Zeiss Argon Ion Beam System User manual

Instruction Manual
Carl Zeiss Microscopy - Electron and Ion Beam Microscopy
Argon Ion Beam System
Optional additional FIB column
for NVision 40
Enabling the Nano-Age World®

Argon Ion Beam System
Optional additional FIB column for NVision 40
Original instructions
Carl Zeiss Microscopy GmbH
Carl-Zeiss-Promenade 10
07745 Jena, Germany
[email protected]
www.zeiss.com/microscopy
Carl Zeiss Microscopy GmbH
Carl-Zeiss-Straße 22
73447 Oberkochen, Germany
Document name: Instruction Manual Argon Ion Beam System
Revision: en02
Effective from: June 2012
© by Carl Zeiss Microscopy GmbH
346000-8070-000
This document or any part of it must not be translated, reproduced or transmitted in any form or by any means, electronic or
mechanical, including photocopying, recording, or by any information or retrieval system. Violations will be prosecuted.
The use of general descriptive names, registered names, trademarks, etc. in this document does not imply, even in the
absence of a specic statement, that such names are exempt from the relevant protective laws and regulations and therefore
free for general use.
Software programs will fully remain the property of Carl Zeiss Microscopy. No program, documentation or subsequent
upgrade thereof may be disclosed to any third party, unless prior written consent of Carl Zeiss Microscopy has been procured
to do so, nor may they be copied or otherwise duplicated, even for the customer’s internal needs apart from a single back-
up copy for safety purposes. Due to an ongoing process of improvement Carl Zeiss Microscopy reserves the right to make
modications of this document without notice.

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Table of contents
1. About this manual ........................................................................................ 5
1.1. Definition of terms ........................................................................................... 7
2. Safety summary ........................................................................................... 8
2.1. Intended use ..................................................................................................... 8
2.2. Prevention of accidents and of improper use ............................................... 8
3. Description ................................................................................................... 9
3.1. Overview ........................................................................................................... 9
3.1.1. Argon FIB modes .................................................................................................... 9
3.2. Principle of operation .................................................................................... 10
3.2.1. Fine-polishing ........................................................................................................ 11
3.3. Technical data ................................................................................................ 12
3.4. Customer service ........................................................................................... 13
4. Installation .................................................................................................. 13
5. Operation .................................................................................................... 14
5.1. Getting started ................................................................................................ 14
5.1.1. Switching on the argon beam ................................................................................ 14
5.1.2. Adjusting the coincidence point ............................................................................. 16
5.2. Adjusting operational parameters ................................................................ 18
5.2.1. Setting the acceleration voltage ............................................................................ 18
5.2.2. Checking the argon gas flow ................................................................................. 19
5.2.3. Checking the argon discharge ............................................................................... 20
5.3. Fine polishing of TEM lamellas ..................................................................... 21
5.4. Switching off the argon beam ....................................................................... 26
6. Maintenance and repair ............................................................................. 27
6.1. Change of consumables and chemicals ...................................................... 27
6.1.1. Replacing the argon supply ................................................................................... 27
6.2. Repair .............................................................................................................. 27
6.3. Troubleshooting ............................................................................................. 28
7. De-installation and disposal ..................................................................... 28
8. Abbreviations ............................................................................................. 29
9. Declaration of conformity .......................................................................... 30
10. Index .......................................................................................................... 31

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1. About this manual
This instruction manual is considered to be part of the Argon Ion Beam System.
Read the instructions carefully. Keep the instruction manual nearby the Argon Ion Beam System
and hand it over to future owners of the instrument.
This instruction manual is designed for users who have been trained by an authorised
Carl Zeiss expert to operate the workstation, the Argon Ion Beam System=is built in.
Operators of the must not deviate from the instructions provided in this document.
IMPORTANT
It is assumed that the operator is already familiar with general functions of SmartSEM®
and the operation of the CrossBeam®workstation.
Reference to
related
documents
For detailed information regarding the CrossBeam®workstation refer to the Instruction Manual of
the workstation.
For detailed information regarding the operating software refer to the Software Manual
SmartSEM®NV.
Safety
instructions The safety instructions in this manual are classified as follows:
DANGER
This safety symbol and signal word indicates an imminently hazardous situation.
Disregarding this warning WILL result in death or serious injury.
WARNING
This safety symbol and signal word indicates a potentially hazardous situation.
Disregarding this warning COULD result in death or serious injury.
CAUTION
This safety symbol and signal word indicates a potentially hazardous situation.
Disregarding this warning MAY result in minor or moderate injury.
CAUTION
This signal word used without a safety symbol indicates a potentially hazardous situation.
Disregarding this warning MAY result in property damage.

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Moreover you will find the following type of information:
IMPORTANT
This symbol and signal word draws your attention to important and useful
information.
Typographical
conventions For the description of software, the following typographical conventions are used:
Typography Meaning
Push <ENTER>. Push the ENTER key on the keyboard.
Type <key1, key2> Type key 1 first, then type key 2 on the keyboard.
Type <Ctrl + Alt + Del>. Simultaneously type CTRL key, ALT key and DEL
key on the keyboard.
Click on the High voltage icon.
Select Aperture size from the drop-down list.
Icons, buttons and menus are printed in bold.
Select Aperture size 30 µm.
Set FIB Fil V Target to zero.
Values to be selected are printed in italics.
Text Meaning
Click... Press the left mouse button.
Right-click... Press the right mouse button.
Double-click.... Press the left mouse button twice.

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1.1. Definition of terms
The following terms are used in this manual:
This instruction manuals relates to the operating software SmartSEM®V05.04.
Argon Ion Beam System Focused ion beam system used for fine polishing of TEM lamellas.
Triple Beam System Combination of FIB/SEM and Argon Ion Beam System
SmartSEM®Operating software for Carl Zeiss field emission scanning electron
microscopes
Operator A trained person, who is assigned to operate the workstation.
Basic operator:
Person who has been trained to perform fundamental operation
sequences
Specially trained operator:
Electrically skilled person who has been trained to perform basic main-
tenance tasks
User A person or organisation that uses products of Carl Zeiss.
Carl Zeiss service
engineer,
Carl Zeiss service staff
Specially trained service expert, either Carl Zeiss staff or
authorised service partner of Carl Zeiss.
FIB Focused ion beam
GEMINI®column Electron optical column
Coincidence point Point where electron beam and ion beam are crossed.

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2. Safety summary
2.1. Intended use
The Argon Ion Beam System is an optional additional ion beam column to the Carl Zeiss
CrossBeam®model NVision 40. With this column, the NVision becomes a triple beam system.
The Argon Ion Beam System allows you to scan a focused beam of argon ions across the
specimen in order to remove material from the specimen surface.
The main use of the Argon Ion Beam System is to remove implanted gallium and amorphous
layers from TEM lamellas by fine polishing with low kV argon ions.
2.2. Prevention of accidents and of improper use
CAUTION
Risk of injury or damage due to improper operation of the option.
Read the user documentation carefully.
Do not operate the option until you have completely read and understood this instruction
manual and the entire user documentation delivered with the workstation. You will find the
user documentation in the document folder.
CAUTION
Risk of property damage due to improper maintenance, service, or repair.
The warranty might be voided.
Follow the instructions given in this instruction manual.
IMPORTANT
All pursuing tasks of maintenance, service, and repair not described in this instruction
manual have to be performed by authorised Carl Zeiss service staff only.

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3. Description
3.1. Overview
Fig. 1.1: Triple Beam System
3.1.1. Argon FIB modes
With the Argon Ion Beam System installed, new imaging modes become available in the
drop-down selection of the FIB toolbar.
•FIB mode Argon
Shows the live image of the argon beam in
scan or spot mode. Electron beam and
focused ion beam are blanked.
•FIB mode Argon + SEM
While working with the argon beam in scan or
spot mode, this mode allows you to monitor
the progress in the live SEM image.
The focused ion beam is blanked.
1FIBcolumn 3GEMINI
®column (SEM)
2 Argon Ion Beam System
3
1
2

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3.2. Principle of operation
In the Triple Beam System, FIB, SEM and Argon Ion Beam System are arranged in a way that
they
intersect at the same point in the specimen chamber. This point is called coincidence point.
Therefore, all Argon Ion Beam System operations can be monitored in high resolution SEM live
imaging.
The Argon Ion Beam System generates argon ions from argon gas. When passing the column,
the condenser aperture and the lens form a microscopic ion beam.
FIB
Ar+
SEM

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3.2.1. Fine-polishing
FIB milling While milling a flow of ions (1) released from the
FIB column (3) hit the surface of the
TEM lamella (2).
Implantation
and
amorphisation
The gallium ion milling causes gallium implanted
and, on crystalline samples, amorphous surface
layers that deteriorate the quality of the TEM
lamella.
Removing
damage layers These damage layers and the implanted gallium
ions (6) can be minimized by fine-polishing with
low-energy argon ions (5) from the Argon Ion
Beam System (4).
This improves the quality of the TEM lamella.
The visibility of fine details improves.
1
3
2
4
5
6

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3.3. Technical data
Environmental requirements
Pollution degree 2
Installation category II
Electrical supplies
Nominal AC voltage AC 100 V 5 A ( 0.5 kVA) ±10%
Nominal frequency 50-60 Hz single phase
Power consumption -
Ground 100 Ohm or less
Specifications
Ion source Gaseous Argon
Lenses Two stage electrostatic lens
Beam deflector Quadrupole electrostatic type
Acceleration voltage 0.5 - 1.0 kV
Maximum beam
current >10 nA
Beam energy 0.5 - 1.0 keV
Beam diameter/ spot size 50 - 150 µm, typically 100 µm at 1 kV, 10 nA
Max. beam shift ± 1.5 mm (at WD 29 mm)
Max. scan range > 3.0 mm (at WD 29 mm)
Ion irradiation angle 0 - 30 °
In situ lift-out The Argon Ion Beam System is compatible with the in-situ lift-out technique
Control
SmartSEM®V05.04 or higher Fully integrated in the SmartSEM®software. The Argon Ion Beam
System is operated via the graphical user interface of SmartSEM®.

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3.4. Customer service
For customer service, contact your local Carl Zeiss service engineer.
A list of Carl Zeiss locations and authorised service partners can be found at:
http://www.zeiss.com/microscopy
4. Installation
The Argon Ion Beam System is either factory-installed or retrofitted by authorised Carl Zeiss serv-
ice staff.

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5. Operation
It is assumed that the operator is already familiar with general functions of SmartSEM®and the
operation of the workstation.
IMPORTANT
Note the instruction manual of your workstation.
For general information about SmartSEM®refer to Software Manual SmartSEM®and
Software Manual SmartSEM®NV.
5.1. Getting started
5.1.1. Switching on the argon beam
1 Select Tools/Goto Panel...
2 Select Argon Gun from the menu.
The Argon Gun panel opens.
3 Click on Standby.
IMPORTANT
When the Argon Ion Beam System powers on, it automatically tests if the gun can achieve
a discharge current greater than 50 mA. This can take up to one minute.

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The Argon Ion Beam System switches to
STANDBY mode.
4 Click on Beam On.
The Argon Ion Beam System switches to
BEAM ON mode.
5 To be able to see the live argon image, select
FIB Mode Argon from the FIB mode
selection.
SmartSEM®switches to the live argon image.
IMPORTANT
The Argon Ion Beam System has the ability to obtain images, but its resolution is not
comparable to SEM imaging. The imaging function is mainly used to align the argon beam
correctly.

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5.1.2. Adjusting the coincidence point
Check daily, if the Argon Ion Beam System is still within the coincidence point of SEM and FIB.
The coincidence point is where all three beams of the Triple Beam System cross.
Preconditions:
•Eucentricity has been adjusted as described in the software manual SmartSEM®NV.
•Coincidence point of FIB and SEM has been adjusted as described in the workstation manual
SmartSEM®NV
Procedure:
1 Load a Faraday cup.
2 Focus on a detail in SEM.
3 To be able to see the live argon image, select
FIB Mode Argon from the FIB mode
selection.
4 Check that the same detail is centered in the
argon image.

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If this detail is not centered in the argon image:
a Go to the Argon Gun panel.
b To center the detail, use the
Argon Beam Shift.
Now, the coincidence point is adjusted.

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5.2. Adjusting operational parameters
The following operational parameters of the Argon Ion Beam System can be adjusted to optimize
milling results.
IMPORTANT
After changing parameters, always adjust the coincidence point as described in
section 5.1.2.
5.2.1. Setting the acceleration voltage
The lower the acceleration voltage, the gentler the polishing process will be, but the milling rate
will also be decreased.
1 To regulate the duration and intensity of the
milling process, adjust the acceleration
voltage with the slider (1).
2 The argon condenser voltage has to be set
according to the acceleration voltage.
Adjust the argon condenser voltage with the
slider (2):
-1200 V at 1000 V acceleration voltage
-1040 V at 750 V acceleration voltage
-900 V at 500 V acceleration voltage
1
2

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5.2.2. Checking the argon gas flow
1 Check that Argon Gas Flow is set to
1.5 - 3.0 %.(Usually 2.0 - 2.3 % is optimal).
The beam current decreases at higher or lower
gas flow.
2 Check that the beam current is high enough:
a Set Argon Energy to 1000 V with the
slider.
b Load a Faraday cup.
c Use the specimen current monitor to
measure the beam current.
It should be at 10 nA.
If the beam current is lower:
d Adjust the argon gas flow with the slider.
IMPORTANT
If the gas flow is set too low or too high, the argon ion beam does not switch on.

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5.2.3. Checking the argon discharge
1 Check, that Argon Discharge is set to
-1000 V (1).
2 Check, that 130 µA are displayed under
Argon Discharge I is (2).
If the value is lower:
a Reduce Argon Gas Flow in 0.1 % steps.
1
2