DuraSiN Silicon Nitride Membranes for TEM and X-ray
DuraSiN Film and Mesh products are durable, non-organic, low scatter support grids for quantitative TEM and X-ray analysis. When seeking the highest possible resolution, DuraSiN Film and Mesh products provide the ideal platform for imaging and analysis. Unlike other support films and grids, DuraSiN Film and Mesh products can withstand harsh chemical and temperature environments. For example, DuraSiN Film or Mesh products could be used as a substrate on which nanowires could be directly grown from a strong acidic solution. Once the nanowires are grown, the specimen is immediately ready for imaging and analysis in the TEM. Direct deposition eliminates the need to prepare a sample on one substrate only to then transfer it to a support grid for imaging.
DuraSiN Film and Mesh for TEM
DuraSiN Film and Mesh products have revolutionized the way samples are prepared for and analyzed in the transmission electron microscope.
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The DuraSiN Advantage
1. DuraSiN sample supports are affordable
DuraSiN is available in quantities as small as a five grids and variety packs can be assembled upon request— this enables users to sample multiple grids without the constraint of large minimum orders. Just as important, the availability of variety packs allows customers to quickly determine which product is ideal for their particular application.
2. DuraSiN support membranes allow multiple microscopy techniques to be performed on the same specimen
The mechanical stability of DuraSiN offers a support film that is ideal for multi-analysis, in particular, TEM or X-ray and AFM. DuraSiN products are strong enough to allow AFM directly on the membrane giving microscopists the ability to analyze both internal structure (with TEM / X-ray) and surface detail (with AFM) on the same support.
The mechanical stability of DuraSiN products provides an ultra-flat surface with wide area membranes free from grid bars. This eliminates the unwanted roughness, contamination or obstruction of other support grids and allows examination of specimens through large tilt angles without loss of data.
3. DuraSiN products are robust to solvents, bases and acids
Able to withstand virtually any acid, base or solvent, DuraSiN allows the synthesis or growth of colloids, fibers, nanoparticles, powders, polymers and wires directly onto the support film. If your samples is grown or synthesized under strong acidic or basic conditions then DuraSiN Film or Mesh needs to be part of your standard protocol.
4. DuraSiN products can withstand high temperatures (up to 1000°C)
The temperature stability of DuraSiN allows direct deposition using standard physical and vapor deposition techniques common in the semiconductor industry, including CVD, sputtering, e-beam and resistive evaporation. With deposition or growth directly on a DuraSiN specimen support, you can eliminate the traditional experimental ambiguity caused by transferring a sample from a larger sample to a TEM grid. Samples grown or deposited directly onto DuraSiN can be annealed or cured at elevated temperatures while mounted to the DuraSiN specimen support.
The temperature stability of DuraSiN also allows the observation of dynamic processes when several samples are removed for analysis at various times in the deposition, growth or anneal process.
5. DuraSiN products are robust to glow discharge & high energy plasma cleaning
Where cleanliness is a concern, particularly for compositional analysis using EDAX, etc., DuraSiN can be vigorously cleaned using processes previously incompatible with carbon-based supports. DuraSiN can be cleaned in sulfuric acid to remove organics, glow discharge can be used to modify the surface of DuraSiN products and high energy plasmas can be used to aggressively remove any organic residuals from the sample preparation process. Using these techniques, a pristine, carbon-free surface can be obtained for subsequent specimen deposition, growth and analysis.
DuraSiN Silicon Nitride Sample Support Film
Perfect for the analysis of colloids, powders, aerosols and polymers. DuraSiN Film provides a durable, non-organic, low scatter substrates for quantitative TEM and X-ray analysis.
DuraSiN Film products are specifically designed to give TEM/STEM and X-ray microscopists a support film that can withstand virtually any environment needed to grow or deposit a specimen. If your specimen requires exposure to high temperatures, acids, bases or solvents, consider growing them directly on DuraSiN Film - samples will not need to be transferred to another support for imaging and the presence of imaging artifacts introduced by specimen preparation are virtually eliminated. Self-assembled monolayers can be formed on a DuraSiN Film membrane for subsequent attachment of nanoparticles. Sandwiched together DuraSiN form a closed environment for wet cell applications. Our films are even robust enough to allow multianalysis, including AFM and TEM using the same grid.
The DuraSiN Film support grids are composed of two materials. The area for specimen observation is fabricated from chemically robust, low-stress, planar silicon nitride films. This area is supported by a 300 micron thick rigid silicon frame. The DuraSiN Film support grids provide a durable platform for sample preparation, cleaning, imaging and analysis. DuraSiN Film products are robust to most cleaning procedures, including acetone, alcohol and oxygen plasma/UV ozone. Products are available in sizes ranging from standard TEM (2.65 mm diameter) to greater than 10 mm for x-ray applications.
DuraSiN Silicon Nitride Sample Support Mesh
DuraSiN Mesh products offer the unique combination of an inorganic support film and regions completely transparent to an electron beam. These two features provide the microscopist and micro-analyst unparalleled capability for imaging and analysis.
Like other holey or lacey support films, DuraSiN Mesh support substrates provide regions completely unobstructed by the support film. However, the fact that the DuraSiN Mesh is made from an inorganic silicon nitride that provides the ability to thoroughly clean (e.g. with an aggressive oxygen plasma) a specimen already fixed to the support substrate. Cleaning the sample after affixing to the support assures that the imaging and analysis is not degraded by unintended contamination. For example, when analyzing carbon nanotubes, DuraSiN provides a clean, carbon-free support to isolate the specimen from carbon contamination.
DuraSiN Mesh support grids are fabricated from chemically robust, low-stress, planar silicon nitride films with an array of holes across the membrane. The membrane area is supported by a rigid silicon frame. The mesh pattern is available in a variety of shapes and sizes, down to even sub-micron features.
DuraSiN Mesh support films are ideal for multi-analysis of samples, including fibers, colloids, nanowires and powders. The rigid silicon frame provides an area for AFM analysis, just microns from the transparent window regions for TEM,STEM and X-ray. Remove the experimental ambiguity of analyzing different specimens by combining microscopy techniques. A specimen can be deposited or grown directly on a DuraSiN Film and then a single specimen can be analyzed with TEM, STEM, AFM and X-ray. Depending upon the DuraSiN window thickness and AFM stylus force, some users have even been able to AFM their specimen directly on the membrane itself.
DuraSiN Film and Mesh products are robust over extreme temperatures and in harsh chemical environments making them an ideal choice for many applications:
1. Quantitative analysis of carbon containing specimens
- DuraSiN Film and Mesh provide a carbon-free support providing more accurate compositional analysis of carbon-containing compounds
- The continuous, ultra-planar surface of DuraSiN Film is ideal for the deposition of polymers allowing the nanostructure of ordered polymer layers to be quantified
2. Chemical deposition and growth
- Surface modification of DuraSiN Film or Mesh silicon nitride membranes allows attachment and analysis of target materials
- Liquid samples can be dried on and supported by DuraSiN Film
- The large, regular array of holes for imaging on DuraSiN Mesh provides numerous electron-transparent analysis sites
3. Nanoparticle analysis
- Fine powders can be deposited and imaged over the electron-transparent holes of DuraSiN Mesh
- Atomized nanoparticles can be deposited and imaged at near-atomic resolution on continuous DuraSiN Film
4. Chemical reactions
- The impact of particle size & separation can be quantified with DuraSiN
- Oxidation and reduction reactions can be observed in situ or ex situ with DuraSiN Film and Mesh
5. New material discovery
- Multiple analysis techniques (e.g. TEM, STEM, XRAY, SEM, XPS, AES and AFM) can all be performed on the same specimen when it is supported by DuraSiN Film or Mesh
There are several standard and immediately available DuraSiN products specifically designed for TEM and X-ray applications as outlined below. Of course given their mechanical durability and robustness to temperature and chemicals, all of the DuraSiN products make ideal substrates for performing and then correlating the results from multiple microscopy techniques all on the same specimen.
DuraSiN Film for TEM
|Window Area||Frame Diameter||Frame Thickness||10 Count|
|DTF-2523||200 nm||.5 mm²||2.65 mm||300 µm||$130|
|DTF-1523||100 nm||.5 mm²||2.65 mm||300 µm||$130|
|DTF-05523||50 nm||.5 mm²||2.65 mm||300 µm||$170|
|DTF-03523||30 nm||.5 mm²||2.65 mm||300 µm||$230|
|DTF-050523||50 nm||50 µm²||2.65 mm||300 µm||$290|
|DTF-030523||30 nm||50 µm²||2.65 mm||300 µm||$290|
DuraSiN Film for X-ray
|Film Thickness||200 nm|
|Window Area||2.5 mm²|
|Frame Diameter||5 mm|
|Frame Thickness||300 µm|
DuraSiN Mesh for TEM
|Film Thickness||200 nm|
|Window Area||0.5 mm²|
|Frame Diameter||2.65 mm|
|Frame Thickness||300 µm|
|Hole Size||2 µm|
|Hole Pitch||12 µm|
|Hole Spacing||10 µm|
Based upon low-Z, inert silicon nitride, the DuraSiN Film and Mesh products are specifically designed to give TEM/STEM and X-ray microscopists a support film that will withstand virtually any environment needed to grow, deposit and image a specimen. DuraSiN Film and Mesh products are ideal if your specimen requires exposure to high temperatures, acids, bases or solvents. If your samples are grown in these conditions, consider synthesizing them directly on support films to prevent transferring to another support for imaging.
DuraSiN Film products are fully specified by 4 parameters: window area (B), frame thickness (D), film thickness(A) and frame diameter (C):
DuraSiN Mesh products use parameters A, B, C and D as above but also require two additional parameters: hole size (E) and center-center hole pitch (F).
Surface roughness AFM data for 100 nm thick DuraSiN films is shown below. The data was acquired from a 5 µm scan across the surface. The average surface roughness in the boxed area (ignoring the dust particle to the left) is 3.39 angstroms. Although some variation is expected from device to device, DuraSiN 100 nm and 200 nm films typically have an average surface roughness in the 3.0-angstrom range.
DuraSiN products with 50 nm films typically have a slightly larger average roughness than the 100 nm and 200 nm films. As determined by AFM, the 50 nm DuraSiN films typically exhibit average surface roughness of about 1.2 nm.
Flatness is a measure of how warped or bowed the surface is. As measured though a 20X DI microscope objective, the images do not demonstrate any measurable deformations. The regions around the 2 micron holes are completely flat, without any lip or curl around the edge of the hole, allowing specimens to lay flat across the holes. The image of the film also does not show any deformations. As a reference, the small specimen viewable in the image stands out because of the difference in surface height with respect to the film.
Solvent and Acid Robustness
DuraSiN™ Films and Meshes are robust to most solvent and acid treatments, and can be cleaned with virtually any process required by your specimen preparation protocol. Solvents such as methanol, ethanol and acetone have no effect on the film. Acids, including sulfuric and nitric, also do not affect the film. Other common cleaning procedures such as the J.T. Baker solution and RCA cleaning are also acceptable.
Plasma and Glow Discharge Robustness
DuraSiN Film and Mesh products are made from silicon nitride and are extremely robust to glow discharge cleaning and high-energy oxygen plasma. This is particularly useful when completely removing organic residues that could either affect the image quality or EDAX measurements. The products have been exposed to high-energy, 300W oxygen plasma systems typically used for removing up to microns of photoresist in the semiconductor industry, and no etching was observed in spectroscopic thickness measurements. In addition, no degradation was observed when inspected through a high-power optical microscope.
Monte Carlo simulations on models of 100 nm thick DuraSiN films, under the presence of a 120 and 200 keV electron beam and probe size of 1 angstrom show almost zero electron scattering even after 10,000 trajectories are simulated. With standard available thickness from 50 nm to 200 nm and the amorphous structure of the film, atomic-scale resolution has been obtained with DuraSiN products.
The only acids which might adversely affect the films are 49% hydrofluoric acid when exposed for several minutes, or phosphoric acid when heated to temperatures greater than 150 °C. The need for these chemicals at these conditions is quite rare.
The films are in the nanometer thickness range and it is not recommended that the grids be exposed to an ultrasonic bath. Cleaning for 30 minutes in concentrated sulfuric acid will generally remove organics and dust particles. Sometimes a final treatment in oxygen plasma or glow discharge is also applied.
DuraSiN has been tested to temperatures near 500 °C in ambient, and near 800 °C in vacuum. No degradation, warping or bowing was observed using a 20X DI microscope objective. DuraSiN is expected to be stable at temperatures up to 1000 °C, which makes the grids well suited for high temperature deposition steps.
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