TEM sample prep CAMM

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Fischione 1010

E.A. Fischione’s Model 1010®Ion Mill® is a state-of-the-art compact, tabletop precision ion milling / polishing system that consistently produces high quality TEM specimens with large electron transparent areas. Unlike electro-polishing, ion milling is equally effective for materials having low (semiconductors and insulators) or high (metals and semimetals) electrical conductivity. It uses an impinging incident HAD (Hollow Anode Discharge) ion to sputter ions from the surface of a sample. The sputtering can be only due to momentum transfer between the incident ion and the sample surface (in case of inert gases like Ar or Ar+) or enhanced by chemical reaction (in case of reactive gases).

Features

The 1010®Ion Mill® is fully programmable with two independently adjustable HAD ion sources having a 0-30º milling angle, which permit either rapid milling or more gradual material polishing. Under an automatic gas control the specimen can be rocked or rotated with an optional liquid nitrogen cooled stage and optional automatic termination. The choice of single or dual ion source operation allows milling from either one or both sides of the specimen. The HAD ion sources operate over user selectable ranges of extractor voltage (0.5kV to 6.0 kV) and current (3mA to 8mA), and are capable of producing ion beam currents up to 400 mamps. Typically varying voltage changes the average ion energy while varying current alters the ion flux. With increase in either of them the milling rate would increase.

The summary of specifications of 1010®Ion Mill®

Ion Source Type

Hollow Anode Design

Ion source settings range

Voltage: 0.5 – 6 kV, Current: 3-8 mA

Specimen motion

Full rotation (360º) or oscillation (0-+/- 179º)

Milling rate

Varies with material

Gas requirements

Argon equal to or greater than 99.998% and supplied at a pressure of 10psi (69 Mpa)

Microscope capability

200-2000X monocular microscope fitted with a CCD camera and color monitor

Turbo-molecular vacuum pump

70 lps (min). With no gas flow, ultimate chamber vacuum is 1 X 10-6 torr. Under normal milling conditions, the system vacuum is between 1 X 10-4 and 2 X 10-5 torr.

The basic procedure of sample preparation and ion milling are:

  1. Mechanically section (cleave, saw) the sample
  2. Ultrasonically cut discs (3mm dia by < 500mm thick)
  3. Rough grind (3mm dia by < 70mm thick)
  4. Dimple grind (3mm dia by 10mm thick)
  5. Ion mill the top and bottom surfaces until they are electron transparent (3mm dia by <100nm thick)
  6. Plasma clean.

Sputtering of specimen due to Ion Milling

Hollow Anode Discharge (HAD) Ion Source

 

Fischione Nanomill (1040)

NanomillTM is a newly developed state-of-the-art low energy ion mill, which is installed in late 2006. In this system, a focused low energy (50-2000V) Argon beam (10-12mm beam size) is rastered on the region of interest at relatively low angles (0-15). The milling occurs at the moderate ion milling rates (0.2-0.3nm/min for Si at 900V and 15o) with a current density of ~1mm/mm2. The main purpose of using low energy focused Argon beam is to remove any kind of surface artifact on TEM samples such as amorphous surface damage layer caused by FIB in a reasonable time period without sacrificing any thin area. In order to achieve this, a scanned argon beam at a proper milling voltage, milling angle and milling rate is applied.  Using a focused Argon beam also avoids the problems that arise due to the geometry of the specimen, so the Argon ion beam can easily reach to the surface of the specimen without any discrepancy. This approach prevents the possible cross contamination caused by the surrounding materials such as the support Cu grid. During the milling process in the NanomillTM, the focused Ar ion beam is used for ion milling and at the same time for imaging and selection of the region of interest.

Features

Source: Focused Argon ion beam
Beam size: 10-12mm
Ion image: max 1000X
Sputtering rate: 0.3nm/min (900V Si at 30o)

Ion energy: 50 - 2000V
Incidence angle: 0o - +30o/-10o

 

Struers Tenupol Electropolisher (Cryo Temp)

The TenuPol-5 is an automatic, micro-processor controlled apparatus for electrolytical thinning of specimens for examination in a transmission electron microscope.  It includes a scanning function for easy determination of parameters and additional enhancement functions parameters so that new materials can be easily established.  Both 2.3 and 3mm diameter specimens are polished from both sides simultaneously to achieve a thin foil with a center hole as small as possible.  The thinning is controlled by an infrared light source, which stops the polishing as soon as the first light passes through. `

Specifications

Control unit
  • Mains voltage: Single-phase, 100-120/220-240V, 50-60 Hz.
  • Power consumption: 220-240V / 1.50A
  • 110-120V / 3.15A
  • Output: 0-100V / 0-2A
Polishing unit
  • Sizes of original 12-21mm dia., max. 1mm thick
  • specimen: 3mm dia., max. 0.5mm thick
  • 2.3mm dia., max. 0.5mm thick
Specifications
  • TenuPol-5 control unit, with electronic thermometer and adapter for the connection of (TENPO) TENFI
  • TenuPol polishing unit, with specimen holder for 3 mm dia. Specimens (TETRI), sets of jets (TETOR), pump, cooling coil, insulated PVC container, non-insulated PVC-container and built-in photo cell TENPO
  • Connection print for data transfer between TenuPol-5 and a PC LECPC
  • Specimen holder for 3mm dia. specimens TETRI
  • Specimen holder for 2.3mm dia. specimens TETTO
  • Specimen holder, 10mm diaphragm for pre-thinning TETMA
  • Set of jets, 1mm bore TETOR
  • Set of jets, 2.5mm bore for use with (TETMA) TETET
  • Tape Kit for electrolytic “punching” TENKI