JP6858607B2 - Method for preparing analytical sample and method for analyzing powder or granular material sample - Google Patents

Method for preparing analytical sample and method for analyzing powder or granular material sample Download PDF

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JP6858607B2
JP6858607B2 JP2017054963A JP2017054963A JP6858607B2 JP 6858607 B2 JP6858607 B2 JP 6858607B2 JP 2017054963 A JP2017054963 A JP 2017054963A JP 2017054963 A JP2017054963 A JP 2017054963A JP 6858607 B2 JP6858607 B2 JP 6858607B2
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正和 木村
正和 木村
昭弘 麻生
昭弘 麻生
木村　昌弘
昌弘 木村
吉田　仁
仁 吉田
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JX Nippon Mining and Metals Corp
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Description

本発明は、分析試料の作製方法、及び粉粒体試料の分析方法に関する。 The present invention relates to a method for preparing an analytical sample and a method for analyzing a powder or granular material sample.

粉粒体試料を分析する場合には、粉粒体試料を樹脂固結後に成型加工し、観察試料を作製する（例えば、特許文献１，２等参照）。例えば、粉粒体試料を走査型電子顕微鏡（ＳＥＭ：Scanning Electron Microscope）を用いて分析する場合、粉粒体試料を樹脂固結させた後に、機械研磨や化学研磨等の水分と接触させながらの研磨を実行し、仕上げにＡｒイオンビームで研磨して観察表面を調整する。 When analyzing the powder or granular material sample, the powder or granular material sample is molded after the resin is consolidated to prepare an observation sample (see, for example, Patent Documents 1 and 2). For example, when analyzing a powder or granular material sample using a scanning electron microscope (SEM), the powder or granular material sample is resin-solidified and then brought into contact with water such as mechanical polishing or chemical polishing. Polishing is performed and the observation surface is adjusted by polishing with an Ar ion beam for finishing.

特開２０１５−４０７２４号公報Japanese Unexamined Patent Publication No. 2015-40724 特開２０１５−１１４２４１号公報Japanese Unexamined Patent Publication No. 2015-114241

しかしながら、粉粒体試料の中には正極材原料のように水分や大気との接触により変質し易いものがある。粉粒体試料が変質すると適切な分析結果を得ることができなくなるおそれがある。 However, some powder or granular material samples, such as the raw material for the positive electrode material, are easily deteriorated by contact with moisture or the atmosphere. If the powder or granular material sample is altered, it may not be possible to obtain appropriate analysis results.

本発明は上記の課題に鑑みてなされたものであり、分析試料の変質を抑制することが可能な分析試料の作製方法、及び適切な分析結果を得ることが可能な粉粒体試料の分析方法を提供することを目的とする。 The present invention has been made in view of the above problems, a method for producing an analytical sample capable of suppressing deterioration of the analytical sample, and a method for analyzing a powder or granular material sample capable of obtaining appropriate analytical results. The purpose is to provide.

本発明の分析試料の作製方法は、粉粒体試料と樹脂の混合試料を第１の治具に形成された断面長方形の貫通孔に注入し、固結後、第２の治具を前記貫通孔に嵌入することで、前記貫通孔から樹脂固結片を押し出し、前記樹脂固結片を大気非暴露状態に保持したまま前記樹脂固結片をイオン研磨する、方法である。 In the method for producing an analysis sample of the present invention, a mixed sample of a powder or granular material sample and a resin is injected into a through hole having a rectangular cross section formed in the first jig, and after consolidation, the second jig is penetrated. This is a method in which a resin solidified piece is extruded from the through hole by being fitted into the hole, and the resin solidified piece is ion-polished while the resin solidified piece is kept in an air-unexposed state.

本発明の粉粒体試料の分析方法は、本発明の分析試料の作製方法を用いて作製した分析試料を、大気非暴露状態を保持した状態で走査型電子顕微鏡により分析する方法である。 The method for analyzing a powder or granular material sample of the present invention is a method for analyzing an analytical sample prepared by using the method for preparing an analytical sample of the present invention with a scanning electron microscope while maintaining an unexposed state in the atmosphere.

本発明の分析試料の作製方法は、分析試料の変質を抑制することができるという効果を奏する。また、本発明の粉粒体試料の分析方法は、適切な分析結果を得ることができるという効果を奏する。 The method for producing an analytical sample of the present invention has the effect of suppressing alteration of the analytical sample. Further, the method for analyzing a powder or granular material sample of the present invention has an effect that an appropriate analysis result can be obtained.

一実施形態に係る粉粒体試料の分析方法について示すフローチャートである。It is a flowchart which shows the analysis method of the powder / granular material sample which concerns on one Embodiment. 図２（ａ）〜図２（ｃ）は、樹脂固結片の作製方法について説明するための図である。2 (a) to 2 (c) are views for explaining a method for producing a resin solidified piece. 樹脂固結片を示す斜視図である。It is a perspective view which shows the resin consolidation piece. 図４（ａ）〜図４（ｃ）は、樹脂固結片をホルダスタンドにセットする手順について説明するための図である。4 (a) to 4 (c) are views for explaining a procedure for setting the resin solidified piece on the holder stand. 図５（ａ）、図５（ｂ）は、樹脂固結片の隣接する２面が９０°の場合のイオン研磨について模式的に示す図である。5 (a) and 5 (b) are diagrams schematically showing ion polishing when two adjacent surfaces of the resin solidified pieces are at 90 °. 図６（ａ）、図６（ｂ）は、樹脂固結片の隣接する２面が９０°でない場合のイオン研磨について模式的に示す図である。6 (a) and 6 (b) are diagrams schematically showing ion polishing when two adjacent surfaces of the resin solidified piece are not 90 °.

以下、一実施形態に係る分析試料の作製方法、および粉粒体試料の分析方法について、図１〜図６に基づいて、詳細に説明する。図１は、粉粒体試料の分析方法について示すフローチャートである。 Hereinafter, the method for producing an analytical sample and the method for analyzing a powder or granular material sample according to an embodiment will be described in detail with reference to FIGS. 1 to 6. FIG. 1 is a flowchart showing a method for analyzing a powder or granular material sample.

図１に示すように、本実施形態においては、樹脂固結片作製工程（Ｓ１０）、仕上げ研磨（イオン研磨）工程（Ｓ１２）。ＳＥＭ分析工程（Ｓ１４）が実行される。以下、各工程について詳細に説明する。 As shown in FIG. 1, in the present embodiment, the resin solidified piece manufacturing step (S10) and the finish polishing (ion polishing) step (S12). The SEM analysis step (S14) is performed. Hereinafter, each step will be described in detail.

（樹脂固結片作製工程（Ｓ１０））
まず、樹脂固結片作製工程（Ｓ１０）について説明する。なお、樹脂固結片の作製作業は、不活性ガス中（グローブボックス内）において行われる。 (Resin Consolidation Fragment Fabrication Step (S10))
First, the resin solidified piece manufacturing step (S10) will be described. The work of producing the resin solidified piece is performed in the inert gas (in the glove box).

まず、作業者は、図２（ａ）に示すように、断面長方形（縦２〜１２ｍｍ、横１〜３ｍｍ）の貫通孔１２が形成された第１の治具としての型枠１００を用意する。そして、型枠１００の下面に高分子フィルム（例えば、ＰＥＴ（Polyethylene terephthalate）フィルム）４０を設け、粘着テープ５０で高分子フィルム４０を固定する。その後、作業者は、図２（ｂ）に示すように、分析対象である粉粒体試料８０を貫通孔１２内に上方から入れるとともに樹脂材料９０を注入する。ここで、樹脂材料は、エポキシ埋込樹脂を１時間程度４０℃の雰囲気内に放置した後、硬化剤を例えば２５：３（＝エポキシ埋込樹脂：硬化剤）の割合で混ぜたものである。 First, as shown in FIG. 2A, the operator prepares a mold 100 as a first jig in which a through hole 12 having a rectangular cross section (length 2 to 12 mm, width 1 to 3 mm) is formed. .. Then, a polymer film (for example, PET (Polyethylene terephthalate) film) 40 is provided on the lower surface of the mold 100, and the polymer film 40 is fixed with the adhesive tape 50. After that, as shown in FIG. 2B, the operator inserts the powder or granular material sample 80 to be analyzed into the through hole 12 from above and injects the resin material 90. Here, the resin material is obtained by leaving the epoxy-embedded resin in an atmosphere of 40 ° C. for about 1 hour, and then mixing the curing agent at a ratio of, for example, 25: 3 (= epoxy-embedded resin: curing agent). ..

次いで、作業者は、常温で真空脱泡（または減圧脱泡）する。これにより、粉粒体試料８０と樹脂材料９０が混合して貫通孔１２の底に沈殿する。その後は、大気で固結するまで放置し、粉粒体試料８０と樹脂材料９０の混合したものが固結するまで待つ。なお、粉粒体試料８０は、大気や水と接触すると変質する性質を有するものとする。 The operator then vacuum defoams (or vacuum defoams) at room temperature. As a result, the powder or granular material sample 80 and the resin material 90 are mixed and settled at the bottom of the through hole 12. After that, it is left to stand until it solidifies in the air, and waits until the mixture of the powder or granular material sample 80 and the resin material 90 solidifies. It is assumed that the powder or granular material sample 80 has a property of deteriorating when it comes into contact with air or water.

次いで、作業者は、図２（ｃ）に示すように、第２の治具としての押し出し治具２００を用いて、型枠１００から粉粒体試料８０と樹脂材料９０を押し出す。これにより、図３に示すような樹脂固結片１８０が押し出されるようになっている。図３の樹脂固結片１８０は、断面長方形の貫通孔１２内で鋳造されているため、後の工程でイオン研磨（イオンミリング）される面８０ａと、該面８０ａに隣接する面８０ｂとがなす角度が９０°となっている。また、イオン研磨される面８０ａは、図２（ｂ）において高分子フィルム４０が接触しているため、凹凸がほとんどない。このため、イオン研磨される面８０ａをイオン研磨する前に研磨する必要はない。すなわち、イオン研磨される面８０ａをイオン研磨する前に機械研磨や化学研磨等を行う必要がない。この場合、水を用いた研磨を行わなくてもよいため、粉粒体試料が水により変質するのを抑制することができる。 Next, as shown in FIG. 2C, the operator extrudes the powder or granular material sample 80 and the resin material 90 from the mold 100 by using the extrusion jig 200 as the second jig. As a result, the resin solidified piece 180 as shown in FIG. 3 is extruded. Since the resin solidified piece 180 of FIG. 3 is cast in the through hole 12 having a rectangular cross section, the surface 80a to be ion-polished (ion milled) in a later step and the surface 80b adjacent to the surface 80a are formed. The angle of formation is 90 °. Further, the surface 80a to be ion-polished has almost no unevenness because the polymer film 40 is in contact with the surface 80a in FIG. 2B. Therefore, it is not necessary to polish the surface 80a to be ion-polished before ion-polishing. That is, it is not necessary to perform mechanical polishing, chemical polishing, or the like before ion polishing the surface 80a to be ion-polished. In this case, since it is not necessary to perform polishing with water, it is possible to prevent the powder or granular material sample from being altered by water.

（仕上げ研磨工程（Ｓ１２））
次に、仕上げ研磨工程（Ｓ１２）について説明する。仕上げ研磨工程においては、作業者は、まず、図４（ａ）に示すような専用の試料ホルダ（ホルダスタンド）１２０を不活性ガス中（グローブボックス内）に用意する。ここで、ホルダスタンド１２０は、平板状の遮蔽板１２２と、位置合わせ面１２４ａを有する位置合わせ部１２４とを有する。遮蔽板１２２の下面と位置合わせ面１２４ａの間の角度は垂直（９０°）となっている。 (Finish polishing process (S12))
Next, the finish polishing step (S12) will be described. In the finish polishing step, the operator first prepares a dedicated sample holder (holder stand) 120 as shown in FIG. 4A in an inert gas (inside the glove box). Here, the holder stand 120 has a flat plate-shaped shielding plate 122 and an alignment portion 124 having an alignment surface 124a. The angle between the lower surface of the shielding plate 122 and the alignment surface 124a is vertical (90 °).

次いで、作業者は、図４（ｂ）に示すように、樹脂固結片１８０を位置決めする。この場合、イオン研磨される面８０ａを位置合わせ面１２４ａに当て、面８０ｂを遮蔽板１２２に当てることで、位置合わせを行う。ここで、面８０ａと面８０ｂのなす角を９０°としておくことで、遮蔽板１２２と樹脂固結片１８０との間には隙間が生じないようになっている。 The operator then positions the resin consolidation piece 180, as shown in FIG. 4 (b). In this case, the ion-polished surface 80a is applied to the alignment surface 124a, and the surface 80b is applied to the shielding plate 122 to perform alignment. Here, by setting the angle formed by the surface 80a and the surface 80b to 90 °, no gap is formed between the shielding plate 122 and the resin solidified piece 180.

次いで、作業者は、樹脂固結片１８０の位置を固定する固定部材１３０をホルダスタンド１２０にネジ止めする。その後は、ホルダスタンド１２０にホルダスタンド１２０内を大気遮断状態にするキャップを装着し、その状態でＡｒイオン研磨装置（例えば、ＩＭ４０００形イオンミリング装置）にホルダスタンド１２０を設置し、イオン研磨を実行する。なお、ホルダスタンド１２０においては、遮蔽板１２２と位置合わせ面１２４ａとの間の距離は１ｍｍ程度であり、また、遮蔽板１２２と固定部材１３０の間で樹脂固結片１８０を挟んで固定するには、１ｍｍ程度の寸法が必要となる。したがって、樹脂固結片１８０の図４（ｂ）の左右方向の寸法は、２ｍｍ以上必要である。 Next, the operator screwes the fixing member 130 for fixing the position of the resin consolidation piece 180 to the holder stand 120. After that, a cap is attached to the holder stand 120 to block the inside of the holder stand 120 from the atmosphere, and in that state, the holder stand 120 is installed in an Ar ion polishing device (for example, IM4000 type ion milling device) to perform ion polishing. To do. In the holder stand 120, the distance between the shielding plate 122 and the alignment surface 124a is about 1 mm, and the resin solidified piece 180 is sandwiched and fixed between the shielding plate 122 and the fixing member 130. Requires a dimension of about 1 mm. Therefore, the dimension of the resin consolidated piece 180 in the left-right direction in FIG. 4B needs to be 2 mm or more.

ここで、イオン研磨装置においては、Ａｒイオン研磨を行うこととする。イオン研磨装置の内部は、ホルダスタンド１２０が設置された後に真空状態とされる。そして、真空状態下で、ホルダスタンド１２０からキャップを外し、樹脂固結片１８０のイオン研磨を実行する。イオン研磨の際には、ホルダスタンド１２０とともに、樹脂固結片１８０が揺動される。また、イオンの加速電圧は３．５〜４．５ｋＶに設定され、イオンビームは間欠照射されるようになっている。更に、イオン研磨装置では、ホルダスタンド１２０を液体窒素により冷却することで、熱伝導により樹脂固結片１８０を冷却しながらイオン研磨を行う。このように、イオン研磨の際に樹脂固結片１８０を冷却することで、樹脂固結片１８０が常温以上の温度に加熱すると変質する性質を有していても、樹脂固結片１８０の変質を防ぐことができる。 Here, in the ion polishing apparatus, Ar ion polishing is performed. The inside of the ion polishing device is evacuated after the holder stand 120 is installed. Then, under a vacuum state, the cap is removed from the holder stand 120, and the resin solidified piece 180 is ion-polished. During ion polishing, the resin solidified piece 180 is shaken together with the holder stand 120. Further, the acceleration voltage of the ions is set to 3.5 to 4.5 kV, and the ion beam is intermittently irradiated. Further, in the ion polishing apparatus, by cooling the holder stand 120 with liquid nitrogen, ion polishing is performed while cooling the resin solidified piece 180 by heat conduction. In this way, by cooling the resin solidified piece 180 during ion polishing, even if the resin solidified piece 180 has the property of deteriorating when heated to a temperature higher than room temperature, the resin solidified piece 180 is denatured. Can be prevented.

ここで、イオン研磨について、図５、図６に基づいてより詳細に説明する。図５（ａ）は、面８０ａと面８０ｂのなす角が９０°の場合を示し、図６（ａ）は、面８０ａと面８０ｂのなす角が９０°でない場合（比較例）を示している。図５（ａ）の場合、イオン研磨を行うと、図５（ｂ）に示すように、観察断面を平滑に研磨することができる。一方、図６（ａ）の場合、面８０ｂと遮蔽板１２２との間には隙間が生じるため、この状態でイオン研磨を行うと、図６（ｂ）に示すように、遮蔽板１２２と面８０ｂとの間にＡｒイオンが入り込んでしまい、観察断面を平滑に研磨することができなくなる。 Here, ion polishing will be described in more detail with reference to FIGS. 5 and 6. FIG. 5A shows a case where the angle formed by the surface 80a and the surface 80b is 90 °, and FIG. 6A shows a case where the angle formed by the surface 80a and the surface 80b is not 90 ° (comparative example). There is. In the case of FIG. 5 (a), when ion polishing is performed, the observed cross section can be smoothly polished as shown in FIG. 5 (b). On the other hand, in the case of FIG. 6A, a gap is generated between the surface 80b and the shielding plate 122. Therefore, when ion polishing is performed in this state, the shielding plate 122 and the surface are formed as shown in FIG. 6B. Ar ions enter between the 80b and the observation cross section cannot be polished smoothly.

このように、本実施形態では、図２（ａ）〜図２（ｃ）に示すような方法で、面８０ａ，８０ｂのなす角が９０°の樹脂固結片１８０を作製しているので、イオン研磨により観察断面を適切な状態にすることができる。 As described above, in the present embodiment, the resin solidified piece 180 having a 90 ° angle formed by the surfaces 80a and 80b is produced by the method shown in FIGS. 2 (a) to 2 (c). The observation cross section can be brought into an appropriate state by ion polishing.

（ＳＥＭ分析工程（Ｓ１４））
次に、ＳＥＭ分析工程（Ｓ１４）について説明する。イオン研磨が終了した後は、作業者は、ホルダスタンド１２０にキャップを装着し、キャップが装着されたホルダスタンド１２０をＡｒイオン研磨装置から取り出し、走査型電子顕微鏡（ＳＥＭ：Scanning Electron Microscope）に設置する。ＳＥＭでは、ＳＥＭ内部を真空にした後、ホルダスタンド１２０からキャップを外し、樹脂固結片１８０の観察面の観察や分析を実行する。本実施形態においては、樹脂固結片１８０を大気や水に触れさせず、かつ加熱もしないため、粉粒体試料が割れたり膨らんだりするのを防ぐことができ、分析精度を向上することができる。 (SEM analysis step (S14))
Next, the SEM analysis step (S14) will be described. After the ion polishing is completed, the operator attaches a cap to the holder stand 120, removes the holder stand 120 with the cap from the Ar ion polishing apparatus, and installs it in a scanning electron microscope (SEM). To do. In the SEM, after the inside of the SEM is evacuated, the cap is removed from the holder stand 120, and the observation surface of the resin solidified piece 180 is observed and analyzed. In the present embodiment, since the resin solidified piece 180 is not exposed to the atmosphere or water and is not heated, it is possible to prevent the powder or granular material sample from cracking or swelling, and it is possible to improve the analysis accuracy. it can.

以上、詳細に説明したように、本実施形態によると、粉粒体試料８０を樹脂材料９０に混合して樹脂固結片１８０を作製し（Ｓ１０）、樹脂固結片１８０を大気非暴露状態に保持したまま樹脂固結片１８０をイオン研磨する（Ｓ１２）。このようにすることで、本実施形態では、樹脂固結片１８０を大気に暴露せずにイオン研磨するため、粉粒体試料８０が大気との接触により変質する物質であっても、変質を抑制または防止することができる。また、作製した樹脂固結片１８０を直接イオン研磨することで、機械研磨や化学研磨等を行わなくてもよいため、樹脂固結片１８０と水の接触を防ぐことができる。これにより、粉粒体試料８０が水と接触し変質するのを防ぐことが可能となる。 As described in detail above, according to the present embodiment, the powder / granular material sample 80 is mixed with the resin material 90 to prepare the resin solidified piece 180 (S10), and the resin solidified piece 180 is not exposed to the atmosphere. The resin solidified piece 180 is ion-polished while being held at (S12). By doing so, in the present embodiment, the resin solidified piece 180 is ion-polished without being exposed to the atmosphere, so that even if the powder or granular material sample 80 is a substance that is altered by contact with the atmosphere, it is altered. Can be suppressed or prevented. Further, by directly ion-polishing the produced resin solidified piece 180, it is not necessary to perform mechanical polishing, chemical polishing, or the like, so that contact between the resin solidified piece 180 and water can be prevented. This makes it possible to prevent the powder or granular material sample 80 from coming into contact with water and deteriorating.

また、本実施形態では、イオン研磨する際に、樹脂固結片１８０を冷却しながら研磨する。これにより、樹脂固結片１８０が常温以上の温度に加熱することで変質する性質を有していても、イオン研磨の際に樹脂固結片１８０が変質するのを防ぐことが可能となる。 Further, in the present embodiment, when ion polishing is performed, the resin solidified piece 180 is polished while being cooled. As a result, even if the resin solidified piece 180 has a property of being altered by heating to a temperature of room temperature or higher, it is possible to prevent the resin solidified fragment 180 from being altered during ion polishing.

また、本実施形態では、樹脂固結片１８０のイオン研磨される面８０ａと近接する面８０ｂとのなす角を９０°としている。これにより、イオン研磨の際に、遮蔽板１２２と面８０ｂとの間に隙間が生じないため、観察表面を適切な状態に研磨することが可能となる。 Further, in the present embodiment, the angle formed by the ion-polished surface 80a of the resin solidified piece 180 and the adjacent surface 80b is 90 °. As a result, during ion polishing, there is no gap between the shielding plate 122 and the surface 80b, so that the observation surface can be polished to an appropriate state.

また、本実施形態では、イオン研磨として、Ａｒイオン研磨を採用し、イオンの加速電圧を３．５〜４．５ｋＶとし、かつ、イオンビームを間欠照射する。これにより、Ａｒイオン研磨を適切な条件下で行うことができる。 Further, in the present embodiment, Ar ion polishing is adopted as the ion polishing, the acceleration voltage of the ions is set to 3.5 to 4.5 kV, and the ion beam is intermittently irradiated. Thereby, Ar ion polishing can be performed under appropriate conditions.

また、本実施形態では、樹脂固結片１８０を作製する際、粉粒体試料８０と樹脂材料９０を型枠１００に形成された断面長方形の貫通孔１２に注入し、固結後、押し出し治具２００を貫通孔１２に嵌入することで、樹脂固結片１８０を押し出す。このようにして樹脂固結片１８０を作製することで、簡易に、樹脂固結片１８０のイオン研磨される面８０ａと近接する面８０ｂとのなす角を９０°にすることができる。 Further, in the present embodiment, when the resin consolidation piece 180 is produced, the powder or granular material sample 80 and the resin material 90 are injected into the through hole 12 having a rectangular cross section formed in the mold 100, and after the consolidation, the resin material 90 is extruded. By fitting the tool 200 into the through hole 12, the resin solidified piece 180 is extruded. By producing the resin consolidated piece 180 in this way, the angle formed by the ion-polished surface 80a of the resin consolidated piece 180 and the adjacent surface 80b can be easily set to 90 °.

また、本実施形態では、樹脂固結片１８０をイオン研磨した観察試料をＳＥＭにより分析するので、大気や水、熱の影響を受けていない観察試料の表面を分析することが可能である。 Further, in the present embodiment, since the observation sample obtained by ion-polishing the resin solidified piece 180 is analyzed by SEM, it is possible to analyze the surface of the observation sample that is not affected by air, water, or heat.

なお、上記実施形態では、粉粒体試料８０が大気、水、熱の少なくとも１つからの影響を受けない（変質しない）場合もある。このような場合には、粉粒体試料８０の性質に応じて、各工程の条件を適宜緩和することとしてもよい。 In the above embodiment, the powder or granular material sample 80 may not be affected (altered) by at least one of air, water, and heat. In such a case, the conditions of each step may be appropriately relaxed according to the properties of the powder or granular material sample 80.

上述した実施形態は本発明の好適な実施の例である。但し、これに限定されるものではなく、本発明の要旨を逸脱しない範囲内において種々変形実施可能である。 The embodiments described above are examples of preferred embodiments of the present invention. However, the present invention is not limited to this, and various modifications can be made without departing from the gist of the present invention.

１２ 貫通孔
８０ 粉粒体試料
９０ 樹脂
１００ 型枠（第１の治具）
１２０ ホルダスタンド（専用の試料ホルダ）
１８０ 樹脂固結片
２００ 押し出し治具（第２の治具） 12 Through hole 80 Powder or granular material sample 90 Resin 100 Formwork (first jig)
120 Holder stand (dedicated sample holder)
180 Resin consolidation piece 200 Extruding jig (second jig)

Claims (12)

粉粒体試料と樹脂の混合試料を第１の治具に形成された断面長方形の貫通孔に注入し、固結後、第２の治具を前記貫通孔に嵌入することで、前記貫通孔から樹脂固結片を押し出し、
前記樹脂固結片を大気非暴露状態に保持したまま前記樹脂固結片をイオン研磨する、
分析試料の作製方法。 A mixed sample of a powder or granular material sample and a resin is injected into a through hole having a rectangular cross section formed in the first jig, and after consolidation, the second jig is fitted into the through hole to form the through hole. Extrude the resin solidified pieces from
The resin solidified pieces are ion-polished while being kept in an air-free state.
How to prepare an analytical sample. 前記イオン研磨する際に、前記樹脂固結片を冷却しながら研磨することを特徴とする請求項１に記載の分析試料の作製方法。 The method for producing an analytical sample according to claim 1, wherein when the ion polishing is performed, the resin solidified pieces are polished while being cooled. 前記樹脂固結片を冷却しながら前記イオン研磨する際に、液体窒素の熱伝導により前記樹脂固結片を冷却することを特徴とする請求項２に記載の分析試料の作製方法。 The method for producing an analytical sample according to claim 2, wherein the resin solidified pieces are cooled by heat conduction of liquid nitrogen when the ion polishing is performed while cooling the resin solidified pieces. 前記樹脂固結片を大気非暴露状態に保持する際に、専用の試料ホルダを使用することを特徴とする請求項１〜３のいずれか一項に記載の分析試料の作製方法。 The method for producing an analytical sample according to any one of claims 1 to 3, wherein a dedicated sample holder is used when the resin consolidated piece is kept in an air-unexposed state. 前記樹脂固結片は、なす角度が９０°である隣接する２面を有することを特徴とする請求項１〜４のいずれか一項に記載の分析試料の作製方法。 The method for producing an analytical sample according to any one of claims 1 to 4, wherein the resin solidified piece has two adjacent surfaces having an angle of 90 °. 前記イオン研磨はＡｒイオン研磨であり、イオンの加速電圧を３．５〜４．５ｋＶとすることを特徴とする請求項１〜５のいずれか一項に記載の分析試料の作製方法。 The method for producing an analytical sample according to any one of claims 1 to 5, wherein the ion polishing is Ar ion polishing, and the acceleration voltage of ions is 3.5 to 4.5 kV. 前記イオン研磨はイオンビームを間欠照射することを特徴とする請求項１〜６のいずれか一項に記載の分析試料の作製方法。 The method for producing an analytical sample according to any one of claims 1 to 6, wherein the ion polishing involves intermittent irradiation of an ion beam. 前記粉粒体試料は大気と接触すると変質する性質を持つ試料であることを特徴とする請求項１〜７のいずれか一項に記載の分析試料の作製方法。 The method for producing an analytical sample according to any one of claims 1 to 7, wherein the powder or granular material sample is a sample having a property of deteriorating when it comes into contact with the atmosphere. 前記粉粒体試料は水分と接触すると変質する性質を持つ試料であることを特徴とする請求項１〜７のいずれか一項に記載の分析試料の作製方法。 The method for producing an analytical sample according to any one of claims 1 to 7, wherein the powder or granular material sample is a sample having a property of deteriorating when it comes into contact with water. 前記粉粒体試料は常温以上の温度に加熱すると変質する性質を持つ試料であることを特徴とする請求項１〜７のいずれか一項に記載の分析試料の作製方法。 The method for producing an analytical sample according to any one of claims 1 to 7, wherein the powder or granular material sample is a sample having a property of deteriorating when heated to a temperature of room temperature or higher. 前記貫通孔は、縦２〜１２ｍｍ、横１〜３ｍｍの断面長方形の貫通孔であることを特徴とする請求項１〜１０のいずれか一項に記載の分析試料の作製方法。 The method for producing an analytical sample according to any one of claims 1 to 10, wherein the through hole is a through hole having a rectangular cross section having a length of 2 to 12 mm and a width of 1 to 3 mm. 請求項１〜１１のいずれか一項に記載の分析試料の作製方法を用いて作製した分析試料を、大気非暴露状態を保持した状態で走査型電子顕微鏡により分析することを特徴とする粉粒体試料の分析方法。
A powder or granular material produced by using the method for producing an analytical sample according to any one of claims 1 to 11 is analyzed by a scanning electron microscope while maintaining an unexposed state in the atmosphere. Analysis method of body sample.
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