Application Note EM... · Metal sheets are thicker than 100 µm. Mechanical pre-preparation is...

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Material Research Life Science Research Medical Research Industrial Manufacturing Natural Resources Application Note Metal films and sheets Sample Preparation for TEM related instrument Leica EM RES102

Transcript of Application Note EM... · Metal sheets are thicker than 100 µm. Mechanical pre-preparation is...

Page 1: Application Note EM... · Metal sheets are thicker than 100 µm. Mechanical pre-preparation is necessary to obtain an acceptable initial thickness and a good surface quality for ion

Material

Research

Life Science

Research

Medical

Research

Industrial

Manufacturing

Natural

Resources

Application Note Metal films and sheetsSample Preparation for TEM

related instrument Leica EM RES102

Page 2: Application Note EM... · Metal sheets are thicker than 100 µm. Mechanical pre-preparation is necessary to obtain an acceptable initial thickness and a good surface quality for ion

Metal films and sheets

FORMULATION OF THE PROBLEMMost metal films already have a thickness that requires no further mechanical pre-preparation. Frequently, how-ever, they are also domed, which can lead to undefined milling angles. This is a disadvantage, particularly for films that contain inclusions, and that therefore mostly require very flat milling angles.

Milling angles that are too high, and which thereby also lead to excessive energy transfer through the ions, often result in the destruction of the sample material. The latter should be proved by the use of various milling angles. To do this, thin Al and Ti films were prepared.

PREPARATION CONDITIONSMechanical pre-preparationDisc puncher to cut out 3 mm discs

Ion millingSample holder: Quick-clamp-holderAcceleration voltage: 7 kV / 2 kV (final thinning)Milling angle: 16° and 6°Sample movement: Rotation

The metal films can be prepared automatically with the Leica EM RES102. In addition, single milling steps or complete programs can be written. These will then be checked by the computer and, with the help of an optical automatic termination, will be stopped at the optimum point in time. The presence of the user during the milling process is not necessary. Time-consuming sample preparations can thereby be carried out overnight.

Programmed milling sequence on the touch screen

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Page 3: Application Note EM... · Metal sheets are thicker than 100 µm. Mechanical pre-preparation is necessary to obtain an acceptable initial thickness and a good surface quality for ion

RESULTSThe metal films can be prepared to be electron-transparent over a wide range. The influence of the milling angle is clearly dis-cernible with Al films. While the sample processed with a milling angle of 6° is free from visible defects (see Fig. 1), the sam-ple prepared with 16° shows a high defect density (Fig. 2).

Fig. 1: TEM image of an Al film that has been ion milled with a milling angle of 6°

Fig. 2: TEM image of an Al film that has been ion milled with a milling angle of 16° with clearly visible defect structures (dislocation network)

TEM images of a Ti film that has been ion milled with a milling angle of 6°

3LNT Application Note - METAL FILMS AND SHEETS

Page 4: Application Note EM... · Metal sheets are thicker than 100 µm. Mechanical pre-preparation is necessary to obtain an acceptable initial thickness and a good surface quality for ion

PURPOSEMetal sheets are thicker than 100 µm. Mechanical pre-preparation is necessary to obtain an acceptable initial thickness and a good surface quality for ion milling. A ultrasonic cutter can be used to get a 3 mm disc. It is also possible to use the core drill of the Leica EM TXP.

PREPARATION CONDITIONSMechanical pre-preparationTXP core drill to get a 3mm disc.TXP for double sided polishing down to a final thickness of 50 µm Diamond foils: 6 µm, 3 µm, 1 µm and 0.5 µm at 2000 rpm.

Ion milling1. Step:Acceleration voltage: 7kVCurrent: 2.6 mAMilling angle: ±6°Sample movement: RotationMilling time: 4h

2. Step:Acceleration voltage: 2kVCurrent: 1.5 mAMilling angle: ±6°Sample movement: Rotation

RESULTSClean and large electron transparent areaSome grains show lattice damages which may be due to the rolling process during manufacture.

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TEM images of ion milled V2A steel sheet

5LNT Application Note - METAL FILMS AND SHEETS

Page 6: Application Note EM... · Metal sheets are thicker than 100 µm. Mechanical pre-preparation is necessary to obtain an acceptable initial thickness and a good surface quality for ion

The statement by Ernst Leitz in 1907, “With the User, For the User,” describes the fruitful collaboration with end users and driving force of innovation at Leica Microsystems. We have developed five brand values to live up to this tradition: Pioneering, High-end Quality, Team Spirit, Dedication to Science, and Continuous Improvement. For us, living up to these values means: Living up to Life.

LIFE SCIENCE DIVISION - NANO TECHNOLOGY LNTThe Leica Microsystems Nano Technology Division’s focus is to provide the most compehensive product portfolio for the preparation of biological, medical and industrial samples for investigation in the Electron and Light Microscope. Excellent Sample Preparation is a prerequisite for perfect microscopy. Your image starts here!

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Leica EM RES102 Application Note Metal films and sheets ∙ 09/2014 ∙ Copyright © by

Leica Mikrosysteme GmbH, Vienna, Austria, 2014. Subject to modifications. LEICA and the

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