The homo- and heteroepitaxial deposition of LGS (langasite, La3Ga5SiO14) thin films on LGS single crystals, Si and SiO2 substrates by pulsed laser deposition (PLD) is demonstrated. PLD is performed at substrate temperatures up to about 700 °C and results initially in Ga deficient films. Two strategies of counterbalancing the Ga deficit are realized. First, off-stoichiometric targets with an enhanced Ga content are applied. Secondly, an increased oxygen partial pressure up to about 6 Pa is used during deposition to suppress evaporation of Ga suboxides. Combining these adaptions results in the growth of stoichiometric LGS thin films. Films deposited on LGS substrates do not show any additional X-ray diffraction reflexes nor broadening of the peaks with respect to the single crystalline substrates. Therefore, the homoepitaxial approach can be considered successful. The deposition on Si and SiO2 substrates under the same conditions leads to the formation of polycrystalline films. However, post-annealing at 800 °C increases crystallinity. Stoichiometry and homogeneous distribution of La, Ga and Si cations are confirmed by secondary neutral mass spectrometry (SNMS). The composition remains constant within the film, implying stable process parameters.

Characterization of three vendor’s bulk semi-insulating GaN:Fe wafers, grown by either hydride vapor phase epitaxy or the ammonothermal method, was performed using: scanning electron microscopy, secondary ion mass spectroscopy, high resolution X-ray diffraction, cathodoluminescence, photoluminescence, and high voltage testing. Although the Fe doping level is significantly different for each growth method, both are promising for the fabrication of PCSS devices operating in the lock-on mode.

A cadmium chloride activation treatment is essential for the production of high efficiency cadmium telluride (CdTe) solar cells. However, the effects of the treatment on the distributions of chlorine and sulphur within the device are not fully understood. Here, the detailed locations of chlorine and sulphur in a treated CdTe cell are determined in three dimensions by high resolution dynamic SIMS measurements. Chlorine is found to be present in grain boundaries, grain interiors, extended defects within the grain interiors, at the front interface, and in the cadmium sulphide layer. In each of these regions, the chlorine is likely to have significant effects on local electronic properties of the material, and hence overall device performance. Sulphur is found to have a U-shaped diffusion profile within CdTe grains, indicating a mixed grain boundary and lattice diffusion regime.

Perovskite-based solar cells, typically CH3NH3PbI3, have reached power conversion efficiencies on par with single crystal silicon solar cells. Perovskite cells prepared with the most common perovskite solvent N,N-dimethylformamide (DMF) by different research groups exhibit disparate efficiencies and stability for nominally identical perovskite films. Although the differences can be related to processing conditions, a consistent physical cause for the differences has been lacking. Highly-sensitive time-of-flight secondary ion mass spectrometry (TOF-SIMS) reveals significant dimethylamine (DMA) included in perovskite films. TOF-SIMS and x-ray photoelectron spectroscopy results suggest DMA levels ranging from roughly 10–50%. Only the highest levels register as perovskite peak shifts in x-ray diffraction; lower levels are invisible. We propose that methylamine (MA) can react with DMF solvent by transamidation to produce dimethylamine (DMA), which then displaces some MA in perovskite crystals, see Fig. 1. Transamidation of DMF can be catalyzed by TiO2, Al2O3, water, or acid, but in perovskite films transamidation is inhibited by water.

We fabricated ferroelectric (Pb,La)(Zr,Ti)O3 (PLZT) capacitors withSn:In2O3 (ITO) or Pt top electrodes and investigatedthe ferroelectric properties of these PLZT capacitors. The shape ofpolarization–voltage hysteresis loops was essentially unchanged andthe decrease in the remnant polarization of the ITO/PLZT/Pt capacitors wassmaller than that of the Pt/PLZT/Pt capacitors after annealing with 3%D2 (in N2) at 200°C and 1 Torr(i.e., FGAD). Time of flightsecondary mass spectrometry revealed that the D atoms were incorporated into thePLZT film of the Pt/PLZT/Pt capacitors after 3% D2 annealing,resulting in a decrease in the ferroelectric properties. In comparison, no D ionsignal was detected in the PLZT film after FGAD for ITO/PLZT/Ptcapacitors.

We fabricated ferroelectric (Pb,La)(Zr,Ti)O3 (PLZT) capacitors with Sn:In2O3 (ITO) top electrodes using chemical solution deposition. Then, the effects of a thin conductive ITO buffer layer between the Pt bottom electrode and PLZT thin film were investigated in combination with top electrode (ITO/PLZT/ITO/Pt). The H2 degradation resistance of ITO/PLZT/ITO/Pt capacitors with a 3- and 28-nm-thick buffer layer was improved to 78 and 85%, respectively, from 60% without a buffer layer. The time-of-flight secondary ion mass spectrometry profiles indicated the intensity of H ion increased after 45 min forming gas (3% H2/balance N2) annealing.

The behavior of the redox-based resistive switching memories is influenced by chemical interactions between the electrode and the solid electrolyte, as well as by local environment. The existence of different chemical potential gradients is resulting in nanobattery effect lowering the stability of the devices. In order to minimize these effects we introduce a graphene layer at the active electrode – solid electrolyte interface. We observe that graphene is acting as an effective diffusion barrier in the SiO2-based electrochemical metallization cells and acts catalytically on the electrochemical processes prior to resistive switching.

Thin-film solid-oxide fuel cells (TF-SOFCs) fabricated using microelectromechanical systems (MEMS) processing techniques not only help lower the cell operating temperature but also provide a convenient platform for studying cathodic losses. Utilizing these platforms, cathode kinetics can be enhanced dramatically by engineering the microstructure of the cathode/electrolyte interface by increasing the surface grain-boundary density. Nanoscale secondary ion mass spectrometry and high-resolution transmission electron microscopy studies have shown that oxygen exchange at electrolyte surface grain boundaries is facilitated by a high population of oxide-ion vacancies segregating preferentially to the grain boundaries. Furthermore, three-dimensional structuring of TF-SOFCs enabled by various lithography methods also helps increase the active surface area and enhance the surface exchange reaction. Although their practical prospects are yet to be verified, MEMS-based TF-SOFC platforms hold the potential to provide high-performance for low-temperature SOFC applications.

Hexagonal boron nitride (hBN) crystals enriched in 10B and 11B isotopes were synthesized using a high temperature (1500° C) Ni-Cr-B reactive-precipitation growth under a N2 atmosphere. Two growth mechanisms were observed: conventional defect-facilitated bulk growth which produced crystals with a platelet-like habit with width and thickness of 20-30 μm and 5 μm, respectively, and vapor-liquid-solid interface growth of hBN whiskers with lengths and diameters as large as 70 μm and 5 μm, respectively. Similar growth mechanisms were seen for samples enriched in either isotope. Isotopic analysis via secondary-ion mass spectrometry showed boron concentrations of 84.4 at% and 93.0 at% for the majority isotopes in the 10B-rich and 11B-rich samples, respectively. Raman spectroscopy showed an increase in peak Raman shift for the 10B-rich sample, having two barely resolved peaks at 1393.5 and 1388.8 cm-1, and a decrease for the 11B-rich sample, having peak at 1359.5 cm-1 (FWHM of 9.4 cm-1), compared to that of natural hBN, with its peak at 1365.8 cm-1 (FWHM of 10.3 cm-1). Raman shift showed a linear trend with increasing 10B concentration allowing for a calibration curve to be developed to estimate 10B enrichment in hBN using non-destructive methods.

Alternate aluminum and arsenic precursors were investigated for InAlAs grown by organometallic vapor phase epitaxy (OMVPE). The quality of the InAlAs growths was investigated by secondary-ion mass spectrometry (SIMS) to measure impurity concentrations. Trends are extracted from SIMS measurements for each precursor as a function of V/III ratio and growth temperature. Two arsenic precursors, arsine and tertiarybutylarsine (TBAs), were chosen to compare InAlAs growth quality. The impurity concentrations measured by SIMS decrease as the V/III ratio increases, for both arsine and TBAs growths. Impurities also decrease as growth temperature increases. Two aluminum precursors, trimethylaluminum (TMAl) and tritertiarybutylaluminum (TTBAl), were used to compare the effect of alumimum precursor on carbon and oxygen impurity levels. TMAl is widely studied in literature, though TTBAl is less common. This study represents the first report using the TTBAl precursor for InAlAs growth. Each aluminum source is used in conjunction with each aforementioned arsenic precursor in order to compare all possible precursor combinations. TMAl growths demonstrated decreasing impurities with increasing V/III ratio. TTBAl growths did not exhibit such a dependence, impurity concentrations remained virtually constant regardless of V/III ratio.

The electrical and electromechanical properties of lithium niobate single crystals are investigated at high-temperatures. The total electrical conductivity is determined as a function of temperature by impedance spectroscopy for Z-cut crystals with different lithium content. For stoichiometric lithium niobate (sLN) the activation energy is found to be (1.49 ± 0.03) eV in the temperature range from 500 to 900 °C.

Further, the piezoelectric properties (resonance frequency, Q-factor) of X-cut lithium niobate crystals are determined at high temperatures for samples with compositions ranging from congruent to stoichiometric and, subsequently, compared to the conductivity data in order to identify loss contributions.

In this context, the high-temperature stability is examined for X- and Z-cut samples with compositions ranging from congruent to stoichiometric. Series of samples with and without additional alumina protection layers are annealed in air at 900 °C for approximately 50 h. Subsequently, depth profiles are measured by SNMS. In all cases, no lithium loss is observed and, therefore, a high-temperature stability of sLN for at least 50 h at 900 °C can be assumed in ambient air.

Further, the influence of protective layers with different thicknesses and compositions is investigated for X- and Z-cut samples. A lithium loss in the first 300 nm is observed for the Z-cut samples, while the X-cut samples show a behavior dependent on the type of protecting layer.

The ability of nano secondary ion mass spectrometry (NanoSIMS) to locate and analyze Raman active gold core nanoparticles (R-AuNPs) in a biological system is compared with the standard analysis using the scanning electron microscope (SEM). The same cell with R-AuNPs on and inside the macrophage was analyzed with both techniques to directly compare them. SEM analysis showed a large number of nanoparticles within the cell. Subsequent NanoSIMS analysis showed fewer R-AuNPs with lower spatial resolution. SEM was determined to be superior to NanoSIMS for the analysis of inorganic nanoparticles in complex biological systems.

Experiments were performed to incorporate Li and N simultaneously into the diamond lattice during hot-filament chemical vapour deposition in an attempt to produce n-type semiconducting diamond with useful electronic characteristics. Microcrystalline diamond films were grown using a mixture of methane/ammonia/hydrogen gases with tantalum as the filament. The Li was added by placing crystals of lithium nitride (Li3N) on the substrate and allowing them to melt and then slowly diffuse into the film. SIMS depth profiles showed that this process produced high levels of Li and N (0.05% - 0.5%) situated in the same region within the diamond film. The crystallinity and morphology of diamond crystals produced were confirmed using laser Raman spectrometry and scanning electron microscopy.

Commercially available bulk silicon carbide (SiC) has a high number (>2000/cm2) of screw dislocations (SD) that have been linked to degradation of high-field power device electrical performance properties. Researchers at the NASA Glenn Research Center have proposed a method to mass-produce significantly higher quality bulk SiC. In order for this bulk growth method to become reality, growth of long single crystal SiC fibers must first be achieved. Therefore, a new growth method, Solvent-Laser Heated Floating Zone (Solvent-LHFZ), has been implemented. While some of the initial Solvent-LHFZ results have recently been reported, this paper focuses on further characterization of grown crystals and their growth fronts. To this end, secondary ion mass spectroscopy (SIMS) depth profiles, cross section analysis by focused ion beam (FIB) milling and mechanical polishing, and orientation and structural characterization by X-ray transmission Laue diffraction patterns and X-ray topography were used. Results paint a picture of a chaotic growth front, with Fe incorporation dependant on C concentration.

The possibility and suitability of micro-Raman spectroscopy as a noncontact, in-line measurement technique for boron (B) concentration in ultrathin (20~35 nm thick) Si1–xGex layers epitaxially grown on 300 mm diameter p−-Si(100) wafers, by ultrahigh vacuum chemical vapor deposition, was investigated. Raman spectra from Si1–xGex/Si(100) wafers were measured under 363.8, 457.9, 488.0, and 514.5 nm excitation. Strong correlation was found between B content and characteristics of the Si–Si Raman peak from the Si1–xGex films. As B concentration increased from undoped to 9.1 × 1020 atoms/cm3, the Si–Si Raman peak broadened and the peak height became smaller for a given Ge content. The B concentration in Si1–xGex film estimated from Raman measurement was in good agreement with secondary ion mass spectroscopy analysis results. Boron concentration as low as 8.7 × 1017 atoms/cm3 can be detected by Raman spectroscopy, which is ~30 times more sensitive than the detection limit (2.7 × 1019 atoms/cm3) of high-resolution x-ray diffraction.

Ion implantation of Ge2Sb2Te5 (GST) enables localized doping of the film by using conventional lithography. Although the doped region dimensions and the doping concentration profile are defined by the opening in the mask and the ion energy, longitudinal and lateral straggling of implanted ions leads to a spread in the ions final location. Additionally, a thermal treatment such as one that induces a phase transition may lead to redistribution of the implanted dopants and further increase the spread. In this work we demonstrate doping of GST by ion implantation. Using Secondary Ion Mass Spectrometry (SIMS) we studied the as-implanted doping profiles obtain by ion implantation of carbon and silicon into GST. We also investigated by SIMS the dopant redistribution following a recrystallization annealing. The as-implanted ion profiles were found to be in fair agreement with TRIM simulation. The dopants profiles show little change after a crystallization annealing at 200°C for silicon doping and at 350°C for carbon doping.

The present work reports surface segregation in polycrystalline yttria-stabilised zirconia (cubic) including 10 mol% Y2O3 (10YSZ). The 10YSZ specimen was annealed in the range 1073 K - 1673 K in the gas phase of controlled oxygen activity. The segregation-induced intensity profiles of 89Y, 40Ca, 28Si, 27Al, 133Cs, 197Au and 90Zr was measured using secondary ion mass spectrometry (SIMS). The data obtained show that (i) annealing of 10YSZ results in the formation of segregation-induced concentration gradients of 89Y, 40Ca, 28Si, 27Al and (ii) segregation-induced profiles depend on oxygen activity.

We propose a new technique to fabricate 4H-SiC metal–oxide–semiconductor field-effect transistors (MOSFETs) with high inversion channel mobility. P atoms were incorporated into the SiO2/4H-SiC(0001) interface by post-oxidation annealing using phosphoryl chloride (POCl3). The interface state density at 0.2 eV from the conduction band edge was reduced to less than 1 × 1011 cm−2eV−1 by the POCl3 annealing at 1000 °C. The peak field-effect mobility of 4H-SiC MOSFETs on (0001) Si-face processed with POCl3 annealing at 1000 °C was approximately 90 cm2/Vs. The high channel mobility is attributed to the reduced interface state density near the conduction band edge.

Following containment failure in the scenario of geological disposal of spent nuclear fuel, the penetration rate of groundwater into the UO2 matrix could cause a rapid increase of the fraction of inventory becoming available for prompt dissolution. In this respect, oxygen and water diffusion mechanisms are key issues to investigate. In this work, secondary-ion-mass-spectrometry (SIMS) depth profiling has been applied to characterize a polycrystalline UO2 pellet exposed to 18O-labelled water at room temperature. 18O depth profiling up to 25 μm beneath the pellet surface clearly indicates a combination of oxygen diffusion into the UO2 lattice and water diffusion along grain boundaries, behaving as high diffusivity paths. The lattice diffusion coefficient of oxygen, DL , and the quantity δDB – product of the grain boundary width, δ, and the grain boundary diffusion coefficient of water, DB – have been measured, resulting in DL = (2.5 ± 0.1) × 10-24 m2 s-1 and δDB = (7.5 ± 0.3) × 10-24 m3 s-1.

At 1100 °C, the diffusion properties of Ti4+ into congruent LiNbO3 crystals codoped with 0.5 mol% Er2O3 and different MgO concentrations of 0.5, 1.0, and 1.5 mol% have been studied by secondary ion mass spectrometry (SIMS). Three Y-cut and three Z-cut plates with different Mg doping levels were coated with a 60-nm-thick Ti film at first and then annealed at 1100 °C for 28 h in a wet O2 atmosphere. SIMS was used to analyze depth profile characteristics of diffused Ti ions and the constituent elements of the substrate as well. The results show that the diffusion reservoir was exhausted and the Ti metal film was completely diffused. All measured Ti profiles follow a Gaussian function. No Mg out-diffusion accompanied the Ti in-diffusion procedure for all crystals studied. The 1/e diffusion depth is similar to 8.3/10.2, 7.4/8.7, and 6.6/8.2 ± 0.2/0.2 μm/μm for the Y/Z-cut crystal with the Mg doping level of 0.5, 1.0, and 1.5 mol%, respectively, yielding a Ti4+ diffusivity of 0.62/0.93, 0.49/0.67, and 0.39/0.60 ± 0.03/0.03 (μm2/h)/(μm2/h), respectively. The diffusion shows definite anisotropy and a considerable MgO doping level effect. Under the same Mg doping level, the diffusion in a Z-cut crystal is faster. The diffusivity decreases with the increase of the Mg doping level. This effect is qualitatively explained from the viewpoint of the Mg doping effect on concentration of the intrinsic defects in LiNbO3 crystal.