氮化铝铬的制备及其光学性质

利用直接氮化法得到了氮化铝和氮化铬,并用两种途径得到Cr³⁺掺杂的氮化铝样品。用X射线衍射仪分析了样品晶相并测试了两种样品的激发和发射光谱,计算了晶体场劈裂参数D_q和Racah参数B及D_q/B分别为1 800,693.69和2.59。光谱数据表明,Cr³⁺在氮化铝中属于强场环境,光发射来自于最低激发态²E能级,与在氧化铝中的环境相似。根据光谱数据给出了Cr³⁺在氮化铝晶体场中的能级。     

FORMATION OF A BURIED LAYER OF ALUMINIUM NITRIDE BY HIGH DOSE N2+ IMPLANTATION INTO ALUMINIUM

Aluminium films with various thickness between 700 nm and 1μm were deposited on Si (100) substrates, and 400 keV N₂⁺ ions with doses ranging from 4.3×10¹⁷ to 1.8×10¹⁸ N/cm² were implanted into the alu-minium films on silicon, Rutherford Backscattering (RBS) and channeling, secondary ion mass spectroscopy (SIMS), Fourier transform infrared spectra (FTIR), X-ray diffraction (XRD), transmission electron microscopy (TEM) and spreading resistance probes (SRP) were used to characterize the synthesized aluminium nitride. The experiments showed that when the implantation dose was higher than a critical dose N_c, a buried stoichiometric AlN layer with high resistance was formed, while no apparent AlN XRD peaks in the as-implanted samples were observed; however, there was a strong AlN(100) diffraction peak appearing after annealing at 500 ℃ for 1h. The computer program, Implantation of Reactive Ions into Silicon (IRIS), has been modified and used to simulate the formation of the buried AlN layer as N₂⁺ is implanted into aluminium. We find a good agreement between experimental measurements and IRIS simulation.     

A combined 14N/27Al nuclear magnetic resonance and powder X-ray diffraction study of impurity phases in beta-sialon ceramics

Beta-sialons are ceramic phases occurring in the SiO(2)-Si(3)N(4)-AlN-Al(2)O(3) system. A series of samples with differing compositions has been investigated by magic-angle spinning nuclear magnetic resonance (NMR) spectroscopy and powder X-ray diffraction (XRD). Although the constituent nitrogen nuclei occupy positions of low symmetry in the beta-sialon structure, 14N NMR spectra could be recorded for the samples examined. The origin of the 14N signal could be traced to the presence of an aluminium nitride (AlN) impurity phase with the help of 27Al NMR and XRD results. Similarly, the existence of Al(2)O(3) grains could be readily detected for a number of samples. Thus, the combination of 14N and 27Al NMR is shown to be an especially effective tool in identifying and characterizing impurity phases in sialon ceramics, complementing the results obtained from standard XRD analysis.     

Effect of Crucibles on Qualities of Self-Seeded Aluminium Nitride Crystals Grown by Sublimation

Self-seeded aluminium nitride （AlN） crystals are grown in tungsten and hot pressed boron nitride （HPBN） crucibles with different shapes by a sublimation method. The qualities of the AlN crystals are characterized by high-resolution transmission electronic microscopy （HRTEM）, scanning electron microscopy （SEM） and Micro-Rarnan spectroscopy. The results indicate that the better quality crystals can be collected in conical tungsten crucible.     

Landscape of s-triazine molecule on Si(100) by a theoretical x-ray photoelectron spectroscopy and x-ray absorption near-edge structure spectra study

The chemisorbed structure for an aromatic molecule on a silicon surface plays an important part in promoting the development of organic semiconductor material science. The carbon K-shell x-ray photoelectron spectroscopy(XPS) and the x-ray absorption near-edge structure(XANES) spectra of the interfacial structure of an s-triazine molecule adsorbed on Si(100) surface have been performed by the first principles, and the landscape of the s-triazine molecule on Si(100) surface has been described in detail. Both the XPS and XANES spectra have shown their dependence on different structures for the pristine s-triazine molecule and its several possible adsorbed configurations. By comparison with the XPS spectra, the XANES spectra display the strongest structural dependency of all of the studied systems and thus could be well applied to identify the chemisorbed s-triazine derivatives. The exploration of spectral components originated from non-equivalent carbons in disparate local environments has also been implemented for both the XPS and XANES spectra of s-triazine adsorbed configurations.     

Influence of N+ ion implantation at different temperatures on nanostructural modifications and characteristics of Al alloy surface

Thick (3.0 mm) Al samples (7049 an alloy with 15 elements) were implanted by N⁺ ions of 30 keV energy and fluence of 5 × 10 ¹⁷ N⁺ cm^?2 at different temperatures. The surface modification of the samples was studied using X-ray diffraction (XRD) and atomic force microscope (AFM) analysis. XRD spectra of the samples clearly showed the formation of different phases of AlN. Crystallite sizes (coherently diffracting domains) obtained from AlN diffraction lines showed that at a certain substrate temperature the crystallite size decreases considerably. AFM images showed the formation of grains on Al samples, and it was observed that both grain size and sample surface roughness first decrease and then increase with temperature (i.e. a minimum at a certain temperature is observed). In addition at this temperature, a minimum of intensity is also observed for the intensity of different phases of AlN and the intensity ratio of AlN (200)/AlN (311). This phenomenon is similar to those obtained for thin films and pure metal foils though the sample studied in this work is an Al alloy and the minimum for Al occurred at a value three times larger than that reported for the above cases. Alloy nature of this sample with 14 elements is responsible for the observed results because they may act as defects. Results may also be affected by the residual gases, substrate temperature, dissociation of water in the chamber and the ion energy. Results also showed that the processes of Al nitride and Al oxide formations are competing with each other; decrease of aluminium nitride phases are associated with increase of aluminium oxide phases.     

Structural and optical studies of thin films of aluminum nitride grown via ion-plasma sputtering on gallium arsenide substrates with different orientations

IR and UV spectroscopy is used to study the properties of nanostructured aluminum nitride films obtained via reactive ion-plasma sputtering on GaAs substrates with different orientations. Nanostructured thin (100–200 nm) films of cubic aluminum nitride with optical bandgaps of ~5 eV and refractive indices varying from 1.6 to 4.0 in the wavelength range of ~250 nm are fabricated. Growth on a misoriented GaAs(100) substrate (4° with respect to the [110] plane) makes it possible to synthesize AlN films with smaller grains and higher refractive indices (n ~ 4). It is shown that misoriented GaAs substrates allow us to control the morphology, surface composition, and optical functional characteristics of AlN/GaAs heterophase systems.     

Growth of AlN on clean and oxidised polycrystalline iron: an Auger study

The growth of aluminium nitride (AlN) thin films on clean and oxidised polycrystalline iron was studied by Auger electron spectroscopy. The films of AlN were deposited by reactive RF sputtering (argon + nitrogen atmosphere). On clean iron, a modelisation of the Auger peak-to-peak intensities evidences a Stranski-Krastanov growth mode (one layer followed by island formation) with an interfacial layer made of iron nitride covered by the AlN. Results on oxidised iron suggested the growth of a two-phase film with stoichiometry gradient of the (AlN)_x(Al₂O₃)_1−x form, x increasing with the film thickness. Grains of AlN in the layer were shown to favour the diffusion of oxygen from the substrate to the film until thicknesses of about 80 monolayers are reached. The presence of grains of both phases supports the hypothesis of an island growth mode for this interface.     

Influence of substrate temperature and ion-beam energy on the syntheses of aluminium nitride thin films by nitrogen-ion-assisted pulsed-laser deposition

Aluminium nitride (AlN) thin films have been grown on Si(100), Si(111) and Sapphire Al₂O₃(001) substrates by pulsed KrF excimer laser (wavelength 248 nm, duration 30 ns) ablation of an AlN target with the assistance of nitrogen-ion-beam bombardment. The influence of process parameters such as substrate temperature and ion-beam energy has been investigated in order to obtain high-quality AlN films. The AlN films deposited by pulsed-laser deposition (PLD) have been characterized by X-ray diffraction (XRD) to determine the crystalline quality, grain size and growth orientation with respect to the substrate. The XRD spectra of AlN films on Si(100), Si(111) and Sapphire substrates yield full-width-half-maximum (FWHM) values of approximately 1.6. The bonding characteristics in the films have been evaluated by Raman spectroscopy. The chemical composition of the films has been characterized by X-ray photoelectron spectroscopy (XPS). The surface morphology of the films has been measured by atomic force microscopy (AFM). At a substrate temperature of at least 600 °C, polycrystalline AlN films with orientations of AlN(100) and AlN(101) have been synthesized. PACS 68.55.-a; 81.15.Fg; 77.84.Bw     

X-ray spectroscopic identification of garnet from the placer deposits of the Taman peninsula

Garnet from recent placer deposits of the Taman peninsula has been investigated by energy-dispersive X-ray fluorescence microanalysis and X-ray absorption near-edge structure (XANES) spectroscopy. Energy-dispersive X-ray fluorescence microanalysis showed that the chemical composition of the garnet under study corresponds to pyrope-almandine-spessartine series. The Fe K-edge X-ray absorption spectra of garnet have been recorded using a Rigaku R-XAS laboratory spectrometer. Iron K-edge XANES spectra for two iron-containing garnet minals (components), almandine and andradite, have been calculated using the full multiple-scattering and finite-difference methods. Based on a comparison of the experimental and theoretical Fe K-XANES spectra, it is concluded that recent magnetite-garnet placer deposits of the Taman peninsula contain garnet in the form of almandine.     

Solvothermal synthesis of nitrides

Abstract

III-V nitrides are large band-gap semiconductors. They are very promising materials for opto-electronic and microelectronic applications.

The present paper deals with a new process for preparing nitrides. Two nitrides, gallium nitride (GaN) and aluminium nitride (AlN), have been synthesiaed through a solvothermal route. This process uses ammonia in supercritical conditions as solvent and metals as source of gallium and aluminium. Moreover, an additive is used to improve the nitridation of the metals.

The resulting microcrystallites of nitrides have been charactensed by X-ray diffraction and the morphology has been observed by scanning Electron Microscopy.     

Electron spectroscopy study in the NbN growth for NbN/AlN interfaces

NbN superconductor and wide band gap AlN thin films were deposited using sputtering at room temperature. Study of the nitride interfaces are forerunner to the growth Josephson junctions that are considered able to work in the terahertz frequency. We find that to be compatible with lithography technology and to have a high critical transition temperature, the substrate should not be overheated, and this means working in low power regime to limit the induced heating of the plasma. X-ray photoelectron spectroscopy and X-ray diffraction analysis were performed on samples deposited on crystalline, amorphous, flexible, and nanostructured substrates. The experimental results suggest us how to improve the deposition process in order to obtain the best nitride films as well as NbN/AlN/NbN trilayers for Josephson junction applications.     

Low-temperature synthesis of AlN films through electron cyclotron resonance plasma-aided reactive pulsed laser deposition

Combination of pulsed laser ablation with electron cyclotron resonance microwave discharge was demonstrated for a novel method for low-temperature thin film growth. Aluminum nitride thin films were synthesized on silicon substrates at temperatures below 80 °C by means of reactive pulsed laser deposition in nitrogen plasma generated from the electron cyclotron resonance discharge. The synthesized films show a very smooth surface and were found to have a stoichiometric AlN composition. X-ray photoelectron spectroscopy analysis evidenced the formation of aluminum nitride compound. Fourier transform infrared spectroscopy revealed the characteristic phonon modes of AlN. The AlN films were observed to be highly transparent in the visible and near-IR regions and have a sharp absorption edge near 190 nm. The band gap of the synthesized AlN films was determined to be 5.7 eV. The mechanisms responsible for the low-temperature film synthesis are also discussed in the paper. The nitrogen plasma facilitates the nitride formation and enhances the film growth. Received: 17 March 2000 / Accepted: 28 March 2000 / Published online: 23 May 2001     

K‐edge XANES analysis of sulfur compounds: an investigation of the relative intensities using internal calibration

Sulfur K‐edge XANES (X‐ray absorption near‐edge structure) spectroscopy is an excellent tool for determining the speciation of sulfur compounds in complex matrices. This paper presents a method to quantitatively determine the kinds of sulfur species in natural samples using internally calibrated reference spectra of model compounds. Owing to significant self‐absorption of formed fluorescence radiation in the sample itself the fluorescence signal displays a non‐linear correlation with the sulfur content over a wide concentration range. Self‐absorption is also a problem at low total absorption of the sample when the sulfur compounds are present as particles. The post‐edge intensity patterns of the sulfur K‐edge XANES spectra vary with the type of sulfur compound, with reducing sulfur compounds often having a higher post‐edge intensity than the oxidized forms. In dilute solutions (less than 0.3–0.5%) it is possible to use sulfur K‐edge XANES reference data for quantitative analysis of the contribution from different species. The results show that it is essential to use an internal calibration system when performing quantitative XANES analysis. Preparation of unknown samples must take both the total absorption and possible presence of self‐absorbing particles into consideration.     

Tensile strength of aluminium nitride films

Two-layered aluminium nitride (AlN)/silicon nitride microbridges were fabricated for microbridge tests to evaluate the elastic modulus, residual stress and tensile strength of the AlN films. The silicon nitride layer was added to increase the robustness of the structure. In a microbridge test, load was applied to the centre of a microbridge and was gradually increased by a nano-indenter equipped with a wedge tip until the sample was broken, while displacement was recorded coherently. Measurements were performed on single-layered silicon nitride microbridges and two-layered AlN/silicon nitride microbridges respectively. The data were fitted to a theory to derive the elastic modulus, residual stress and tensile strength of the silicon nitride films and AlN films. For the AlN films, the three parameters were determined to be 200, 0.06 and 0.3?GPa, respectively. The values of elastic modulus obtained were consistent with those measured by conventional nano-indentation method. The tensile strength value can be used as a reference to reflect the maximum tolerable tensile stress of AlN films when they are used in micro-electromechanical devices.     

X-ray spectra and electronic band structure of nitrogen in Al<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>Ga<Subscript>1−<Emphasis Type="Italic">x</Emphasis></Subscript>N solid solid solutions

The electronic energy structure of the valence band and the x-ray absorption near edge structure (XANES) region of nitrogen in Al _x Ga_1?x N solid solutions and binary crystals of gallium nitride GaN and aluminum nitride AlN are calculated using the local coherent potential method and the cluster version of the muffin-tin approximation within the framework of the multiple scattering theory. It is demonstrated that the calculated electron densities of states correlate with the nitrogen K x-ray emission and nitrogen K x-ray absorption spectra. The electronic energy structure of the top of the valence band and the XANES region in Al _x Ga_1?x N solid solutions are compared with those in the binary crystals of the GaN and AlN nitrides, and an interpretation of their specific features is proposed. An analogy is drawn between the evolution of the electronic energy structure of the valence band and the XANES region in the alloys under investigation and the evolution of the electronic band structure in the Al _x B_1?x N and B _x Ga_1?x N alloys. General trends in the transformation of the structure and variations in properties of these alloys are discussed.     

Spiral resonator manufactured on AlN ceramics to filter the coupled wave between patch antennas

The objective of this paper was to present an alternative technique of manufacturing the unit cells of spiral-shaped resonators (SR) on the aluminium nitride (AlN) ceramics. In this technique the AlN plane surface is irradiated by the Yb:glass medium-power laser (1.06 µm). As a result of the irradiation by a focused laser beam (a laser beam power up to 20 W), the rupture of the aluminium and nitrogen physical bonds occurs. Under such circumstances the conductive aluminium “paths” are formed on the originally insulating ceramic surface. Upon obtaining low ohmic conductive paths, this method makes for the feasible manufacturing of metamaterial structures. In carried out studies, the usage of such structures to suppress the coupling between pairs of patch antennas has been examined. The improvement of the mutual coupling at the level of 10 dB has been obtained. One of the advantages of the demonstrated method is a possibility to perform the selective and direct metallization of the AlN ceramics surface without using any mask as opposed to photolithography. It greatly reduces the implementation time of the projected metamaterial structures.     

Chloride Assisted Growth of Aluminum Nitride Nanobelts and Their Enhanced Dielectric Responses

通过氯化物辅助的气-固生长方法成功地制备出了大量单晶的氮化铝纳米带. X射线衍射、透射电子显微镜以及选区衍射分析表明,所制备的纳米带是纯度高、结构均匀的单晶体,并具有六方的晶体结构. 显微观察表明所获得的氮化铝纳米带没有缺陷,其生长方向为[0001]方向. 测量了产物在50 Hz 到5 MHz范围内的介电频谱,谱图分析表明样品中的界面对样品的介电特性有很大的影响. 室温条件下,与氮化铝微米粉相比,氮化铝纳米带的介电常数高得多,并在低频情况下尤为显著.     

Luminescence of thulium-activated cubic boron nitride

Under high pressure and temperature conditions, we have obtained samples of thulium-activated cubic boron nitride in the form of micropowders, ceramics, and polycrystals activated by thulium in the presence of aluminum. We studied the cathodoluminescence (CL), photoluminescence (PL), and photoluminescence excitation spectra of the samples. In the luminescence spectra we observe structured bands with maxima at ∼370, ∼475, ∼660, and ∼ 800 nm, assigned to electronic transitions in the triply charged thulium ions. We have established that the most efficient method for excitation of “blue” luminescence at ∼475 nm for thulium ions in cBN is excitation by an electron beam. The cBN samples synthesized in the presence of Al have photoluminescence spectra with a more complex structure compared with samples not containing Al, with the band of dominant intensity at about 660 nm. Hypothetically, this is a consequence of incorporation of thulium ions into the crystalline phases cBN and AlN, which are equally likely to be formed during synthesis. The observed photoluminescence spectrum of the indicated samples is the superposition of the photoluminescence spectra of the Tm³⁺ ions located in the crystal fields of cBN and AlN of different symmetries. The presence in the photoluminescence excitation spectra (at 450, 490, and 660 nm) of structure, with features at wavelengths shorter than the excited photoluminescence, suggests a nonresonant mechanism for its excitation. We have established that luminescence of Tm³⁺ ions is less intense than for other rare earth elements incorporated into cubic boron nitride. __________ Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 75, No. 4, pp. 547–555, July–August, 2008.