Product Overview

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. 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 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.

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

 

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 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 make the grids well suited for high temperature deposition steps.

Publications using DuraSiN

Iron assisted growth of copper-tipped multi-walled carbon nanotubes.
Nanotechnology, Volume 18, Number 49, p. 495602, December 2007.
Z. R. Abrams, D. Szwarcman, Y. Lereah, G. Marovich, and Y. Hanein

A Complete Scheme for Creating Predefined Networks of Individual Carbon Nanotubes.
Nano Letters Volume 7, Issue 9, pp. 2666 -2671, 2007.
Z. R. Abrams, Z. Ioffe, A. Tsukernik, O. Cheshnovsky, and Y. Hanein

Characteristics of solid-state nanometre pores fabricated using a transmission electron microscope.
Nanotechnology, Volume 18, Number 20, p. 205302, May 2007.
M. J. Kim, B. McNally, K. Murata, A. Meller

Radial deformation measurements of isolated pairs of single-walled carbon nanotubes.
Carbon, Volume 45, Issue 4, pp. 738-743, April 2007.
Z.R. Abrams and Y. Hanein.

Scanning Transmission Electron Microscopy of Biological Specimens in Water.
Microscopy and Microanalysis. Volume 13, Supplement S02, pp. 242-243, 2007.
N. de Jonge, D.B. Peckys, G.M. Veith, S. Mick, S. Pennycook and D. Joy.

Chemically Modified Solid-State Nanopores.
Nano Letters, Volume 7, Number 6, pp. 1580-1585, 2007.
M. Wanunu and A. Meller

Transmission electron microscope imaging of single-walled carbon nanotube interactions and mechanics on nitride grids.
Nanotechnology, Volume 17, Number 18, pp.4706-4712, September 2006.
Z. R. Abrams, Y. Lereah and Y. Hanein

Rapid Fabrication of Uniformly Sized Nanopores and Nanopore Arrays for Parallel DNA Analysis.
Advanced Materials, Volume 18, Issue 23, pp. 3149 - 3153, 2006.
M. J. Kim, M. Wanunu, D. C. Bell, and A. Meller

Tube-Tube and Tube-Surface Interactions in Straight Suspended Carbon Nanotube Structures.
Journal of Physical Chemistry B, Volume 110, Number 43, pp. 21419-21423, 2006.
Z.R. Abrams and Y. Hanein

Growth and Characterization of Self-assembled Nanofibers.
Microscopy and Microanalysis, Volume 11, Supplement S02, pp. 372-373, 2005.
M.E. Salmon, P.E. Russell and E.B. Troughton

 

DuraSiN™ is a trademark of Protochips, Inc. All rights reserved