材料技術研究所の共同利用設備を利用する場合、下記、設備ごとの試料条件、必須前処理を満たすこと
真空装置へ挿入する試料についての共通注意事項
原則として無機固体のみ。粉末試料及び樹脂包埋試料不可
10mm×3mm (厚さ10 mm)または 8mm×5mm (厚さ2mm)以下
EBSP測定をする試料は下記工程(例)により、表面を鏡面研磨する
原則として無機固体試料のみ。
樹脂包埋試料は加熱プレス装置を使った場合必ず脱泡処置を施し、樹脂内部からの放出ガスをなくす。アクリル樹脂の場合は真空含浸埋め込み装置を使う事。
直径25mm、高さ約20mm以下または直径32mm、高さ約20mm以下
これより小さい試料については問題なし。
大きい試料については要相談のこと。
EPMA測定をする試料は下記工程(例)により、表面を鏡面研磨する
原則として無機固体のみ。粉末試料及び樹脂包埋試料は不可
通常:1cm×1cm 厚さ2mm以下
非導電性試料:1cm×0.5cm 厚さ2mm以下
最大:直径26mm以下 厚さ3mm以下
FE-AES測定をする試料は原則鏡面研磨、もしくはそれに等しい表面性状を有するものとする 下記工程(例)により、表面を鏡面研磨する
原則として無機試料のみ。生物・有機試料不可
5mm×5mm 高さは5mm以下の低い方が良い
樹脂包埋試料は加熱プレス装置を使った場合必ず脱泡処置を施し、樹脂内部からの放出ガスをなくす。アクリル樹脂の場合は真空含浸埋め込み装置を使う事。
最終洗浄はアセトンもしくはエタノールで超音波洗浄を施すこと
FE-SEM付属の分析装置はEDSで検出限界に制限があるため微量濃度検出は不得意。試料作成はEPMAとほぼ同様
原則として、半導体(Si.GaAs)単結晶基板上の材料を加工する。
ガラス基盤は不可
加工サイズ:通常 横10μm×縦5μm
深さ方向は最大10μmの加工
最大:5cm×5cm×1cm
原則無機試料のみ生物・有機試料不可
5mm×2mm 高さは2mm以下の低い方が良い
最終洗浄はアセトンもしくはエタノールで超音波洗浄を施すこと
樹脂包埋試料と試料洗浄はFE-SEMと同様。試料移動範囲に制限があるためなるべく10mm直径に入るようにカットすること。
原則として、無機試料のみ生物・有機試料及び磁性体試料は不可
また電子線により損傷し、腐食性ガスが発生する試料〔イオン結合結晶等)も不可
試料前処理については、利用者が行うこと
TEM試料作成については要相談
一からの作成の場合最低1ヶ月はかかるので要注意
原則として、無機固体試料であること
粉末及び樹脂包埋試料不可
導電性が無い場合測定できない事があります。(特にペロブスカイト構造の基板上の絶縁性薄膜)
通常1cm×1cmの固体平板 (高さ2mm以下)
その他のサンプルについては要相談
When using the joint usage facilities at ZAIKEN, users should ensure the following sample conditions and essential pretreatment in the respective facilities.
As a rule, only inorganic solids are acceptable. Powdered samples and resin-embedded samples are not acceptable.
10 mm × 3 mm (10 mm thick) or smaller, or 8 mm × 5 mm (2 mm thick) or smaller
To prepare samples for EBSP measurement, perform mirror polishing according to the following steps (example).
As a rule, only inorganic solid samples are acceptable.
For resin-embedded samples, if a heat press machine is used, be sure to perform degassing treatment so as not to emit the gas from inside the resin. For acrylic resin, be sure to use the vacuum impregnation embedding equipment.
25 mm in diameter and less than about 20 mm in height, or 32 mm in diameter and less than about 20 mm in height
Samples smaller than the abovementioned sizes are acceptable.
Consultation is required for larger samples.
To prepare samples for EPMA measurement, perform mirror polishing according to the following steps (example).
As a rule, only inorganic solids are acceptable. Powdered samples and resin-embedded samples are not acceptable.
Normally: 1 cm × 1 cm, 2 mm or less in thickness
Non-conductive samples: 1 cm × 0.5 cm, 2 mm or less in thickness
Maximum: 26 mm in diameter, 3 mm in thickness
Samples for FE-AES measurement should, as a rule, have the surface quality of mirror polishing or equivalent. Perform mirror polishing according to the following steps (example).
In principle, only inorganic samples are acceptable. Living things and organic samples are not acceptable.
5 mm × 5 mm; 5 mm or less in thickness (the thinner, the better)
For resin-embedded samples, if a heat press machine is used, be sure to perform degassing treatment so as not to emit the gas from inside the resin. For acrylic resin, be sure to use the vacuum impregnation embedding equipment.
Finally, perform ultrasonic cleaning with acetone or ethanol.
The analysis equipment equipped with the FE-SEM is EDS equipment, which has a restricted detection limit; thus, it is not good at detecting trace concentrations. Sample preparation procedures are similar to those for the EPMA.
As a rule, process the materials on semiconductor (Si.GaAs) single-crystal substrate.
Glass substrates are not acceptable.
Cutting size: Normally, 10 μm (width) × 5 μm (length)
The maximum processing depth is 10 µm.
Maximum: 5 cm × 5 cm × 1 cm
As a rule, only inorganic materials are acceptable. Living things and organic samples are not acceptable.
5 mm × 2 mm; 2 mm or less in thickness (the thinner the better)
Finally, perform ultrasonic cleaning with acetone or ethanol.
For resin-embedded samples, if a heat press machine is used, be sure to perform degassing treatment so as not to emit the gas from inside the resin. For acrylic resin, be sure to use the vacuum impregnation embedding equipment.
Finally, perform ultrasonic cleaning with acetone or ethanol.
Cut samples to within 10 mm in diameter whenever possible, because the sample movement range is limited.
As a rule, only inorganic samples are acceptable. Biological/organic materials and ferromagnetic materials are not acceptable.
Also, samples that may be damaged by the electron beam and produce corrosive gases (e.g., ion bonded crystals) are not acceptable.
Users of the facility should perform sample pretreatment.
Consultation is required for TEM sample preparation.
Note that preparation from scratch requires least one month.
As a rule, only inorganic solid samples are acceptable.
Powdered samples and resin-embedded samples are not acceptable.
If the sample does not have electrical conductivity, it may be unable to be measured (especially in the case of insulation thin film on a board with perovskite-type structure)
Normally, a solid plate of 1 cm × 1 cm (2 mm or less in thickness)
Consultation is required for other sample sizes.