David D. Allred received Alumni Professorship Award

Abstract: We investigated the correlation between growth efficiency and structural parameters of single-walled carbon nanotube (SWCNT) forests and report the existence of a SWCNT “sweet spot” in the CNT diameter and spacing domain for highly efficient synthesis. Only within this region could SWCNTs be grown efficiently. Through the investigation of the growth rates for ~340 CNT forests spanning diameters from 1.3 to 8.0 nm and average spacing from 5 to 80 nm, this “sweet spot” was found to exist because highly efficient growth was constrained by several mechanistic boundaries that either hindered the formation or reduced the growth rate of SWCNT forests. Specifically, with increased diameter SWCNTs transitioned to multiwalled CNTs (multiwall border), small diameter SWCNTs could only be grown at low growth rates (low efficiency border), sparse SWCNTs lacked the requirements to vertically align (lateral growth border), and high density catalysts could not be prepared (high catalyst density border). As a result, the SWCNTs synthesized within this “sweet spot” possessed a unique set of characteristics vital for the development applications, such as large diameter, long, aligned, defective, and high specific surface area.

Abstract: High-aspect-ratio metallic microstructures have a variety of potential applications in sensing and actuation. However, fabrication remains a challenge. We have fabricated nickel microstructures with over 20:1 aspect ratios by electroplating patterned carbon-coated carbon-nanotube forests using a nickel chloride bath. Pulse plating allows nickel ions to diffuse into the interior of the forest during off portions of the cycle. Done properly, this solves the problem of the formation of an external crust, which otherwise blocks nickel deposition in the interior of the structures. Thus, densities of 86 ± 3% of bulk Ni for the composite structures are achieved. Cantilever structures do not yield under load, but break. Measurements of the material properties of this composite material indicate an elastic modulus of ~42 GPa and a strength of 400 MPa. We demonstrate the utility of this method with an external field magnetic actuator consisting of a proof mass and two flexures. We achieved 1-mN actuation forces. [2014-0274]

Abstract: We report an inverse relationship between the carbon nanotube (CNT) growth rate and catalyst lifetime by investigating the dependence of growth kinetics for ~330 CNT forests on carbon feedstock, carbon concentration, and growth temperature. We found that increased growth temperature led increased CNT growth rate and shortened catalyst lifetime for all carbon feedstocks, following an inverse relationship of fairly constant maximum height. For increased carbon concentration, the carbon feedstocks fell into two groups where ethylene/butane showed increased/decreased growth rate and decreased/increased lifetime indicating different rate-limiting growth processes. In addition, this inverse relationship held true for different types of CNTs synthesized by varied chemical vapor deposition techniques and continuously spanned 1000-times range in both growth rate and catalyst lifetime, indicating the generality and fundamental nature of this behavior originating from the growth mechanism of CNTs itself. These results suggest it would be fundamentally difficult to achieve a fast growth with long lifetime.

Abstract: Carbon nanotubes (CNTs) can be grown in dense lithographically patterned forests to form framework structures that can be filled in via chemical vapor deposition to form solid structures. These solid structures can then be used in microelectromechanical systems (MEMS) applications. Initial testing with these structures suggests that when these frameworks are filled with carbon, the resulting material exhibits favorable properties for use in compliant MEMS. To better understand this material's properties, we conducted tests to measure its Young's modulus, failure stress, and stress relaxation in the direction perpendicular to the CNT growth, as well as the modulus and stress in the direction parallel to the CNTs. To determine the properties in the transverse direction, we applied vertical loads to the tips of simple cantilever beam samples, and recorded the force and deflection until failure. The results showed failure strain up to 2.48%. Cantilever samples prepared from the same pattern were also used to measure the stress relaxation of the material. The first test for each sample showed an average force relaxation of 3.72%, while successive tests only produced 1.23% after 24 h. To determine the properties in the direction parallel to the CNTs, we prepared simple rectangular beams and subjected them to 3-point bending tests. The average strain calculated in the parallel direction was 8.17%.

Abstract: Conventional magnetic tape is the most widely used medium for archival data storage. However, data stored on it need to be migrated every ca. 5 years. Recently, optical discs that store information for hundreds, or even more than 1000 years, have been introduced to the market. We recently proposed that technology in these optical discs be used to make an optical tape that would show greater permanence than its magnetic counterpart. Here we provide a detailed optical characterization of a sputtered thin film of bismuth, tellurium, and selenium (BTS) that is a proposed data storage layer for these devices. The methodology described herein should be useful in the future development of related materials. Spectroscopic ellipsometry (SE) data are obtained using interference enhancement, and the modeling of this data is guided by results from atomic force microscopy (AFM), scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray reflectivity (XRR). By AFM, ca. 40 nm BTS films show ca. 10 nm roughness. SEM images also suggest considerable roughness in the films and indicate that they are composed of 13.1 ± 5.9 nm grains. XRD confirms that the films are crystalline and predicts a grain size of 17 ± 2 nm. XRD results are consistent with the composition of the films – a mildly oxidized BTS material. Three models of increasing complexity are investigated to explain the SE data. The first model consists of a smooth, homogeneous BTS film. The second model adds a roughness layer to the previous model. The third model also has two layers. The bottom layer is modeled as a mixture of BTS and void using a Bruggeman effective medium approximation. The upper layer is similarly modeled, but with a gradient. The first model was unable to adequately model the SE data. The second model was an improvement – lower MSE (4.4) and good agreement with step height measurements. The third model was even better – very low MSE (2.6) and good agreement with AFM results. The third SE model predicted ca. 90% void at the film surface. XRR modeling of the film agreed well with the predictions from SE. The uniquenesses of the SE models were confirmed.

Abstract: Most data today, including pictures, videos, documents, technical data, etc., is stored digitally. Much of this information is of great importance both to individuals, e.g., pictures and video, and to governmental organizations and corporations, e.g., documents and technical data. Unfortunately, almost all of the data storage options available today show high degrees of volatility – they are for the most part ephemeral, lasting in general only a few years to about a decade.1 Our group has been actively working in this area to develop new materials and data storage options that will offer greater permanence. In particular, we have recently been developing permanent solid-state storage devices that use nanofuses as the basic storage elements. Clearly, to be competitive with current data storage densities, features sizes will need to be around those in current Flash technology. Accordingly, tools are need for prototyping at these dimensions. Here we will present electron beam lithography as an effective patterning/prototyping tool for this kind of work, and then describe its use in the fabrication of contact pads and carbon nanofuses for permanent solid-state storage devices.