Nano-Reactor
A revolutionary technology for understanding chemical reactions
The Nano-Reactor is the MEMS based device that acts as a functional sample carrier enabling the gas-heating environment within the TEM. The Nano-Reactor, once loaded into the Climate Sample Holder, allows a defined amount of gas to be flowed through an inert Nano-Reactor chamber where the sample temperature is controlled by an integrated micro-heater and temperature sensor.
Replicating the real-world industrial chemical reactor, the Nano-Reactor allows sub-Angstrom resolution imaging and analysis of gas-solid reactions.
Easy Sample Preparation
Directly deposit your sample onto the Nano-Reactor
Loading the sample onto the MEMS based sample carrier called the Nano-Reactor, is easy and fast to perform. Catalyst nanoparticles are typically in powder form and are prepared in an ethanol solution for direct drop casting onto the Nano-Reactor’s electron transparent windows.
Nano-Reactor Overview
Replicating real-world chemical reactions on the nano-scale
Atomic Resolution Imaging
Observe catalyst dynamics with full S/TEM performance
The Nano-Reactor enables users to achieve real-world gas conditions pressures of up to 2 Bar, while imaging at atomic resolution. The Nano-Reactor has been designed such that the thickness of the gas flow at the position of the sample is in the 10 um range, giving close to zero interaction with the electron beam. As a sample carrier, the Nano-Reactor’s lower SiNx window has a quadruple benefit of supporting the sample for S/TEM imaging, thermally insulating the heated sample area from the bulk material (at RT) of the Nano-Reactor and being chemically inert to most samples and gases enclosing the gas safely within the Nano-Reactor.
The single top window (EDS version, 50 nm thick) and the bottom SiNx windows (30 nm thick) have almost no interaction with the S/TEM primary beam so to minimize the background signal. For low contrast samples an Ultra High Resolution Nano-Reactor is available with a top chip window of just 30nm thick. Each Nano-Reactor MEMS device is thoroughly tested to ensure safe operation in the high-vacuum S/TEM environment.
EDS top chips
Receive more information and achieve a higher resolution
Our EDS top chips allow for a large solid angle of X-ray detection. Thanks to the extra bulk material removed around the electron (and X-ray) transparent membrane even quanta with low take-off angles can leave the Nano-Reactor and find their way to an EDS detector (1). A small alpha tilt of the in situ holder (20 – 30 deg) will result in a significant increase of the EDS count rate. This enables elemental mapping of the sample in a short period of time (typically less than 30 minutes). In combination with the exceptional high stability of our Nano-Reactor this allows for high resolution elemental mapping.
The thin membrane at the center of the EDS top chip (2) has no windows, which allows for much larger tilt angles compared to the traditional top chips. Also, the chip alignment procedure becomes much easier since the required accuracy of this alignment is relaxed by two orders of magnitude.
Crossing the Pressure Gap
Observing the effects of pressure on sample dynamics
Micro-heater
Temperature accuracy, stability and reliability
The Nano-Reactor’s micro-heater is based on the proven and well established DENSsolutions MEMS technology that offers superior performance in temperature accuracy, reliability and stability. The micro-heater is encapsulated in inert SiNx to ensure that the metal of the heater doesn’t interact with the gas or the sample. Through a process of Joule heating, an electric current is passed through the metal micro-heater creating a homogeneous temperature environment up to 1,000 °C. The center of the micro-heater has a homogeneous temperature area that surrounds each of the ten electron transparent windows where the S/TEM sample is supported and creates the homogeneous environment. The 4-point contact design of the micro-heater allows for the 4-point-probe method of controlling the local temperature around the sample being studied – two contacts for heating and two contacts for measuring the local resistance of the micro-heater. The inherent physical advantage of a metal heater shows that resistance has a linear relationship to temperature, enabling the fast feedback to the electronics/software to accurately increase/decrease the temperature as desired by the user. Additionally, the 4-point-probe method compensates for any changes in the gas environment surrounding the sample as the fast feedback adjusts the power accordingly to counteract any change in thermal conductance and maintain the target temperature.
Calorimetry
Monitoring heat dissipation & absorption
A clean environment is essential to in situ microscopy and the modularity of the Sample Holder allows for all components that come into contact with the reaction gases to be replaced or cleaned on-site by the user. This includes the gas tubing, metal tip & lid, O-rings and consumable Nano-Reactor.
Consumable MEMS Device
Stay at the forefront of science with the latest in MEMS technology
Ensuring a clean and contamination free environment is crucial to every TEM experiment, which is why the Nano-Reactor has been designed as a consumable sample carrier. Therefore, the Nano-Reactor ensures reliability of results and prevents the data from being contaminated by particles with a high adhesion co-efficient (which are the majority) or the gases which have been in contact with the Nano-Reactor. Secondly, the DENSsolutions R&D team is continually developing and improving the Nano-Reactor as MEMS technology advances and this ensures the Climate user will always be at the forefront of in situ TEM technology.
Climate Nano-Reactor for Thermo Fisher Scientific Microscopes
Climate Nano-Reactor for JEOL Microscopes
Assembling Nano-Reactor & Tip
Fast and easy assembly with all tools included
The assembly of the Nano-Reactor into the Sample Holder tip is easy to perform (see video 1) and all required tools / components are included. Following sample preparation and feed through of the replaceable internal tubing, the Nano-Reactor is loaded into the precision made slot at the base of the Sample Holder tip. Small screws are used to lightly secure the Sample Holder tip together , before the Alignment Tool can be used to center the membrane of the top chip around the heater on the bottom chip is used to align the electron transparent windows of the top chip (10 um ⌀) with those in the bottom chip (6 um ⌀). Finally, the screws are tightened and the Sample Holder is ready for testing in the Gas Supply System Vacuum Test Tube.
1. Climate Holder & Nano-Reactor Assembly
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