Fischione 1010 ION MILL Manuale utente
MODEL 1010 ION MILL
Standard Magnification Version
INSTRUCTION MANUAL
E.A. Fischione Instruments, Inc.
9003 Corporate Circle
Export, PA 15632 USA
Phone (724)325-5444
FAX (724)325-5443
www.fischione.com
PN 009-0988 Rev.3
Contents
Model 1010 Ion Mill – Standard Magnification Version
Contents
SAFETY 1
BACKGROUND 2
Ion Milling Theory 2
Model 1010 Features 2
Ion Sources 3
Basic Procedure for Sample Preparation and Ion Milling 3
SYSTEM OVERVIEW 4
Sample Chamber 5
Vacuum System 6
Gas Flow 7
Water Flow 7
Sample Cooling Capability (Optional) 7
Endpoint Detection Capability (Optional) 7
Visual Monitoring 8
Control System and Software 8
Specifications 8
INSTALLATION AND SETUP 9
Warnings, Cautions, and Notes 9
Assessing initial condition 9
Unpacking and Inspecting 9
Accessories 10
Connections 11
Process gas 11
Exhaust gas 12
Water 12
Microscope Installation 12
Process Control Computer 13
Laser Installation (optional) 14
Power Connections 14
For US application 14
For non-US application 14
To change operating voltage 15
OPERATION 16
Basic Startup Procedure 16
Dewar Bakeout 17
Laser Calibration 18
Loading TEM Specimens 19
Specimen Cooling (optional) 20
Ion Milling 21
Insert specimen 22
Microscope 22
Endpoint determination (optional) 22
Set milling parameters 22
Set data logging options 24
Save recipe 24
Start milling 25
View Data 27
Basic Shutdown Procedure 29
MAINTENANCE 30
Contents
Model 1010 Ion Mill – Standard Magnification Version
Preventive Maintenance Schedule 30
Cleaning the Air Filters 30
Changing the Fuses 31
Opening the Enclosure 32
Enclosure removal 32
Window Cleaning 33
Front access door window 33
Bottom light window 34
Cleaning o-rings 36
Lamp Replacement 36
Ion Source Maintenance 38
Disconnect gas line 39
Remove ion source cartridge 39
Remove cathode 41
Remove anode and extractor 41
Inspect components 42
Clean components 43
Service ion source body components 43
Ultrasonically clean and inspect components 45
Reassemble ion sources 45
Verify electrical connections 45
Replace ion source 46
Attach gas and electrical connections 46
Check leaks 46
Start up ion source 47
Ion Source Alignment 47
Adjust source alignment 47
Verify alignment 48
Dewar Maintenance 48
Remove Dewar 48
Change Zeolite® desiccant 51
Install Dewar 52
Evacuate Dewar wall space 52
Chamber and Specimen Stage Cleaning 52
Stage maintenance 52
Ion source flange 56
Pirani gauge tube 58
Bottom plate 59
Mass Flow Controllers 60
Verify electronics 60
Evaluate flow 61
Replace mass flow controller 61
Leak Detection 62
High pressure 62
Vacuum 63
Turbomolecular Vacuum Pump 64
Reinstall Enclosure 64
Back Panel 64
TROUBLESHOOTING 65
Diagnosis chart 65
Error messages 67
Laser 68
SPARE PARTS AND CONSUMABLES 69
REFERENCES 71
Contents
Model 1010 Ion Mill – Standard Magnification Version
Safety
1 Model 1010 Ion Mill
Standard Magnification Version
Safety
The following hazards are associated with the Model 1010 Ion Mill.
ELECTRICAL HAZARD. High voltages can cause severe injury or death. Do not
connect the power cord until after the initial inspection and after making gas connections.
Do not attempt to operate the instrument with the cover removed.
Before disconnecting the power cord from the instrument, wait one minute to ensure that
any charged electronic component will discharge.
HAZARDOUS MATERIALS. Toxic, reactive, or radioactive materials can cause
severe injury or death. If hazardous materials will be inserted into the Model 1010 for
processing, the ion mill must be connected directly to an exhaust system capable of
accommodating the hazardous material. If radioactive materials will be milled, the
instrument must be enclosed in protective shielding.
LASER HAZARD. Laser beams can cause severe eye damage. Do not point the laser
beam into your eye or into any other person’s eye. The ion mill contains a 670 nm red
(visible) Class II laser.
COMPRESSED GAS. High-pressure gas stream can injure exposed skin or eyes. Point
tubing away from personnel while connecting or disconnecting gas cylinders.
MECHANICAL HAZARD. Moving parts can injure fingers and hands. Do not attempt
to operate the instrument with the cover open.
Background
2 Model 1010 Ion Mill
Standard Magnification Version
Background
For many of today's advanced materials, ion milling is an excellent preparation technique
for specimens that require TEM analysis. Electron microscopy needs samples that are
clean, representative of the bulk state, and free of physical or chemical artifacts. To
prepare them for microscopy, samples are first mechanically sectioned and ground and
then polished or milled to remove additional material.
Electropolishing requires that a sample material possess a certain level of electrical
conductivity.
Ion milling is effective for all materials, including those that are relatively nonconductive
such as semiconductors and insulators as well as those that are conductive (metallic or
semimetallic). Ion mills bombard the substrate surface with an energetic ion beam.
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.
Ion Milling Theory
Ion milling uses an impinging incident HAD (Hollow Anode Discharge) ion to remove
(“sputter”) ions from the surface of a sample.
If an inert gas (for example, Ar or Ar+) is used for milling, sputtering is the result of
momentum transfer between the incident ion and the sample surface. If a reactive gas is
used, sputtering is enhanced by chemical reactivity.
Model 1010 Features
The Model 1010 is fully programmable, with features including two independently
adjustable Hollow Anode Discharge (HAD) ion sources which permit either rapid milling
or more gradual specimen polishing, automatic gas control, an oil-free vacuum system, a
milling angle range of 0 to 45°, specimen rotation or rocking, an optional liquid nitrogen
cooled specimen stage and optional automatic termination.
Sam
p
le Material
θ= 0 to 90o
Ar +
Sputtered
Sample
Material
Background
3 Model 1010 Ion Mill
Standard Magnification Version
The choice of single or dual ion source operation allows milling from either one or both
sides of the specimen. When using the Model 1010, total ion milling time is typically less
than two hours depending on the specimen material and its initial thickness.
Ion Sources
The Hollow Anode Discharge (HAD) ion sources operate over user-selectable ranges of
extractor voltage (0.5 kV to 6.0 kV) and current (3 mA to 8 mA), and are capable of
producing ion beam currents up to 400 microamps. To a first approximation, varying
voltage varies the average ion energy, while varying current varies the ion flux. The
milling rate for a given material generally increases as either parameter is increased. They
are fabricated from a combination of aluminum, brass, ceramics, polymers, and stainless
steel.
Hollow Anode Discharge (HAD) ion source.
Basic Procedure for Sample Preparation and Ion Milling
1. Mechanically section (cleave, saw) the sample.
2. Ultrasonically cut disks (3 mm diameter by <500 µm thick).
3. Rough grind (3 mm diameter by <75 µm thick).
4. Dimple grind (3 mm diameter by <10 µm center thickness).
5. Ion mill the top and bottom surfaces until they are electron transparent (3 mm
diameter by <100 nm thick).
6. Plasma clean.
System Overview
4 Model 1010 Ion Mill
Standard Magnification Version
System Overview
Turbomolecular pump (TMP)
Ion source
Mass flow
controller (MFC)
LN2
Dewar
Dewar rod
Microscope
Sample chamber
Process control
computer
Front access door
System Overview
5 Model 1010 Ion Mill
Standard Magnification Version
Sample Chamber
The sample chamber is fabricated from a single block of aluminum. The ion sources are
connected to the chamber via mounting and alignment flanges. Radial o-ring seals ensure
the vacuum integrity between the ion sources and the chamber.
Bottom: A vacuum flange mounted on the chamber bottom contains:
●The Pirani gauge for sensing vacuum.
●The bottom lamp assembly for observing the specimen using transmitted light.
●The detector for milling termination.
Rear: The rear of the chamber includes:
●The specimen stage rotator assembly.
●A series of electrical connections.
System Overview
6 Model 1010 Ion Mill
Standard Magnification Version
●The specimen rotation drive motor.
●The angle adjustment drive motor.
●The vacuum pumping port for the liquid nitrogen Dewar flask.
●The optical pick-up and encoder, which provides the milling angle indication.
Top: The top chamber surface includes:
●The top light assembly
Front: The front of the chamber includes:
•The electro-mechanical leak valve
•The chamber access door
Vacuum System
The Model 1010 is equipped with a 70 lps (minimum) turbomolecular vacuum pump. A
fan creates a constant air flow across the turbo pump cooling vanes to minimize the heat
associated with maintaining a vacuum under gas flow conditions. The Model 1010 also
includes an external rough pump. This is a diaphragm pump that provides backing
vacuum for the turbomolecular pump.
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. Total pump down
time is typically less than four minutes, although this time may vary based on ambient
temperature and relative humidity as well as the length of time that the chamber front
access door was open exposing the chamber to ambient conditions. Pump down times are
also increased following ion source cleaning or chamber maintenance.
The turbomolecular pump is directly mounted to the chamber by two bolts. An inlet
protection screen prevents debris from entering the pump and damaging the turbine
blades.
An electro-mechanical vent valve is installed directly onto the chamber and all venting is
controlled through the computer. Vacuum is sensed by a Pirani gauge and is continuously
indicated in the Ion Milling Program screen. In order to improve ion source performance,
argon flows through the ion sources during the venting process.
The specimen chamber vents through the normally closed solenoid valve located on the
front of the chamber. When the vacuum system is de-energized, both the diaphragm and
the turbomolecular pumps are turned off and voltage is applied to the vent valve. The
vent valve slowly bleeds ambient air into the chamber over approximately 20 seconds to
minimize stress on the rotary turbine blades in the turbo pump.
When liquid nitrogen is being used, venting will not occur until the specimen stage
temperature reaches +10°C, to prevent contamination of the specimen.
If the main instrument power switch is turned off while the vacuum system is energized,
the vacuum will be maintained, keeping the chamber sealed and free from ambient
contamination.
Indice
