Non-classical crystallization, in which charged nanoparticles (NPs) are the building blocks of film growth, has been extensively studied in chemical vapor deposition (CVD). Here, the deposition behavior of silicon oxide films by the two-step growth process, where NPs are generated in the gas phase at high temperature and deposited as films at low temperature, was studied in the CVD process. Although we supplied SiH4, H2, and N2, the deposited film turned out to be silicon oxide, which is attributed to relatively poor vacuum. Also, silicon oxide NPs were captured on transmission electron microscopy (TEM) carbon membranes of a copper grid for 10 s under various conditions. When the quartz tube with a conical nozzle was used, the size of nanoparticles increased drastically with increasing processing time (or delay time) and porous films with a rough surface were deposited. When the quartz tube without a nozzle was used, however, the size did not increase much with increasing processing time and dense films with a smooth surface were deposited. These results suggest that the size of nanoparticles is an important parameter for the deposition of dense films for two-step growth at low temperatures.
The possibility that charged nanoparticles (CNPs) are generated in the gas phase during direct current (DC) magnetron sputtering of Ag is studied. Sputtered Ag particles could be captured on an ultrathin amorphous carbon membrane for transmission electron microscopy (TEM) observation. It is confirmed that the average particle size and the total area of deposition under the condition of the positive bias applied to the substrate are bigger than those under the condition of the negative bias applied to the substrate. The results indicate that some of the sputtered Ag particles are negatively charged. To evaluate the contribution of negatively-charged particles to the film growth, Ag thin films were deposited for 30 min on the Si substrate with the substrate biases of −300, 0 and +300 V and analyzed by field-emission scanning electron microscopy (FESEM), X-ray diffraction (XRD) and four-point probe. When +300 V was applied to the substrate, the film growth rate was highest with the film thickness of 85.0 nm, the crystallinity was best with the smallest full width at half maximum (FWHM) value of 0.44 and the resistivity was smallest with 3.67 μΩ·cm. In contrast, when −300 V was applied to the substrate, the film growth rate was lowest with the film thickness of 68.9 nm, the crystallinity was worst with the largest FWHM value of 0.53 and the resistivity was largest with 8.87 μΩ·cm. This result indicates that the charge plays an important role in film growth and can be a new process parameter in sputtering.
Nanoparticles (NPs) in contact with each other observed in a transmission electron microscope (TEM) tend to undergo rapid coalescence. Similarly, isolated NPs show unstable fluctuations and changes in orientation due to active vibration and rotation; these behaviors are accompanied by a rapid diffusion of surface atoms and are likely related to the rapid coalescence of NPs, which has been widely attributed to bombardment by highenergy electrons. However, indirect experimental results have suggested that these phenomena are due to the built-up charge.Here, we used TEM to examine the behavior of gold NPs between insulating and conducting membranes to discern between electron bombardment and built-up charge effects. Our observations indicated that the rapid coalescence and active motion of NPs originate mainly from the built-up charge. This novel finding of charge-enhanced atomic diffusion in NPs helps clarify the mechanisms of many phenomena, such as the almost liquid-like rapid coalescence of NPs that produces smooth, single-crystalline nanowires. In contrast, NPs of the same size may show very sluggish coalescence, producing pearl-like chains, which may be attributed to the absence of charge.
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