Protochips Heating Poseidon E-chips User Guide

Protochips Heating Poseidon E-chips

Atmosphere E-chips

The Atmosphere E-chip family of sample supports provides an unparalleled level of flexibility for your in situ gas environment experiments. Atmosphere experiments utilize a small and large E-chip that form the bottom and top of the closed-cell design, respectively. Because each experiment requires both E-chips, Prototypes offers multiple combinations to optimize your imaging conditions whether you are imaging with JEOL or Thermo Fisher Scientific microscopes. E-chips containing a durable ceramic heating membrane are uniquely calibrated for thermal accuracy, and all E-chips utilize an amorphous silicon nitride window that creates a strong barrier for containing gases with minimal beam scatter.

Three Key Parameters for Atmosphere E-chips

Optimized for STEM and EDS

When conducting STEM and EDS experiments, sample placement at the top of the closed cell is preferred in order to minimize beam scatter and maximize EDS counts per second (CPS). Because Atmosphere is assembled with the large E-chip on top of the small E-chip, it is recommended to pair EAT-33AA and EAB-33W E-chips for these imaging modes. In this configuration, the heating membrane is integrated into the large chip, so samples should be placed or deposited on the large E-chip.

Optimized for TEM and HRTEM
When conducting TEM and HRTEM experiments, sample placement at the bottom of the closed cell is preferred in order to minimize beam scatter and maximize imaging resolution. Because Atmosphere is assembled with the large E-chip on top of the small E-chip, it is recommended to pair EAB-33AB and EAT-33W E-chips for these imaging modes. In this configuration, the large E-chip creates an electrical connection between the small E-chip spacers and the electrical contacts on the holder. The heating membrane is integrated into the small E-chip, so samples should be placed or deposited on the small E-chip.

Spacer Height
The thickness of the gaseous layer is established through embedded spacers on the small E-chips. This spacer sets the minimum spacing between the two E-chips, and all Atmosphere E-chip spacer heights are fixed at 5 μm.

How to Order?
Please contact us directly at orders@protochips.com including part
numbers and quantities (multiples of 10).
Note: One large and one small E-chip will be required for each experiment.
For additional information, please visit: www.protochips.com
www.protochips.com/success
Call us at 919.377.0800

Guidelines for Use

1. Use the provided calibration file for each heating E-chip, before the experiment. Download calibration files at echips.protochips.com
2. An ex situ leak check is required before every experiment.
3. Atmosphere E-chips are compatible with a variety of samples and sample preparation techniques including drop casting, FIB preparation, and other lift out techniques. For more information, visit success.protochips.com or consult the Atmosphere manual and sample prep guides.

Thermo Fisher Scientific, JEOL, Nion are registered trademarks of their respective companies.

Streamline Your Workflow

Tools for Sample Preparation and Characterization

Sample preparation is an important step to your in situ experiment as it sets the foundation for every step you take thereafter. The ability to reproduce your experiment in the future can be heavily dependent on the reproducibility of the sample preparation process. Prototypes has developed several tools that will help you create a highly reproducible sample preparation process that will save time and prevent wasted sample and E-chips.

Shadow Mask
Enables precise sample deposition on a targeted area of the E-chip. Compatible with Poseidon Select, Atmosphere, and Fusion Select E-chips:

• Prevents electrical shorts
• Keeps spacers on closed-cell E-chips clean
• Compatible with common PVD instrumentation (sputter coaters, evaporators, etc.), drop casting, and dry powder depositions
• Request part number: SHW-MSK-PKG

Inspection Holder
Optimize your sample distribution & concentration and perform pre-and post- mortem characterization of your sample right on the E-chip. Primarily used alongside Poseidon Select and Atmosphere experiments, but will also hold a Fusion E-chip.

• Check for agglomerations and sample concentration before assembling and leak checking
• Compatible with TEM plasma cleaners – deposit sample and plasma clean your E- chip all while held securely in the holder
• Complement your in situ data by performing high-resolution imaging, EDS, EELS, and diffraction of your sample on the E-chip before and after the experiment
• Observe areas that were and were not exposed to the beam during the in situ experiment and analyze how the combination of beam and environment affected the sample
• Request part number: APA-WKFL-TFS (Thermo Fisher Scientific microscopes) or APA-WKFL-JEOL (JEOL microscopes)

FIB Stub
The FIB stub in combination with our step-by-step guide for FIB sample deposition onto membrane and membrane-free E-chips will help ensure your time spent at the FIB does not go to waste. Compatible with Poseidon Select, Atmosphere, and Fusion Select E-chips with a special notch for the Fusion Select FIB-optimized electrical E-chips.

• Designed specifically to securely hold E-chips
• Step-by-step guides give specific angles and instructions for successful deposition and thinning on the E-chip (guides are located on the Success Community)
• Top notch is designed to hold our Fusion Select FIB-optimized electrical E-chip vertically so the deposition process mimics using a typical half-grid for a familiar feel.
• Request part number: FIB-STUB

If you have a question or would like to place an order for any of the above workflow items, please email ordes@protochips.com. For supporting documentation and troubleshooting guides for all in situ systems, please visit success.protochips.com or email support@protochips.com.

550μm x 20μm window E-chips

(Schematics not to scale)

Part Number| 0 nm| 50 nm| Spacer Height
150 nm       500 nm| 1 μm| 5 μm| Spacer Configuration

Static                              Flow

---|---|---|---|---|---|---
EPB-52A| •| | | | | | |
EPB-52BNS| | •| | | | | •|
EPB-52BNF| | •| | | | | | •
EPB-52DNS| | | •| | | | •|
EPB-52DNF| | | •| | | | | •
EPB-52GS| | | | •| | | •|
EPB-52GF| | | | •| | | | •
EPB-52JS| | | | | •| | •|
EPB-52JF| | | | | •| | | •
EPB-52MS| | | | | | •| •|
EPB-52MF| | | | | | •| | •

Small E-chips
These E-chips are used in combination with many different large E-chips and form the bottom of the closed-cell that safely confines liquid samples. Small E-chips are 2mm x 2mm in size, so they can be placed into the holder with the window aligned parallel or perpendicular to the window on the large E-chip. Check the recommended configuration and E-chip pairing using the table on Page 10 to see if these E-chips are optimized for your experiment. These E-chips can be used with most samples including whole cells, biological and soft materials, nanomaterials, and FIB lamellae.

Notes: Due to liquid layer thickness, STEM mode is necessary when using a 5 μm spacer.

All feature dimensions listed should be considered nominal. Variations in dimensions can occur.

550μm x 50μm window E-chips

(Schematics not to scale)

__

Part Number

| __

0 nm

| __

50 nm

| Spacer Height

150 nm         500 nm

| __

1 μm

| __

5 μm

| Spacer Configuration

Static                       Flow

---|---|---|---|---|---|---
EPB-55A| •| | | | | | |
EPB-55BNS| | •| | | | | •|
EPB-55BNF| | •| | | | | | •
EPB-55DNS| | | •| | | | •|
EPB-55DNF| | | •| | | | | •
EPB-55GS| | | | •| | | •|
EPB-55GF| | | | •| | | | •
EPB-55JS| | | | | •| | •|
EPB-55JF| | | | | •| | | •
EPB-55MS| | | | | | •| •|
EPB-55MF| | | | | | •| | •

Small E-chips
These E-chips are used in combination with many different large E-chips and form the bottom of the closed-cell that safely confines liquid samples. Small E-chips are 2mm x 2mm in size, so they can be placed into the holder with the window aligned parallel or perpendicular to the window on the large E-chip. Check the recommended configuration and E-chip pairing using the table on Page 10 to see if these E-chips are optimized for your experiment. These E-chips can be used with most samples including whole cells, nanomaterials, FIB lamellae, and biological and soft materials.

Notes: The thicker the spacer, the lower the resolution. Due to liquid layer thickness, STEM mode is necessary when using a 5 μm spacer.

All feature dimensions listed should be considered nominal. Variations in dimensions can occur.

300μm x 90μm Window E-chips

(Schematics not to scale)

__

Part Number

| Window Size| Spacer Thickness
---|---|---
300 μm x 90 μm| No Spacer| 500 nm
ECB-39A| •| •|
ECB-39GF| •| | •

Small Microwell E-chips
Microwell E-chips integrate microfabricated reinforcement features into the window that minimize window bowing and provide an array of 170 nm deep wells with windows only 30 nm thick that better confine your sample for longer imaging sessions. Microwell E-chips provide a substantial field of view with a very thin, uniform liquid thickness and are optimal for most samples that are <100 nm in size. Small microwell E-chips are preferred when imaging in TEM mode. The number of visible wells is dependent on the window dimensions and orientation of the large E-chip, and recommended E-chip pairings can be found on Page 10.

Microwell Dimensions

• Membrane thickness: 30 nm
• Microwell depth: 170 nm

All feature dimensions listed should be considered nominal. Variations in dimensions can occur.

Large Microwell E-chips

(Schematics not to scale)

__

Part Number

| Window Size| Microwell Size| Array
---|---|---|---
400 x 200 μm| 10 x 10 μm| 20 x 20 μm| 8 x 16| 4 x 8
EPB-42A1| •| •| | •|
EPB-42A2| •| | •| | •

Large Microwell E-chips
Microwell E-chips integrate microfabricated reinforcement features into the window that minimize window bowing and provide an array of 170 nm deep wells with windows only 30 nm thick that better confine your sample for longer imaging sessions. Microwell E-chips provide a substantial field of view with a very thin, uniform liquid thickness and are optimal for most samples that are <100 nm in size. Large microwell E-chips are preferred when imaging in STEM mode or conducting EDS analysis. The number of visible wells is dependent on the window dimensions and orientation of the small E-chip, and recommended E-chip pairings can be found on Page 10.

Microwell Dimensions

• Membrane thickness: 30 nm
• Microwell depth: 170 nm

Large E-chips

(Schematics not to scale)

__Part Number| Window Size| Microwell Size| Array
---|---|---|---
400 x 200 μm| 10 x 10 μm| 20 x 20 μm| 8 x 16| 4 x 8
EPT-42A1| •| •| | •|
EPT-42A2| •| | •| | •

Large E-chips
These E-chips are used in combination with many different small E-chips and form the top of the closed-cell that safely confines liquid samples. Check the recommended configuration and E-chip pairing using the table on Page 10 to see if these E-chips are optimized for your experiment. These E-chips can be used with most samples including whole cells, nanomaterials, FIB lamellae, and biological and soft materials.
All feature dimensions listed should be considered nominal. Variations in dimensions can occur.
SP-00004 5.7

EDS Optimized E-chips

(Schematics not to scale)

EDS Optimized E-chips
Featuring reduced chip material around the window, these E-chips deliver improved EDS performance, improving Counts Per Second (CPS) up to six times* from traditional E-chips. When paired with a recommended small E-chip found on Page 10, you enable direct line-of-sight from your sample to the EDS detectors even at zero tilt. These E-chips can be used with most samples including whole cells, nanomaterials, FIB lamellae, and biological and soft materials.

*Improvement can vary based on detector configuration.

All feature dimensions listed should be considered nominal. Variations in dimensions can occur.

Liquid Heating E-chips

(Schematics not to scale)

Poseidon Select Liquid Heating E-chips
The Poseidon Heating E-chips are used with the optional Poseidon Select Liquid Heating Package to heat liquids in situ. The liquid temperature is controlled using the Clarity software package, which provides closed-loop temperature control to heat the entire volume of liquid up to 100ºC. These E-chips are commonly used to heat liquid solutions or liquids containing nanoparticles. For recommended small E-chip pairing, use the table on Page 10.

Key Features

• Temperature Range: RT to 100 °C
• Temperature Accuracy: <4%
• Temperature Resolution: +/- 0.01 °C
• Temperature Control Method: Closed-Loop, on chip sensor

All feature dimensions listed should be considered nominal. Variations in dimensions can occur.

Electrochemistry E-chips

Poseidon Electrochemistry E-chips
When used with the Poseidon Select system and the optional Electrochemistry package, these E-chips enable quantitative electrochemistry experiments on samples and electrolytes of interest. Two different electrode geometries are offered and both can be used with a variety of small E-chips which can be found on the compatibility chart on page 10.

Concentric Electrode E-chips

Part Number| Working Electrode Material Electrode Location
---|---
Platinum| Glassy Carbon| Working Electrode on Window (nanomaterials)| Working Electrode off Window

(FIB lamella)

ECT-45CR| | •| •|
ECT-45PT| •| | •|
ECT-45PTF| •| | | •

Concentric Electrode E-chips
The concentric electrode configuration ensures the most uniform field distribution around the working electrode. There are two configurations of the concentric electrode design: one designed for use with nanomaterials (working electrode on window) and one designed for use with FIB lamella (working electrode off window). When working with nanomaterials, the working electrode is centered on the 550 µm x 40 µm silicon nitride window to maximize viewing area. When working with FIB lamella, the working electrode is located just off the silicon nitride window to provide a robust area for lamella deposition and allows the lamella to extend into the viewing area for imaging.

Linear Electrode E-chips

Part Number| Working Electrode Material Electrode Location
---|---
Platinum| Number of Electrodes in Viewing Area
ECT-15WR| •| 2
ECT-15WO| •| 1

Linear Electrode E-chips
The linear electrode configuration allows for flexibility in electrode location and provides you with an option to have two electrodes within the viewing area, allowing an environment where you can see the anode and cathode simultaneously in the TEM. For experiments where two electrodes are desired in the viewing area, ECT-15WR’s electrodes are all 5 µm wide, two of them are located 30 µm apart from each other on the silicon nitride viewing window and the third is 200 µm off the window. For experiments where one electrode is desired in the viewing area, ECT-15WO’s electrodes are all 10 µm wide with one located in the center of the viewing window and the others located 75 µm and 200 µm away, respectively.

Note: The small E-chip with the 300μm x 90μm window (page 4) is recommended for broadest viewing area of the electrode; the small E-chips with the 550μm x 50μm window (page 3) are recommended for highest resolution.
All feature dimensions listed should be considered nominal. Variations in dimensions can occur.
SP-00004 5.7

E-chip Compatibility

Recommended E-chip pairings
In order to ensure compatibility between the small and large E-chips you have selected, make sure that they are compatible with each other using the chart below. Certain E-chips combinations work better in different window alignment configurations, so make sure to consider this when ordering E-chips for your experiment.

Tip Consumables & Special Purpose E-chips

Special Purpose E-chips (Not for TEM Imaging)
Special purpose E-chips, not designed for imaging. See Product Description for more information.

Part Number| Type| Quantity| Description| Specifications
---|---|---|---|---
EPT-001-10| Blank E-chip: Large| 10| Large E-chip without viewing window. Used for testing vacuum and storage.|
EPB-001-10| Blank E-chip: Small| 10| Small E-chip without viewing window.
Used for testing vacuum and storage|
E-MSK-21A-10| Shadow Mask E-chip: Narrow Opening|

10

| E-chip mask for depositing sample with the mask jig. Not for use in the TEM.| 240 x 120 Micron

Deposit Area

E-MSK-11A-10| Shadow Mask E-chip: Square Opening|

10

| E-chip mask for depositing sample with the mask jig. Not for use in the TEM.| 120 x 120 Micron

Deposit Area

Gaskets & O-rings
Gaskets should be replaced periodically when surface wear is observed, excessive debris does not respond to cleaning, or when working with aggressive solvents.

Compatible Tip (PJES)
APA-GK-PF05| 5| Perfluoroelastomer gasket-style O-rings for sealing E-chips in tip of gasket compatible* Poseidon or Atmosphere TEM holders.| Standard Tip (JEOL and ThermoFisher)
APA-OR-PF05| 5 Sets| Perfluoroelastomer O-ring Kit – set of 5: Includes: 5 small O-rings (1.3 x 0.30mm) and 5 large O-rings (3.7 x 0.30mm). Compatible with both Poseidon and Atmosphere. Not Compatible with JEOL UHR compatible tip.|

Standard Tip (JEOL and ThermoFisher)

| * Please reach out to customer support if you are unsure if your holder is gasket compatible

Lid Screws
The brass screws that attach the lid of the Atmosphere holder to the tip should be replaced whenever the threading begins to show signs of wear or thread stripping.

Atmosphere.

All feature dimensions listed should be considered nominal. Variations in dimensions can occur.
SP-00004 5.7

Poseidon Select Spare & Replacement

Internal Tubing Replacements
Internal PEEK tubing assembly replacements. Includes 6 spare capillary O-rings.

TEM holder.
PJ-CT-PF01|

3

| Internal using assembly replacements for JEOL Poseidon Select TEM holder.

Poseidon Select Accessories Case

Everything you need for preparation, assembly, setup and running your experiment, in a convenient, portable carrying case. Includes storage areas for E-chips.

The following items are included in the Poseidon Select Accessories Case. Certain individual components are available separately from our partner, Electron Microscopy Sciences on page 15. Smaller groupings of items are available on page 14.

• Carrying Case (1)
• Micropipette (1)
• PEEK Tubing Cutter (1)
• 1 mL Glass Syringes (2)
• 5 mL Glass Syringe (1)
• Carbon Tipped Tweezers: Straight (1)
• Carbon Tipped Tweezers: Curved (1)
• Watch Glass
• Teflon Cleaning Dishes (2)
• Tip assembly jig
• Waste container holder (1)
• Red 1 mm OD PEEK Tubing (1.5 m)
• Yellow 1mm OD PEEK Tubing (1.5 m)
• PEEK Tubing T-Splitter
• P-REX Gaskets
• Torque Screw Driver
• Lid Screws
• Liquid Port One-piece fitting (3)
• Liquid Port Plug
• Syringe Luer Lock Assembly Set (1)

Request Part #PSEL-ACC-KIT-AS or #PSEL-ACC-KIT-ES (PJES Holders, JEOL UHR EDS Compatible Tip)

Poseidon Select Spare & Replacement Components

Do you need to replace missing or worn parts, or add a second set for multiple users? Small components and accessories are available as convenient packages.

**Poseidon Select Spare Part C***
Spare parts kit for Poseidon Select systems. Kit includes the following items:

• Tip Assembly Jig
• 1 mL glass Hamilton syringe (1)
• Syringe Luer Lock Assembly Set (1)
• Red 1 mm OD PEEK Tubing (1.5 m)
• Yellow 1mm OD PEEK Tubing (1.5 m)
• Liquid Port One-piece fitting (3)
• Liquid Port Plug (3)

Request Part #PSEL-SPARE-C

**Poseidon Select Flushing Kit***
Spare parts kit for Poseidon Select systems. Kit includes the following items:

• 5 mL Glass Syringe (1)
• Syringe Luer Lock Assembly Set (1)
• T-Splitter for flushing both input ports simultaneously (1)

Request Part #PSEL-FLUSH-KIT

Protochips-Heating-Poseidon-E-chips-16

Miscellaneous Supplies

Many accessory items that work well with the Atmosphere system are available as part of the Poseidon Select Toolkit, which is available from our partner, Electron Microscopy Sciences (EMS).

Orders may be placed directly through EMS

https://www.emsdiasum.com/microscopy/products/tem/holder.aspx

Small Volume Pipette 0.1-2µl – Autoclavable. Small volume allows for precise deposition of sample onto the Poseidon E-chip. Requires compatible pipette tips

Pipette Tips – 10 ul disposable pipette tips, required for the small volume pipette.

Watch Glass – 75 mm diameter. Used to plasma clean E-chips to ensure they are clean and hydrophilic. Curved watch glass makes placing and picking up E-chips easier.

Torque Screw Driver – for tightening lid screws.

Torque Driver Bit – for Torque Screw Driver

Torque Driver Adapter – Insert Bit 1/4″ Dr Hex Adapters. Adapter holds the torque driver bit, so it can be inserted into the torque driver

Style 2A Straight-Tip PVDF Tweezers – Carbon tip tweezers help to avoid chipping the E-chip silicon

Style 7 Curved-Tip PVDF Tweezers – Carbon tip tweezers help to avoid chipping the E-chip silicon SA-00004 5.5

Replacement Parts
Did something not listed above get lost or damaged? Replacement tip lids, holder stands, cables, and electrochemistry dongles are available. Contact orders@Protochips.com with a description of the part you need and holder serial number for a quote.

Add More Capability to Your Existing System
Accessories for increased workflow efficiency that integrate seamlessly with your existing Poseidon Select system.

Syringe Pump
Add a second syringe pump for mixing experiments or upgrade your existing pump to infuse/withdraw capability

• Harvard Apparatus Syringe Pump
• Request Part Number: SP-500 (Infuse Only) or SP-506 (Infuse/Withdraw)

Ex-Situ Electrochemistry Cell
Optimize your electrochemical experiments on the benchtop without tying up your Poseidon TEM holder. The ex-situ cell replicates the exact
tip conditions of the TEM holder in a convenient footprint for standalone use or with an optical microscope.

• Poseidon Select Ex Situ System with 3 Liquid Ports and 3 Electrodes for Sample and Experiment Optimization. Specification
• Request Part Number: EXP-3031

Leak Check System
Protochips’ recommended system for performing leak checks and storing the holder to minimize contamination.

• Highvac turbo dry pumping station with full-scale gauge, auto vent valve.
• Detachable flange for TEM holder
• Request part number: LKCK-AV-TFS (Thermo Fisher Scientific microscopes) or LKCK-AV-JEOL (JEOL microscopes)

Ready to Upgrade?
Your existing Poseidon Select Base System can be upgraded at any time to add more in-situ capabilities.

For a quote to add more functionality to your system

Please contact sales@Protochips.com for a personalized quote.

Poseidon Select Heating Package
Package contains everything required to add liquid heating capabilities to your existing Poseidon Select system. Harvard Apparatus Syringe
Pump

• Control liquid temperature between room-temperature and 100C in static, liquid flow and liquid mixing configuration.
• Power Supply & Clarity Software
• All necessary cabling.
• Contact your local Protochips’ representative for a quote.

Poseidon Select Electrochemistry Package
Package contains everything required to add electrochemical capabilities to your existing Poseidon Select system.

• High performance potentiostat/Galvano stat & software.
• Ex-situ electrochemistry cell for for experiment optimization outside
• All necessary cabling
• Contact your local Protochips’ representative for a quote.

AXON Machine Vision Software Platform
Redefine your in situ experience by linking the transmission electron microscopy detectors and in situ systems together with a revolutionary new tool.

• Improves data quality, enhances and extends your current microscope capabilities and makes in situ experiments easier for the novice to most advanced users.
• The AXON platform is a module-based software solution. Easily plug in new modules as they are released, and your system will stay up to date with the latest features.
• Contact your local Prototypes’ representative for a quote optimized for your setup.

Support
Not sure what E-chip or tool you need? Our applications scientists are always happy to help you find the right configuration for your experiment.
Contact support@Protochips.com and we’ll connect you with one of our highly-skilled applications scientists.

WE’RE HERE TO HELP!

References

• Customer Community
• Protochips | Advanced in situ TEM Solutions & Sample Supports
• Omniprobe Lift-Out Grids, TEM Holders, and Thinning

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