Leica EM ACE600 User manual

From Eye to Insight
OPERATING MANUAL
EM ACE600
167202032 Version 01/19

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 con-
tinuously 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, photocopy-
ing, 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 ACE600
Operating Manual
Leica EM ACE600 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 instruction manual carefully
before operating the instrument.
For Research use only!

Operating Manual Leica EM ACE600 Version 01/19 Page 1
Foreword
Please read this instruction manual carefully before operating the instrument. This
user manual is intended to provide essential information about the Leica EM
ACE600 coating system. It includes important information regarding correct
operation, servicing, and troubleshooting. Following these instructions will help
prevent hazards, reduce repair and downtime costs, and prolong the system's life.
The Leica EM ACE600 coater system can be handled safely
and easily when operated in accordance to the instructions in
this manual. Ignoring safety instructions may endanger the
user(s) and the system itself.
Users must familiarize themselves with the system before operation. Special
attention must be paid to comply with the safety requirements. The Leica EM
ACE600 must not be used beyond the limits specified in the provided technical
data sheet.
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 subjected to vacuum and/or coating procedures.
Warranty claims will only be considered if the instrument is used according to the
guidelines specified in this user manual.
In addition, all generally applicable legal and otherwise binding regulations for
accident and environmental protection must be observed and communicated.
Leica reserves the right to change technical specifications as well as
manufacturing processes without prior notice. Only in this way, Leica can
continuously improve the technology and manufacturing techniques used to
provide its 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) as well
as handing over to third parties requires approval of Leica Mikrosysteme GmbH.

Operating Manual Leica EM ACE600 Version 01/19 Page 2
Table of Contents
1.Introduction ..................................................................................................................... 4
1.1Identification .................................................................................................................. 6
1.1.1Product ................................................................................................................................ 6
1.1.2Name and address of the manufacturer .............................................................................. 6
2.Product description ........................................................................................................ 7
2.1Field of application and proper use ............................................................................... 7
2.2Dimensions and weight ................................................................................................. 8
2.3Environmental conditions for operation and storage .................................................... 8
2.4Safety information ......................................................................................................... 9
2.4.1General instructions ............................................................................................................. 9
2.4.2Safety measures at the installation site ............................................................................. 10
2.4.3Qualification of operating personnel .................................................................................. 10
2.4.4Residual hazards ............................................................................................................... 10
2.4.5Safety measures when working with nitrogen ................................................................... 11
2.4.6Emergency procedure ....................................................................................................... 15
3.Installation and set up .................................................................................................. 15
3.1.Warranty ..................................................................................................................... 1 5 
3.2. Instrument overview .................................................................................................... 16
3.3.Delivery of the instrument ........................................................................................... 17
3.4.Installation requirements for the instrument ................................................................ 17
3.5.Unpacking and connection ......................................................................................... 18
3.6Inserting chamber shielding ........................................................................................ 22
3.7Shutter installation ...................................................................................................... 26
3.8.Quartz crystal measurement installation ..................................................................... 28
3.8.1Eccentric quartz holder ...................................................................................................... 30
3.9.Stage installation ........................................................................................................ 32
3.9.1Rotating stage .................................................................................................................... 35
4.Operating instructions .................................................................................................. 37
4.1General functions ........................................................................................................ 38
4.1.2Software update................................................................................................................. 42
4.2Pump and Vent ........................................................................................................... 44
4.3Vacuum test ................................................................................................................ 45
4.4Process start and stop ................................................................................................ 45
4.5Thickness monitoring and geometrical correction (QSG) ........................................... 45
4.6Carbon thread coating ................................................................................................ 46
4.6.1Loading a carbon thread .................................................................................................... 47
4.6.2Choosing a carbon thread protocol ................................................................................... 51

Operating Manual Leica EM ACE600 Version 01/19 Page 3
4.6.3Carbon thread materials .................................................................................................... 53
4.7Sputter coating ............................................................................................................ 54
4.7.1Loading the sputter target .................................................................................................. 55
4.7.2Choosing a sputtering protocol .......................................................................................... 57
4.7.3Parameters for sputter coating .......................................................................................... 60
4.7.4 Sputter materials............................................................................................................... 60
4.8E-beam coating ........................................................................................................... 61
4.8.1Loading an e-beam evaporation source ............................................................................ 63
4.8.2Choosing an e-beam protocol ........................................................................................... 80
4.8.3Parameter suggestion e-beam coating ............................................................................. 82
4.8.4E-beam material ................................................................................................................ 83
4.9.Carbon rod coating ..................................................................................................... 84
4.9.1Loading a carbon rod ......................................................................................................... 85
4.9.2Choosing a carbon rod protocol ........................................................................................ 91
4.9.3 Carbon rod materials ......................................................................................................... 94
4.10Glow discharge ........................................................................................................... 95
4.10.1Choosing a glow discharge protocol.................................................................................. 95
4.11.Sequence ............................................................................................................. 98
4.12Rotating stage: difference in user interface and set-up ............................................ 102
4.13 Running a process ............................................................................................. 103
4.14 Load lock ............................................................................................................ 106
5.Maintenance and service ............................................................................................ 110
5.1General instructions for maintenance and cleaning .................................................. 110
5.1.1Source cover .................................................................................................................... 111
5.2Cleaning of the Leica EM ACE600 ........................................................................... 111
5.2.1Removing and cleaining the door with a metal polisher .................................................. 115
5.2.2Removing shutter and internal shielding ......................................................................... 116
5.2.3Exchanging the glass shielding for the chamber light ..................................................... 116
6.Troubleshooting .......................................................................................................... 117

Operating Manual Leica EM ACE600 Version 01/19 Page 4
1. Introduction
In order to ensure the safety of operators and service technicians, and to prevent
any damage to the Leica EM ACE600, it is essential to read this manual carefully
before beginning to work with the system.
This user manual is intended to provide the user a complete understanding of the
system (including its specified limits and capabilitites), as well as to maintain and
service it in accordance with its physical parameters.
This user manual includes important information regarding proper and economical
installation, operation, servicing, troubleshooting and repair. Following these
instructions will help prevent hazards, reduce repair and downtime costs, and
prolong the system's service life.
In this user manual, symbols are used to alert the user about important
information, such as necessary safety precautions, activites relating the operation
and/or maintenance of the system, and relevant process-oriented descriptions or
remarks.
Symbols used in this manual and their meaning:
Danger!
Instructions regarding possible hazards are identified with this
symbol. Ignoring 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 that may
endanger staff or result in damage to the system if it is ignored.
Lifting hazard. Single person lift could cause injury.
Use assistance when moving or lifting the coater.

Operating Manual Leica EM ACE600 Version 01/19 Page 5
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.
Wear clean, powder-free gloves.
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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.

Operating Manual Leica EM ACE600 Version 01/19 Page 6
Warning! Improper use of the instrument can cause
serious harm. Read the manual before operating the
system.
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.
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1.1 Identification
1.1.1 Product
Leica EM ACE600 High Vacuum Coater
1.1.2 Name and address of the manufacturer
Leica Mikrosysteme GmbH
Hernalser Hauptstraße 219
A-1170 Vienna
Tel.: [phone]
Fax: [phone]
Internet: www.leica-microsystems.com

Operating Manual Leica EM ACE600 Version 01/19 Page 7
2. Product description
2.1 Field of application and proper use
The Leica EM ACE600 coating system is used for precise coating of samples for
subsequent examination with an electron microscope (EM). Up to two angled
sources can be configured. Automated stage rotation is integrated for best
distribution. Integrated quartz crystal measurement accurately determines the
layer thickness Automated height and tilt adjustment is optional, otherwise tilt and
height are set manually. The optional glow discharge makes grids hydrophilic. A
planetary drive stage for even distribution of coating material is available.
The samples are metal coated using the sputtering method where argon plasma
erodes a target material or e-beam evaporation. Carbon coating is achieved by
carbon thread, carbon rod or e-beam evaporation. Any sample can be processed
as long as it is not sensitive to vacuum, argon plasma or the heat generated
during carbon coating.
The Leica EM ACE600 coater can be configured with up to two (some limitations)
of the following processes: sputtering, carbon thread evaporation, carbon rod
evaporation, e-beam evaporation.
The removable shielding, shutter, source and door are designed to enable easy
and comprehensive cleaning of the system.
The vacuum system creates an ultimate vacuum ≤ 2x10-6 mbar. Pressure is
monitored by a combined thermal and cold cathode vacuum gauge.
Main components:
The Leica EM ACE600 coating system includes the following main functional
units, depending on the configuration:
 Vacuum Chamber
 Touch screen control panel (see 4.)
 Rotating sample stage, 24 positions for 12,7mm SEM stubs (exchangeable,
see 3.9)
 Removable shielding, shutter and door (see 3.6, 3.7)
 Housing
 Quartz (QSG) thickness measurement (3.8)
 Carbon thread source or sputter source or e-beam source or carbon rod
source (see 4.6 – 4.9)
Optional:
 Planetary drive stage (see 3.9)
 Automated or manual height and tilt adjustment (see 3.9)
 Sample stage for two 76 mm x 26 mm (3” x 1”) glass slide, sample stage for
low angle rotary shadowing and clamping grids (60mm diameter)
(exchangeable, see 3.9)
 VCT Stage with four positions
 Glow discharge (see 3.7)

Operating Manual Leica EM ACE600 Version 01/19 Page 8
2.2 Dimensions and weight
Basic unit: app. 65 kg
Instrument packed app. 74 kg
Note: e-beam instruments are about 20 mm more in depth and 5 kg heavier.
Dimensions for the Leica EM ACE600 with a VCT500 are in the technical data
sheet and the manual for cryo outfits.
2.3 Environmental conditions for operation and storage
Indoor use, altitude up to 2000 m
Power supply 100/115/230 V
Humidity 80% RH (no condensation)
Temperature range > 15° C < 30° C
Pollution degree (IEC 61010-1) 2

Operating Manual Leica EM ACE600 Version 01/19 Page 9
2.4 Safety information
2.4.1 General instructions
Covers protect all electronic components: door lock (1), source cover (2), and
housing (3). The door and source covers are equipped with sensors that cut off
power supply when opened. Only authorized Leica representatives are allowed to
remove the housing. Additionally, there are software switches, which cut off power
when a malfunction is noticed.
The coating sources are protected against overheating. If at any time, the source
temperature reaches 65° C, the system automatically pauses the current process
only to continue after the temperature has sank below 45° C.
In case of a sudden and unexpected vacuum break, the instrument switches off
automatically to protect the pump and electric parts.
All electrical parts are safely separated from the user by the front cover and back
housing.
If the Leica EM ACE600 coating system is damaged or malfunctions, all use of the
system should be suspended until the issue has been corrected.
All modifications and conversions to the system are prohibited and invalidate the
warranty.
3
2
1

Operating Manual Leica EM ACE600 Version 01/19 Page 10
2.4.2 Safety measures at the installation site
The following measures must be implemented to prevent incorrect use:
 A technically qualified person must carry out connecting to electricity and
gas.
 Gas bottles must be secured and stand upright when connected. A
technically qualified person must connect the system to the gas supply.
 Repairs may only be made by Leica authorized service staff or authorized
representatives.
 If the Leica EM ACE600 coating system is installed incorrectly, the system
may be damaged and may incur injury to the user
Maintenance and Service may only be conducted by technicians authorised
only by the manufacturer's service department.
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Leica EM ACE600 coating system should not be operated unless all safety
regulations, technical requirements and conditions are fulfilled.
2.4.3 Qualification of operating personnel
The operating personnel must be familiar with and follow the recognized rules for
safety at work.
The operating personnel responsible for operating and maintaining the Leica EM
ACE600 coating system must satisfy the specific professional requirements for
their respective duties.
The operating personnel must have received training and must be familiar with the
duties that have been assigned to them and for which they are responsible.
2.4.4 Residual hazards
The Leica EM ICE ACE600 coating system represents the latest technology and
conforms to recognized safety regulations: even so, hazards still exist.
All modifications and conversions to the system are prohibited!
Only accessories which meet the manufacturer’s specifications shall be used.
Electrical socket acts as disconnecting device. Make sure an easy access to the
disconnecting device is granted.
Install or update software only with data media supplied by Leica
Microsystems.
The Leica EM ACE600 must not be used to process any hazardous materials,
such as radioactive, highly corrosive, explosive, toxic or human pathogenic
substances. The machine must not be used for medical or in-vitro-
diagnostic applications unless specifically certified for this purpose by the
local authorities.

Operating Manual Leica EM ACE600 Version 01/19 Page 11
2.4.5 Safety measures when working with nitrogen
The volume of the LN2 Dewar is 25 l. When working with liquid nitrogen (LN2)
please bear in mind LN2 is extremely cold. It boils at -196 °C. Nitrogen gas (GN2)
escapes at very low temperature from the boiling LN2. Both LN2 and GN2 as 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 LN2 evaporates, it expands in a ratio of 1:700. 1 liter LN2 produces 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.
Removing LN2 waste: dump LN2 into an outdoor pit or container filled with gravel,
where it will evaporate rapidly and safely.
GN2 is odorless and tasteless and will be inhaled like air. GN2 is non-toxic, but a
high GN2 content 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 analyzer (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 LN2 Dewars in a closed storage room or
chamber. The evaporation rate from Dewar vessels can rise to several liters 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 LN2 evaporates. However, once the object has cooled down there may
occur unexpected strong boiling and spurting of LN2.
In the case of burns from LN2 splashes, 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
liters 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 LN2 in a
glass Dewar.

Operating Manual Leica EM ACE600 Version 01/19 Page 12
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
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 LN2cannot 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 cryopreparation
metal troughs (1 cm Styrofoam insulation), Styrofoam containers or plastic troughs
are eminently suitable and ensure low risk cryopreparation.

Operating Manual Leica EM ACE600 Version 01/19 Page 13
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 liter of LN2 per day.
Defective Dewar vessels with higher evaporation rates are a safety risk, and
should be taken out of work or repaired.
Do not leave LN2 standing 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 air will be taken up in exchange for nitrogen. LN2 with high liquid oxygen
content has a faintly bluish color. Concentrated liquid oxygen promotes vigorous
burning!
Make sure that your Dewar vessel is filled only with LN2. Apply a note in the
central distribution place stating clearly
ONLY LIQUID NITROGEN
or similar if different liquefied gases are delivered from there. Check the color of
cryogen: Bluish color indicates the presence of a high percentage of liquid oxygen.
The concentration of liquid oxygen increases during long periods of storage as its
boiling point (-183 °C) is higher than the boiling point (-196 °C) of LN2.
Main supply must be assured: 100 – 240 VAC, 50 / 60 Hz
The instruments are equipped with protected ground. Before connecting it to the
local electrical supply make sure that the mains has the required ground and that
the instrument is connected to it according to the local regulations.
Unplug the instrument before installing or changing fuses.

Operating Manual Leica EM ACE600 Version 01/19 Page 14
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HAZARD WARNING
LIQUID NITROGEN, LN2
Suffocation
- Any vessel containing LN2 is a potential hazard
- One litre LN2 produces 700 litres N2 gas
- N2 gas is odourless and tasteless
- Oxygen levels can quickly drop in confined spaces due to displacement of
oxygen
- by N2 when using or dispensing large volumes of LN2
- This can cause immediate fainting and unconsciousness
- Always use LN2 in well-ventilated areas
- Treat it with respect!
Storage
- For reasons mentioned above do not store full LN2 Dewars in confined
spaces
Burns
- LN2 boils at -196 °C. It is extremely cold and can cause serious burns. Please
read the safety instructions provided with all Leica products for the correct
handling of liquid nitrogen!

Operating Manual Leica EM ACE600 Version 01/19 Page 15
2.4.6 Emergency procedure
Caution
If unusual operating conditions or unaccustomed noises occur, the system
must be switched off using the mains switch on the rear of the system.
If firefighting measures are called for, a CO2fire extinguisher must be used.
Technical Service must be consulted before resuming work with the system.
Note
For maintenance and servicing the system must be switched off!
Caution
There is a danger of electric shock when the housing is removed.
Injuries may be sustained that could lead to death.
The Leica EM ACE600 coating 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.
Caution!
There is danger from the edges of the metal sheet of the internal
shielding and shutter.
Personal injury (e.g. cuts) may occur.
3. Installation and set up
3.1. Warranty
The Leica EM ACE600 is covered by a WARRANTY according to the conditions
of sale. If functional errors should occur or if the components of the system
sustain damage that is subject to warranty coverage during the warranty period,
the manufacturer will repair or replace the faulty components following
examination thereof.
The manufacturer’s warranty covers the system in its original configuration.
Only original replacement parts may be used. The manufacturer accepts no
liability for damage caused by use of other replacement parts.
The manufacturer will not accept liability for damage caused by misuse of the
system or its use for purposes other than the intended use, nor for damage
caused by work on the system that is not described in this manual.