Leica EM TIC 3X User manual

From Eye to Insight
OPERATING MANUAL
EM TIC 3X
167190032 Version 07/17

Important Note
Leica Mikrosysteme GmbH reserves the right to change technical specications as
well as manufacturing processes without prior notice. Only in this way is it possible to
continuously improve the technology and manufacturing techniques used to provide our
customers with excellent products.
Any copyrights of this document are retained by Leica Mikrosysteme GmbH,
Vienna. Any reproduction of text and illustrations (or any parts thereof) by printing,
photocopying, or other methods (including electronic systems and media) requires
express prior permission in writing.
Issued by:
Leica Mikrosysteme GmbH
Hernalser Hauptstrasse 219
A-1170 Vienna

Leica EM TIC 3X
Operating Manual
Leica EM TIC 3X Serial Number:
Date of purchase:
For the instrument serial number, please refer to the name type label on the
back of the instrument!
Please read this operating manual carefully
before operating the instrument.
For Research use only!

Page 1 Leica EM TIC 3X Operating Manual 07/17
Foreword
This operating manual is intended to provide essential information about the proper
operation and servicing of the Leica EM TIC 3X Triple Ion Beam Cutter system. The
appendix helps with specific processing of solid samples for subsequent investigation
with an electron microscope (EM) or light microscope (LM).
This operating manual describes commissioning of the Leica EM TIC 3X Triple Ion
Beam Cutter system, phased testing and adjustment of all components and
movement sequences, and restoring the basic functionality.
Service and operating staff must familiarize themselves with all components of the
system before commissioning. Particular attention must be paid to the aspect of
safety.
This operating manual must be retained for future reference.
Texts, schedules and tables may not be copied, reproduced, or divulged to third
parties without our express consent.
It should be noted that this operating manual does not constitute a part of any
existing, prior agreement or covenant or legal relationship.
All obligations are derived from the purchase agreement, which is also the sole
document of record regarding the terms of the warranty. Contractual provisions are
not affected by the operating manual.
The documentation issued by the respective suppliers shall apply in addition to this
manufacturer's documentation (see attachment).
In addition, all generally applicable legal and otherwise binding regulations for
preventing accidents and protecting the environment must be observed and
communicated.

Page 2 Leica EM TIC 3X Operating Manual 07/17
Table of contents
1.Introduction..............................................................................................................................5
1.1 Identification..........................................................................................................................8
1.1.1 Product..............................................................................................................................8
1.1.2 Name and address of the manufacturer............................................................................8
2.Product description................................................................................................................. 9
2.1 Field of application and proper use.......................................................................................9
2.2 Instrument overview............................................................................................................10
2.3 Dimensions and weight.......................................................................................................11
2.4 Electrical and gas requirements..........................................................................................11
2.5 Energy consumption, energy conditions.............................................................................11
2.6 Sound emissions.................................................................................................................11
2.7 IP code of the electrical devices .........................................................................................11
2.8 Environmental conditions and limits for operation and storage ..........................................11
2.9 Safety information...............................................................................................................12
2.9.1 General instructions.........................................................................................................12
2.9.2 Design safety measures..................................................................................................12
2.9.3 Safety measures at the installation site...........................................................................13
2.9.4 Safety measures before use............................................................................................13
2.9.5 Qualification of operating personnel................................................................................13
2.9.6 Residual hazards.............................................................................................................14
2.9.7 Emergency procedure .....................................................................................................14
2.9.8 Liquid Nitrogen (LN2) used for the cooling stage (optional).............................................14
3.Installation and set up...........................................................................................................18
3.1 Transportation and storage conditions................................................................................18
3.2 Installation requirements.....................................................................................................18
3.2.1 Working area conditions..................................................................................................18
3.2.2 Connections requirements............................................................................................... 18
3.3 Installing, assembling and commissioning..........................................................................19
3.3.1 Unpacking and installing on a table.................................................................................19
3.3.2 Installing the Leica EM TIC 3X on Leica instrument table...............................................23
3.3.3 Installing the arm rests of the Leica instrument table ......................................................24
3.3.4 Clamping device (Argon bottle, LN2pump) of the instrument table.................................26
3.3.5 Assembling the stereo microscope S9E..........................................................................27
3.3.6 Assembling the stereo microscope M80 (with 0.8x objective).........................................30
3.3.7 Assembling the stereo microscope M80 (highest magnification) ....................................36

Page 3 Leica EM TIC 3X Operating Manual 07/17
3.3.8 Assembling the movable lens adapter for M80 objectives ..............................................42
3.3.9 Safe storage of the packing material...............................................................................43
3.3.10 Electrical and gas connections........................................................................................43
3.3.11 Initial operation................................................................................................................44
3.4 Repacking to prevent damage during transportation..........................................................44
3.5 Storage location for the instructions....................................................................................44
4.Operating instructions.......................................................................................................... 45
4.1 Introduction.........................................................................................................................45
4.2 Main components of the Leica EM TIC 3X Triple Ion Beam Cutter....................................45
4.3 Functional description.........................................................................................................45
4.3.1 Chamber..........................................................................................................................45
4.3.2 Vacuum system...............................................................................................................46
4.3.3 Standard sample stage (optional)....................................................................................46
4.3.4 Multiple sample stage (optional)......................................................................................48
4.3.5 Cooling stage (optional)...................................................................................................49
4.3.6 Rotary Stage (optional)....................................................................................................51
4.3.7 Leica EM VCT500 docking port (optional).......................................................................52
4.3.8 Triple Ion source..............................................................................................................53
4.3.9 Gas supply control...........................................................................................................54
4.3.10 LCD touch control panel..................................................................................................54
4.3.11 Stereo microscopes.........................................................................................................55
4.4 Principle operating and display functions............................................................................56
4.4.1 Exchanging the stages (when different stages are ordered)...........................................56
4.4.2 User Interface..................................................................................................................62
4.4.2.1 Setting the parameters.....................................................................................................63
4.4.2.2 Status information and programming..............................................................................64
4.4.2.3 Guns status ......................................................................................................................68
4.4.2.4 Illumination.....................................................................................................................69
4.4.2.5 Command line, Start/Pump/Vent ....................................................................................70
4.4.2.6 Menu................................................................................................................................71
5.Maintenance and service...................................................................................................... 74
5.1 General...............................................................................................................................74
5.2 Safety measures during maintenance and service.............................................................74
5.3General instructions for maintenance and cleaning............................................................74
5.4 Daily maintenance activities before beginning work...........................................................75
5.5 Daily maintenance activities after ending work...................................................................75
5.6 Components requiring maintenance...................................................................................75

Page 4 Leica EM TIC 3X Operating Manual 07/17
5.6.1 View port..........................................................................................................................75
5.6.2 Triple ion source..............................................................................................................80
5.6.2.1 Assembly..........................................................................................................................80
5.6.2.2 Function...........................................................................................................................81
5.6.2.3 Ion Source Lifetime vs. Replacement Cycle...................................................................81
5.6.2.4 Replacement of Ion source..............................................................................................82
5.6.2.5 Maintenance of the ion source ........................................................................................83
5.6.2.6 Dismantling the ion source..............................................................................................84
5.6.2.7 Disassembling and assembling the triple ion source.......................................................86
5.6.2.8 Exchange of the complete ion source..............................................................................88
5.6.2.9 Cleaning the ion source components...............................................................................90
5.6.2.10 Instability of the ion source with a high life time and low kV setting............................95
5.6.3 Exchanging fuses ............................................................................................................95
5.7 Cleaning the Leica EM TIC 3X............................................................................................96
5.8 Maintenance schedule (summary)...................................................................................... 96
6.Troubleshooting .................................................................................................................... 97
6.1 Error messages...................................................................................................................97
6.2 Malfunction..........................................................................................................................97
7.Servicing and repair by Customer Service .........................................................................98
Appendix:
EC Declaration of Conformity

Page 5 Leica EM TIC 3X Operating Manual 07/17
1. Introduction
In order to ensure the safety of service technicians and operators, and to prevent any
damage to the Leica EM TIC 3X Triple Ion Beam Cutter system, it is essential to read
this manual carefully before beginning any work with the system.
This operating manual is intended to help the user to understand the system more
completely, to use it within the specified limits of its working capabilities, and to
maintain and service it in accordance with its physical parameters.
This operating manual includes important information regarding proper and
economical installation, operation, servicing, troubleshooting and repair. Following
these instructions will help to prevent hazards, reduce repair and downtime costs,
and prolong the system's service life.
In certain chapters, a certain symbol refers to the function or respective section of
text and is relevant for the operation or maintenance of the system, or indicates
important descriptions or additional remarks:
Symbols in this manual and their meaning:
Danger!
All paragraphs in the operating manual that contain instructions regarding
possible hazards are identified with this symbol. Failure to observe these alerts
may result in serious injury! Users of the instrument must comply with
instructions at all times.
Caution!
This symbol alerts the user to important information which may endanger staff
or result in damage to the system if it is ignored.
Note!
This symbol indicates further information relating to a previous explanation,
which does not have a safety-critical function. However, it is important to
follow this information to ensure that the system functions optimally.
This symbol indicates the necessary work processes for scheduled and
unscheduled maintenance with consideration of the safety equipment. Another
symbol indicates the qualification that is required in order to carry out such
work.
Wear work gloves!

Page 6 Leica EM TIC 3X Operating Manual 07/17
Symbols and indications on the instrument and their meaning:
The plug is equipped with a locking
mechanism. Please do not pull on the cable!
Grasp the knurled part of the plug and retract
for disconnecting the cable.
Hazardous Voltage! Enclosed Voltage or
current hazard is sufficient to cause shock,
burn or death. Disconnect and lockout power
before servicing.
Danger of pinching the fingers when closing
the flange (stage).
Hot surface during and right after processing
the sample. Allow to cool before servicing the
ion source.
LN2is used to cool down the sample. To avoid
serious burns or frostbite, follow safety
information before disconnecting fluid lines.
Lifting hazard. The volume of the LN2Dewar is
25 l. Single person lift could cause injury. Use
assistance when moving or lifting the Dewar.

Page 7 Leica EM TIC 3X Operating Manual 07/17
This Dewar contains LN2, follow safety
procedures when handling with liquid
nitrogen.
Warning! Improper use of the instrument can
cause serious harm. Read the manual before
operating the system.
LN2connection for the LN2tube from the LN2
pump in case the system is equipped with the
cooling device.
Connection for ring LED or coaxial LED
illumination.
Port to connect a <= 16GB USB memory stick
for data up and download.
This product has been tested to the
requirements of CAN/CSA C22.2 No. 61010-1,
second edition, including Amendment 1, or a
later version of the same standard
incorporating the same level of testing
requirements.
LN2
(left side of the instrument)

Page 8 Leica EM TIC 3X Operating Manual 07/17
1.1 Identification
1.1.1 Product
Leica EM TIC 3X Triple Ion Beam Cutter system
1.1.2 Name and address of the manufacturer
Leica Mikrosysteme GmbH
Hernalser Hauptstrasse 219
A-1170 Vienna
Tel.: [phone]
Fax: [phone]
Internet: http:// www.leica-microsystems.com

Page 9 Leica EM TIC 3X Operating Manual 07/17
2. Product description
2.1 Field of application and proper use
The Leica EM TIC 3X Triple Ion Beam Cutter system is used for precise processing
of samples for subsequent examination with an electron microscope (EM) or light
microscope (LM). For this purpose, a cross-section or ion beam polished surface of a
sample is created with the Leica EM TIC 3X Triple Ion Beam Cutter system.
The samples are processed with ion beams in a vacuum. The system generates ions
in the energy range from 1 keV to 10 keV.
A variety of sample preparation equipment (stages) can be used to adapt the Leica
EM TIC 3X to the application needs (e.g. cryo stage). Hence, almost any material can
be processed, e.g. semiconductors, metals, rocks, ceramics, polymers, rubber,
paper, environment sensitive and even biological material.
Please refer to separate operating manuals of stages you ordered!
The ion energy causes the temperature of the sample to increase during processing.
The operator must ensure that this does not cause the sample's state of aggregation
to change. If so, using the cooling stage is recommended.
The Leica EM TIC 3X must not be used beyond the limits specified in its technical
data sheet.
An inert gas, preferably argon, is used as the working gas. If other gases are used for
reactive processing of samples, the appropriate safety measures (purging, removal of
exhaust air) must be put in place, not only for the working gas, but also for the
reaction by products created during processing. To make sure the system will be
suitable for other gases than argon please contact the Leica representative prior to
use.
When hazardous substances (e.g., radioactive, toxic or explosive substances) are
processed the substance-specific safety precautions must be implemented. It is
forbidden to process substances that release corrosive or poisonous gases when
they are cut with an ion beam. When hazardous substances have been processed
the system (chamber) must be decontaminated before servicing the instrument.
Applications other than those described are inconsistent with proper use and are
therefore prohibited. If the system is used incorrectly, all claims under warranty will
be not accepted.
In cases of doubt, please consult your local Leica representative.

Page 10 Leica EM TIC 3X Operating Manual 07/17
2.2 Instrument overview
1. Stereo Microscope
2. Drawer unit to load the
sample in the vacuum
chamber
3. Touch sensitive control
panel
4. Instrument table
5. LN2pump (optional)
6. LN2Dewar (optional)
7. Microscope support column
8. LED illumination
9. Access to E-W traverse
knob. Opposite side is sample
Z-movement
10. USB port
1
1
2
3
4
5
6
7
8
9
10

Page 11 Leica EM TIC 3X Operating Manual 07/17
2.3 Dimensions and weight
Dimensions of the system with without light microscope and sound suppressor:
Width: 500 mm
Height: 485 mm
Depth: 738 mm
Weight: approx. 62 kg
Dimensions of the shipping container:
Width: 650 mm
Height: 820 mm
Depth: 950 mm
The weight of the transport-ready system is about 90 kg.
Volume of LN2Dewar: 25 l
2.4 Electrical and gas requirements
Voltage: 100 –230 VAC, 50/60 Hz
Mains supply fluctuations: ± 15% of the nominal voltage
Fuses: 4 AT
Working gas: preferably 99.999 % (Ar 5.0)
Gas flow: <1 sccm/ion source with automatic control
2.5 Energy consumption, energy conditions
Power consumption:
Maximum: 300 W
2.6 Sound emissions
The continuous sound level emitted by the Leica EM TIC 3X Triple Ion Beam Cutter
system is about 50 dB (A).
2.7 IP code of the electrical devices
The electrical devices are equipped with housings and covers, and are therefore
designed to provide degree of protection IP 20 (contact protection: blocking finger
access; protection from foreign bodies: protected from foreign bodies > d = 12 mm,
no special water protection).
2.8 Environmental conditions and limits for operation and storage
Operating temperature: +15 °C to +30 °C
Storage temperature: +5 °C to +40 °C
Atmospheric humidity for operation and storage: max. 80 % RH; non-condensing
Protection from dust and aggressive media must be provided during operation and
storage.

Page 12 Leica EM TIC 3X Operating Manual 07/17
2.9 Safety information
2.9.1 General instructions
Danger!
The Leica EM TIC 3X Triple Ion Beam Cutter system can be handled safely and
easily provided it is operated in accordance with the instructions in this
manual.
Non-observance of these safety instructions may endanger people and the
system.
2.9.2 Design safety measures
All electronic components are protected by covers (doors, panels, etc.). These covers
must not be opened except for servicing by authorized Leica representative.
Caution!
There is a danger of electric shock when the cover is removed.
Injuries may be sustained that could lead to death.
The Leica EM TIC 3X Triple Ion Beam Cutter system must not be operated
unless all covers are properly in place.
Caution!
Some of the components inside the system may become hot and present a
danger of injury.
Burns may be sustained.
The Leica EM TIC 3X Triple Ion Beam Cutter system must not be operated
unless all covers are properly in place.
Caution!
When working with liquid nitrogen (LN2) please bear in mind LN2is extremely
cold. It boils at -196 °C. Nitrogen gas (GN2) escapes at very low temperature
from the boiling LN2. Both LN2and GN2as well as cooled elements (e.g. pipes,
valves, hoses, containers or stoppers) can cause severe frost bite and burns to
the skin and eyes.
Please pay particular attention to the safety information about the use of LN2!

Page 13 Leica EM TIC 3X Operating Manual 07/17
2.9.3 Safety measures at the installation site
The following measures must be implemented to prevent incorrect use at the
installation site:
•The electrical and gas connections for the system must be carried out by
qualified technicians.
•Gas bottles must be stood up securely and connected professionally. The
system must be connected to the operator's mains supply by qualified
technicians.
•The system must not be operated except by trained and authorized personal.
•Repairs may only be made by authorized staff of Leica representatives.
•If the Leica EM TIC 3X Triple Ion Beam Cutter system is installed incorrectly,
the system may be damaged.
2.9.4 Safety measures before use
The Leica EM TIC 3X Triple Ion Beam Cutter system must be installed by authorized
staff of Leica representatives.
Note!
The system should be switched off for maintenance and servicing only, not at
the end of a work session.
The system must be installed correctly before it is commissioned by the technical
service. The supply of power and gas must be assured according requirements
described at point 3.
2.9.5 Qualification of operating personnel
The operating personnel must be familiar with and follow the recognized provisions
for safety at work.
The operating personnel must be trained and familiar with the duties that have been
assigned to them and for which they are responsible.
The professional profiles for operating personnel responsible for the system are
outlined in the following.

Page 14 Leica EM TIC 3X Operating Manual 07/17
Operator
Personnel with technical training, able to perform simple tasks, i.e., operate the Leica
EM TIC 3X Triple Ion Beam Cutter system and load / unload samples.
Administrator
Staff with technical training, able to perform the tasks of qualification 2, and also
typical simple maintenance, adjustment and start-up activities with protective devices
switched off as well as restarting the system.
Manufacturer's service technician
Trained technician provided by the Leica representative, who is able to carry out
more complex work in exceptional situations or in cases where such has been
agreed with the user.
2.9.6 Residual hazards
The Leica EM TIC 3X Triple Ion Beam Cutter system represents the latest technology
and conforms to recognized safety regulations: even so, hazards still exist.
If the Leica EM TIC 3X Triple Ion Beam Cutter system is damaged or malfunctioning,
all use of the system should be suspended until the malfunction or damage has been
corrected.
All modifications and conversions to the system are prohibited and leads to exclusion
of guarantee!
2.9.7 Emergency procedure
If unusual operating conditions or unaccustomed noises occur, the system must be
switched off using the main switch on the system if necessary.
If firefighting measures are called for, a CO2fire extinguisher must be used.
The Technical Service must be consulted before resuming work with the system.
2.9.8 Liquid Nitrogen (LN2) used for the cooling stage (optional)
The volume of the LN2Dewar is 25 l. When working with liquid nitrogen (LN2) please
bear in mind LN2is extremely cold. It boils at -196 °C. Nitrogen gas (GN2) escapes at
very low temperature from the boiling LN2. Both LN2and GN2as well as cooled
elements (e.g. pipes, valves, hoses, containers or stoppers) can cause severe frost
bite and burns to the skin and eyes.
When LN2evaporates, it expands in a ratio of 1:700. 1 litre LN2produces almost 1 m3
of GN2. Care should therefore be taken to ensure that when large quantities of
nitrogen evaporate (e.g. when transferring LN2), the room should always be well
ventilated.

Page 15 Leica EM TIC 3X Operating Manual 07/17
Removing LN2waste: dump LN2into an outdoor pit or container filled with gravel,
where it will evaporate rapidly and safely.
GN2is odourless and tasteless and will be inhaled like air. GN2is non-toxic, but a
high GN2content in the air (> 78%) reduces the oxygen-content (< 21%) and
produces immediate fainting and deep unconsciousness without any previous
symptoms.
When there is doubt about the adequacy of ventilation, use an oxygen analyser (0 to
25% scale) to check for oxygen. The content of oxygen must not drop below 18%.
If an unconscious person stays in a low oxygen environment then death may occur.
If breathing stops, apply artificial respiration at once and notify doctor and ambulance
immediately!
For the reasons given above, never put LN2Dewars in a closed storage room or
chamber. The evaporation rate from Dewar vessels can rise to several litres a day if
they are defective due to improper handling or to natural wear over many years of
use.
Always keep the working area well ventilated.
Bring objects at room temperature carefully into contact with LN2. Initially an
insulating gas layer is formed preventing a large transfer of heat. During this initial
period little LN2evaporates. However, once the object has cooled down there may
occur unexpected strong boiling and spurting of LN2.
In the case of burns from LN2splashes, rinse the affected skin immediately with
plenty of water at hand temperature. For serious burns arrange for a skin specialist to
see them at once.
In the case of LN2 affecting the eyes, rinse immediately with water at hand
temperature and arrange for an eye specialist to see it at once.
Never use glass Dewar vessels in the lab (especially glass Dewars larger than 2
litres capacity) without complete metal envelope: Glass Dewars often burst for no
obvious reason or due to unintentional mishandling (e.g. contact with metal
instruments etc.). Never work without open protective glasses when using LN2in a
glass Dewar.
Estimation of lethal GN2 –concentration in closed rooms.
Full-load values (10 kV, 3.5 mA, -150 °C), room temperature ~25 °C
Size of the room [m3]
10
21
31
42
52
62
73
83
94
104
Time to achieve critical
concentration [h]
1
2
3
4
5
6
7
8
9
10

Page 16 Leica EM TIC 3X Operating Manual 07/17
Fig.1.1: When working with LN2for refilling the Dewar avoid protective glasses
(a), boots (c), walking shoes (e) and protective gloves (g) out of which the LN2
cannot easily escape if entered. LN2splashing into the closed protective
glasses (a), open boots (c), shoes (e) or protective gloves (g) evaporates
suddenly and can cause serious burns.
Always use protective glasses (b) with side protection which are open at the
top and at the bottom. Only use boots if you have loose (not narrow) trousers
coming outside the boots (d) and completely covering the gap. Wear only open
slip-on sandals (f) in the lab, no walking shoes or court shoes. Always wear
cuffless trousers if you wear slip-on sandals. Never wear protective gloves
when pouring LN2or when putting the Dewar head on the Dewar vessel. Just
use an open flannel cloth (h) to protect your hands from the cold. Gloves
should be used only to grasp dry cold parts. They are unsuitable for LN2work.
Only use metal Dewars specifically designated for storage of LN2, since only
containers of this kind exclude risks during storage. For routine cryo-preparation
metal troughs (1 cm Styrofoam insulation), Styrofoam containers or plastic troughs
are eminently suitable and ensure low risk cryo-preparation.
Check the evaporation rate of your metal Dewar regularly every three months and
compare these rates with the rate given by the manufacturer. The evaporation rate of
an undamaged metal Dewar should be well below 1 litre of LN2per day. Defective
Dewar vessels with higher evaporation rates are a safety risk, and should be taken
out of work or repaired.
Do not leave LN2standing in open vessels where it can exchange with the room
atmosphere. The boiling point of LN2(-196 °C) is lower than liquid oxygen’s boiling
point (-183 °C). When the exchange surfaces are extensive enough, oxygen from the