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DuraSIN™ Silicon Nitride Membranes for TEM and X-ray | ||||
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DuraSiN™ Film and Mesh products have revolutionized the way samples are prepared for and analyzed in the transmission electron microscope.
Overview DuraSiN™ Film and Mesh products are affordably-priced, 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 onto 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. With direct deposition, no longer will you have to prepare a sample on one substrate only to then have to transfer it to a support grid for imaging. DuraSiN™ Film
Perfect for the analysis of colloids, powders, aerosols and polymers. The DuraSiN™ Film provides durable, non-organic, low scatter substrates for quantitative TEM and X-ray analysis at affordable prices. 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 and/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 can be virtually eliminated. Self-assembled monolayers can be formed on a DuraSiN™ Film membrane for subsequent attachment of nanoparticles. Sandwich them together and 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 and this area is supported by a rigid silicon frame where the frame thickness available for these products ranges from 200 - 600 microns. The DuraSiN™ Film support grids provide a cost-effective and 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 (2.65mm diameter) to greater than 10mm for x-ray applications. DuraSiN™ Mesh
DuraSiN™ Mesh products are a completely novel product, offering 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 with 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 inorganic silicon nitride provides the ability to thoroughly clean (e.g. with an aggressive oxygen plasma) a specimen already fixed to the support substrate and to assure that the imaging and analysis is done only upon on the specimen rather than 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 multianalysis 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 when combining microscopy techniques. A specimen can be deposited or grown directly on DuraSiN™ Films 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. 
The DuraSiN™ Advantage (TOP 5) 1. DuraSiN™ products are affordable DuraSiN™ is available in quantities as small as a single grid and variety packs can be assembled upon request— this enables users to sample multiple grids at a reasonable cost without the constraint of large minimum orders. Just as important, the availability of single grid and variety packs allows customers to quickly and inexpensively determine which product is ideal for their particular application. 2. DuraSiN™ products 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. That is, 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) either in the same viewing area or in areas on the support frame. 
Moreover, the mechanical stability of DuraSiN™ products provide 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 from grid bars. 3. DuraSiN™ products are robust to solvents, bases and acids Able to withstand virtually any acids, bases or solvents, DuraSiN™ allows the synthesis or growth of colloids, fibers, nanoparticles, powders, polymers or wires directly onto the support film itself. If your samples is grown or synthesized under strong acidic or basic conditions consider using DuraSiN™ Film or Mesh as 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. By deposition or growth directly onto a DuraSiN™ specimen support, you can eliminate the normal experimental ambiguity introduced 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 not possible 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 or growth and analysis. Applications 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 allowing 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 Publications using DuraSiN ™: Iron assisted growth of copper-tipped multi-walled carbon nanotubes. A Complete Scheme for Creating Predefined Networks of Individual Carbon Nanotubes. Characteristics of solid-state nanometre pores fabricated using a transmission electron microscope. Radial deformation measurements of isolated pairs of single-walled carbon nanotubes. Scanning Transmission Electron Microscopy of Biological Specimens in Water. Chemically Modified Solid-State Nanopores. Transmission electron microscope imaging of single-walled carbon nanotube interactions and mechanics on nitride grids. Rapid Fabrication of Uniformly Sized Nanopores and Nanopore Arrays for Parallel DNA Analysis. Tube-Tube and Tube-Surface Interactions in Straight Suspended Carbon Nanotube Structures. Growth and Characterization of Self-assembled Nanofibers.
Product Line 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 can withstand virtually any environment needed to grow, deposit and/or image a specimen. DuraSiN™ Film and Mesh products are ideal if your specimen requires exposure to high temperatures, acids, bases and/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-D as above but also require two additional parameters: hole size (E) and center-center hole pitch (F). 
Standard Products 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
DuraSiN™ Film for X-ray
DuraSiN™ Mesh for TEM
We realize that each customer has unique needs. Because specimens vary greatly in composition and size, and because DuraSiN™ finds use in numerous analytical and imaging techniques, there is no "ideal" product shape and size. To meet the diverse and demanding needs of the research community, DuraSiN™ Film and Mesh products were designed to facilitate customization and meet a user's specific requirements. For example, X-ray microscopists may be interested in DuraSiN™ products with a larger window area and with a thicker silicon nitride membrane. Users with microscopes that have a unique sample support fixture may be interested in DuraSiN™ products with a larger frame diameter. Finally, for the most demanding applications, ultra-thin silicon nitride membranes (<50nm) may be required. DuraSiN™ products can be customized to target a specific silicon nitride membrane thickness, silicon frame thickness, window area, and/or frame area. Most custom dimensional changes can be accommodated in only 3-4 weeks, and most other custom requests can be completed within 4-6 weeks. Please note that customized products may be more expensive, and minimum quantities may apply. Requests for customized parts can be made directly to Protochips via e-mail to sales@protochips.com. While almost any parameter defining the structure of DuraSiN™ products can be customized, there are ranges for these parameters that generally need to be considered:
Membrane Thickness Standard DuraSiN™ products are available with 50nm, 100nm, and 200nm silicon nitride membrane thickness. Custom membranes can be manufactured with silicon nitride film thickness ranging from 20nm up to several microns thick. Typically, very thin windows (<50nm) are compatible with small window area while thicker windows can be used with any window area, including large area windows. It should be noted that extremely thin windows must be handled very carefully due to their fragile nature. Window Area Standard DuraSiN™ products have square windows are available with edge length ranging from 500um to 5mm. Custom window areas can be manufactured with window area ranging from um to mm . The maximum window area is a function of the membrane thickness, and larger windows can produced from thicker nitride. Very small windows can also be manufactured, but, due to process constraints, these small windows may exhibit a larger window size variation among samples, for example 50um +/- 20um. Rectangular windows (sometimes known as "slot grids") with custom dimensions can also be produced. Frame Diameter Standard DuraSiN™ products have frame diameter ranging from 2.65mm to 10mm. Custom frame diameters can be manufactured with frame diameter ranging from 2.65mm to 10mm. Typically, larger window areas require a larger frame diameter. The minimum frame diameter than can be produced is the TEM size (2.65mm), presently offered through EMS along with 5mm and 10mm frame sizes. However, any size between 2.65mm and 15mm can be custom ordered. Technical Data Surface Roughness Surface roughness AFM data for 100nm thick DuraSiN™ films is shown below. The data was acquired from a 5µm 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 and 200nm films typically have an average surface roughness in the 3.0-angstrom range. DuraSiN™ products with 50nm films typically have a slightly larger average roughness than the 100nm and 200nm films. As determined by AFM, the 50nm DuraSiN™ films typically exhibit average surface roughness of about 1.2nm. 
Surface Flatness 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 there is a need to completely remove 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. Electron Transparency Monte Carlo simulations on models of 100nm thick DuraSiN™ films, under the presence of a 120 and 200keV 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 50nm to 200nm and because of the amorphous structure of the film, atomic-scale resolution has been obtained with DuraSiN™ products, depending on the exact specimens under evaluation. Chemical Robustness 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 generally quite rare. Because the films are in the nanometer thickness range, it is also 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. Temperature Robustness 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.
DuraSiN™ Film for TEM
DuraSiN™ Film for X-ray
DuraSiN™ Mesh for TEM
DuraSiN™ is a trademark of Protochips, Inc. All rights reserved |
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DuraSiN™ Film
and Mesh for TEM