In-depth analysis of InAlN/GaN HEMT heterostructure after annealing using angle-resolved X-ray photoelectron spectroscopy

During high-electron-mobility transistor elaboration process, a thermal treatment of In_0.2Al_0.8N (InAlN) barrier layer is performed in order to improve electrical performances. We showed previously that In_0.2Al_0.8N/GaN heterostructures, annealed at 850°C under O₂ partial pressure, present a specific in-depth organization. Angle-resolved X-ray photoelectron spectroscopy is a powerful tool to precisely determine the spatial localization and relative position of the different interfaces, from InAlN until buried GaN layer. The proposed in-depth model of the stack evidences (1) an Al-rich surface oxide with embedded N₂ molecules, (2) an interlayer of InAlN_<1 governed by nitrogen lattice defects, (3) a stable In_0.2Al_0.8N matrix, and finally (4) the GaN buffer layer underneath.     

An IR Spectroscopic Investigation of Nanostructured AlN and GaN Powder Surfaces

By combining the results of IR spectroscopy experiments, both in the transmission and diffuse reflectance modes, with data obtained by HRTEM, XRD and XPS an overall picture of AlN and GaN nanoparticle surface structures and functionality were deduced. The surface species from the IR data analysis indicated that the nanostructured AlN powder surfaces had acidic and weak basic sites in the form of Al³⁺ and Al₃N^–, respectively. Also present were -OH, -NH₂, and -NH. For GaN, the bulk core of the particle had a zincblendel (FCC) structure with nitrogen vacancies, and the only functionality detected was Ga–H. The surface of the particles had a wurtzite(HCP) structure, with abundant NH and NH₂ groups as well as OH and Ga³⁺ functionalities.     

纳米六方相氮化铝的合成和光学性能研究

报道了以AlCl₃和Mg₃N₂为反应物, 在500 ℃条件下, 用简易的设备, 合成六方相AlN纳米材料. 样品的XRD和XPS图谱表明, 实验得到的AlN样品是纯的六方相AlN, 其中的杂质相含量均小于仪器的探测灵敏度. TEM图表明, AlN样品呈多孔网络状结构, 网络的骨架大小在10～20 nm之间. 对AlN样品的光学性能的研究表明, AlN样品的禁带宽度值约为6.12 eV; 红外吸收谱以680 cm^－1为中心形成一个很宽的红外吸收带; 其拉曼散射峰较AlN薄膜和AlN单晶向低波数方向移动.     

利用高分辨X射线衍射仪表征GaN薄膜的结构特性

使用高分辨X射线衍射法(HRXRD)对金属有机物化学气相沉积(MOCVD)外延生长GaN薄膜进行微结构表征.首先采用绝对测量法精确测试了GaN薄膜的晶格常数,由此获得该GaN薄膜的应变与弛豫的信息.采用面内掠入射(IP-GID)法测定了GaN薄膜的位错密度以及位错扭转角.     

Quantitative SIMS depth profiling of Al in AlGaN/AlN/GaN HEMT structures with nanometer‐thin layers

The possibilities of quantitative secondary ion mass spectrometry (SIMS) depth profiling of Al in AlxGa1 ? xN/AlN/GaN transistor heterostructures are shown. Using a series of test structures for a TOF.SIMS‐5 time‐of‐flight mass spectrometer, we obtained a refined linear calibration dependence of the secondary‐ion yield on the composition ×, namely, Y(CsAl+)/Y(CsGa+) = K × x/(1 ? x), with a high linear correlation coefficient, Rl = 0.9996, which permits quantitative SIMS analysis of relatively thick AlGaN barrier layers. The method of profile reconstruction with allowance for the main artifacts of ion sputtering has been first applied for the analysis of GaN/AlGaN/AlN/GaN high electron mobility transistor structure. This method permits to perform quantitative analysis of the thickness and composition of a nanometer‐thin AlN sublayer and to estimate the measurement error. For the structure being studied, the AlN sublayer is 1.2 ± 0.2 nm thick. Copyright © 2016 John Wiley & Sons, Ltd.     

Properties of nanostructured GaN prepared by different methods

Various methods have been employed to prepare nanostructured GaN exhibiting reasonable surface areas. The methods include ammonolysis of γ-Ga₂O₃ or Ga₂O₃ prepared in the presence of a surfactant, and the reaction of a mixture of Ga₂O₃ and Ga(acac)₃ with NH₃. The latter reaction was also carried out in the presence of H₃BO₃. All the methods yield good GaN samples as characterized by X-ray diffraction, electron microscopy and photoluminescence measurements. Relatively high surface areas were obtained with the GaN samples prepared by the ammonolysis of γ-Ga₂O₃ (53 m² g⁻¹), and of Ga₂O₃ prepared in the presence of a surfactant (66 m² g⁻¹). GaN obtained by the reaction of NH₃ with a mixture of Ga₂O₃, Ga(acac)₃ and boric acid gave a surface area of 59 m² g⁻¹. GaN nanoparticles prepared by the nitridation of mesoporous Ga₂O₃ samples generally retain some porosity.     

Deposition of Gallium Nitride Thin Films by MOCVD in Microwave Plasma

The deposition of GaN thin films in a nitrogen–hydrogen microwave plasma using Ga(CH ₃ ) ₃ as a gallium precursor was investigated. The deposit was identified as stoichiometric GaN by XPS and XRD. The substrate was dielectrically heated in the microwave discharge and the substrate temperature was lower than that in usual thermal MOCVD. The NH radicals, which were the primary N-atoms precursors, and fragments of Ga(CH ₃ ) ₃ were identified in the plasma by OES. The NH radical formation and the decomposition of Ga(CH ₃ ) ₃ in the plasma may be one of the reasons for the lower deposition temperature of GaN. The position dependence of the substrate temperature showed similar tendency as the position dependence of the electron temperature. The plasma state contributes to the deposition of GaN thin films. The deposited GaN exhibited a wide optical band gap of 3.4eV. Material highly oriented along the c axis was detected in the deposit, and a PL spectrum which has the band head at about 450 mm was obtained.     

Evaluation of GaN and In0.2Ga0.8N Semiconductors as Potentiometric Anion Selective Electrodes

The response of potentiometric anion selective electrodes consisting of undoped GaN or In_0.2Ga_0.8N films grown on Al₂O₃ (sapphire) was measured in electrolyte solutions of F^?, NO₃^?, Cl^?, SCN^?, ClO₄^? or Br^? anions at concentrations ranging from 10^?6 to 10^?1 M. The slope of the linear regions varied between ?32.8 and ?51.9 mV/decade for the GaN electrode and between ?31.0 and ?72.0 mV/decade for the In_0.2Ga_0.8N electrode. The drift of the GaN electrode reached 1.57 mV/day in KNO₃ solutions, whereas the drift of the In_0.2Ga_0.8N electrode could not be evaluated due to large drops in the slope of its linear range over time. Both electrodes were sensitive to pH variations over the pH range from 12.8 to 1.3. The GaN electrode surface could be electrochemically etched under anodic polarization; however, both GaN and In_0.2Ga_0.8N electrodes remained chemically stable and mechanically intact under open circuit conditions even after prolonged use.     

Structural and magnetic impact of Cr+-implantation into GaN thin film

Thin films of GaN with thickness of 2 μm were synthesized on sapphire. Cr⁺ ions were implanted into GaN with150 keV energy at a fluence of 3 × 10¹⁵ cm⁻². The annealing of the samples was carried out for a short time using rapid thermal annealing (RTA). Structural properties of the implanted samples were undertaken by XRD and Rutherford backscattering. The annealed samples demonstrated lattice recovery and damages caused by implantation. The structural properties were also studied by High-resolution X-ray Diffraction (HRXRD). Magnetic measurements of the samples were performed by Alternating Gradient Magnetometer (AGM) at room temperature and by SQUID in the range of 5–380 K. The SQUID results showed ferromagnetic behavior at T = 5 K and above 380 K for Cr⁺-implanted GaN.     

A study on electrodeposited of ZnO/ZnS heterostructures

ZnO/ZnS heterostructures were synthesized by a two steps electrochemical deposition method. Firstly, ZnS layer was deposited from an aqueous solution containing Na₂S₂O₃ and ZnSO₄ onto indium-doped tin oxide (ITO) coating glass substrate at two deposition potentials. Then, ZnO nanostructures were deposited from an aqueous solution of Zn(NO₃) onto ZnS surface. The as-obtained samples were characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray diffraction (XRD), Raman and UV-visible analysis. The results indicate that the electrodeposition of ZnS layer at ?0.9 V give the best proprieties of ZnO/ZnS heterostructures. Homogeneous and uniform surface of ZnO/ZnS heterostructure was confirmed by AFM images. The XRD patterns indicates a high crystallinity of ZnO/ZnS. A high transmittance of 65% was also noted from UV-Visible spectra and band gap energy as large as 3.6?eV was found.     

Ion induced controlled modifications in structural and optical properties of indium oxide thin films – studies with 25‐keV Co− and N+ beam implantations

Two sets of indium oxide thin films (~150 nm) grown on quartz substrates using thermal evaporation technique were processed separately with 25‐keV Co^? and N⁺ ions with several fluences ranging from 1.0 × 10¹⁵ to 1.0 × 10¹⁶ ions/cm². The pristine and the ion implanted films were characterized by Rutherford backscattering spectroscopy (RBS), X‐ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and UV–Vis spectrometry. The RBS spectra reveal signature of only cobalt and nitrogen in accordance to their fluences confirming absence of any contamination arising due to ion implantation. An increase in the average crystallite size (from 13.7 to 15.3 nm) of Co^? ions implanted films was confirmed by XRD. On the other hand, the films implanted with N⁺ ions showed a decrease in the average crystallite size from 20.1 to 13.7 nm. The XRD results were further verified by SEM micrographs. As seen in AFM images, the RMS surface roughness of the samples processed by both ion beams was found to decrease a bit (29.4 to 22.2 nm in Co^? implanted samples and 24.2 to 23.3 nm in N⁺ implanted samples) with increasing fluence. The Tauc's plot deduced from UV–visible spectroscopy showed that the band gap decreases from 3.54 to 3.27 eV in Co^? implanted films and increases from 3.38 to 3.58 eV for films implanted with N⁺ ions. The experimental results suggest that the modifications in structural and optical properties of indium oxide films can be controlled by optimizing the implantation conditions. Copyright © 2017 John Wiley & Sons, Ltd.     

Structural,morphological, optical and sensing properties of SnSe and SnSe2 thin films as a gas sensing material

In this work, orthorhombic tin selenide thin films were grown onto three different substrates using an organophosphorus precursor (Ph₃PSe) via chemical vapor deposition. Structural, microstructural and morphological properties of the as-grown films were systematically investigated using XRD, ESEM and AFM respectively. Grain size, microstrain and dislocation were calculated and correlated with different factors. The effects of selenization temperature and substrate type on different film properties and gas sensing response of films deposited onto alumina substrates were investigated. XRD analysis reveals the appearance of a mixed phase as a function of temperature. Furthermore, substrate type plays a key role in the rate of appearance of each phase. EDAX analysis confirms the existence of the desired elements and detect the evaporation of selenium and the appearance of oxygen at higher temperatures. Atomic force microscopy (AFM) was used to investigate the surface topography of the grown thin films.Optical properties of the films grown onto glass and silicon substrates were studied. From the recorded optical data, a direct optical band gap in the range of 0.9–1.3 eV was obtained with an absorption coefficient α > 10⁴ cm⁻¹ throughout large spectral regions. Optical studies were remarkably affected by the obtained phase as well as the selenization temperature. Gas sensing properties of the samples deposited onto alumina substrates were examined as a new sensing material for detection of methane gas at different concentrations. SnSe sensors show high sensitivity, are reversible and exhibit fast response and recovery times compared to SnSe₂ sensors.     

Powder‐XRD and 14N magic angle‐spinning solid‐state NMR spectroscopy of some metal nitrides

Some metal nitrides (TiN, ZrN, InN, GaN, Ca₃N₂, Mg₃N₂, and Ge₃N₄) have been studied by powder X‐ray diffraction (XRD) and ¹⁴N magic angle‐spinning (MAS) solid‐state NMR spectroscopy. For Ca₃N₂, Mg₃N₂, and Ge₃N₄, no ¹⁴N NMR signal was observed. Low speed (ν_r = 2 kHz for TiN, ZrN, and GaN; ν_r = 1 kHz for InN) and ‘high speed’ (ν_r = 15 kHz for TiN; ν_r = 5 kHz for ZrN; ν_r = 10 kHz for InN and GaN) MAS NMR experiments were performed. For TiN, ZrN, InN, and GaN, powder‐XRD was used to identify the phases present in each sample. The number of peaks observed for each sample in their ¹⁴N MAS solid‐state NMR spectrum matches perfectly well with the number of nitrogen‐containing phases identified by powder‐XRD. The ¹⁴N MAS solid‐state NMR spectra are symmetric and dominated by the quadrupolar interaction. The envelopes of the spinning sidebands manifold are Lorentzian, and it is concluded that there is a distribution of the quadrupolar coupling constants Q_cc's arising from structural defects in the compounds studied. Copyright © 2015 John Wiley & Sons, Ltd.     

Effects of nitridation durations on the synthesis of wurtzite GaN thin films by spin coating method

In this paper, the effects of nitridation durations on the structural, surface morphologies and lattice vibrational properties of gallium nitride (GaN) thin films grown via spin coating method were reported. X-ray diffraction (XRD) results revealed that all the deposited GaN thin films have wurtzite structure and with GaN(002) preferred orientation. In addition, the crystallinity of the GaN thin films increases with increasing of nitridation durations from 15 to 75 min while it degrades at 105 min. Field-emission scanning electron microscopy observations showed that GaN thin films with hexagon grains were formed at nitridation duration of 45 and 75 min, whereas rose-like microstructures were formed at nitridation duration of 105 min. P-polarized infrared reflectance measurements demonstrated that the reststrahlen feature of GaN thin films gradually increases from 15 to 75 min and diminished at 105 min, which is consistent with the XRD results. Finally, all the results revealed that the duration of 75 min was the most efficient time for the nitridation process.     

Metal-Organic Chemical Vapor Deposition (MOCVD) Synthesis of Heteroepitaxial Pr0.7Ca0.3MnO3 Films: Effects of Processing Conditions on Structural/Morphological and Functional Properties

Calcium-doped praseodymium manganite films (Pr_0.7Ca_0.3MnO₃, PCMO) were prepared by metal-organic chemical vapor deposition (MOCVD) on SrTiO₃ (001) and SrTiO₃ (110) single-crystal substrates. Structural characterization through X-ray diffraction (XRD) measurements and transmission electron microscopy (TEM) analyses confirmed the formation of epitaxial PCMO phase films. Energy dispersive X-ray (EDX) and X-ray photoelectron spectroscopy (XPS) characterization was used to confirm lateral and vertical composition and the purity of the deposited films. Magnetic measurements, obtained in zero-field-cooling (ZFC) and field-cooling (FC) modes, provided evidence of the presence of a ferromagnetic (FM) transition temperature, which was correlated to the transport properties of the film. The functional properties of the deposited films, combined with the structural and chemical characterization collected data, indicate that the MOCVD approach represents a suitable route for the growth of pure, good quality PCMO for the fabrication of novel spintronic devices.     

XPS study of impurities in Si‐doped AlN film

This paper reports an XPS study of impurities in a 100‐nm‐thick AlN film grown by metalorganic chemical vapor deposition (MOCVD) under low pressure on the n‐type 6H‐SiC substrate. The Si‐doped AlN film was characterized by the X‐ray photoelectron spectroscopy (XPS) in a high vacuum system, which reveals the content distribution and chemical states of impurities along depth. The XPS analysis of AlN film before and after argon‐ion etching indicates that there always exist Ga, O and C contaminations in AlN film. Especially, O contamination on the AlN film surface is mostly introduced during the growth of AlN layer by MOCVD. Meanwhile, most of O atoms bind with Al or Ga in Al―O and Ga―O chemical states. In particular, the Ga atoms in AlN film are always in two chemical states, i.e. Ga―Ga bond and Ga―O bond, which demonstrates that the aggregation of Ga is accompanying with AlN growth. Copyright © 2016 John Wiley & Sons, Ltd.     

The investigation of Ag decorated double‐wall hollow TiO2 spheres as photocatalyst

In this paper, a novel TiO₂ nanosheets assembled double‐wall hollow sphere (DHS)has been prepared successfully via hydrothermal treatment of SiO₂@TiO₂ with the assistant of CTAB.The prepared samples are characterized with transmission electron microscopy (TEM), scanning electron microscopy (SEM), electron spin resonance (ESR), X‐ray diffraction (XRD) and X‐ray photoelectron spectra (XPS), etc.Results show that redeposited silica species play a key role in the formation of the double‐wall structure. The as‐synthesized DHS nanostructure exhibits a large surface area (417.6 m² g^‐1) and excellent mechanical strength. Furthermore, after decoration of Ag and calcination treatment, the double‐shelled TiO₂/Ag heterostructures show an enhanced photocatalytic performance in the degradation of RhB under UV or visible light irradiations for the following reasons: the surface plasmon resonance effect of Ag, strong interaction between Ag and TiO₂ nanosheets, large surface area, excellent adsorption capacityand unique double‐wall structure. On the basis of the experimental results, a possible mechanism for pollutantdegradation under visual light irradiation has been proposed.     

Effect of repetition nanoindentation of GaN epilayers on a‐axis sapphire substrates

In this work, gallium nitride (GaN) epilayers were deposited on a‐axis sapphire substrate by means of metal organic chemical vapor deposition (MOCVD). Berkovich nanoindentation was used to explore the repetition pressure‐induced impairment of the GaN film. The observation of load‐displacement vs stress‐strain curves concludes that basal slip is implicated in the deformation on the A plane GaN. The increase in the hardness (H) and elastic modulus (E) was determined from cyclic nanoindentation, and resulted in a crack due to the formation of incipient slip bands and/or the to‐and‐fro motion of mobile dislocation. It is indicated that the generation of individual dislocation and residual deformation of the GaN films are showed by CL mapping analysis. From the morphological studies, it is revealed that the crack was found by means of atomic force microscope (AFM) technique at nine loading/reloading cycles even after the indentation beyond the critical depth on the residual indentation impression. Copyright © 2010 John Wiley & Sons, Ltd.     

Coating of anatase titania on clinoptilolite by metal organic chemical vapor deposition method: enhanced mesoporosity and photocatalytic activity

Clinoptilolite-supported TiO₂ (TiO₂/CP_MOCVD) has been synthesized by metal organic chemical vapor deposition method (MOCVD). Titanium precursor was evaporated at 110 °C under nitrogen flow rate to promote the surface interaction between titanium species and clinoptilolite. The effect of titanium precursor on the crystalline structure and the surface area of clinoptilolite were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), transformed infrared spectroscopy (FT-IR), Raman spectroscopy, and Brunauer–Emmett–Teller measurement. XRD and SEM results indicate that TiO₂ precursor interacted with the support, decreasing the crystallinity of the clinoptilolite. The analysis by FT-IR spectroscopy further confirms that the titanium species were bound to clinoptilolite through Ti–O–Si bonds. The TiO₂/CP_MOCVD catalyst showed a mesoporous structure with the distribution of pores in several dimensions 3.7–7.1 nm, with high specific surface area (~ 471 m²/g). MOCVD improved the adsorption capacity of the catalyst surface towards the pollutants. TiO₂/CP_MOCVD particles turn yellow after adsorption of salicylic acid. The development of the yellow color is a clear indication of the formation of charge transfer titanium (IV) salicylate surface complex. Photocatalytic decomposition of SA in aqueous solution was carried out using TiO₂/CP_MOCVD. Experimental results revealed that TiO₂/CP_MOCVD required shorter irradiation time (120 min) for complete decomposition of SA than commercial P25 Degussa and TiO₂/CP_imp (clinoptilolite-supported TiO₂ using impregnation method). The TiO₂/CP_MOCVD can be recycled at least four times without loss in activity, indicating their magnificent stability.     

Ag作催化剂制备的GaN的形貌及其性能

用化学气相沉积法(CVD)在Si(100)衬底上以Ag纳米颗粒为催化剂制备了微纳米结构的GaN,原料是熔融态的金属Ga和气态的NH3。采用X射线衍射仪(XRD)、透射电镜(TEM)、X-ray能谱仪(EDS)、场发射扫描电子显微镜(SEM)、光致发光能谱(PL)和霍尔效应测试对样品进行了结构、成分、形貌和发光、电学性能分析。结果表明:生成的自组装GaN为六方纤锌矿的类似小梯子的微纳米单晶结构,且在不同的温度下,GaN的发光性能和电学性能也有所不同,相对于强的紫外发光峰,其它杂质发光峰很微弱,且均呈p型导电。对本实验所得到的GaN微纳米结构的可能形成机理进行了探讨。