Linkam Scientific Instruments TS1500 TS100 TS1000 High Temperature Stage USER GUIDE
Contents Before Setting Up your Equipment... 3 Important Notice... 4 Warranty... 4 Technical Support... 4 Equipment Maintenance... 4 Using Vacuum with the High Temperature Vacuum Stage... 4 Using the Vacuum Pump... 4 Safety Precautions... 5 Symbol Reference... 5 Introduction... 6 High Temperature Stage Specifications... 6 High Temperature Stage System... 6 Stage Anatomy... 7 Stage Assembly... 7 Lid Assembly... 7 Windows Assembly... 8 Lid Window Assembly... 8 Bottom Window Assembly... 8 Mounting Stage to Microscope with Dovetail Substage... 9 Setting up the Condenser for Koehler Illumination... 9 Pirani Gauge and Vacuum Port Connection... 10 ECP Water Circulator Pump Tubing Connection... 10 ECP Water Circulator Pump Tubing Connection for Ellipsometer Lid... 11 Sample Preparation for Ellipsometer Lid... 11 MV196 setup... 1 Vacuum Pump Setup... 1 MV196 Motorised Valve Setup... 1 Mounting the MV196... 1 Sample Preparation... 13 Using The High Temperature Stage... 14 Atmospheric Control... 14 Appendix... 15 High Temperature Stage with Options... 15 High Temperature Stage with Internal Electrical Contacts... 15 Using the Internal Electrical Contact... 15 Lemo Connector... 16 Blanking Plates... 17 Connecting the 991 Gas Purge Kit... 18 Contact Details... 4
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. 3
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 1 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. Using Vacuum with the High Temperature Vacuum Stage If the system is supplied with vacuum ports, read the following for safety. 1. WEAR APPROPRIATE SAFETY PROTECTION APPAREL such as gloves and eye protection.. DO NOT exceed the vacuum specification of 10-3 mbar. Using the Vacuum Pump 1. Read the included vacuum pump manual for more details.. Disconnect power before moving or servicing the vacuum pump. 3. Improper use or connections may cause ELECTRICAL SHOCK hazards. Be sure that all associated devices are properly grounded before switching them on. 4. Care must be exercised if touching the pump, as certain components may be hot. 5. The Exhaust Gas from the vacuum pump is composed of oil and gases entering the pump. The exhaust gas therefore should be well ventilated. Never operate the pump with locked or restricted outlet. 6. The vacuum pump supplied is not designed for pumping corrosive, aggressive or explosive gases, or for use in flammable or explosive environment. 4
Safety Precautions 1) Read this guide before using the equipment. Save these instructions for later use. ) 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: The user must not make or remove any connections while the equipment is powered on. To avoid electric shock do not remove the cover. Refer servicing to qualified service personnel. This warning symbol indicates that the surface labelled with this symbol may be hot. 5
Introduction Thank you for purchasing the High Temperature Stage System. Please take the time to read through the manual as it will help you to make the most out of the equipment. High Temperature Stage Specifications Temperature range. TS1500: ambient to 1500ºC TS100: ambient to 100ºC TS1000: ambient to 1000ºC Maximum sample: 10mg Maximum heating rate: 00 C/min Objective Lens WD: 6.0mm (7/3cup) 9.0mm (7/6cup) Condenser lens WD: 14.8mm (7/3cup) 1.6mm (7/6cup) Aperture hole: 1.7mm Weight: 0.5Kg High Temperature Stage with vacuum option. Maximum vacuum: 10-3 mbar High Temperature Stage with internal electrical contact option. Maximum voltage: 50V Maximum ampere: 0.A High Temperature Stage System The system is supplied with a T95 System Controller. An ECP water circulator pump is included and is used to keep the Lid and stage body cool. LINK System Control software and digital video capture can be added as an option to control from PC. The High Temperature Stage is mounted onto the microscope by using either specific stage clamps, an adaptor plate or by simply placing on the XY table of the microscope, using double sided adhesive tape. 6
Stage Anatomy Stage Assembly 1. Ceramic Heating Crucible. Water Cooling Connector 3. Bypass Water Cooling Connector 4. Gas Connector 5. Temperature sensor cable 6. Stage Cable 3 4 6 1 5 3 4 Lid Assembly The lid is removed by unscrewing it from the stage. 7. Stage Lid 8. Inner Lid 9. Viewing Window (8mm diameter) 7 8 9 7
Windows Assembly 1. O-rings (ORTS1500). Quartz window (W55Q, 55x1mm) 3. Ceramic Radiation Shield with 1.7mm diameter aperture 4. Sapphire Sample Disc with sample 5. Silicon Rubber O-rings 6. Quartz Window (WQ, x 0.5mm) 7. Window Locking Ring 8 Lid Window Assembly To replace the Lid Windows (), unscrew the Inner Lid (8) from the Stage Lid (9) and reassemble the Lid as shown in the diagram. 1 9 3 4 Bottom Window Assembly To replace the bottom window (6), use the Window Tool (10) to unscrew the Window Locking Ring (7) and reassemble the window as shown in the diagram. 5 6 7 10 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. 954) 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 (1) and the Locking Thumbscrew () so that approximately 5mm of thread is exposed on the inside edge of the clamp. This will roughly position the stage in the centre of the dovetail. Curved Clamp 954 Place the stage onto the dovetail then focus a 10X objective lens on the aperture of the heating crucible. Using the two positioning screws ensure that the aperture is in the centre of the field of view and tighten the Locking Thumbscrew () to lock the stage in position For other types of microscope substage, see the included diagram for fitting instruction. 1 1 Setting up the Condenser for Koehler Illumination. Place a small sample on a Sapphire Sample Disc and place into the Ceramic Heating Crucible. 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 Linkam Imaging Station with dovetail substage Dovetail 9
Pirani Gauge and Vacuum Port Connection The vacuum ports used the standard KF16 or KF10 vacuum flange. If a Pirani vacuum gauge is ordered with the system please connect the gauge as shown. 1. Vacuum flange. Vacuum o-ring 3. Clamping ring 4. Pirani vacuum gauge 1 3 4 To vacuum pump Note: make sure the flange and the rubber part of the vacuum o-ring are lightly coated with vacuum grease. ECP Water Circulator Pump Tubing Connection The water circulator is necessary to keep the stage body and Lid Window cool during heating experiments. Make sure the water is running before heating up the stage. Connect the Inlet and Outlet tubing from the ECP to the High Temperature Stage as shown. Note: An ECP pump filled with cool water, 15-18 C, has large enough capacity for upto hours operation of the stage at 1000 C or over. It is not recommenced for longer term work at these temperatures. Refer to the ECP, Water Circulator Pump Manual for setting up the ECP. Inlet Outlet Note: DO NOT touch the viewing window when the stage is being heated. The window will be hot. Bypass cooling loops 10
ECP Water Circulator Pump Tubing Connection for Ellipsometer Lid. The Elipsometer lid for the TS1000 uses one extra bypass cooling loop. In let Connect the Inlet and Outlet tubing from the ECP to the High Temperature Stage as shown. Refer to the ECP, Water Circulator Pump Manual for setting up the ECP. Note: DO NOT touch the viewing window when the stage is being heated. The window will be hot. Bypass cooling loops Out let Sample Preparation for Ellipsometer Lid. To ensure the full 140 optical angle of the ellipsometer lid, samples must be mounted onto a Ø10.0x1.0mm sapphire window within the heater. Note: the sapphire disk must be clean, sample residue stuck to the disk may melt and leak into the crucible and damage the heater. When loading a sample take care that it does not spill over the edges. Molten sample is not easily removed from the ceramic heating element. If sample comes into contact with the thermocouple it will cause permanent damage. Warning When heating above 800 C the heating element will begin to glow brightly. Use a light filter in the trinocular (or binocular) head of the microscope to view the sample. 11
MV196 set-up Only read the following section if you have purchased the High temperature stage with MV196 system. NOTE: Do not operate the MV196 while the stage temperature exceeds 00 C. the stage must be evacuated at a lower temperature and then heated. Vacuum Pump Setup Please read the Vacuum Pump manual to fill the pump with oil and to install the mist filter (1). 1 MV196 Motorised Valve Setup The MV196 Motorized Vacuum Control System consists of a motorized valve () 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. 4 3 Mounting the MV196 The MV196 has an vacuum flange just like the vacuum ports on the sides of the High temperature 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). 5 6 1
Sample Preparation Note: the sapphire disk must be clean, sample residue stuck to the disk may melt and leak into the crucible and damage the heater. The samples are loaded into the ceramic heating crucible on either a sapphire disc (1) or in a platinum crucible (). 1 Note: when using the platinum crucible a sapphire sample disc must first be placed inside the ceramic heating cup and then the platinum crucible placed on top. The total mass of sample and sample carrier (sapphire disc or platinum crucible) must not exceed 10mg as this will overload the heating element and equipment will not perform to specification. When loading a sample take care that it does not spill over the edges. Molten sample is not easily removed from the ceramic heating element. If sample comes into contact with the thermocouple it will cause permanent damage. Place the ceramic Radiation Shield (3) on top of the crucible, this will create a closed furnace to ensure uniform sample heating. The heat shield also prevents a majority of volatiles condensing on the quartz lid window when heating. Warning When heating above 800 C the heating element will begin to glow brightly. Use a light filter in the trinocular (or binocular) head of the microscope to view the sample. 3 13
Using the High Temperature Stage The High Temperature Stage responds very quickly to changes in temperature on the sample, so to prevent any damage to the heater it is strongly advised that no COLD samples be introduced at higher temperatures. Use a gas flow rate of no more than 60cc/min. Use a sample as thin and as light as possible. Samples must always be placed on either the sapphire disc or platinum crucible as the sample can fuse into the ceramic cup or can attack the thermocouple causing incorrect temperatures and leading to failure of the heater. For the same reasons quartz discs should not be used at temperatures >1000 C. Atmospheric Control If purging with gas, please DO NOT USE HYDROGEN OR HELIUM. These gases have very high thermal conductivity and will cause the heater to burn out very quickly. Gas Outlet It is recommended that other reactive gases are diluted with 95% of an inert gas such as nitrogen or argon. Please use a gas flow of less than 60CC/min. High gas flow has a cooling effect on the heater and will overload the heating element. To control the atmosphere in the stage there are gas valve ports on either side of the stage. Push the Valve Insert (1) into the Gas Connector (), there should be a click when the two parts are connected. Attach tubing (3) with 3mm inner diameter to this. Gas Inlet Note: To remove the Gas Valve Insert, hold the outer sleeve of the Gas Connector and push towards the stage. The Gas Connector is sealed when it is not connected. 1 3 14
Appendix High Temperature Stage with Options Only read the following if the stage is supplied with vacuum ports (e.g. TS1500V) or internal electrical contacts (e.g. TS1500E) and / or both options. Picture opposite shows a TS1500EV Stage with both options High Temperature Stage with Internal Electrical Contacts The stage is supplied with two internal electrical contact connectors (1) wired to an external Lemo connector (). 1 Using the Internal Electrical Contact The internal electrical contact has a self-closing spring loaded pin (3). 3 15
Using a finger tip push in the pin to open the electrical contact and insert a platinum wire into the contact (1). Release the finger when the wire is in place. 1 Lemo Connector Remove the Lemo plug by holding it firmly and pull it gently away from the Stage. Wire up the Lemo to your instrument. To reconnect the Lemo, line up the red dot on the Lemo plug () to the red mark on the Lemo socket (3) and push the Lemo firmly into place. 3 16
Blanking Plates Use the supplied blanking plates (1) if either/both vacuum ports are not being used. Use a M.5 hex key to remove the two screws () on either side of the vacuum port. 1 3 Do the reverse to fit the blanking plate in place. Make sure that the aluminium vacuum seal (3) insert is placed between the stage and connector. The picture opposite shows the stage with both blanking plates fitted. 17
Connecting the Gas Purge Kit If you have purchased a vacuum compatible stage with a 991 Gas purge kit, the following diagrams will help you connect up and use the equipment. 18
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. Fully close the vacuum valve 3. Purge the stage with Argon to evacuate Oxygen from the stage and gas tubes. b) Purge the stage for 10 seconds. Make sure that the purge fitting is removed and the valve is closed afterwards a) Open the in line gas valve (regulator set at psi) 4. Turn on vacuum pump, then open the vacuum valve. Leave for 15 minutes so that the maximum achievable vacuum is reached. a) Turn on the vacuum pump Open the vacuum valve b) NOTE : There is no vacuum gauge, these gauges leak and have an effect on test results 0
5. After 15 minutes close the vacuum valve and open the gas valve a) Close the vacu- b) Open the gas valve um valve 6. Heat the stage to 00 C and hold the temperature for minutes. 7. Heat the stage to the desired experimental temperatures. Let the stage cool down to room temperature before turning off the gas supply. 1
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Linkam Scientific Instruments Ltd Tel: +44(0)1737 363 476 Fax: +44(0)1737 363 480 Email: support@linkam.co.uk Unit 8 Epsom Downs Metro Centre Waterfield, Tadworth, Surrey, KT0 5LR, UK www.linkam.co.uk Version: 1.05 4