention is not limited to the above-described embodiments, and various modifications and improvements may be made within a range in which specific effects obtained by the constituent features of the invention and combinations thereof can be derived. Including.
図４は、変形例に係る搬送用治具１をＺ１からＺ２に向かう方向で見た時の概略平面図である。 FIG. 4 is a schematic plan view of the carrying jig 1 according to the modified example when viewed in the direction from Z1 to Z2.
本実施形態に係る図１においては、第１固定部材（爪３）が１個の場合を例示した。その一方、爪３の数には限定は無く、例えば図４に示すように、土台２に爪３を複数設けても構わない。爪３の数は４つでもよく、それ以外の複数個数でも構わない。例えば、図４に…で記載のように、Ｘ１−Ｘ２方向で３列以上の爪３を設けてもよいし、Ｙ１−Ｙ２方向で３行以上の爪３を設けてもよい。また、爪３の向きはいずれも同じ向きであってもよいし、別の向きであってもよい。 In FIG. 1 according to this embodiment, the case where the number of the first fixing members (the claws 3) is one is illustrated. On the other hand, the number of the claws 3 is not limited, and a plurality of the claws 3 may be provided on the base 2 as shown in FIG. 4, for example. The number of the claws 3 may be four or may be a plurality of other numbers. For example, as described in FIG. 4..., the claws 3 in three or more rows may be provided in the X1-X2 direction, or the claws 3 in three or more rows may be provided in the Y1-Y2 direction. Further, the directions of the claws 3 may be the same or different directions.
また、爪３の利用態様についてであるが、市販品等を利用した場合で土台２に既にねじが形成されている場合にはこれを使用してもよい。すなわち雌ねじ穴と雄ねじとの間に爪３を挟み込み、雄ねじを雌ねじ穴に螺合させることにより、爪３を固定してもよい。つまり、爪３と雌ねじ穴（すなわち土台）との間に試料Ｓを挟み込むことにより試料Ｓを固定してもよい。ねじが形成されていない場合にはねじを形成し上記の状況を可能にしてもよい。 As for the usage of the claw 3, when a commercially available product or the like is used and a screw is already formed on the base 2, this may be used. That is, the claw 3 may be fixed by sandwiching the claw 3 between the female screw hole and the male screw and screwing the male screw into the female screw hole. That is, the sample S may be fixed by sandwiching the sample S between the claw 3 and the female screw hole (that is, the base). If not threaded, threads may be threaded to allow the above situation.
また、図４の爪３の位置に、市販品等を利用した場合で既にねじが形成されている場合にはこれを使用してもよい。その場合、各爪３の代わりに、例えばＸ１−Ｘ２方向またはＹ１−Ｙ２方向で隣接する各雌ねじ穴を架け渡す長尺の押さえ部材を第１固定部材として使用してもよい。ねじが形成されていない場合にはねじを形成し上記の状況を可能にしてもよい。この構成を採用することにより、架け渡された長尺の押さえ部材の下に複数の試料Ｓを固定することができ、作業効率が向上する。 Further, if a commercially available product or the like is used and a screw is already formed at the position of the claw 3 in FIG. 4, this may be used. In that case, instead of the claws 3, for example, a long pressing member bridging the female screw holes adjacent in the X1-X2 direction or the Y1-Y2 direction may be used as the first fixing member. If not threaded, threads may be threaded to allow the above situation. By adopting this configuration, a plurality of samples S can be fixed under the extended long pressing member, and the working efficiency is improved.
例えば本実施形態においては試料をＦＩＢ装置内へと搬送することを前提としたが、バルク試料から試料片を摘出可能な装置（更に言えば摘出可能な空間、所定の装置内への搬送、更に広義には所定の作業領域）内への搬送用途にも上記の搬送用治具は使用可能である。この搬送用治具の構成は以下の通りである。
「試料を搬送する搬送用治具であって、
前記試料を前記搬送用治具に固定する第１固定部材と、
前記試料から摘出された試料片を保持する保持部材を前記搬送用治具に固定する第２固定部材と、
を備えた、搬送用治具。」
この搬送用治具を用いた試料片作製方法および試料片分析方法も同様にＦＩＢ装置以外に適用可能である。
For example, in the present embodiment, it is premised that the sample is transported into the FIB device, but a device capable of extracting the sample piece from the bulk sample (more specifically, an extractable space, transportation into a predetermined device, In a broad sense, the above-mentioned transportation jig can be used for transportation to a predetermined work area). The structure of this carrying jig is as follows.
"A transfer jig for transferring samples,
A first fixing member for fixing the sample to the carrying jig;
A second fixing member for fixing the holding member, which holds the sample piece extracted from the sample, to the transport jig;
A jig for transportation. "
The sample piece preparation method and the sample piece analysis method using this transportation jig can be similarly applied to other than the FIB apparatus.
また、本実施形態においては試料を機械的に固定する第１固定部材を備えた搬送用治具について述べたが、それに限定されない。例えば、導電ペーストや導電テープにより試料を非機械的に固定する搬送用治具であっても、試料とグリッドとを共に搬送可能であることには違いなく、真空を破る回数を減らせることから、本発明の課題は解決される。 Further, in the present embodiment, the carrying jig including the first fixing member that mechanically fixes the sample has been described, but the present invention is not limited thereto. For example, even with a transfer jig that non-mechanically fixes a sample with a conductive paste or conductive tape, it must be possible to transfer both the sample and the grid, and the number of vacuum breaks can be reduced. The problems of the present invention are solved.
１………搬送用治具
２………土台
３………爪（第１固定部材）
４………クリップ（第２固定部材）
Ｇ………グリッド
Ｓ………（バルク）試料
ＳＰ………試料片
1---Transfer jig 2---Base 3...-Claw (first fixing member)
4.........Clip (second fixing member)
G ......... grid S ......... (bulk) samples S P ......... specimen
Claims (4)
前記試料を前記搬送用治具に固定する第１固定部材と、
前記ＦＩＢ装置内にて前記試料から摘出された試料片を保持する保持部材を前記搬送用治具に固定する第２固定部材と、
を備えた、搬送用治具。 A transport jig for transporting a sample into a focused ion beam (FIB) device,
A first fixing member for fixing the sample to the carrying jig;
A second fixing member for fixing the holding member, which holds the sample piece extracted from the sample in the FIB device, to the transport jig;
A jig for transportation.
前記第２固定部材にて前記保持部材を固定する第２固定工程と、
前記第１固定工程および前記第２固定工程後、前記搬送用治具を前記ＦＩＢ装置内に搬送する搬送工程と、
前記ＦＩＢ装置内にて前記試料から前記試料片を摘出する摘出工程と、
前記摘出工程の雰囲気のまま前記ＦＩＢ装置内にて前記保持部材に対し前記試料片を保持させる保持工程と、
を有する、試料片作製方法。 A first fixing step of fixing the sample by the first fixing member in the carrying jig according to claim 1 or 2;
A second fixing step of fixing the holding member with the second fixing member;
A carrying step of carrying the carrying jig into the FIB device after the first fixing step and the second fixing step;
An extracting step of extracting the sample piece from the sample in the FIB apparatus,
A holding step of holding the sample piece with respect to the holding member in the FIB device in the atmosphere of the extracting step;
A method for producing a sample piece, comprising:
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| JP2018116860A (en) * | 2017-01-19 | 2018-07-26 | 株式会社日立ハイテクサイエンス | Charged particle beam apparatus |
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| JP2015185457A (en) * | 2014-03-25 | 2015-10-22 | 株式会社日立ハイテクフィールディング | Three-dimensional information reproducing device |
| JP2018116860A (en) * | 2017-01-19 | 2018-07-26 | 株式会社日立ハイテクサイエンス | Charged particle beam apparatus |
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