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

試料条件、必須前処理

試料条件

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

試料サイズ

10mm×3mm　（厚さ10 mm）または　8mm×5mm　（厚さ2mm）以下

必須前処理

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

• 切断機を使い、適した大きさにサイズ調整
• 正確な面保持と荷重調整のため樹脂込め（アセトン等で溶解する樹脂を使用）
• 機械研磨を行い、表層部の凸凹、傷および加工変質層を除去
  面出し、面削りによる粗研磨（耐水ぺーパー）
  バフによる精密研磨1（9 μm、3 μm、1 μm　ダイヤモンド粒子）
  バフによる精密研磨2（0.1 μm、0.05 μm　コロイダルシリカ） 
• 必要に応じて電解研磨等の化学研磨
• 研磨終了後、樹脂を溶解させ試料を取り出す
• 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し研磨剤等を洗浄

試料条件、必須前処理

試料条件

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。

試料サイズ

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。

必須前処理

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

• 切断機を使い、適した大きさにサイズ調整
• 正確な面保持と荷重調整のため樹脂込め
• 機械研磨を行い、表層部の凸凹、傷および加工変質層を除去
  面出し、面削りによる粗研磨（耐水ぺーパー）
  バフによる精密研磨（9 μm、3 μm、1 μm　ダイヤモンド粒子）
• 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し研磨剤等を洗浄

試料条件、必須前処理

試料条件

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

試料サイズ

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

必須前処理

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

• 切断機を使い、適した大きさにサイズ調整
• 正確な面保持と荷重調整のため樹脂込め（アセトン等で溶解する樹脂を使用）
• 機械研磨を行い、表層部の凸凹、傷および加工変質層を除去
  面出し、面削りによる粗研磨（耐水ぺーパー）
  バフによる精密研磨1（9 μm、3 μm、1 μm　ダイヤモンド粒子）
  バフによる精密研磨2（0.1 μm、0.05 μm　コロイダルシリカ） 
• 必要に応じて電解研磨等の化学研磨
• 研磨終了後、樹脂を溶解させ試料を取り出す
• 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し研磨剤等を洗浄

試料条件、必須前処理

試料条件

原則として無機試料のみ。生物・有機試料不可

試料サイズ

5mm×5mm　高さは5mm以下の低い方が良い

必須前処理

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

EDS試料

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

試料条件、必須前処理

試料条件

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

＊試料サイズ

最大：5cm×5cm×1cm

試料条件、必須前処理

試料条件

原則無機試料のみ生物・有機試料不可

＊試料サイズ

5mm×2mm　高さは2mm以下の低い方が良い

必須前処理

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

試料条件、必須前処理

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。

試料条件、必須前処理

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

試料条件、必須前処理

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）

＊試料サイズ

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

Pretreatment by facility

When using the joint usage facilities at ZAIKEN, users should ensure the following sample conditions and essential pretreatment in the respective facilities.

Precautions for insertion of samples into vacuum equipment

• Never touch the samples directly with your hands.
• Do not use re-closable poly bags or similar packages to house samples, in order to prevent the samples from gathering carbon powder or dust.
  (If it is necessary to use such packages, wrap the samples in paper before putting them in the package.)
• When carrying samples, station them in a fixed position in a lidded plastic container.

EBSP

 Sample conditions, essential pretreatment

Sample conditions

As a rule, only inorganic solids are acceptable. Powdered samples and resin-embedded samples are not acceptable.

Sample size

10 mm × 3 mm (10 mm thick) or smaller, or 8 mm × 5 mm (2 mm thick) or smaller

Essential pretreatment

To prepare samples for EBSP measurement, perform mirror polishing according to the following steps (example).

• Adjust the sample to an appropriate size for measurement, using a cutting machine.
• Insert resin for accurate surface retention and load adjustment (use resin that is dissolvable in acetone, etc.).
• Perform machine polishing to remove asperities and/or scratches on the surface and processed alteration layer.
  Rough grinding by figuring and facing (with water-resistant paper)
  Precise polishing with a buff 1 (9 μm, 3 μm, 1 μm; particles; diamond particles)
  Precise polishing with a buff 2 (0.1 μm, 0.05 μm; colloidal silica)
• Perform chemical polishing, such as electrolytic polishing, if necessary.
• After polishing, dissolve the resin and remove the sample.
• Finally, wash out the abrasive (etc.), by performing ultrasonic cleaning with acetone or ethanol.

EPMA

 Sample conditions, essential pretreatment

 Sample conditions

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.

Sample size

 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.

Essential pretreatment

To prepare samples for EPMA measurement, perform mirror polishing according to the following steps (example).

• Adjust the sample to an appropriate size for measurement, using a cutting machine.
• Insert resin for accurate surface retention and load adjustment.
• Perform machine polishing to remove asperities and/or scratches on the surface and processed alteration layer.
  Rough grinding by figuring and facing (with water-resistant paper)
  Precise polishing with a buff (9 μm, 3 μm, 1 μm; diamond particles)
• Finally, wash out the abrasive (etc.), by performing ultrasonic cleaning with acetone or ethanol.

FE-AES

Sample conditions, essential pretreatment

 Sample conditions

As a rule, only inorganic solids are acceptable. Powdered samples and resin-embedded samples are not acceptable.

Sample size

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

Essential pretreatment

 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).

• Adjust the sample to an appropriate size for measurement, using a cutting machine.
• Insert resin for accurate surface retention and load adjustment (use resin dissolvable in acetone, etc.).
• Perform machine polishing to remove asperities and/or scratches on the surface and processed alteration layer.
  Rough grinding by figuring and facing (with water-resistant paper)
  Precise polishing with a buff 1 (9 μm, 3 μm, 1 μm; particles; diamond particles)
  Precise polishing with a buff 2 (0.1 μm, 0.05 μm; colloidal silica)
• Perform chemical polishing, such as electrolytic polishing, if necessary.
• After polishing, dissolve the resin and remove the sample.
• Finally, wash out the abrasive (etc.), by performing ultrasonic cleaning with acetone or ethanol.

FE-SEM

 Sample conditions, essential pretreatment

 Sample conditions

In principle, only inorganic samples are acceptable. Living things and organic samples are not acceptable.

Sample size

5 mm × 5 mm; 5 mm or less in thickness (the thinner, the better)

Essential pretreatment

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.

 EDS samples

 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.

FIB

 Sample conditions, essential pretreatment

 Sample conditions

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.

Sample size

Maximum: 5 cm × 5 cm × 1 cm

HR-SEM

 Sample conditions, essential pretreatment

 Sample conditions

As a rule, only inorganic materials are acceptable. Living things and organic samples are not acceptable.

Sample size

 5 mm × 2 mm; 2 mm or less in thickness (the thinner the better)

Essential pretreatment

Finally, perform ultrasonic cleaning with acetone or ethanol.

LV-SEM

 Sample conditions, essential pretreatment

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.

TEM

 Sample conditions, essential pretreatment

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.

XPS

Sample conditions, essential pretreatment

 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)

Sample size

 Normally, a solid plate of 1 cm × 1 cm (2 mm or less in thickness)
Consultation is required for other sample sizes.