The K1250X Independent Cryogenic Freezing, Preparation & Transfer System

A 'self contained' (independent) preparation system, with a turbo molecular, high vacuum pumping unit to allow the freezing, preparation, transferring, and subsequent examination of frozen hydrated specimens in a Scanning Electron Microscope and Field Emission SEM, without the need to utilise the SEM vacuum system.

The System will interface to all the current range of SEMs and the component parts will allow reverting to ambient temperature applications to be readily achieved.

System Items

System Performance

Freezing Chamber: Integral high vacuum chamber to produce sub-cooled liquid nitrogen for specimen plunge freezing. Pump down time 30 secs. Sub-cooled (slushy) nitrogen at -210^oC. Fitted with locating collar to suit transfer device, and excess pressure relief valve.

Preparation Chamber: Integral high vacuum chamber, axial mounted, with single action, self locking, access gate valve, and dead space pumping to suit transfer device, to facilitate all preparation facilities 'in-situ', and subsequently, with turbo pumping unit.

Turbo pumping unit 'axial' mounted on preparation chamber, with full 'throat' ISO63 flange to ensure maximum pumping efficiency. Pumping speed 60L/Sec. Vacuum better than 1 x 10^-5mbar. Safe shut down to atmosphere in event of vacuum failure, without damage.

Preparation chamber cold stage with four (x4) working positions, and copper to copper conduction, maintaining stage temperature colder than -170^oC, fitted with full cold shield contamination protection. Preparation chamber liquid nitrogen dewar. Double walled vacuum pumped, with one (x1) Litre internal capacity at atmosphere pressure maintaining stage temperature under quiescent conditions for 60 minutes without 'top up' or 'autofeed'. (Approx. 10 Litres per day.)

Sublimation stage integral to preparation chamber cold stage, with controlled temperature and timer.< br />
Micrometer Adjustable Knife with cooled 'blade' and adjustable height and push / pull action, with sample clearance feature on return stroke.

Macro manipulator with cooled 'point', and adjustable pivot positioning.

Sputter head (Standard), low energy input, high resolution. With Gold target (0.1mm thick x 20mm Dia.) fitted as standard. At 20mA, 100V dc (mean) for 2 minutes, thickness 20nm. Grain size 2nm.

Specimen temperature increase less than 3^oC/minute. Vacuum control for sputtering needle valve range 5X10^-1 to 2 x 10^-1mbar with electromagnetic 'back up' valve.

Sputter head Chromium coating head.

Carbon head for flash evaporation technique using carbon cord/string, with high vacuum turbo pumping giving fine coatings and allowing several evaporations from carbon cord without changing source.

Control Unit with plug in modular electronics and low voltage (24V dc) control circuitry. Liquid Crystal Display with small compact keypad. Controller "black box" can be situated away from keypad.

Sputter Coating Module with variable deposition 0-50nm/minute (Gold), and current control 0-50mA on analogue meter, with sputter voltage range 80-120 volts mean dc., and 0-4 minutes reset deposition timer.

Carbon coating module with low voltage 20V ac supply for carbon evaporation 'flash' typically one second, with 0-50A ammeter and variable outgas current control 0-20A.

Radiant heater with low voltage 20V ac supply with variable current control 0-20A.
Vacuum sequence module with electromagnetic valves, and automatic turbo backing pressure interlocking. Continuous vacuum monitoring of preparation chamber analogue meter 0 to 1x10^-5mbar. Auto select vacuum monitor of all other points of the system analogue meter 0 to 1x10^-5mbar.

Turbo control unit interlocked to vacuum sequential with normal (high vacuum) indication, and failure mode sensing.

Temperature monitoring units for preparation chamber cold stage and SEM cold stage. Set point control in range +50^oC to -200^oC, with P.I.D. (Proportional, Integral and Derivative) control parameters, and digital display +50^oC to -200^oC controlling input stage heaters, with adjustable timing 0-20 minutes. (Full range of controls -200^oC to +400^oC) Accuracy better than +/- 1^oC.

Transfer Unit Transfer chamber actively vacuum pumped for contamination-free applications. (Vacuum better than ^-2mBar during Transfer.)Transfer rod with thermal insulated tip, and integral single action, self locking gate valve, with dead space pumping facility.

Specimen stub, polished copper, with good thermal transfer characteristics and 'holding' properties. Warm up less than 10oC/minute during transfer activities when not located on cold stage. Facilities for longitudinal, crossectional, and fracture rivet applications.

SEM Components: Liquid nitrogen dewar, with interface to SEM port, to facilitate cold stage cooling and anti-contamination shield. Double walled vacuum pumped, with one (x1) Litre internal capacity at atmosphere pressure maintaining stage temperature under quiescent conditions for 60 minutes without 'top up' or 'autofeed'. (Approx. 5 Litres per day.)

SEM single action, self locking, access gate valve with interface to SEM port, and dead space pumping to suit transfer device.

System General

Valves: Three (x3) manually operated access gate valves are single action, self locking, to prevent inadvertent operation.

Needle valve for sputtering control fitted with non damaging seat, with pre-set position control, and electromagnetic back up.

All other operational valves are electromagnetic, with push button control, with full mimic status indication.

Input valve for argon gas supply.

Input valve for nitrogen gas supply.

Specifications of the K1250X Cryo SEM System

• Instrument Case: 450mm W x 350mm D x 175mm H International Standard DIN 41494, with integral air flow, and E.M.C. Standard (Electro Magnetic Compatibility)
• Cylindrical Work Chamber: 130mm Dia x 250mm Long, with Vacuum Gate Valve
• Slushing Chamber: 125mm Dia x 150mm Deep
• Liquid Nitrogen Dewar: 100mm Dia x 150mm Deep, Capacity 1.0 Litre
• Turbo Molecular Pump 60 L/Sec.
• Weight: 36Kg
• Control Unit: 450mm W x 350mm D x 175mm H.
• Control Electronics: Fitted
• Weight: 28Kg.
• Transfer Unit: with Vacuum Gate Valve - Vacuum Pumped
• SEM Coldstage: With Vacuum Gate Valve and Liquid Nitrogen Dewar 1 Litre Capacity.
• Weight: 16Kg
• Total Weight of System: 82Kg
• Sputter Coating: 20mm Dia x 0.1mm Thick Target (Gold fitted as standard)
• Timer: 0 - 4 Minutes.
• Sputter Gauge: 0 - 50mA.
• Carbon Coating: Deposition 0-10nm/min Carbon Fibre/Carbon Cord (with Integral Radiant Heater)
• Ammeter Gauge: 0 - 50 Amps
• Evaporate Button
• Outgas Control: 0 - 25 Amps
• Cooled Knife Assembly
• Cooled Probe Assembly
• Specimen Transfer Stub: For Multipurpose applications (special stubs available)
• Vacuum Gauge: 0 - 1 x 10^-5mBar.
• High Vacuum Condition Indicator
• Turbo Molecular Pump Unit: Better than 1x10^-5mBar.
• Preparation Stage Temperature: Better than -170^oC.
• Temp. Monitor & Control: -200^oC to +50 (Control full range - 200^oC to + 400)
• Timer: 0 - 20 Minutes
• SEM Stage Temperature: Better than -170^oC.
• Temp. Monitor & Control: -200^oC to +50 (Control full range -200^oC to +400)
• Timer: 0 - 20 Minutes
• Viewing Light Source

Accessories

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