The solid-state reaction and agglomeration of thin nickel-silicide films was investigated from sputter deposited nickel films ͑1-10 nm͒ on silicon-on-insulator ͑100͒ substrates. For typical anneals at a ramp rate of 3°C / s, 5-10 nm Ni films react with silicon and form NiSi, which agglomerates at 550-650°C, whereas films with a thickness of 3.7 nm of less were found to form an epitaxylike nickel-silicide layer. The resulting films show an increased thermal stability with a low electrical resistivity up to 800°C. © 2010 American Institute of Physics. ͓doi:10.1063/1.3384997͔Nickel-silicides are currently used as contacting materials in state-of-the-art microelectronic devices.1,2 Feature size has shrunk to a few tens of nanometers, and for nickel monosilicide ͑NiSi͒ layers, this results in a particularly severe tendency to agglomerate, 3 leading to a large increase in the electrical resistance of the contact, and an increased mobility of the nickel as it starts to move on the defects, both resulting in a low yield. Since the agglomeration of thin films is driven by a minimization of interface energy, it is expected that thinner films will agglomerate faster ͑i.e., have a lower agglomeration temperature͒. 4 In this letter, we show that this holds true only for films with a thickness of at least 5 nm ͑as-deposited thickness of the nickel layer͒, while for thinner layers the resulting nickel-silicide layer is much more resistant to agglomeration.Nickel films with a thickness between 1 and 10 nm were sputter deposited onto lightly p-doped ͑ =14-22 ⍀ cm͒, Radio Corporation of America ͑RCA͒ cleaned, and HF dipped silicon-on-insulator substrates, with a top layer of 117 nm of Si ͑100͒. The deposition chamber was first evacuated to 10 −4 Pa during deposition, the samples were mounted on a rotating carousel to ensure a uniform deposition thickness. An argon pressure of 0.5 Pa and a sputtering power of 100 W were used, resulting in a deposition rate of 0.04 nm/s. After deposition, the samples were annealed in a high-purity He atmosphere, from 100 to 850°C at a rate of 3°C / s, and the surface roughness ͑using laser light scattering, recording the intensity of nonspecular reflection of the laser light͒, and the sheet resistance ͑using a four point probe͒ were recorded in situ. The thickness of both the as-deposited and annealed films was determined using x-ray reflectivity and cross section transmission electron microscopy, resulting in the reported thicknesses with a precision of Ϯ0.2 nm.An overview of the in situ sheet-resistance is shown in Fig. 1. All of the samples with more than 3.7 nm of nickel ͑6, 8, and 10 nm are shown͒, exhibit a sheet resistance qualitatively similar to what was previously reported 5 for 10 nm layers of nickel on Si ͑100͒; a complex phase sequence of high-resistive metal rich nickel-silicides at low temperatures, and the formation of the low-resistive NiSi phase at 400-450°C. This layer then agglomerates at 550-650°C, leading to the observed increase in sheet resistance. In contrast, for the thinn...
We studied the effects of preconceptional exposure to multiwalled carbon nanotubes (MWCNTs): mature, female C57BL/6J mice were intratracheally instilled with 67μg NM-400 MWCNT, and the following day co-housed with mature males, in breeding pairs. Time to delivery of the first litter, litter parameters, maternal inflammation and histopathology of lung and liver were recorded. In male offspring, locomotor activity, startle response, and daily sperm production (DSP) were assessed. In the dams, lung and liver bore evidence of MWCNT exposure when assessed 6 weeks and 4 months after exposure. A short delay in the delivery of the first litter was observed in exposed females. Litter parameters, behavior and DSP were similar in control and exposed groups. In conclusion, instillation of a single dose of MWCNT induced long lasting pathological changes in dam lung and liver. Theoretically, lung inflammation due to particle exposure could interfere with female reproductive parameters. Whether the observed lag in delivery of a first litter was in fact caused by exposure to MWCNT should be addressed in a study designed specifically to elucidate effects on the early processes involved in establishment of pregnancy. Exposure was not associated with changes in the assessed gestational or offspring parameters.
E171 (titanium dioxide) is a food additive that has been authorized for use as a food colorant in the European Union. The application of E171 in food has become an issue of debate, since there are indications that it may alter the intestinal barrier. This work applied standardized and validated methodologies to characterize representative samples of 15 pristine E171 materials based on transmission electron microscopy (TEM) and single-particle inductively coupled plasma mass spectrometry (spICP-MS). The evaluation of selected sample preparation protocols allowed identifying and optimizing the critical factors that determine the measurement of the particle size distribution by TEM. By combining optimized sample preparation with method validation, a significant variation in the particle size and shape distributions, the crystallographic structure (rutile versus anatase), and the physicochemical form (pearlescent pigments versus anatase and rutile E171) was demonstrated among the representative samples. These results are important for risk assessment of the E171 food additive and can contribute to the implementation of the European Food Safety Authority (EFSA) guidance on risk assessment of the application of nanoscience and nanotechnologies in the food and feed chain.
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