This study is based on the film growth by non-classical crystallization, where charged nanoparticles (NPs) are the building block of film deposition. Extensive studies about the generation of charged NPs and their contribution to film deposition have been made in the chemical vapor deposition (CVD) process. However, only a few studies have been made in the physical vapor deposition (PVD) process. Here, the possibility for Ti films to grow by charged Ti NPs was studied during radio frequency (RF) sputtering using Ti target. After the generation of charged Ti NPs was confirmed, their influence on the film quality was investigated. Charged Ti NPs were captured on amorphous carbon membranes with the electric bias of −70 V, 0 V, +5 V, +15 V and +30 V and examined by transmission electron microscopy (TEM). The number density of the Ti NPs decreased with increasing positive bias, which showed that some of Ti NPs were positively charged and repelled by the positively biased TEM membrane. Ti films were deposited on Si substrates with the bias of −70 V, 0 V and +30 V and analyzed by TEM, field-emission scanning electron microscopy (FESEM), X-ray diffraction (XRD) and X-ray reflectivity (XRR). The film deposited at −70 V had the highest thickness of 180 nm, calculated density of 4.974 g/cm3 and crystallinity, whereas the film deposited at +30 V had the lowest thickness of 92 nm, calculated density of 3.499 g/cm3 and crystallinity. This was attributed to the attraction of positively charged Ti NPs to the substrate at −70 V and to the landing of only small-sized neutral Ti NPs on the substrate at +30 V. These results indicate that the control of charged NPs is necessary to obtain a high quality thin film at room temperature.
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.
Non-classical crystallization suggests that crystals can grow with nanoparticles as a building block. In this case, the crystallization behavior depends on the size and charge of the nanoparticles. If charged nanoparticles (CNPs) are small enough, they become liquid-like and tend to undergo epitaxial recrystallization. Here, the size effect of SiC CNPs on film crystallinity was studied in the hot-wire chemical vapor deposition process. To do this, SiC nanoparticles were captured under different processing conditions—in this case, wire temperature, precursor concentration and the filament bias. Increasing the temperature of tungsten wires and decreasing the ratio of (SiH4 + CH4)/H2 reduced the size of the SiC nanoparticles. When the nanoparticles were small enough, an epitaxial SiC film approximately 100-nm-thick was grown, whereas larger nanoparticles produced polycrystalline SiC films. These results suggest that the size of the CNPs is an important process variable when growing films by means of non-classical crystallization.
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