Challenges for Metrology and Nanotechnology Donald R. Baer, Pacific Northwest National Laboratory Opportunity and Challenge - Although some areas of nanotechnology, such as the semiconductor industry, have current and well defined near term measurement needs, many areas of nanotechnology, and the related metrology needs, are much less developed. At a 2001 National Academy of Science Arthur Sackler Colloquium on Nanoscience, George Whitesides observed that those of us doing nanoscience don’t really know what it is and we certainly don’t know what nanotechnology is. My understanding is that this statement is not an expression of pessimism but a statement of the nearly unlimited potential for scientific and technological impact. The impacts may be incremental at first, but dramatic and revolutionary changes will occur. At this time it is not possible to clearly identify the long term instrumental and metrological needs. None the less, it is essential to begin to establish the framework and approach to meet long term needs and to address areas identified as important. Nomenclature - NASA’s Dr. Meyyappan, Director of the Center for Nanotechnology, Ames Research Center, says that nanotechnology is like ice cream, it comes in many flavors. This seemingly simple statement has very significant implications. There are many different things that we call nanoscience and nanotechnology for a variety of different reasons. These cover different disciplines and a wide variety of technologies as well as different physical, chemical, and biological phenomena. As stated by Prof. Alexandra Navrotsky in the book Nanoparticles and the Environment,1 a “consistent nomenclature” is needed. Well thought out terminology is an essential element for identification and clarification of the concepts associated with nanoscience and nanotechnology. It is also a critical component in the development of accurate, reproducible and meaningful metrology. Most ASTM (American Society for Testing and Materials) and ISO (International Organization for Standards) activities start with efforts to define the critical terms.2 Nanoparticle Characterization – Challenges with accurate and useful characterization of nanoparticles highlight a few topics of importance. Several different methods are used to measure and report the size and size distribution of nanoparticles. Well defined and generally accepted standard methods will be essential if nanoparticles are to be widely used and distributed as “industrial” materials, particularly for size dependent applications. However, the information needs for nanoparticles do not even begin to be satisfied by knowing the size. At a September 2003 Nanoparticles and the Environment workshop, Bob Hwang, director of the Center for Functional Nanomaterials (CFN) at Brookhaven National Laboratory noted that the nature and properties of nanoparticles require a multidimensional analysis because the properties can vary with time and size. Jill Banfield’s research group3 has observed that the structure of nanoparticles( depend upon the environment. Any useful reporting of nanoparticle properties must include information related to production process, time after production, environmental conditions and handling history. There are also complications associated with the collection of nanoparticles for analysis or storage and the movement or transport of nanoparticles from one environment to another for analysis (or use) without contamination or unwanted alteration. Descriptions of the structure and composition of nanoparticles are no less challenging than measurements of size. Although traditional measurements of structure such as transmission electron microscopy (TEM) and x-ray diffraction (XRD) are critically important, it appears that they do not always provide an adequate picture of the detailed structures of nanoparticles. Synchrotron based small angle scattering measurements provide an indication of structure not apparent in the TEM or XRD data. Contamination and surface structure will play a major role for chemical applications of nanoparticles and our ability to accurately obtain such information on very small particle surfaces is very limited. For nano-structured materials, it may be essential to interactively combine multiple types of data to enhance the information obtained. For example, X-ray Photoelectron Spectroscopy (XPS) can be used to obtain information about the elemental distribution of contaminants on nanoparticles when information about the particle size is known from other methods. Such combined approaches to data collection and analysis are not well know, not well tested and not widely applied. Distributions, Statistics and other Challenges - It will ultimately be both unfeasible and undesirable to characterize each nano-component of any system or assembly. However, as already noted for nanoparticles, it is essential to have an accurate sense of the structure and size distribution of the components of nano-structured materials. This is an immediate issue for current and near future generations of integrated circuits. The importance of variations in geometry and time sensitive response can be demonstrated by single molecule Raman data collected by H. Peter Lu’s group.4 Time resolved single molecule spectra show a significant variation with time. The relative magnitudes of various spectral components reflect many factors including flexing of the molecular structure. Although the time averaged signal is identical to the spectrum of bulk material, a series of time resolved single molecule spectra contain significant additional information. In some situations it may be that the statistical distribution of data as collected can be analyzed to provide information about the distributions, sizes, motions and even function of nano-structured materials. In most cases nano-sized components will need to be integrated into larger meso- to macro-sized systems. There are significant challenges in designing, assembling (including registry and electrical contacts) and verifying the nature of the structures achieved. In addition to contamination issues, there are issues related to the stability of nano-structures when exposed to photon or particle irradiation. Methods of confirming the robustness of the final material and functional properties will need to be developed. 1 Nanoparticles and the Environment, Reviews in Mineralogy and Geochemistry 44, ed J. Banfield and A. Navrosky, Mineralogical Society of America 2001. 2 ISO TC 201 on Surface Chemistry is initiating a subcommittee on Scanning Probe Microscopy that will be involved with terminology and standards relevant to nanoscience and nanotechnology. 3 HENGZHONG ZHANG*, BENJAMIN GILBERT*, FENG HUANG & JILLIAN F. BANFIELD Nature 424, 1025 - 1029 (28 August 2003); 4 Yung Doug Suh, Gregory K. Schenter, Leyun Zhu, H. Peter Lu, Ultramicroscopy 97 (2003) 89–102