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 1 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 10 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 a top chip with 30nm thick windows (10x) is available. Each Nano-Reactor MEMS device is thoroughly tested  to ensure safe operation in the high-vacuum S/TEM environment.

CuO in 500 mBar H+ N2 at 350 °C

FFT showing better than 1 Å resolution

Crossing the Pressure Gap

Observing the effects of pressure on sample dynamics

Since the first days of electron microscopy, working in high vacuum has been a major limitation on research. The effects of  more significant pressures (>20 mBar) on sample dynamics are starting to be discovered right now. Crossing the pressure gap and transitioning to a 1 Bar pressure environment will take the community that next step closer to replicating the nano-scale real-world conditions needed for industrial catalysis investigations. Recent studies using MEMS based cells in at 1 Bar environment have shown that there is a direct link between (1) pressure and (2) sample dynamics, which is significantly impacting what’s currently known and modelled. For this reason, the Nano-Reactor technology is required to observe. at pressures up to 1 bar, the true mechanisms and dynamics at work during chemical reactions.

1 Bar Pressure

Fast Gas Switching

Programmable & Automated

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.

RT- 1,000 °C

Ultimate Stability

4-Point-Probe

Calorimetry

 

Monitoring heat dissipation & absorption

 

The amount of heat dissipated or absorbed by the specimen during endo- or exo-thermic reactions can be measured with the highest accuracy using the Nano-Reactor’s 4-point-probe micro-heater. Both the resistance across and the power dissipated by the micro-heater are monitored and displayed with ultra-high resolution to observe any changes in sample temperature and/or heat dissipation. This data can provide new insights and give an indication of the energy produced or consumed relating to the activity and interactions of the sample based on the gas conditions of flow, pressure and composition within the Nano-Reactor.

Heat Dissipation or Absorption

Local Measurement

Real-time Monitoring

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

2. Nano-Reactor Alignment Tool

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