Cross-sectional Transmission Electron Microscopy Observations Research Articles

Finishing of 4H-SiC (0001) by Combination of Thermal Oxidation and Abrasive Polishing

4H-SiC is considered as one of the most promising next-generation semiconductor power-device materials. An atomically flat 4H-SiC surface with a well-ordered step/terrace structure was essential for epitaxial growth or applications in electrical devices. Plasma assisted polishing (PAP), in which the irradiation of atmospheric-pressure water vapor plasma and ceria (CeO2) abrasive polishing were combined, was successfully applied to the atomic-scale flattening of 4H-SiC. To clarify the atomic-scale flattening mechanism of 4H-SiC in PAP process, investigations of thermal oxidation of 4H-SiC were conducted. Cross-sectional transmission electron microscopy (XTEM) observations revealed that the interfaces between the thermal oxidized oxide layer and SiC were very flat regardless of the thickness of the oxide layer. Dipping in hydrofluoric acid for 10 min and CeO2 abrasive polishing for 3 h were respectively conducted on a 4H-SiC surface which was thermally oxidized for 2 h. A flat surface was obtained after dipping in HF acid. However, no step/terrace structure, which corresponds to the inclination of the crystal plane, could be observed due to the residual of silicon oxycarbide. A well-ordered step/terrace structure was obtained on the surface polished by CeO2 abrasive. The step height was about 0.25 nm, which corresponds to a one-bilayer structure of 4H-SiC. The different oxidation rates of Si atoms on the cubic face and Si atoms on the hexagonal face were considered the reason why two kinds of terraces with different width were generated.

Structural, optical, spectroscopic and electrical properties of Mo-doped ZnO thin films grown by radio frequency magnetron sputtering

Undoped and Mo-doped ZnO (2% Mo) films about 1μm thick were deposited by radio-frequency magnetron sputtering on Si(100) and glass substrates at 30 and 300°C. X-ray diffraction patterns show that all films exhibit the hexagonal wurtzite crystal structure with a preferred orientation of the crystallites along the [002] direction. Plane view and cross-section transmission electron microscopy observations showed that the films present a columnar growth. Rutherford backscattering spectrometry indicates that Mo is homogeneously distributed inside the films. Scanning electron microscopy and atomic force microscopy show that Mo doping leads to a reduction of the grain size and surface roughness. According to X-ray photoelectron spectroscopy measurements, the valence of the Mo ions in the ZnO matrix is +5 and +6. Optical measurements in the UV–Visible range show a transmittance increasing from about 60 to 80% when increasing the wavelength from 400 to 800nm. A sharp absorption onset is observed at about 375nm corresponding to the fundamental absorption edge of ZnO at 3.26eV. This gap value remains unchanged upon Mo doping. The Hall effect measurements carried out at room temperature show that both undoped and Mo-doped ZnO films present an n-type conduction. The 2% Mo doping increases the carrier concentration and decreases the resistivity measured in pure ZnO by about three orders of magnitude. A comparison with 2% Al-doped ZnO films grown in the same conditions underlines the important role of the preparation conditions on the transport properties of ZnO based transparent conductive oxides.

Leakage current under high electric fields and magnetic properties in Co and Mn co-substituted BiFeO3 polycrystalline films

Co and Mn co-substituted BiFeO3 films were prepared on Pt/Ti/SiO2/Si(100) substrates, and the effect of co-substitution on the structural, electric, and magnetic properties of the prepared films was systematically investigated. Cross-sectional transmission electron microscopy observations showed that the films were homogeneous; moreover, no magnetic secondary phases were observed in the films. Nano-beam energy-dispersive X-ray spectroscopy, carried out at various points in the films, revealed that Co and Mn were distributed in the films. Further, the average concentration of Bi, Co, Mn, and Fe was 59, 2, 2, and 37at.%, respectively; these values were almost consistent with the nominal composition of the precursor solution used. X-ray diffraction profiles of the films showed that the (012)-d-spacing decreased and (104) and (110) peaks merged into a single peak with increasing co-substitution content. The leakage current in films under high electric fields drastically decreased upon co-substitution without any degradation of ferroelectricity; moreover, this effect was also observed for single Mn-substituted materials. Saturation magnetization of the films monotonically increased with the co-substitution content, and this increase was quantitatively identical to that in the case of single Co-substituted materials. These results indicate that Co and Mn play significant roles in determining the properties of co-substituted BiFeO3 films.

Low-frequency magnetic susceptibility and photoelectric properties of glass/Fe40Pd40B20/ZnO and glass/ZnO/Fe40Pd40B20

The following conditions are deposited: (a) glass/Fe40Pd40B20(Xnm)/ZnO(50nm) and (b) glass/ZnO(50nm)/Fe40Pd40B20(Ynm), where each of X and Y is 2.5nm, 5nm, 7.5nm or 10nm. The sputtering sequence and the thickness of the FePdB film were varied to investigate their effects on the low-frequency alternative-current magnetic susceptibility (χac), maximum phase angle (θmax), maximum χac and corresponding optimal resonance frequency (fres), electrical resistivity (ρ), and transmission and reflection percentages. Experimental results reveal that Fe40Pd40B20(Xnm)/ZnO(50nm) is better than ZnO(50nm)/Fe40Pd40B20(Ynm) because the nanocrystallization Fe40Pd40B20 at the bottom of the material can improve its magneto nanocrystalline anisotropy and increase the crystallization of ZnO, improving its magnetic and electrical properties. X-ray diffraction patterns (XRD) demonstrate that the ZnO (002) peak of Fe40Pd40B20(Xnm)/ZnO(50nm) is stronger than that of ZnO(50nm)/Fe40Pd40B20(Ynm). In particular, a comparison of high-resolution cross-sectional transmission electron microscopic (HR X-TEM) observations of Fe40Pd40B20(10nm)/ZnO(50nm) and ZnO(50nm)/Fe40Pd40B20(10nm) indicates that the Fe40Pd40B20 texture induces magneto nanocrystalline anisotropy into the nanocrystalline FePdB layer of Fe40Pd40B20(10nm)/ZnO(50nm), yielding the highest χac of around 0.79 with an fres of 10Hz and an θmax of 179°. Furthermore, ρ is reduced as the thickness of FePdB increases, because grain boundaries and the surface of thin films scatter electrons, causing thinner films to have greater resistance. The ρ of Fe40Pd40B20(Xnm)/ZnO(50nm) is lower than that of ZnO(50nm)/Fe40Pd40B20(Ynm) because stronger ZnO crystallization and nanocrystalline FePdB improve the scattering of electrons by the surface of the films. Finally, with respect to the optical transmittance and reflectance of Fe40Pd40B20(Xnm)/ZnO(50nm) and ZnO(50nm)/Fe40Pd40B20(Ynm), as the FePdB thickness increases, the transmittance gradually decreases, because transmittance and reflectance are inversely related to film thickness, increasing reflective efficiency. The results reveal that the magnetic and photoelectric properties of glass/Fe40Pd40B20(Xnm)/ZnO(50nm) are better than those of glass/ZnO(50nm)/Fe40Pd40B20(Ynm) owing to the tightly nanocrystalline FePdB crystallization and stronger ZnO crystallization. Glass/Fe40Pd40B20(10nm)/ZnO(50nm) is particularly effective for magnetic and photoelectric applications.

Evaluation of the performance correlated defects of metamorphic InGaAs photodetector structures through plane-view EBIC

To evaluate the performance correlated imperfection or defect features of metamorphic InGaAs photodetector structures, a scanning electron microscopy scheme including both plane-view electron beam induced current (EBIC) and secondary electron (SE) images have been used. The abilities, merits and limitations as well as some case-dependent properties of EBIC have been discussed in detail. The devices of similar structures grown on InP or GaAs substrates with quite different lattice mismatch show discriminated defect distribution patterns, prompting their distinct origins, which have been confirmed by cross-sectional transmission electron microscopy observation. Using self-developed image processing software the EBIC features of the samples are statistically analyzed, which validated the qualitative correlation between the EBIC data and device dark current. Fusing of EBIC and SE images has also been attempted to enhance the defect visibility. Results indicate that EBIC is feasible to investigate the effects of defects on the device performance not only in research work, but also for product quality monitor purposes.

High-Mobility Electron Conduction in Oxynitride: Anatase TaON

We report on a new route for synthesizing metastable anatase tantalum oxynitride (TaON) in thin film form on lattice-matched (LaAlO3)0.3-(SrAl0.5Ta0.5O3)0.7 (LSAT) single crystals by using nitrogen plasma assisted pulsed laser deposition. Epitaxial stress from the substrate stabilized the anatase structure without the need for doping an impurity, such as Sc or Mg, which is required in conventional bulk synthesis by ammonolysis. X-ray diffraction measurements and cross-sectional transmission electron microscope (TEM) observations demonstrated the growth of phase-pure anatase TaON thin films with the epitaxial relationships (001)TaON ∥ (001)LSAT and [100]TaON ∥ [100]LSAT. A high growth temperature (≥750 °C) and a balanced supply of oxygen and nitrogen are crucial for obtaining high-quality anatase TaON thin films. The films grown at 800 °C exhibited good n-type conduction with a resistivity of ∼1 × 10–2 Ω cm. The source of the carrier electrons was likely anion vacancies. The Hall mobility of anatase TaON (∼17 cm2 V–1 s–1 at 300 K) is comparably high to that of anatase TiO2, which is a well-known oxide semiconductor with the same crystal structure and d0 electronic configuration. The bandgap and refractive index of anatase TaON thin films were 2.37 eV and approximately 3.0, respectively, in the visible region.

Band gap and function engineering for novel functional alloy semiconductors: Bloomed as magnetic properties at room temperature with α-(GaFe)2O3

Highly crystalline corundum structured α-(Ga0.42Fe0.58)2O3 alloy thin film showed magnetic properties at room temperature. Microstructure analysis of cross-sectional transmission electron microscope (TEM) observation and TEM energy dispersive X-ray spectroscopy measurement indicated that different crystal phase could not be detected as well as there is no remarkable phase separating area, that is, Fe and Ga ions are distributed uniformly in the film. Magnetic measurements were performed on α-(Ga1−xFex)2O3 (x = 0.24, 0.44, 0.58, 1.00) alloy thin films at 110 K. The induced magnetic moment per a Fe ion of α-(Ga0.42Fe0.58)2O3 at 5000 Oe is about 6 times larger than α-Fe2O3 thin film. Compared to the α-Fe2O3 thin films, the value of coercivity is also about 6 times in α-(Ga0.42Fe0.58)2O3, in contrast, there is no significant difference in value of coercivity of α-(Ga1−xFex)2O3 (x = 0.24, 0.44, 1.00) thin films. These means that the origin of magnetism is not the separation region of α-Fe2O3 in α-(Ga0.42Fe0.58)2O3 thin film.

Development of REBCO Coated Conductors by TFA-MOD Method With High Characteristic in Magnetic Field

YxGd(1 - x)Ba2Cu3 Oy coated conductors (CCs) with artificial pinning centers (APCs) were fabricated by the trifluoroacetates-metal organic deposition method using a batch heat-treatment process. This process has been industrially applied to fabricate long superconducting tapes that have high critical current (Ic). From the viewpoint of applications, the characteristics in magnetic fields become further important, and one solution has been shown previously as introduction of APCs such as BaZrO3. We applied the technique to our CCs fabrication process. The heat-treatment conditions, specifically total gas pressure, oxygen concentration, and crystallization temperature, were optimized for the batch heat-treatment process. As a consequence, fabricated CC showed extremely high characteristic Jc value of 3.5 MA/cm2 in self field, and 0.3 MA/cm2 at 3 T in liquid N2. Moreover, by cross-sectional transmission electron microscopy observation, it was confirmed that the APC was distributed uniformly. Furthermore, the anisotropy of the pinning center is also examined based on the evaluation result of the angular dependence of Jc in 3T.

Formation of Carbon Nanotube/n-Type 6H-SiC Heterojunction by Surface Decomposition of SiC and Its Electric Properties

Carbon nanotube (CNT)/n-type SiC heterojunctions were formed by surface decomposition of 6H-SiC(0001), where each CNT directly bonded to SiC crystal at the interface without any interlayer. Through heating temperature and heating time, the CNT length could be controlled up to 4 µm. For the sample with CNTs of 180 and 230 nm in thickness, distinct rectifying behavior was observed in the current–voltage measurements, with the forward direction observed at positively biased CNTs. When the CNT length was 1500 nm, the leakage current was increased. From cross-sectional transmission electron microscopy (TEM) observations, we conclude that the increase of the leakage current was due to the deterioration of crystalline quality of CNTs near the interface between CNTs and SiC, which was caused by the obstruction of the desorption of Si atoms by the lengthening of CNTs.

Crystalline Defects in Silicon Wafer Caused by Prolonged High-Temperature Annealing in Nitrogen Atmosphere

A floating zone (FZ) silicon wafer produced from a Czochralski (CZ) single-crystal ingot was subjected to prolonged annealing at a high temperature. Precipitates were formed in a N2(70%)+O2(30%) ambient atmosphere. The precipitate regions manifested themselves as dark concentric rings in the X-ray topographs. According to the results of cross-sectional transmission electron microscopy observations and energy-dispersive X-ray spectroscopy elemental analyses, nitrogen was distributed throughout the precipitate regions, while oxygen was rich in the periphery of the regions. A high concentration of nitrogen was also directly detected by secondary ion mass spectrometry in the mid-depth of the wafer in the precipitate regions. Electron diffraction analysis of the precipitates showed that their phase was α-Si3N4.

Optically Pumped Lasing Action with Unusual Wavelength of Approximately 390 nm in Hexagonal GaN Microdisks Fabricated by Radio-Frequency Plasma-Assisted Molecular Beam Epitaxy

Hexagonal GaN microdisks exhibiting lasing action with unusual wavelengths of approximately 390 nm under an optically pumped condition have been investigated. The lasing action was caused by the resonant modes of the whispering gallery mode and/or quasi-whispering gallery mode in the hexagonal microdisks. A cross-sectional transmission electron microscopy observation indicated that multiple crystalline boundaries, which are formed by stacking faults, were included in the specific GaN microdisks exhibiting such an unusual lasing action. The origin of the optical gain was discussed, based on the modification of the crystal structure associated with the stacking faults.

The low-frequency alternative-current magnetic susceptibility and electrical properties of Si(100)/Fe40Pd40B20(X Å)/ZnO(500 Å) and Si(100)/ZnO(500 Å)/Fe40Pd40B20(Y Å) systems

The two deposition conditions are (a) Si(100)/Fe40Pd40B20(X Å)/ZnO (500 Å) and (b) Si(100)/ZnO(500 Å)/Fe40Pd40B20(Y Å), where X and Y are 25 Å, 50 Å, 75 Å, and 100 Å. The sputtering sequence and the thickness of the FePdB film were varied to examine their effects on the low-frequency alternative-current magnetic susceptibility (χac), maximum phase angle (θmax), maximum χac with corresponding optimal resonance frequency (fres), and electrical resistivity (ρ). Experimental results show that ZnO(500 Å)/Fe40Pd40B20(Y Å) is superior to Fe40Pd40B20(X Å)/ZnO(500 Å) because the ZnO(002) texture at the bottom can improve the magneto nanocrystalline anisotropy of Fe40Pd40B20, improving its magnetic properties. In particular, a comparison of high-resolution cross-sectional transmission electron microscopy observations of Fe40Pd40B20(100 Å)/ZnO(500 Å) and ZnO(500 Å)/Fe40Pd40B20(100 Å) demonstrates that the ZnO(002) texture induces a magneto nanocrystalline anisotropy in the nanocrystalline FePdB layer of ZnO(500 Å)/Fe40Pd40B20(100 Å), yielding a highest χac of approximately 2.8 with an fres of 1000 Hz and an θmax of 169°. Additionally, the ρ is reduced as the FePdB thickness increases, because grain boundaries and the surface of thin films scatter the electrons, so thinner films have a greater resistance. The ρ of ZnO(500 Å)/Fe40Pd40B20(Y Å) is lower than that of Fe40Pd40B20(X Å)/ZnO(500 Å) because stronger ZnO crystallization and nanocrystalline FePdB improve the scattering of electrons by the surface of the films.

Remarkably enhanced surface plasmon resonance absorption of Cu nanoparticles in SiO2 by post Zn ion implantation

Cu nanoparticles (NPs) embedded in SiO2 glasses were subjected to implantation of 50 keV Zn ions at fluences of 0.5 × 1016 and 1.0 × 1016 ions/cm2. Remarkable enhancement and shift in the surface plasmon resonance (SPR) absorption signal of Cu NPs have been revealed after subsequent annealing for the sample implanted at the fluence of 1.0 × 1016 ions/cm2. According to cross-sectional transmission electron microscope observations and energy dispersive X-ray spectroscopy analyses, increase of partial dielectric constant around the Cu NPs in the matrix is probably responsible for the dramatic changes of the Cu SPR absorption. The results provide an available route to modulate the SPR signal of Cu NPs in SiO2.

Controlled growth of epitaxial CeO2 thin films with self-organized nanostructure by chemical solution method

Chemical solution deposition is a versatile technique to grow oxide thin films with self-organized nanostructures. Morphology and crystallographic orientation control of CeO2 thin films grown on technical NiW substrates by a chemical solution deposition method are achieved in this work. Based on an enhanced understanding of the effect of oxygen partial pressure during film crystallization, a strong texture can be obtained on the surface of the CeO2 films annealed at temperatures as low as 900 °C followed by a two-step annealing procedure. Crystallization at high temperature (e.g., 1100 °C) in a reducing atmosphere leads to the formation of an oxygen deficient CeO2−x phase coexisting with a small amount of a polycrystalline CeO1.67 phase. Further surface phase and texture analysis by an electron backscattering diffraction technique reveals that the off-stoichiometric CeO2−x phase retains a fluorite structure but exhibits an alternative in-plane texture with eight fold symmetry on the surface. According to phase and texture stability studies, these off-stoichiometric phases gradually transform back to fully oxidized CeO2 with a 45° rotated cube texture during storage in ambient air. Moreover, the morphology of the CeO2 thin films is controlled by precisely regulating the film thickness and crystallization temperature. A temperature-induced transition from the commonly observed granular grain to an atomically flat surface is found in the CeO2–NiW constitution. Cross-sectional transmission electron microscope observation also reveals that this phenomenon is mainly attributable to the surface re-organization, which is strongly associated with the critical film thickness, crystallization temperature, reducing ability of the crystallization atmosphere as well as the interface properties.

Atomic-scale flattening mechanism of 4H-SiC (0 0 0 1) in plasma assisted polishing

Plasma assisted polishing (PAP), in which the irradiation of atmospheric pressure water vapor plasma and ceria (CeO2) abrasive polishing are combined, is a novel finishing technique for single-crystal silicon carbide (4H-SiC). An atomically flat 4H-SiC surface (rms about 0.2nm) with a well-ordered step/terrace structure was obtained by PAP. Cross-sectional transmission electron microscopy (XTEM) observation revealed that plasma oxidation atomically flattened the interface of SiO2/SiC. Angle-resolved X-ray photoelectron spectroscopy (ARXPS) measurement results showed the existence of a thin silicon oxycarbide layer, which is corrosion-resistant to hydrofluoric acid, at the interface. The combination of water vapor plasma oxidation and the mechanical removal of silicon oxide as well as silicon oxycarbide layers by a soft abrasive is effective in obtaining an atomically flat surface of 4H-SiC (0001) without introducing crystallographic subsurface damage.

Epitaxial growth of Sb-doped nonpolar a-plane ZnO thin films on r-plane sapphire substrates by RF magnetron sputtering

► Sb-doped nonpolar a -plane ZnO layers were epitaxially grown on sapphire substrates. ► Crystallinity and electrical properties were studied upon growth condition and doping concentration. ► The out-of-plane lattice spacing of ZnO films reduces monotonically with increasing Sb doping level. ► The p-type conductivity of ZnO:Sb film is closely correlated with annealing condition and Sb doping level. In this study, the epitaxial growth of Sb-doped nonpolar a -plane ( 1 1 2 ¯ 0 ) ZnO thin films on r -plane ( 1 1 ¯ 0 2 ) sapphire substrates was performed by radio-frequency magnetron sputtering. The influence of the sputter deposition conditions and Sb doping concentration on the microstructural and electrical properties of Sb-doped ZnO epitaxial films was investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM) and the Hall-effect measurement. The measurement of the XRD phi-scan indicated that the epitaxial relationship between the ZnO:Sb layer and sapphire substrate was 1 1 2 ¯ 0 ZnO / / ( 1 1 ¯ 0 2 ) Al 2 O 3 and 1 1 ¯ 0 0 ZnO / / 1 1 2 ¯ 0 Al 2 O 3 . The out-of-plane a -axis lattice parameter of ZnO films was reduced monotonically with the increasing Sb doping level. The cross-sectional transmission electron microscopy (XTEM) observation confirmed the absence of any significant antimony oxide phase segregation across the thickness of the Sb-doped ZnO epitaxial film. However, the epitaxial quality of the films deteriorated as the level of Sb dopant increased. The electrical properties of ZnO:Sb film are closely correlated with post-annealing conditions and Sb doping concentrations.

Coherent growth of GaGdN layers with high Gd concentration on GaN(0001)

We report on the coherent growth of GaGdN with high Gd concentration on a GaN template using radio-frequency plasma-assisted molecular beam epitaxy under elevated growth conditions. X-ray diffraction and cross-sectional transmission electron microscopy observations revealed that at a growth temperature of 700 °C or below, GaGdN layers are coherently grown on the GaN templates without segregation of the secondary phases. As the GdN mole fraction x was increased to 0.08, the c-axis lattice parameter in Ga1−xGdxN increased linearly. Increasing the growth temperature to 750 °C causes lattice relaxation in GaGdN. All GaGdN samples exhibited photoluminescence emissions near the band-edge, a blue luminescence band emission, and a green luminescence band emission. The origin of the green luminescence band emission is discussed in relation to the compressive strain existing in the GaGdN layers coherently grown on GaN.

Evaluation of Irradiation Effects on Fracture Strength of Silicon Carbide using Micropillar Compression Tests

Micro-scale material testing techniques (e.g., nanoindentation, micropillar compression, etc.) have been developed and applied for the evaluation of radiation effects on the mechanical properties of nuclear reactor materials. These techniques can measure the mechanical properties from small volumes, which can be beneficial in the investigation of both neutron and ion-irradiated materials. In this study, we evaluated the compressive fracture strength of ion-irradiated silicon carbide (SiC) using micropillar compression tests. SiC and SiC-based composites are considered as candidate materials for micro electronics, sensors, and various components in next-generation reactors. Micropillars with a nominal diameter of 0.65 μm were fabricated on a monolithic polycrystalline cubic SiC plate using a lithography and plasma etching technique. Half of the total micropillars were irradiated with Si2+ ions. The SiC micropillars were uniaxially compressed using a flat diamond punch. A finite element model was used to compute the elastic stress state of the pillar. The results showed irradiation-induced strengthening, which is consistent with other investigations. In addition, plastic deformation of SiC at room temperature was observed. A slip was found to occur on {111} planes from a cross-sectional transmission electron microscopy observation. The micropillar tests are expected to significantly contribute to the study of irradiation and size effect on the mechanical properties of ceramic materials to be used in a radiation environment.

In-depth multi-technique characterization of chromium–silicon mixed oxides produced by reactive ion beam mixing of the Cr/Si interface

The great interest of mixed metal–silicon oxides lies in their suitability, among other applications, as optical coatings with an adjustable refractive index. In this paper we investigate a new method to obtain chromium and silicon mixed oxides. Using as starting point a metallic chromium film deposited on a silicon substrate by magnetron sputtering, we induce the formation of mixed oxides using reactive ion beam mixing by bombarding the Cr/Si interface with oxygen. We have varied the ion fluence (between 5 × 1016 and 1 × 1018 ions cm−2) at a fixed implantation energy of 80 keV in order to modify the final composition of the coating. The composition profiles have been obtained with Rutherford backscattering spectroscopy (RBS), by changing the He energy from 3.035 up to 3.105 MeV, and with elastic recoil detection analysis using a time of flight configuration (ERDA-ToF). Results have been compared with those obtained from secondary ion mass spectrometry (SIMS) depth profiles and Monte Carlo TRIDYN simulations. Concentration depth profiles (CDP) have been also measured using X-ray photoelectron spectroscopy (XPS) and simultaneous Ar+ bombardment, as well as angle-resolved X-ray photoelectron spectroscopy (ARXPS). All the obtained depth profiles agree remarkably well with cross-section transmission electron microscopy (TEM) observations made on the sample implanted at the highest fluence.

Surface damage versus defect microstructures in He and H ion co-implanted Si3N4/Si

Cz n-type Si (100) wafers with a top Si3N4 layer of about 170nm in thickness were sequentially implanted with 40keV He ions at a fluence of 5×1016/cm2 and 35keV H ions at fluences of 1×1015, 5×1015 and 1×1016/cm2, respectively. Creation and evolution of surface damage as well as micro-defects have been studied. Our results clearly show that production of surface damage depends strongly on both the H implant fluence and annealing temperature. Only blistering or localized exfoliation of the top Si3N4 layer has been observed for post H implantation at fluences of 1×1015 and 5×1015/cm2 upon 800°C annealing. However, serious surface exfoliation has been found for the 1×1016/cm2 H co-implanted samples after annealing at 450°C and above. The exfoliation occurs at a depth of about 360nm from the surface, which is obviously larger than the He or H ion range. Moreover, the exfoliated craters show clear two-step structures. Cross-sectional transmission electron microscopy (XTEM) observations reveal formation of micro-cracks in Si bulk and along the original interface, which is mainly responsible for the observed surface phenomena. The formation mechanism of micro-cracks has been discussed in combination of He and H implant-induced defects, impurities as well as their interactions upon annealing.