Bingjun Yu

Friction-induced nanofabrication on monocrystalline silicon

Fabrication of nanostructures has become a major concern as the scaling of device dimensions continues. In this paper, a friction-induced nanofabrication method is proposed to fabricate protrusive nanostructures on silicon. Without applying any voltage, the nanofabrication is completed by sliding an AFM diamond tip on a sample surface under a given normal load. Nanostructured patterns, such as linear nanostructures, nanodots or nanowords, can be fabricated on the target surface. The height of these nanostructures increases rapidly at first and then levels off with the increasing normal load or number of scratching cycles. TEM analyses suggest that the friction-induced hillock is composed of silicon oxide, amorphous silicon and deformed silicon structures. Compared to the tribochemical reaction, the amorphization and crystal defects induced by the mechanical interaction may have played a dominating role in the formation of the hillocks. Similar to other proximal probe methods, the proposed method enables fabrication at specified locations and facilitates measuring the dimensions of nanostructures with high precision. It is highlighted that the fabrication can also be realized on electrical insulators or oxide surfaces, such as quartz and glass. Therefore, the friction-induced method points out a new route in fabricating nanostructures on demand.

Towards a deeper understanding of the formation of friction-induced hillocks on monocrystalline silicon

Friction-induced hillocks can be produced on monocrystalline silicon by scratching under given conditions. Results show that the height of these hillocks increases with the applied normal load or number of scratching cycles, but decreases with the sliding velocity. Transmission electron microscope (TEM) and energy dispersive x-ray (EDX) analysis show that the hillock contains a thin superficial oxidation layer and a thick disturbed (amorphous and deformed) layer in the subsurface. Although the formation of the silicon hillock is the combined results of mechanical interaction and tribochemical reaction, the mechanical interaction plays a more dominant role. Further analysis indicates that the formation of hillock is mostly induced by the amorphization of crystal silicon during scratching. Low sliding speed is found to facilitate the formation of a thick amorphization layer under the same loading condition. Since the friction-induced hillock is the initial surface damage on the nanoscale, the results will shed new light on understanding and controlling the nanowear process of silicon in micro/nanoelectromechanical systems.

Fabrication mechanism of friction-induced selective etching on Si(100) surface.

As a maskless nanofabrication technique, friction-induced selective etching can easily produce nanopatterns on a Si(100) surface. Experimental results indicated that the height of the nanopatterns increased with the KOH etching time, while their width increased with the scratching load. It has also found that a contact pressure of 6.3 GPa is enough to fabricate a mask layer on the Si(100) surface. To understand the mechanism involved, the cross-sectional microstructure of a scratched area was examined, and the mask ability of the tip-disturbed silicon layer was studied. Transmission electron microscope observation and scanning Auger nanoprobe analysis suggested that the scratched area was covered by a thin superficial oxidation layer followed by a thick distorted (amorphous and deformed) layer in the subsurface. After the surface oxidation layer was removed by HF etching, the residual amorphous and deformed silicon layer on the scratched area can still serve as an etching mask in KOH solution. The results may help to develop a low-destructive, low-cost, and flexible nanofabrication technique suitable for machining of micro-mold and prototype fabrication in micro-systems.

Effect of surface hydrophilicity on the nanofretting behavior of Si(100) in atmosphere and vacuum

With an atomic force microscopy, the effect of surface hydrophilicity on the nanofretting behavior of Si(100) against SiO2 microsphere was investigated under vacuum and atmosphere conditions, respectively. The surface hydrophilicity revealed a strong effect on the motion behavior, adhesion force, friction force, and nanofretting damage of Si(100)/SiO2 pairs. The increase in the hydrophilicity of Si(100) surface could expand the stick regime of Si(100)/SiO2 pairs into a higher value of displacement amplitude. While the nanofretting ran in atmosphere, both adhesion and friction forces in the initial cycle would be larger when the Si(100) surface was more hydrophilic. However, because of the in situ chemical modification of SiO2 tip in nanofretting, they might reveal a decrease with increasing nanofretting cycles. Either in vacuum or in atmosphere, the nanofretting damage was weaker when the Si(100) surface was more hydrophobic. Because of the lack of oxygen and vapor in vacuum, the nanofretting damage on th...

Nondestructive nanofabrication on Si(100) surface by tribochemistry-induced selective etching

A tribochemistry-induced selective etching approach is proposed for the first time to produce silicon nanostructures without lattice damage. With a ~1 nm thick SiOx film as etching mask grown on Si(100) surface (Si(100)/SiOx) by wet-oxidation technique, nano-trenches can be produced through the removal of local SiOx mask by a SiO2 tip in humid air and the post-etching of the exposed Si in potassium hydroxide (KOH) solution. The material removal of SiOx mask and Si under low load is dominated by the tribochemical reaction at the interface between SiO2 tip and Si/SiOx sample, where the contact pressure is much lower than the critical pressure for initial yield of Si. High resolution transmission electron microscope (HRTEM) observation indicates that neither the material removal induced by tribochemical reaction nor the wet etching in KOH solution leads to lattice damage of the fabricated nanostructures. The proposed approach points out a new route in nondestructive nanofabrication.

Maskless and low-destructive nanofabrication on quartz by friction-induced selective etching.

A low-destructive friction-induced nanofabrication method is proposed to produce three-dimensional nanostructures on a quartz surface. Without any template, nanofabrication can be achieved by low-destructive scanning on a target area and post-etching in a KOH solution. Various nanostructures, such as slopes, hierarchical stages and chessboard-like patterns, can be fabricated on the quartz surface. Although the rise of etching temperature can improve fabrication efficiency, fabrication depth is dependent only upon contact pressure and scanning cycles. With the increase of contact pressure during scanning, selective etching thickness of the scanned area increases from 0 to 2.9 nm before the yield of the quartz surface and then tends to stabilise after the appearance of a wear. Refabrication on existing nanostructures can be realised to produce deeper structures on the quartz surface. Based on Arrhenius fitting of the etching rate and transmission electron microscopy characterization of the nanostructure, fabrication mechanism could be attributed to the selective etching of the friction-induced amorphous layer on the quartz surface. As a maskless and low-destructive technique, the proposed friction-induced method will open up new possibilities for further nanofabrication.

Effect of crystal plane orientation on the friction-induced nanofabrication on monocrystalline silicon

Although monocrystalline silicon reveals strong anisotropic properties on various crystal planes, the friction-induced nanofabrication can be successfully realized on Si(100), Si(110), and Si(111) surfaces. Under the same loading condition, the friction-induced hillock produced on Si(100) surface is the highest, while that produced on Si(111) surface is the lowest. The formation mechanism of hillocks on various silicon crystal planes can be ascribed to the structural deformation of crystal matrix during nanoscratching. The silicon crystal plane with lower elastic modulus can lead to larger pressed volume during sliding, facilitating more deformation in silicon matrix and higher hillock. Meanwhile, the structures of Si-Si bonds on various silicon crystal planes show a strong effect on the hillock formation. High density of dangling bonds can cause much instability of silicon surface during tip disturbing, which results in the formation of more amorphous silicon and high hillock during the friction process. The results will shed new light on nanofabrication of monocrystalline silicon.

Nanofabrication on monocrystalline silicon through friction-induced selective etching of Si3N4 mask

A new fabrication method is proposed to produce nanostructures on monocrystalline silicon based on the friction-induced selective etching of its Si3N4 mask. With low-pressure chemical vapor deposition (LPCVD) Si3N4 film as etching mask on Si(100) surface, the fabrication can be realized by nanoscratching on the Si3N4 mask and post-etching in hydrofluoric acid (HF) and potassium hydroxide (KOH) solution in sequence. Scanning Auger nanoprobe analysis indicated that the HF solution could selectively etch the scratched Si3N4 mask and then provide the gap for post-etching of silicon substrate in KOH solution. Experimental results suggested that the fabrication depth increased with the increase of the scratching load or KOH etching period. Because of the excellent masking ability of the Si3N4 film, the maximum fabrication depth of nanostructure on silicon can reach several microns. Compared to the traditional friction-induced selective etching technique, the present method can fabricate structures with lesser damage and deeper depths. Since the proposed method has been demonstrated to be a less destructive and flexible way to fabricate a large-area texture structure, it will provide new opportunities for Si-based nanofabrication.

Maskless micro/nanofabrication on GaAs surface by friction-induced selective etching

In the present study, a friction-induced selective etching method was developed to produce nanostructures on GaAs surface. Without any resist mask, the nanofabrication can be achieved by scratching and post-etching in sulfuric acid solution. The effects of the applied normal load and etching period on the formation of the nanostructure were studied. Results showed that the height of the nanostructure increased with the normal load or the etching period. XPS and Raman detection demonstrated that residual compressive stress and lattice densification were probably the main reason for selective etching, which eventually led to the protrusive nanostructures from the scratched area on the GaAs surface. Through a homemade multi-probe instrument, the capability of this fabrication method was demonstrated by producing various nanostructures on the GaAs surface, such as linear array, intersecting parallel, surface mesas, and special letters. In summary, the proposed method provided a straightforward and more maneuverable micro/nanofabrication method on the GaAs surface.

Investigation of silicon wear against non-porous and micro-porous SiO2 spheres in water and in humid air

Tribochemical wear, a method to achieve controlled material removal without residual damage on substrates, plays a very important role in super-smooth silicon surface manufacturing. By using non-porous SiO2 spheres and micro-porous SiO2 spheres, the wear of silicon substrates was comparatively investigated in DI water, humid air (50% RH) and dry air. The wear behaviors presented entirely different cases at the same load in DI water and humid air: (a) less material removal of silicon against non-porous SiO2 spheres than micro-porous SiO2 spheres in water and (b) more serious wear of silicon substrate against non-porous SiO2 spheres in humid air. When the wear tests were operated in dry air, no obvious damage was incurred on the silicon surface against the non-porous SiO2 spheres but slight wear was observed against micro-porous SiO2 spheres under the given conditions. Raman results revealed that a hydrolysis reaction was involved in the tribochemical wear of the silicon substrate and the micro pores in SiO2 spheres could accelerate this process. The corresponding analysis suggests an exponential dependence of wear rate on contact stress, which is consistent with the stress-assisted chemical kinetics model. Although with much lower elastic modulus, micro-porous SiO2 spheres caused a larger wear rate of silicon substrate than non-porous SiO2 spheres at the same contact pressure both in water and humid air. The results indicate that the micro-porous SiO2 spheres can promote the tribochemical reaction due to the storage of water molecules in micro pores.