As materials science researchers look to drive new product innovations, they inspire—and are aided by—sophisticated analytical and imaging instruments.
The nanoIR from Anasys Instruments combines atomic force microscopy (AFM) and infrared spectroscopy to enable materials scientists to study the morphology and chemical composition of complex samples with spatial resolution below 100 nm. The instrument provides high-resolution AFM images and an infrared absorption spectrum from any point on the sample. The nanoIR includes a pulsed, tunable infrared laser that illuminates the sample; the tip of the AFM is used to detect rapid thermal expansion resulting from any absorbed infrared light. By measuring the AFM tip response as a function of the laser wavelength, the nanoIR creates IR absorption spectra with less than 100 nm spatial resolution. The nanoIR platform can perform complementary nanoscale mapping of mechanical and thermal properties of a sample.
Materials research scientists are exploring a range of disciplines, including tribology, corrosion prevention, and biotechnology. However, the most prevalent sector is nanomaterials.
“Nanostructured materials are being actively used in materials like polymer composites, coatings, and multilayer films and novel structures and novel nanoscale characterization techniques are being extensively studied for detection and treatment of disease,” says Craig Prater, CTO, Anasys Instruments.
Solar cells and batteries are another area of interest. “In both cases, the nanostructure of the material has a crucial impact on the function and efficiency of the material, and describing nanometer-size structures is one of the applications of SAXS,” says Gerd Langenbucher, sales manager SAXSess, Anton Paar USA Inc., Ashland, Va.
Anton Paar’s Small-Angle X-ray Scattering (SAXS) method allows users to obtain information about the morphology of a variety of materials, from proteins, nutrients, and active pharmaceuticals to polymers, fibers, paints, and catalysts. The method provides a precise understanding of the inner arrangements of super-molecular structures ranging from 1 to 200 nm. This helps researchers to elucidate the material’s properties on the macroscopic scale.
Nanoscale characterization techniques also are being studied for the detection and treatment of disease. Jeremy Warren, CEO, NanoSight, Salisbury, U.K., says, “The nanotechnology world is trending strongly to ‘warm and wet’, meaning bio-nano and life sciences, as opposed to the cold and hard world of inorganic chemistry.”
Hybrid biomaterials or nanomaterials based on biological systems have become of particular interest to the life sciences industry, to mimic nature to produce stronger, more durable materials, or to incorporate nanomaterials into biological frameworks for drug delivery or medical research.
Bruker’s Nano Surfaces Division designs optical and stylus products for 3D topography measurements down to sub-nanometer vertical and sub-micron lateral scales. Surface measurements characterize a variety of critical material properties and examine stress, surface roughness, shape changes, crack propagation, wear, and corrosion. Advanced analyses allow identification of key features such as cracks, pits, crystal boundaries, or steps. Depth, lateral dimensions, volumes, and a wide variety of roughness-related parameters can be calculated for rapid, automated quantification of key characteristics. New measurement techniques, such as the AcuityXR measurement mode (a 2011 R&D 100 Award winner), allow features as small as 120 nm to be accurately measured. This allows a single system to measure lateral features spanning 5 orders of magnitude (100 nm to 10 mm) and vertical featureorders of magnitude (0.1 nm to 10 mm).
Drug delivery particles are coming of age and beginning to fulfill their promise of targeted and controlled dosimetry and disease specificity, explains Nanosight‘s Warren.
Regulatory agencies spell out standards for new materials for medical devices and implants, creating a long, costly lag time between identification of a new material and adoption in products for human use. Similar regulations apply to drug delivery and drug development.
“As therapeutic drugs tend increasingly to deliver as suspensions, aggregation of nanoparticles is a big issue. Nanoparticles are inherently sticky anyway, but this is especially so with protein suspensions,” Warren says. “Both academics and the FDA (Food and Drug Administration) share concerns about changes to immunogenicity as protein-based therapeutics aggregate.”
Prater says one of the key roadblocks for new material developments has been the lack of nanoscale material properties characterization tools for material scientists.
Tailoring chemical composition at the nanoscale is crucial to achieving the material properties.
The imaging and analytical technology advances include modular characterization systems, which means that more accessories can fit a base setup and hence offer the scientist various different aspect to approach a research topic,” says Anton Paar’s, Langenbucher.
“If you can’t measure size you can’t control it,” says Warren. For many years, electron microscopy (EM) and dynamic light scattering (DLS) were the only techniques used for characterization of materials in the range of 10 to 1,000 nm. Electron microscopy, despite its resolving power, is difficult to employ to provide statistically useful particle size distributions. Dynamic light scattering, while it is a fast and reliable technique, struggles when faced with a wide distribution of sizes, explains Warren. “Of course there is no silver bullet to nanoparticle characterization,” says Warren, “but Nanoparticle Tracking Analysis (NTA), when used in parallel with EM or DLS techniques, provides the missing insight into complexity through particle-by-particle analysis.”
NanoSight’s Nanoparticle Tracking Analysis (NTA) detects and visualizes populations of nanoparticles in liquids down to 10 nm, dependent on material, and measures the size of each particle from direct observations of diffusion. This particle-by-particle methodology goes beyond traditional light scattering and other ensemble techniques in providing high-resolution particle size distributions. Additionally, NanoSight measures concentration and validates data with information-rich video files of the particles moving under Brownian motion. A fluorescence mode provides differentiation of suitably labeled particles. Real-time monitoring of the subtle changes in the characteristics of particle populations with all of these analyses are confirmed by visual validation. The NanoSight NS500 Instrument (above) provides a reproducible platform for specific and general nanoparticle characterization.
“We are constantly modifying and enhancing our instrumentation to keep up with the pace of the nanoscale research,” says JEOL’s Erdman. “We are offering a full suite of instruments to address any characterization needs.”
Instrument technology development will heavily influence materials science in the future, many vendors report. Thesen sees low-voltage transmission electron microscopes used for the investigation of beam-sensitive, low-z materials as becoming more and more effective, opening up new possibilities in the optimization of materials characteristics. He believes correlative light and electron microscopy will speed up development processes.
“Energy-efficient materials and their commercialization will be a ‘hot’ topic in the next few years. Biomaterials as well as materials for disease diagnostics and drug delivery will continue to be important research areas,” Erdman says. “There will be additional focus on multi-disciplinary approaches to solving materials problems, essentially pulling expertise from various fields in addition to traditional materials science to design ‘smart’ materials.”
Predicting the future is not easy, says Martin, since the materials science field is so broad and there are so many avenues in which it can progress.
“Obviously, with the amount of money being spent on photovoltaics, we can expect progress in that field,” he says. “And in Asia, many governments are aggressively funding research into biotechnology and biomaterials. We have already seen a number of developments in that field and will see many more in the years to come.”
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