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PP3010T Cryo-SEM/Cryo-FIB/SEM Preparation System

The PP3010T is a highly automated, easy to use, column-mounted, gas-cooled cryo preparation system suitable for most makes and models of SEM, FE-SEM and FIB/SEM.
Key features
  • High resolution performance on SEM, FE-SEM and FIB/SEMs
  • Totally gas cooled, including cryo preparation chamber - no boiling nitrogen on the SEM
  • Efficient cooling (typically down to at least -190ºC)
  • 24 hours plus run times on one fill of LN2 are typical - allowing unattended overnight operation (at typical operating temperatures)
  • Large recipe driven touch-screen interface
  • Automated sublimation, coating and system start up
  • Superb specimen visibility (including preparation chamber CCD camera)
  • Fully compatible with SEM beam deceleration/stage bias modes up to 5kV
  • Off column cooling and pumping systems - minimum mass on the SEM
  • On-screen data logging and diagnostics
  • Pumped storage of the cryo transfer device
  • Prepdek workstation - self contained work area, extra bench space not required
  • Cryo workflow options
  • Specialist support and extended warranty option
Click to download Brochure

The PP3010T is a highly automated, easy-to-use, column-mounted, gas-cooled cryo preparation system suitable for most makes and models of SEM, FE-SEM and FIB/SEM. 

The PP3010T has all the facilities needed to rapidly freeze, process and transfer specimens. The cryo preparation chamber is turbomolecular pumped and includes tools for cold fracturing, controlled automatic sublimation and sputter coating. After processing, the specimen is transferred from the cryo preparation chamber onto a highly stable SEM cold stage for observation. Cold trapping in the cryo preparation chamber and SEM chamber ensures the whole process is frost-free. Specimen process times are typically between five and ten minutes.

For cryo-SEM and cryo-FIB/SEM applications examples please visit: Application Images.


Detailed description

Mounting, freezing and transferring specimens – easy with the Prepdek™ workstation

Freezing and specimen handling and workflow

The PP3010T PrepdeKtm workstation is fitted with a slushy nitrogen freezing station, connected to the pumping system. Rapid freezing reduces ice crystal damage and results in improved specimen preservation. For handling pre-frozen material the PrepdekTM freezing system allows specimens that have been frozen by alternative freezing methods (or stored field specimens) to be manipulated - in or just above liquid nitrogen - and then transferred under vacuum into the PP3010T preparation chamber for subsequent processing and observation. 

Additionally the 25314 TEM Prep Slusher and 25852 glove box interface/airlock options allow workflow amongst a range of other platforms, including cryo-TEM, cryoultramicrome, XPS and glove box. Please see below for details.

Cryo transfer device – including vacuum storage

The vacuum transfer device is compact (fits easily into one hand), reliably vacuum-tight and has a bayonet connection to the specimen shuttle to ensure rapid pick up and transfer.

Set into the Prepdektwork surface is a pumped storage tube for the cryo transfer device (see Prepdektm  workstation section below).

Specimen stubs, shuttles

The PP3010T is supplied with universal 10 mm specimen stubs with surface slots, holes and a flat area - useful for most specimen types. Blank and slotted stubs are also included. In addition a range of optional holders is available, including shuttles for large specimens and top-loading holders for high pressure freezing, TEM Autogridstm (for cryo-FIB/SEM applications) and clamping shuttles for hard specimens.

You can view examples of these in the Additional Information section, or download a PDF from this link: PP3010T holders.

Cryo preparation chamber

The cryo preparation chamber is connected directly to the microscope and includes a highly efficient nitrogen gas cold stage, extensive cold trapping and facilities to fracture, sublimate and sputter coat specimens. The chamber is fitted with two fully integrated and interlocked gate valves. The outer load-lock valve includes a pumped airlock which accepts the cryo transfer device - the inner SEM valve ensures rapid high-vacuum to high-vacuum specimen exchange.

Highly efficient gas cooled stage and cold traps

At the heart of the cryo preparation chamber is a nitrogen gas cooled specimen stage. The stage has a dovetail fitting to accept a cryo shuttle and can be precisely controlled over a temperature range from 100oC to -190oC or lower. Large gas cooled cold traps located above, below and behind the specimen stage ensure clean, high vacuum conditions in the chamber.

Both the cold stage and cold traps are cooled with the fully integrated CHE3010 off-column cooling system (see below), which at normal operating temperatures give typical hold times of at up to 24 hours between fills (provided the nitrogen gas is dry).

High visibility – plus CCD camera

There is superb visibility into the preparation chamber. In addition to the large front window (75 x 150 mm) there are two top viewing ports. The chamber is lit by three LEDS and a CCD camera allows the specimen cold stage area to be viewed on the control screen and the images saved. 

An optional stereo microscope can also be fitted to the cryo preparation chamber

Cold fracturing

Twin fracturing tools manipulators (actively cooled) are available and allow a range of specimen types to be cold fractured. 

The PP3010T is fitted as standard with a front mounted fracturing and manipulation device. The ball-jointed mount offers flexible movement of the blade which can be used both as a surface pick (probe) and a fracturing knife. 

An optional micrometer-advanced fracturing tool with rigid blade is available in addition to the standard front-mounted tool.

Fractured fragments are captured in the large cold trap located below the specimen stage. 

Automatic sublimation and sputtering

Sublimation temperatures and times can be preset and stored for easy retrieval. The process is fully automatic and graphically displayed on the control screen, showing the actual verses the predicted temperature curves.

The high resolution sputter coater is an in-house design, being based on the market leading Quorum "Q" series of bench top coaters. The coating system will give fine grain films essential for FE-SEM applications. A platinium target is fitted as standard – optional metals include gold, gold/palladium, chromium and iridium. An optional fully integrated carbon fibre evaporation head (11920) can also be fitted.

An optional terminating film thickness monitor is available (12147).

Turbomolecular pumping - high vacuum performance

The preparation chamber is pumped by a remotely-positioned 70 L/s turbomolecular pumping system. Typical preparation chamber vacuums when cold are in the region of 10-7mbar or better. Positioning the turbomolecular pump away from the SEM ensures total elimination of mechanical vibration and has the advantage of significantly reducing the total cryo system mass connected to the SEM. A vacuum buffer tank (remotely located in the PrepdekTM) is automatically pumped when required. The pumping system is connected to the preparation chamber by flexible stainless-steel bellows, which allows flexible positioning of the pumping system.

A 5 m3/hr  rotary vacuum pump (13034) is required to "back" the turbomolecular pump and for slushing and rough pumping operations. The rotary pump can be located up to five metres from the system, allowing remote location if required. Dry pumping alternatives are available – see Ordering Information.

Prepdek™ workstation

The Prepdek™ workstation has been designed to allow specimen mounting, freezing (plus pre-frozen specimen manipulation) and transfer device storage on one ergonomically designed work surface. The control electronics are mounted in a sealed but accessible cabinet beneath the Prepdek™.

Set into the work surface is a pumped storage tube which allows the cryo transfer device to be stored under vacuum conditions when not in use.

Panel PC touch screen user interface

The PP3010T is controlled using a large touch screen panel PC, mounted on the Prepdek™ workstation. User-defined 'recipes' can be entered and stored for instant future access. The screen can be set to suit operator preferences; for example, vacuum measurement can be displayed in millibar, Pascal or Torr.

Many of the key steps in the specimen preparation process are automated (system set up, gas flow control, sublimation and sputter coating). Further help is available through a series of on-screen videos. 

SEM cold stage, cold trap and cooling system

A highly stable, thermally isolated, nitrogen gas-cooled stage attaches to the SEM stage. The SEM stage and cold trap are cooled by separate cold gas circuits - both capable of reaching temperatures of -190°C or lower. This configuration allows the operator to select stage and cold trap temperatures that are optimised for specific specimens. For example, for some non-biological materials it is useful to hold the specimen at very low temperatures – for example, a cold stage temperature of -175°C. This is possible with the PP3010T as cold trap temperatures of -190°C or lower can be selected - but not possible with conduction cooled systems.
The SEM cold stage has a temperature range of down to -190°C and a temperature stability of < 0.5°C.

Compatibility with SEM stage bias mode

The PP3010T cold stage is fully compatible with SEM stage bias/beam deceleration modes of up to 5kV.

CHE3010 off-column cooling

The CHE3010 is a fully integrated, remotely mounted cooling system which comes as standard with every PP3010T. The CHE3010T is used to cool the SEM stage, SEM cold trap and cryo preparation chamber cold stage and cold traps and will typically reach temperatures down to -190°C or lower.

The CHE3010 is remotely positioned (typically on the floor behind the microscope) and at normal operating temperatures can run for up to 24 hours between fills. This greatly simplifies the cryo process (no more checking on dewar status and topping up), but also allows overnight, unattended operation – particularly useful for some automated FIB/SEM "slice and view" protocols.

Single port interface to the SEM or FIB/SEM

Where SEM geometry allows, both the cryo preparation chamber and the SEM cooling system can be fitted to a single chamber port (the minimum port diameter is 38 mm). This gives a tidy installation and frees up a valuable chamber port.


Options and accessories

Specimen shuttles and stubs
The PP3010T is supplied with a selection of holders and a range of additional specimen shuttles and stubs is also available.(See Ordering Information for details).

Carbon evaporation and film thickness monitor
A carbon evaporation attachment (20996) and a terminating film thickness monitor (12147) can be fitted. Both are fully integrated (no external control boxes required).

Pressurised LN2 dewar
The PP7450/60L is a highly recommended option that generates dry nitrogen gas used for cooling the SEM cold stage & cold trap and cryo preparation chamber and cold shields. In addition LN2 can be decanted for slushing (freezing). During normal operation the PP7450/60L will generate dry nitrogen gas for up to eight days usage.

If the PP7450/60L is not included then appropriate, locally sourced, nitrogen gas cylinders can be used. It is important to ensure that it has low moisture content – if in doubt please contact Quorum.

Cryo workflow options

Glove box valve/airlock interface (25852) - for vacuum or inert gas transfer

The airlock is connected to a glove box using a generic NW fitting and for most applications requires a suitable pumping system (13034 rotary pump or 2336 turbomolecular plus diaphragm pumping system). 

The airlock is designed to accept the PP3010T vacuum transfer device.

For full details of this and other accessories please see Ordering Information.

TEM Prep Slusher option (25314)

Offers an easy and convenient way of transporting pre-frozen specimens to and from the PP3010T

  • Conveniently locates into the Prepdek workstation of the PP3010T
  • Freely transportable, e.g. between high pressure freezer, cryoultramicrotome and the PP3010T
  • Ideal for loading/unloading TEM grids and grid holders
  • Tilting holder for cryo shuttles (holders). Allows the easy transfer of specimens from external freezers (e.g. high pressure, jet, slam etc) 
  • Option for PP3010T and previous PP3000T and PP2000/PP2000T models.

Installation and training

Installation and training typically takes four days and is carried out at the customer site. In most cases installation and training is by a specialist Quorum Technologies cryo installation engineer, normally working in conjunction with our local distributor or microscope manufacturer's engineer. For further information, please contact Quorum Technologies (service@quorumtech.com). 

For a full quotation, including on-site installation and customer training, please visit the Global Distributors section or our UK sales team for further assistance.

PP3010T Cryo Preparation system for SEM and FIB/SEM

Including: column-mounted cryo-preparation chamber with off-column turbo pumping system. SEM cold stage and cold trap, PrepdekTM workstation with freezing and specimen manipulation facilities, automatic sputtering and sublimation. CHE3010 off-column gas cooling system.Touch screen, panel PC user interface mounted on the Prepdek  workstation. Cryo transfer device, 2 x AL200077B and 1 x 10246 specimen shuttles and the following specimen stubs: E7402 (pkt. 10), 5 x E7449, 5 x 11541, E7406 (pkt. 5), E7407 (pkt. 5) and 328116510 brass fracturing rivets (pkt. 100). 13761 230 V Sircal gas dryer (13762 foe 110 V). Microscope interfaces, start-up kit and operation manual.


Pumping requirements

The PP3010T requires one rotary vacuum pump or dry pump.

13034. Rotary pump. 5 m3/hr Pfeiffer DUO 6 rotary vacuum pump with oil mist filter.

20063. Edward nXDS6i dry scroll pump


Options and accessories

PP7450/60L. Pressurised liquid nitrogen dewar (60 L). Generates dry nitrogen gas used for cooling the SEM cold stage and cold trap plus cryo preparation chamber and cold traps. Liquid nitrogen can also be decanted for slushing (freezing). If not ordered then locally-sourced nitrogen cylinder gas can be used.

20996. Carbon fibre evaporation head and power supply, including 1 m carbon fibre (C5421).

12147. Film thickness monitor (FTM). Fully integrated (no additional boxes) and terminates sputtering at a pre-set thickness defined by the user.

12145. Micrometer controlled fracturing device with tool steel blade. Note: the ball-joint mounted fracturing tool is fitted as standard - the 12145 can be fitted in addition.

25852. Glove box valve/airlock interface for vacuum or inert gas transfer using the PP3010T cryo transfer device.

25314. TEM prep slusher.


Specimen shuttles

For images and descriptions see: Shuttles and Stubs.

AL200077B. Standard specimen shuttle with insert for 10 mm stubs.

12434. Specimen shuttle with large, flat surface (22 mm x 13 mm surface).

13524. Shuttle for large, flat specimens (with light microscope-style stage clips).

13524. Dual-clamping shuttle for clamping hard, flat specimens. Suitable for clamping flat and side-on for cross-fracturing.

13419.Tilt-rotate shuttle. Tilt and rotation can be altered on the preparation chamber cold stage using system knife/probe.

Shuttles for high pressure freezing holders and rivets

13054. Shuttle for high pressure freezer “top hat” style (3 mm) specimen holders.

10245. Top loading shuttle for "Balzers" style freeze-facture planchettes or similar small, flat holders or specimens.

20529 (formerly 10246). Top loading 10 mm specimen stub shuttle (similar to AL200077B, but with stub clamping mechanism located on the top). Useful for handling pre-frozen specimens mounted on a stub.

20530 (formerly 10247). Top loading rivet holder shuttle (vice style). Holds two rivets (see: 328116510).

E7433. Rivet holder specimen stub, screw-down style (for use with 10246).

Special shuttle for cryo-FIB/SEM of TEM autogridstm

12406. Shuttle to accept two TEM Autogridstm

STEM holders

Specimen holder requirements will vary according to make and model of SEM. In addition a modified SEM cold stage may be required, depending upon the SEM type. Please contact Quorum for further information.

13359. STEM shuttle for 3 mm TEM grid, including loading took. For STEM detectors mounted below the SEM cold stage.


Specimen stubs

E7449. Universal specimen stub with holes and slots 10 mm diameter  x 7 mm high.

11541. Universal specimen stub with holes and slots. 10 mm diameter x 5 mm high.

E7402. Blank aluminum (Al) stubs (pack of 10).

E7403. Blank copper (Cu) stubs (pack of 10).

E7405. Screw-down stub for thin, hard specimens.

E7406. Copper (Cu) stubs with 3 x 3 mm slots (pack of 5).

E7407. Copper (Cu) stubs with 1 x 3 mm slot (pack of 5).

32816510. Brass rivets for fracturing liquids (pack of 100).


Sputter targets and carbon fibre

All targets 24 mm diameter.

E7400-314IA. Gold (Au) target 0.2 mm thick.

E7400-314B. Gold/palladium (Au/Pd - 80:20) target 0.2 mm thick.

E7400-314C. Platinum (Pt) target 0.2 mm thick.

E7400-314F. Chromium (Cr) target 0.3 mm thick.

E7400-314IR. Iridium (Ir) target 0.3 mm thick.

C5421. Carbon fibre cord for use with optional 20996 carbon attachment (1 m).

C5421-10. Carbon fibre cord for use with optional 20996 carbon attachment (10 m).

Examples of PP3010T installations

Carl Zeiss

Left: Carl Zeiss Merlin FE-SEM.

Right: Carl Zeiss EVO W-SEM.







FEI

From left to rights: 

Nova NanoSEM 650 FE-SEM)

Versa 3 D FIB/SEM)

Helios 650 (FIB/SEM).






JEOL

JEOL 7800F FE-SEM.








Hitachi High Technologies

Left: Hitachi SU500 FE-SEM.

Right: Hitachi SU8230 FE-SEM.






Tescan

Tescan VEGA 3 XMU.






PP3010T Product Brochure

PP3010T specimen holders (version 16)

Please note special holders can be designed to meet specific requirements - please contact Quorum for details.