Nano-Chip

Sample carrier for in situ heating

The Nano-Chip is a functional ‘sample carrier’ that replaces traditional TEM Cu grids. Based on Micro-Electro-Mechanical Systems (MEMS), Nano-Chips provide an elevated temperature environment while maintaining the resolution power of a transmission electron microscope. Controlling the temperature environment locally on the device via the 4-point-probe, each Nano-Chip creates a micro-laboratory environment within your TEM. Imaging across the entire temperature range can now be performed with the ultimate in sample stability and temperature accuracy.

Micro-heater

A ‘micro-sized’ heater
for ‘nano-sized’ materials

Based on the most advanced MEMS technology and engineering knowledge, the Nano-Chip scales down the micro-heater to the ‘sample size’ for heating the region of interest – the sample. Fabricated using highly accurate chemical deposition techniques, the 300 x 300 um metal micro-heater is very low in mass and has a very low thermal expansion co-efficient. This in conjunction with the 4-point-probe provides researchers with extremely fast ramp / quench rates and the highest temperature accuracy and stability – 0.001 °C at any temperature.

Easy Sample Preparation

Directly deposit your sample onto the Nano-Chip

Loading the sample onto the Nano-Chip is easy and fast to perform. Nanoparticles are typically in powder form and are prepared in an ethanol solution for direct drop casting onto the Nano-Chip’s electron transparent windows.

Technology Leadership

Nano-Chip = Performance

Calculating the temperature at the source dramatically improves the temperature accuracy and minimises the effects of the specimen size, column temperature or gas environment – such as the Climate Nano-Reactor. The Nano-Chip combines the optimal heater material (metals for their fast responsiveness and linear R-T dependence) and the best known MEMS measurement system (4-point-probe). As shown in the figure on the left, two contacts deliver the ‘current’ (I) and two contacts measure the ‘resistance’ (R).

The figure on the right shows the key unique feature of metal heaters, that across the temperature range of RT – 1,300 °C, temperature (T) has a linear relationship to the locally measured resistance (R). This important feature of metal heaters allows for calibration to be performed to guarantee the high temperature accuracy across the entire temperature range. Cross correlation of the temperature accuracy and Nano-Chips is performed using a number of methods – IR Pyrometry & Raman Spectroscopy – and ensures the highest temperature accuracy in the researcher area.

Features & Benefits

1. Unique Design For Optimal Stability

Nano-Chips are fabricated to ensure a stable, chemically inert and electrically insulated environment that guarantees your TEM’s performance is preserved.

3. Reliable Output

The closed-loop temperature feedback system offers a major advantage in temperature accuracy, stability and response times. Additionally, Nano-Chips are cross-referenced with Raman thermometry to increase system reliability and accuracy

2. Heat At The Source

The Nano-Chip localizes the heating to the same scale dimensions of your sample, allowing for greater control, response time, accuracy and reliability.

4. Long Life-Time

Each individual Nano-Chip offers unrivalled stability and experimental lifetime (>90 hours) at elevated temperatures. The replaceable nature of the Nano-Chips offers you full experimental freedom and guaranteed contamination free analysis.

Nano-Chip Support Film Range

Most samples such as nanoparticles or 2D materials for in situ TEM must be ‘supported’ on a thin electron transparent film to hold the specimen in place during investigation inside the TEM. Only samples that are ‘self-supporting’ do not require additional support film including FIB prepared lamellas.

Silicon Nitride

Silicon nitride support films (or Si3N4 membranes) is the standard configuration for the heating experiments for all Wildfire systems. Made by state-of-the-art MEMS fabrication techniques using Low Pressure Chemical Vapor Deposition (LPCVD), this results in high quality, low-stress and amorphous silicon nitride thin films. Silicon nitride has many advantages including being chemically inert, mechanically robust and can withstand harsh chemical and temperature environments (up to 1,000 °C).

  • Elevated temperatures up to 1,000 °C
  • HRTEM
  • Typical samples: drop casted particles and thin films

Configurations: Nano-Chip ST and Nano-Chip XT

Carbon

This Nano-Chip offer researchers a ~5 nm thin layer of carbon substrate for the sample. These extremely thin membranes are highly transparent to electrons and provides a low background that does not interfere with the contrast of the sample. The carbon support is best for moderate temperature studies (up to 800 °C) and nanoparticle experiments.

  • Moderate temperatures up to 800 °C
  • Ultrathin windows
  • Typical samples: nanoparticles and thin films

Configuration: Nano-Chip XT

Through-Hole

Through-hole Nano-Chips are fabricated for FIB lamella applications. This Nano-Chip has no support as the lamella that span the window size of 5 by 20 micron can be prepared across the window. Having a number of windows in the homogeneous temperature viewable area, a number of lamellas can be prepared onto the same Nano-Chip.

  • Ultra high temperatures > 1,300 °C
  • High contrast
  • FIB prepared lamellas and nano-tubes

Configuration: Nano-Chip XT

Frequently Asked Questions

What is a Nano-Chip or MEMS device?
Nano-Chips are functional consumable ‘sample carriers’ that replace traditional TEM Cu grids. Based on Micro-Electro-Mechanical Systems (MEMS), they offer the unique ability to expand your application space and experiments by controlling the environment locally on the Nano-Chip. Each Nano-Chip creates a micro-scale laboratory environment within your TEM, and due to its very low mass and minimal power consumption, the response times are extremely fast and performance highly reliable.

Is the heater of a Nano-Chip conductive with the sample?
No. The metal heater lines are encapsulated in SiNx, ensuring that the same is insulated from the heater.

What is the thickness of the electron transparent windows?
This is dependent on the type of window – Silicon nitride, carbon or through-hole.

  1. Silicon Nitride
    1. Nano-Chip ST – 30 nm
    2. Nano-Chip XT – 20 nm
  2. Carbon
    1. Nano-Chip XT – 5 nm
  3. Through-hole
    1. Nano-Chip XT – No window present.

What is the temperature accuracy of the Nano-Chip?
DENSsolutions guarantees every Nano-Chip provides better than 5% error in temperature accuracy in the research area of the heater.

What is the life-time of a single Nano-Chip?
The life-time of our Nano-Chips has been extensively tested for the heater life-time and related temperature performance:

  • The Nano-Chip ST set at the maximum rated temperature of 800 °C showed no change in performance after 90 hours of continuous use.
  • The Nano-Chip XT set at the maximum rated temperature of 1,300 °C showed no change in performance after 26 hours of continuous use.

What TEM specimens can be used on a Nano-Chip
Generally speaking, all particle-like samples can be dispersed in ethanol or alcohol and drop cast onto the membrane of the Nano-Chip. Thin films can be sputtered onto the backside of the membrane of the Nano-Chip. Micro-manipulators can be used to transfer one single nanowire, micron-size particle or flake to one specific window of the heater. FIB lamella can be prepared, transferred and polished on the Nano-Chip.

How is the Nano-Chip calibrated for temperature accuracy?
Each package of Nano-Chips (10x per pack) is delivered to the customer with a calibration number called the ‘b value’. This b value is the number which is entered into the software to calibrate the system to that Nano-Chip. No calibration is needed to be done by the user. A number of methods are cross-correlated to calibrate and measure the temperature of the heater and sample ‘research area’. IR Pyrometry and Raman Spectroscopy is used to calibrate the parameters to the central research area of the Nano-Chip.

Can I exceed the maximum temperature range of the Nano-Chip?
DENSsolutions guarantees the performance of the device within the rated temperature range of each device.

  • Nano-Chip ST (RT to 800 C)
  • Nano-Chip XT (RT to 1,300 C)

Note: For SiNx windows, the maximum temperature of the membrane is ~1,000 C even though the device can easily go to high temperatures. For short experiments, it is possible to extend the temperature ~200 C above the rating before the device performance degrades. E.g. the Nano-Chip XT can be used at 1,500 C for short period. Note: DENSsolutions does no guarantee the length or time and performance at temperatures above the rated temperature.

How robust are the Nano-Chips to fast heating and cooling?
Our Nano-Chips are very robust, capable of cycling between the rated temperature (e.g. Nano-Chip XT from RT – 1,300 C) without damaging the device.

Can I damage the Nano-Chip by going to temperatures above the rated temperature?
The Nano-Chip device is capable of going beyond the rated temperature, for example, the Nano-Chips can be heated past the 1,300 C to 1,500 C. However, in doing this the heater starts to degrade and for long experiments the local resistance measurement cannot be guaranteed within our specifications. If you set (Tset) the temperature to 3,000 C in the software, the system will try and reach that temperature no matter what you set. In this case of 3,000 C, the Nano-Chip will fail and will need to be replaced. To avoid going to such high temperatures accidentally by typing one to many 0, the software prompts you for a maximum (Tmas) temperature to ensure that you don’t enter the incorrect temperature.

Can Nano-Chips be used more than once?
Our Nano-Chips are designed as a consumable sample carrier, for a one time use. In principle, each Nano-Chip can be used in excess of 100 hours and therefore re-used. However, we do not recommend using the same Nano-Chip more than once due to the difficulty in successfully removing specimens from the Nano-Chip windows. Experimentally, ensuring a clean environment free from contamination of a prior experiment is key to obtaining correct data. For this reason we recommend that a Nano-Chip is NOT cleaned and reused.

Can Nano-Chips be plasma cleaned?
The Nano-Chip ST and Nano-Chip XT devices with SiN or through-hole windows can be plasma cleaned when using low power. Nano-Chips with carbon windows cannot be plasma cleaned as carbon is etched away by plasma. To clean Nano-Chips, it is recommended to be done with the Nano-Chip loaded into the holder. Recommended parameters for Nano-Chips with SiN and through-hole windows:

  • Oxygen plasma (it is the most effective in breaking most of the organic bonds (i.e. C-H, C=C, C-O, C-N, etc.) that are present in surface contaminants).
  • Power: < 5 -10 W
  • Flow rate: 5 sccm flow
  • Time: 30 seconds

Argon plasma is possible, although not as efficient as the oxygen. In this case, you may need to increase the time from 30 seconds to 1 minute. NOTE: Be aware that most plasma cleaners for holders are set by default to high powers (typically >100 W) which can be harmful for the Nano-Chip. If the power is too high (> 100W) it will etch the contact pads of the Nano-Chips and induce stress to the SiN window membrane.

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For more information on workflow, applications and specifications.

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Contact us

Feel free to contact us with any further questions.

Request a Demo or Quote

Request a quotation or demonstration at your lab.