Temperature Effects on ion Irradiation Damage in MgAl2O4 Spinel Single Crystals

1994 ◽  
Vol 373 ◽  
Author(s):  
Ning Yu ◽  
Kurt E. Sickafus ◽  
Michael Nastasi

AbstractSingle crystalline samples of magnesium aluminate spinel (MgAl2O4), <100> oriented, were irradiated at 100 K and 670 K with 370-400 keV Xe ions to doses of (1-2)x1016 Xe/cm2. The microstructures of irradiated samples were subsequently examined by cross-sectional transmission electron microscope. A uniform layer of amorphous phase was observed on the surface of spinel irradiated at 100 K. At the end of the damage range underlying the amorphous layer, a disordered transition layer resided on the undamaged substrate. Both high resolution electron microscopy and microdiffraction revealed that the transition layer retained single crystallinity with epitaxial relationship to the underlying substrate. However, the intensity of <220> reflections in the transition layer was significantly weaker than that of the undamaged spinel. No evidence of amorphization was found in the spinel sample irradiated at 670 K to a dose of 2x1016 Xe/cm2. The <220> reflections exhibit only limited diminution in the heavily damaged region. The observation of reduced intensity of <220> reflections or absent reflections suggests that spinel experiences a structural transition from its original cubic phase (a=0.808 nm) to a new cubic phase (a=0.404 nm). A transition sequence from the original phase to a metastable phase and then to an amorphous phase has been observed. The temperature dependence of metastable and amorphous phase formation has revealed that the accumulation efficiency of cation disorder decreases with increasing irradiation temperature due to the enhancement of interstitial-vacancy recombination.

1989 ◽  
Vol 4 (6) ◽  
pp. 1385-1392 ◽  
Author(s):  
K. Pampus ◽  
K. Dyrbye ◽  
B. Torp ◽  
R. Bormann

The structure of Nb–Al thin films after ion mixing was studied for compositions from 20 to 85 at. % Al as a function of temperature in the range between 40 and 620 K. The phase formation was determined by transmission electron microscopy. At lower temperatures, only supersaturated bcc-solid solution, NbAl, and amorphous phase were found throughout the studied composition range. Besides these phases irradiation at temperatures above 470 K causes the formation of a metastable crystalline compound at an overall composition close to Nb25Al75, and for T = 623 K the equilibrium compound NbAl3 is formed. The other intermetallic phases Nb2Al and Nb3Al have not been observed at any irradiation temperature. Calculations of the Gibbs free energies of the various phases are presented, and the reliability of extrapolations to regions of metastability with respect to temperature and composition is commented on. The phase formation during heavy-ion irradiation is discussed in the context of the calculated free energies and kinetic constraints. For temperatures above 300 K, the attainment of a metastable phase equilibrium between the bcc solid solution and the amorphous phase is proposed due to the influence of radiation enhanced diffusion.


1998 ◽  
Vol 540 ◽  
Author(s):  
Fuxin Li ◽  
Ping Lu ◽  
Kurt E. Sickafus ◽  
Caleb R. Evans ◽  
Michael Nastasi

AbstractRutile (TiO2) single crystals with (110) orientation were irradiated with 360 keV Xe2+ ions at 300K to fluences ranging from 2×1019 to 1×1020 Xe/m2. Irradiated samples were analyzed using: (1) Rutherford backscattering spectroscopy combined with ion channeling analysis (RBS/C); and (2) cross-sectional transmission electron microscopy (XTEM). Upon irradiation to a fluence of 2×1O19 Xe/m2, the sample thickness penetrated by the implanted ions was observed to consist of three distinct layers: (1) a defect-free layer at the surface (thickness about 12 nm) exhibiting good crystallinity; (2) a second layer with a low density of relatively large- sized defects; and (3) a third layer consisting of a high concentration of small defects. After the fluence was increased to 7×1019 Xe/m2, a buried amorphous layer was visible by XTEM. The thickness of the amorphous layer was found to increase with increasing Xe ion fluence. The location of this buried amorphous layer was found to coincide with the measured peak in the Xe concentration (measured by RBS/C), rather than with the theoretical maXimum in the displacement damage profile. This observation suggests the implanted Xe ions may serve as nucleation sites for the amorphization transformation. The total thickness of the damaged microstructure due to ion irradiation was always found to be much greater than the projected range of the Xe ions. This is likely due to point defect migration under the high stresses induced by ion implantation.


1993 ◽  
Vol 316 ◽  
Author(s):  
B.A. Turkot ◽  
D.V. Forbes ◽  
H. Xiao ◽  
I.M. Robertson ◽  
J.J. Coleman ◽  
...  

ABSTRACTThe development of the damage structure produced in (100) GaAs/Al0.6Ga0.4As/GaAs by 1 MeV Kr+ ion irradiation at 77 and 293 K has been investigated by RBS channeling and cross-sectional high-resolution TEM techniques. Following an implantation to a dose of 1014 ions cm-2 at 77 K, RBS channeling spectra indicate that the Al0.6Ga0.4 layer contained a high defect density and was possibly amorphous. Warming to room temperature resulted in a change in the channeling spectrum, which indicated that the damage in the Al0.6Ga0.4As layer had partially recovered. The degree of recovery was greatest at the GaAs/ Al0.6Ga0.4As interface, and decreased with increasing depth. TEM observations show the damage in the Al0.6Ga0.4As to be comprised of planar defects, the density of which increases with depth, and an amorphous layer at the bottom interface. This difference in the damage distribution is consistent with the asymmetry in the channeling spectrum. A model based on the depth variation of cascade density is proposed to account for the observations.


Author(s):  
X.W. Lin ◽  
Z. Liliental-Weber ◽  
J. Washburn ◽  
J. Desimoni ◽  
H. Bernas

Epitaxy of semiconducting β-FeSi2 on Si is of interest for optoelectronic device technology, because of its direct bandgap of ≈0.9 eV. Several techniques, including solid phase epitaxy (SPE) and ion beam synthesis, have been successfully used to grow β-FeSi2 on either Si (001) or (111) wafers. In this paper, we report the epitaxial formation of β-FeSi2 upon thermal annealing of an Fe-Si amorphous layer formed by ion implantation.Si (001) wafers were first implanted at room temperature with 50-keV Fe+ ions to a dose of 0.5 - 1×1016 cm−2, corresponding to a peak Fe concentration of cp ≈ 2 - 4 at.%, and subsequently annealed at 320, 520, and 900°C, in order to induce SPE of the implanted amorphous layer. Cross-sectional high-resolution electron microscopy (HREM) was used for structural characterization.We find that the implanted surface layer ( ≈100 nm thick) remains amorphous for samples annealed at 320°C for as long as 3.2 h, whereas annealing above 520°C results in SPE of Si, along with precipitation of β-FeSi2.


1990 ◽  
Vol 187 ◽  
Author(s):  
E. Ma ◽  
L.A. Clevenger ◽  
C.V. Thompson ◽  
K.N. Tu

AbstractThe growth of an amorphous Ti-Si phase and subsequent formation of crystalline silicides during solid-state reactions in Ti/a-Si multilayer films have been studied using power-compensated differential scanning calorimetry, cross-sectional transmission electron microscopy, and thin-film x-ray diffraction. By analyzing calorimetric data we have determined the activation energies for the formation of the various silicides (amorphous Ti-silicide, TiSi, C49-TiSi2, Ti5Si3) as well as their heats of formation. An amorphous silicide is the first phase to form during heating and we have measured the composition profile of this amorphous layer using scanning transimission electron microscopy. Metastable phase equilibria in the Ti-Si system are discussed in light of the thermodynamic and compositional information obtained in our experiments.


1995 ◽  
Vol 395 ◽  
Author(s):  
K. DOVIDENKO ◽  
S. OKTYABRSKY ◽  
J. NARAYAN ◽  
M. RAZEGHI

ABSTRACTThe microstructural study of wide-band gap semiconductor AlN thin films grown on (0001) and (1012) sapphire and (111), (100) Si was carried out using plan-view and cross-sectional high-resolution electron microscopy and x-ray diffraction. The films were grown by MOCVD from TMAl + NH3 + N2 gas mixture. Epitaxial relationship for AIN grown on (0001)α 01-Al2O3 was determined to be the following: (0001)AIN ║ (0001)sap with the 30° in-plane rotation - [0110]AIN ║ [1210]sap. We report also TEM observation of the following epitaxial relationship of the AlN/(1012)α-Al2O3 heterostructure: (1120)AIN ║ (1012)sap; [0001]AIN ║ [1011]sap and [1100] AIN ║ [1210]sap. These epitaxial relationships were determined to be controlled by the bonding of Al and O ions at the interface. The study of interfaces and the defects present in the film was also carried out. Main type of defects were established to be inverted domain boundaries, misfit and threading dislocations - in the films on (0001) sapphire, and stacking faults of high density in the films on (1012) sapphire. The epitaxial AIN films on (0001) sapphire contained dislocation density about 1010 cm−2 and exhibited device quality electrical characteristics. The films on both orientations of Si were found to be highly <0001> textured polycrystalline.


Author(s):  
Y. Cheng ◽  
J. Liu ◽  
M.B. Stearns ◽  
D.G. Steams

The Rh/Si multilayer (ML) thin films are promising optical elements for soft x-rays since they have a calculated normal incidence reflectivity of ∼60% at a x-ray wavelength of ∼13 nm. However, a reflectivity of only 28% has been attained to date for ML fabricated by dc magnetron sputtering. In order to determine the cause of this degraded reflectivity the microstructure of this ML was examined on cross-sectional specimens with two high-resolution electron microscopy (HREM and HAADF) techniques.Cross-sectional specimens were made from an as-prepared ML sample and from the same ML annealed at 298 °C for 1 and 100 hours. The specimens were imaged using a JEM-4000EX TEM operating at 400 kV with a point-to-point resolution of better than 0.17 nm. The specimens were viewed along Si [110] projection of the substrate, with the (001) Si surface plane parallel to the beam direction.


Author(s):  
H. Watanabe ◽  
B. Kabius ◽  
B. Roas ◽  
K. Urban

Recently it was reported that the critical current density(Jc) of YBa2Cu2O7, in the presence of magnetic field, is enhanced by ion irradiation. The enhancement is thought to be due to the pinning of the magnetic flux lines by radiation-induced defects or by structural disorder. The aim of the present study was to understand the fundamental mechanisms of the defect formation in association with the pinning effect in YBa2Cu3O7 by means of high-resolution electron microscopy(HRTEM).The YBa2Cu3O7 specimens were prepared by laser ablation in an insitu process. During deposition, a substrate temperature and oxygen atmosphere were kept at about 1073 K and 0.4 mbar, respectively. In this way high quality epitaxially films can be obtained with the caxis parallel to the <100 > SrTiO3 substrate normal. The specimens were irradiated at a temperature of 77 K with 173 MeV Xe ions up to a dose of 3.0 × 1016 m−2.


Author(s):  
Yoshinori Fujiyoshi

The resolution of direct images of biological macromolecules is normally restricted to far less than 0.3 nm. This is not due instrumental resolution, but irradiation damage. The damage to biological macromolecules may expect to be reduced when they are cooled to a very low temperature. We started to develop a new cryo-stage for a high resolution electron microscopy in 1983, and successfully constructed a superfluid helium stage for a 400 kV microscope by 1986, whereby chlorinated copper-phthalocyanine could be photographed to a resolution of 0.26 nm at a stage temperature of 1.5 K. We are continuing to develop the cryo-microscope and have developed a cryo-microscope equipped with a superfluid helium stage and new cryo-transfer device.The New cryo-microscope achieves not only improved resolution but also increased operational ease. The construction of the new super-fluid helium stage is shown in Fig. 1, where the cross sectional structure is shown parallel to an electron beam path. The capacities of LN2 tank, LHe tank and the pot are 1400 ml, 1200 ml and 3 ml, respectively. Their surfaces are placed with gold to minimize thermal radiation. Consumption rates of liquid nitrogen and liquid helium are 170 ml/hour and 140 ml/hour, respectively. The working time of this stage is more than 7 hours starting from full LN2 and LHe tanks. Instrumental resolution of our cryo-stage cooled to 4.2 K was confirmed to be 0.20 nm by an optical diffraction pattern from the image of a chlorinated copper-phthalocyanine crystal. The image and the optical diffraction pattern are shown in Fig. 2 a, b, respectively.


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