Linkam Scientific Instruments FDCS196 User manual

FDCS196 / THMS350V
Vacuum Stage
Linkam Scientific Instruments
USER GUIDE

2
Contents
Stages covered by this manual ............................................................................................ 3
Before Setting Up Your Equipment....................................................................................... 3
Important Notice ................................................................................................................ 4
Warranty............................................................................................................................ 4
Technical Support............................................................................................................... 4
Equipment Maintenance...................................................................................................... 4
Handling Liquid Nitrogen..................................................................................................... 4
Safety Precautions .............................................................................................................. 5
Symbol Reference......................................................................................................... 5
Introduction. ...................................................................................................................... 6
FDCS196 Stage Specification ......................................................................................... 6
FDCS196 System ................................................................................................................ 6
Stage Anatomy................................................................................................................... 7
Mounting Stage to Microscope with Dovetail Substage .......................................................... 8
Setting up the Condenser for Koehler Illumination .......................................................... 8
Vacuum Tweezers .............................................................................................................. 9
Connecting the Pirani Gauge ............................................................................................. 10
Flexible Stainless Steel Vacuum Tube Connection ............................................................... 11
FDCS196 Pro System Setup............................................................................................... 12
Vacuum Pump Setup................................................................................................... 12
MV196 Motorised Valve System Setup.......................................................................... 12
Mounting the MV196................................................................................................... 12
Sample Preparation and Loading ....................................................................................... 13
Sample Loading Using G16.3 Sample Holder................................................................. 13
Sample Loading Using FDCS196/CC Crucible Carrier and Quartz Crucible ....................... 16
Cooling Connections ......................................................................................................... 19
Filling the Liquid Nitrogen Dewar ................................................................................. 19
Appendix.......................................................................................................................... 20
Using The Stage with Gas Connectors................................................................................ 20
Installing Gas Connectors............................................................................................ 20
Window Assembly............................................................................................................. 21
Lid Window Assembly ................................................................................................. 21
Bottom Window Assembly ........................................................................................... 21
Troubleshooting ............................................................................................................... 22
Alternative Configuration: THMS350V ................................................................................ 23
THMS350V Stage Anatomy.......................................................................................... 24
Alternative Configuration: THMSEL350V............................................................................. 25
THMSEL350V Stage Anatomy ...................................................................................... 26
Using the Ellipsometer stage with vacuum port............................................................. 27
Ellipsometer windows assembly................................................................................... 28
Contact Details ................................................................................................................. 32

3
Stages covered by this manual
The following Linkam stages are covered in this manual:
FDCS196 Freeze drying cryo stage.
THMS350V High temperature vacuum stage
THMSEL350V High temperature vacuum stage with ellipsometry
Before Setting Up Your Equipment
Please register your products by going to the technical support section of our web site www.linkam.co.uk
You will need to register your equipment with us to:
 Activate your warranty and technical support
 Access the online setup videos
 Permanently unlock LINK software (if purchased)
If you have purchased LINK software, or want to try a demonstration of it, please install it first. You will
be guided through the LINK software registration process the first time that the software is used, and will
need the LINK software registration card to complete this.

4
Important Notice
Please check that your Linkam equipment has not been damaged during transit. If there is any evidence of
external damage DO NOT SWITCH ON ANY ELECTRICAL ITEMS.
Contact LINKAM SCIENTIFIC or their appointed distributor immediately. Your warranty may be
impaired if Linkam is not informed of any transport damage within 7 working days of delivery.
NO attempt should be made to repair or modify the equipment in any way, as there are no user replaceable
parts.
No attempt should be made to open the case except by qualified personnel as hazardous voltages are
present.
In order to use this equipment successfully, please take time to read this manual all the way through before
using it.
Warranty
This equipment has a warranty against defects in material and workmanship for a period of 12 months.
Linkam will either repair or replace products that prove to be defective. For warranty service or repair, this
product must be returned to Linkam or a designated service facility.
The warranty shall not apply to defects resulting from interfacing, unauthorized modification or misuse,
operation outside of the environmental specifications for the product, or improper site preparation or
maintenance.
Technical Support
Any technical questions or queries should be addressed to the Technical Support Department at the
address shown on the back of this manual.
Equipment Maintenance
Use a small quantity of isopropyl alcohol with a soft cloth and gently wipe the surface. To clean the
hotstage, use isopropyl alcohol (IPA) and cotton swabs. Take great care not to touch the platinum
temperature sensor protruding from the side of the heating element. The sensor is very fragile.
Handling Liquid Nitrogen
To cool samples below room temperature a LNP95 liquid nitrogen pump is required. Please refer to your
health and safety manual for instructions on how to handle liquid nitrogen safely. Always use in a well
ventilated room.

5
Safety Precautions
1) Read this guide before using the equipment. Save these instructions for later use.
2) Follow all warnings and instructions which may be placed on the stage.
3) Never use the equipment if any cables have been damaged. Do not allow any heavy objects to rest on
the cables. Never lay the cables on the floor.
4) Do not obstruct any ventilation holes. Do not attempt to insert anything into these openings. Provide
adequate ventilation of at least 75mm all around the equipment.
5) Do not expose the equipment to water. If for any reason it gets wet then unplug it from the mains and
contact Linkam Scientific Technical Support.
6) The equipment is not intended to be used outdoors.
7) If any problems occur then turn all Linkam equipment off and contact Linkam Scientific Technical
Support.
8) Do not remove any covers from the equipment, any servicing should be carried out by qualified
service personnel.
Symbol References
Caution:
This warning symbol indicates that the surface labelled with this symbol may be hot.

6
Introduction
Thank you for purchasing the FDCS196 Freeze
Drying Stage system. Please take the time to read
through the manual as it will help you to make the
most out of the equipment.
FDCS196 Stage Specifications
Objective Lens WD: 4.6mm
Condenser lens WD: 12.5mm
Objective light
approach angle: 115°
Maximum temperature: 125°C
Minimum temperature: -196 °C
Maximum heating rate: 150°C/min
Maximum cooling rate: 60°C/min
Maximum cooling Rate
under vacuum: 130°C/min
Maximum vacuum: 10-3mBar
XY-Manipulators travel: 16mm
Vacuum flange type: KF10 / KF10
Aperture hole: 1.3mm
Weight: 0.6Kg
FDCS196 System
The system consists of a FDCS196 stage, a T95-
LinkPad System Controller, LNP95 liquid nitro-
gen cooling pump system, Pirani vacuum gauge
and LINK software.
The FDCS196 Pro System has an additional 1.5L
Vacuum Pump and MV196 motorised vacuum
valve control System.
LINK System control software and digital video
capture can be added as an option to control from
PC.
The FDCS196 stage is mounted onto the
microscope by using specific stage clamps or an
adaptor plate.
This manual will describe instruction for setting
up a standard FDCS196 System.
FDCS196 System

7
Stage Anatomy
1. Lemo connector for Stage Connection Lead
2. Heating element carrier assembly
3. Platinum temperature sensor
4. 22mm Diameter heating block
5. Sample chamber
6. X-Sample manipulator
7. Door locking thumbscrew
8. Liquid nitrogen cooling connector
9. Heating element wire
10. Stainless steel cooling tube
11. Vacuum port
12. Sample holder ramp
13. Y-Sample manipulator
14. Stage lid
15. Lid insert
16. Quartz window (0.5mm thick)
17. Tube Clip Holder and tubing for Nitrogen
de-fogging stage window
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17

8
Mounting Stage to Microscope
with Dovetail Substage
The following description is for mounting the
stage on to microscopes which have a circular
dovetail substage assembly.
Attach the curved stage clamps (part no. 9542) to
the base of the stage using the supplied hex
screws and the outer most holes in the base plate.
Adjust the two positioning screws so that approxi-
mately 5mm of thread is exposed on the inside
edge of the clamp. This will roughly position the
stage in the centre of the dovetail.
Place the stage onto the dovetail then focus a 10X
objective lens on the aperture of the silver block.
Using the two positioning screws ensure that the
aperture is in the centre of the field of view.
For other types microscope’s substage, see the
included diagram for fitting instruction.
Setting up the Condenser for Koehler
Illumination.
Place a small sample on a cover slip and place
onto the surface of the silver block. Use the 10X
lens to focus on the sample. Now close down the
microscope field diaphragm and adjust the
condenser focus so that the edges of the
diaphragm are in focus. Now use the condenser
positioning screws to centre the condenser in your
field of view. Open the diaphragm so that it just
fills the field of view.
For more information about Koehler illumination
see the extremely informative ‘microscopy
Primer’ on the Molecular Expressions website.
http://micro.magnet.fsu.edu/primer/index.html
9542 curve clamps set
Dovetail substage

9
Vacuum Tweezers
The vacuum tweezers are used to manipulate the
glass sample slides onto the silver block to
prevent fingerprints on the glass and scratching
the surface of the silver block when using
standard fine tip metal tweezers.
The System is supplied with a Vacuum Tweezers
Kit which consists of a Vacuum Pump (1) and
tweezers (2).
Connect the tubing at the end of the tweezers to
the Regulator Valve (3) connection.
Use the dial on the valve to adjust the vacuum for
the tweezers.
Use a finger to block the hole of the tweezers to
pick up a sample cover slip with the suction cup.
Release the finger to drop the sample cover slip.
1
2
To vacuum pumpTo tweezers
3

10
Connecting the Pirani Gauge
The surfaces where the O-ring (1) sits should be
completely free of dirt. The O-rings should be
smeared with a small amount of vacuum grease
before loading in between the Pirani Gauge (2)
and the Stage Vacuum Connector (3).
Ensure that the O-ring is correctly seated in the
gauge and vacuum connector before tightening
the Clamping Bracket (4) screw (5).
Connect the Pirani Cable with the LAN type
connector (5) to the Pirani and the other end of
the cable to the back of the T95; Slot 4; labelled
‘VAC’, see page 9.
1
2
3
4
5
5

11
Flexible Stainless Steel Vacuum
Tube Connection
The surfaces where the O-ring (1) sits should be
completely free of dirt. The O-rings should be
smeared with a small amount of vacuum grease
before loading in between the Flexible Stainless
Steel Vacuum Tube (2) and the stage Vacuum
Connector (3).
Ensure that the O-ring is correctly seated in the
Steel Vacuum Tube and vacuum connector before
tightening the Clamping Bracket (4) screw (5).
Connect the other end of the Flexible Stainless
Steel Vacuum Tube to a Vacuum Pump.
Note: the FDCS196 is tested with a vacuum of
10-3mBar. Do not use a vacuum lower than this.
Vacuum Pump
123
4
5

12
FDCS196 Pro System Setup
Only read the following section if you have
purchased the FDCS196 Pro System.
Vacuum Pump Setup
Please refer to the Vacuum Pump manual to fill
the pump with oil and to install the mist filter (1).
MV196 Motorised Valve System
Setup
The MV196 Motorized Vacuum Control System
consists of a motorized valve (2) connected to a
T-piece (3) on top of the Vacuum Pump (4).
Please note that the motorized valve accurately
controls the vacuum within the stage but the
maximum vacuum possible is not as great as
when using a simple on/off style valve.
Mounting the MV196
The MV196 has an vacuum flange just like the
vacuum ports on the sides of the FDCS196 Stage.
Use a small amount of vacuum grease to coat a
thin layer on the surface where the O-ring will sit.
Coat the surfaces of the T-piece with vacuum
grease as well. The valve has two ports, there is
one in line and one protruding perpendicularly out
of the side of this valve. The side port (5) is for
the controlled vacuum vent and therefore should
not have anything attached to it.
Use the Clamping Bracket (6) to secure the
T-piece to the port as seen in the opposite picture.
Secure the vacuum pipe between the stage and
T-piece using the supplied O-rings and clamping
rings (6).
2
3
FDCS196
4
1
6
5

13
Sample Preparation
and Loading
The stage chamber must first be prepared for
vacuum. Ensure that the chamber is completely
clean and dry inside. Finger grease and dirt must
be cleaned off with IPA (isopropanol).
Sample Loading Using G16.3 Sample
Holder
A Freeze Drying Sample is prepared using a
G16.3 Sample Holder (1).
To load the G16.3 into the FDCS stage, open the
door of the stage by unscrewing the door
thumbscrew. The G16.3 slides into the brass
housing located just inside the door.
The Sample Holder Ramp (2) will guide the
G16.3 up on to the silver block.
Close the door and tighten the thumbscrew to seal
the stage.
Adjust the XY manipulators so the holder is in the
middle of the silver block
1
2

14
At standard atmospheric pressure the contact
between the sample and the silver block is enough
to establish good thermal contact as the air
molecules in any minute scratches will conduct
the heat, but when pulling a vacuum these are
drawn out of the stage. Objective immersion oil
(supplied) has the same refractive index as quartz
and ensures an almost perfect thermal seal
between block and crucible.
Using either the dropper or micropipette place a
tiny drop of oil on the silver block. Be careful not
to place the oil over the aperture hole of the silver
block.
Use the supplied Vacuum Tweezers or a pair of
tweezers place a clean 16 x 0.3mm Quartz Sample
Window directly on top of the oil inside the
G16.3 Sampler Holder.
Adjust the XY manipulators by a few turns in
both directions to spread out the oil underneath
the Quartz Sample Window evenly.
Using a pair of tweezers place a Shim Spacer (1)
in the middle of the Sample Holder.
1

15
Pipette 2μl of sample on the Quartz Sample Win-
dow inside the Shim Spacer.
Use the supplied Vacuum Tweezers or a pair of
tweezers place a clean W13G, (13 x 0.17mm)
Glass Sample Window on top of the sample,
ensuring it touches the Shim Spacer.
Use the XY manipulators to move the Sample
Holder so the edge of the sample sits across the
aperture hole of the silver block. This makes
visual location of the sample easier once analysis
starts.

16
Sample Loading Using FDCS/CC
Crucible Carrier and Quartz Crucible
This method is used if you are preparing the
sample away from the FDCS196 stage.
The crucible carrier has two spring clips to hold
the crucible flat against the silver block. This is to
ensure good thermal contact.
To load the quartz crucible into the carrier, lift the
two spring clips about 2mm upward and slide the
crucible in to the holder.
Release the two spring clips to hold the Crucible
in place.
Use a pair of tweezers to place a Shim Spacer
inside the Quartz Crucible.
1
2

17
Pipette 2μl of sample inside the Shim Spacer.
Use the supplied Vacuum Tweezers or a pair of
tweezers to place a clean W13G, (13 x 0.17mm)
Glass Sample Window on top of the sample,
ensure it touches the Shim Spacer.
Before loading the Crucible Carrier the silver
block must be prepared with silicon oil to provide
a good thermal contact between the crucible and
the silver block when the stage is under a vacuum.
Using either the dropper or micropipette place a
tiny drop of oil on the silver block. Be careful not
to place the oil over the aperture hole of the silver
block.

18
Load the Crucible Holder with the prepared
sample into the FDCS196 stage. Unscrew the Y
manipulator (the one screwed into the stage door)
so that when you close the door, the FDCS/CC
doesn’t push the crucible right off the edge of the
block and the silicon oil with it.
Open the door of the stage by unscrewing the
door thumbscrew. The FDCS/CC slides into the
brass housing located just inside the door. There
is a Sample Holder Ramp just before the silver
block which guides the crucible up on to the
block.
With one hand push the FDCS/CC and with the
other hand lift the edge of the crucible up the
ramp and over the drop of oil. When the drop of
oil is roughly in the centre of the crucible gently
lower the crucible on the block. Now close the
door of the stage and screw in the door locking
screw. This screw only needs to be finger tight.
Adjust the XY manipulators by a few turns in
both directions to spread out the oil underneath
the Quartz Crucible.
Use the XY manipulators to move the FDCS/CC
so the edge of the sample sits across the aperture
hole of the silver block. This makes visual
location of the sample easier once analysis starts.

19
Cooling Connections
These connections need only be made if the
experiments are to be carried out below room
temperature.
The Dewar Siphon (1) is the thick white foam
tubing and is attached to the liquid nitrogen Dew-
ar. The thin black capillary tube inside the white
foam tube must be inserted into the liquid nitro-
gen cooling connectors on the stage.
The white tubing slides on to the outside of the
connector. Twist the siphon whilst sliding it on
and push until it comes to a stop. It does not need
to go all the way to the base of the connector.
The thicker silicon tube from the LNP95 cooling
pump ends in a white PTFE connector (2), this is
pushed over the end of the other stainless steel
connector as seen in the image.
The smaller tube from the outlet on the LNP95
should be placed in position on the top of the lid
using the Tube Clip Holder (3). This tube blows
warm recycled nitrogen gas across the lid window
to prevent condensation on the viewing window
surface.
Filling the Liquid Nitrogen Dewar
Please follow your health and safety manual for
directions on how to handle liquid nitrogen and
ensure that you have the correct safety equipment
including gloves and safety goggles.
Fill the Dewar until approximately 2/3 full and
replace the lid with siphon attached.
DO NOT FASTEN THE CATCHES.
Wait for the nitrogen to stop bubbling before
fastening the catches.
Take care when placing lid on a table to always
have the black capillary pointing upwards. It is
easily damaged which will impair N2 flow.
3
12

20
Appendix
Using The Stage With Gas
Connectors
Installing Gas Connectors
This is used when vacuum is not needed.
To replace the vacuum port with a gas port con-
nector (1), use the hex key provided to remove the
two screws that hold the vacuum port in place.
Do the reverse to fit in the gas port connector and
make sure that the vacuum/gas seal (2) insert is
placed between the stage and connector.
The Gas Connector is self closing, it is open when
the Gas Insert is pushed into the Gas Connector.
To close the connector, the Gas Insert is removed.
To use the Gas Insert, connect one end to a tube
(3mm inner diameter, 6mm outer diameter) and
push the other end into the Gas Connector. You
should hear a “click” when the two parts are
connected properly.
To remove the Gas Insert, just push back the outer
sleeve of the Gas connector toward the base of the
FDCS196 Stage and the Gas Insert should drop
out.
Gas Connector
Gas Insert
2
1