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Mechanical properties, i.e. hardness and elastic modulus, of amorphous SiO2 and Si3N4 PE-CVD coatings have been studied for two coating thicknesses (0.1 and 1.0 µm) and two substrate materials (fused silica, i.e. Herasil, and borosilicate glass, i.e., BK7) using low load instrumented indentation. The coating systems are being considered for possible use as reference materials for thin film mechanical property test methods. Single layers of SiO2 and Si3N4 and a multilayer stack consisting of five double layers of SiO2/Si3N4 (individual layer thickness: 0.1 µm) were investigated on both substrate materials. A special plasma pre-treatment of the substrates prior to deposition ensured that coating adhesion exceeded inner film stress for all systems considered. The applied indentation load ranged from 700 down to 0.1 mN and resulted in indentation depths from more than 1 µm to about 15 nm. The influence of coating thickness and the effect of the substrate on the measurement of hardness and elastic modulus of the films are discussed, with emphasis on the effects of indentation depth vs. coating thickness on the observed coating properties. One coatingsubstrate system (1.0 µm Si3N4 on Herasil) out of ten was found to be above a critical threshold for tensile cracking of the coating. In this system, termed overcritical, tensile cracks occurred both prior to, and as a result of, indentation, indicating that Berkovich indentation may also be used to probe residual film stress.
The removal of a 75- to 90-nm-thick passivating silicon nitride antireflection coating from standard textured multicrystalline silicon photovoltaic wafers with a typical diffused 90-Ω/sq-emitter upon irradiation with near-infrared femtosecond laser pulses (790 nm central wavelength, 30 fs pulse duration) is studied experimentally. The laser irradiation areas are subsequently characterized by complementary optical microscopy, scanning electron microscopy and depth profiling chemical analyses using secondary ion mass spectrometry. The results clarify the thin-film femtosecond laser ablation scenario and outline the process windows for selective antireflection coating removal.
Results of rolling contact fatigue (RCF) tests by balls-on-rod (BOR) method and two-roller methods have been compared to those by the balls-on-flat (BOF) method by using three different silicon nitride grades. The results suggest that the two-roller method could differentiate the bearing grade materials in terms of wear behavior.
In this study, a new direct functionalization method of silicon nitride (Si3N4) using azidation and click chemistry is presented. First, amino groups (NHx) were created on a Si3N4 substrate by fluoride etching. These NHx-terminated Si3N4 surfaces were analyzed by chemical derivatization X-ray photoelectron spectroscopy (CD-XPS) with 4-trifluoromethylbenzaldehyde (TFBA) and a derivatization yield of 20% was concluded. In the second step freshly prepared NHx surfaces were transformed into azides which were used immediately in a click reaction with halogenated alkynes. The presented combination of amination, azidation and click reaction is a promising alternative for common silane-based Si3N4 functionalization methods.
The friction and wear behaviour of SiC, Si3N4 and SiC/Si3N4 composite ceramics were investigated with oscillating sliding (gross slip fretting) at room temperature. The influence of counter body material and the humidity of the surrounding air was studied with a ball-on-disc configuration with different ball materials (1000Cr6, Al2O3 SiC and Si3N4). The effect of RH on friction is marginal with exception of SiC (low friction) as counter body material. The wear behaviour, however, is strongly affected by humidity, showing inverse trends for different counter body materials. Consequently, the wear behaviour of a tribo couple can be improved by selecting an adequate mating material. The results reveal the necessity to control RH in tribological tests. For estimation of the performance of tribo couples under varying environmental conditions, a variation of RH is required. In tribo couples with single phase SiC, either as ball or disc, the tribological behaviour of the system is dominated by SiC. The friction behaviour of the composite material is in between the behaviour of the two single phase materials, Si3N4 and SiC, whereas the wear behaviour is very similar to that of single phase Si3N4.
Porous silicon nitride ceramics were prepared via sintered reaction bonded silicon nitride at 1680 °C. The grain size of nitrided Si3N4 and diameter of post-sintered ß-Si3N4 are controlled by size of raw Si. Porosity of 42.14–46.54% and flexural strength from 141 MPa to 165 MPa were obtained. During post-sintering with nano Y2O3 as sintering additive, nano Y2O3 can promote the formation of small ß-Si3N4 nuclei, but the large amount of ß-Si3N4 (>20%) after nitridation also works as nuclei site for precipitation, in consequence the growth of fine ß-Si3N4 grains is restrained, the length is shortened, and the improvement on flexural strength is minimized. The effect of nano SiC on the refinement of the ß-Si3N4 grains is notable because of the pinning effect, while the effect of nano C on the refinement of the ß-Si3N4 grains is not remarkable due to the carbothermal reaction and increase in viscosity of the liquid phase.
Gradient porous silicon nitride (Si3N4) was fabricated by a novel vacuum foaming and freeze drying process. Aqueous Si3N4 slurries were foamed at vacuum pressure of 50–90 kPa, the green body was obtained by the freeze drying process, a gradient pore structure with porosities of 72–90% was achieved after pressureless sintering at 1680 °C. The porosity was increased with decreasing vacuum pressure. The pore structure consists of large pores (~100 μm) on top, medium pores (~45 μm) on the wall of the large pores, and small pores (~0.7 μm) in the matrix. Such gradient porous Si3N4 with macro- and micro-pores has potential application as high temperature filters.