scholarly journals Low Temperature Nitridation Combined With High Temperature Buffer Annealing for High Quality GaN Grown by Plasma-Assisted MBE

Author(s):  
Gon Namkoong ◽  
W. Alan Doolittle ◽  
Sangbeom Kang ◽  
Huang Sa ◽  
April S. Brown ◽  
...  

The effect of the initial nitridation of the sapphire substrate on the GaN crystal quality as a function of substrate temperature was studied. GaN layers were grown by plasma-assisted molecular beam epitaxy (MBE) on sapphire substrates nitridated at different substrate temperatures. A strong improvement in the GaN crystal quality was observed at 100 °C nitridation temperature. Symmetric (0004) and asymmetric (10-5) full widths at half maximum (FWHM) of the x-ray rocking curves were 136 and 261 arcsec, respectively. This compares to an x-ray rocking curve full width at half maximum of 818 arcsec (0004) for conventional MBE buffer conditions. For our conventional buffer conditions, sapphire substrates were exposed to a N plasma at temperatures above 500 °C for 10min and then 25~50nm buffers were deposited without annealing at high temperature. The low temperature nitridation also shows an enhancement of the lateral growth of the GaN, resulting in larger grain sizes. The largest grain size achieved was approximately 2.8μm, while the average grain size was approximately 2.4μm at 100 °C nitridation temperature.

2021 ◽  
pp. 174751982098472
Author(s):  
Lalmi Khier ◽  
Lakel Abdelghani ◽  
Belahssen Okba ◽  
Djamel Maouche ◽  
Lakel Said

Kaolin M1 and M2 studied by X-ray diffraction focus on the mullite phase, which is the main phase present in both products. The Williamson–Hall and Warren–Averbach methods for determining the crystallite size and microstrains of integral breadth β are calculated by the FullProf program. The integral breadth ( β) is a mixture resulting from the microstrains and size effect, so this should be taken into account during the calculation. The Williamson–Hall chart determines whether the sample is affected by grain size or microstrain. It appears very clearly that the principal phase of the various sintered kaolins, mullite, is free from internal microstrains. It is the case of the mixtures fritted at low temperature (1200 °C) during 1 h and also the case of the mixtures of the type chamotte cooks with 1350 °C during very long times (several weeks). This result is very significant as it gives an element of explanation to a very significant quality of mullite: its mechanical resistance during uses at high temperature remains.


2001 ◽  
Vol 672 ◽  
Author(s):  
Kathleen A. Dunn ◽  
Katharine Dovidenko ◽  
Anna W. Topol ◽  
Serge R. Oktyabrsky ◽  
Alain E. Kaloyeros

ABSTRACTZinc sulfide doped with manganese is extensively used for thin film electroluminescent device applications. In order to assess the key material and process challenges, ZnS:Mn layers were fabricated by metalorganic chemical vapor deposition in the 250°-500°C range on an AlTiO/InSnO/glass stack. The microstructure of the ZnS:Mn films was examined by Transmission Electron Microscopy (TEM) as part of a larger study which fully characterizes these films by a variety of structural and chemical characterization techniques, including Rutherford Backscattering, Secondary Ion Mass Spectroscopy, Atomic Force Microscopy, Scanning Electron Microscopy and X-ray Diffraction. For all the growth conditions, the films were found to be polycrystalline having predominantly 2H hexagonal ZnS structure. The ZnS grains are found to grow columnar as the film thickness increases, also widening in the direction parallel to the substrate surface and reaching the 100 - 200 nm average lateral size at the 650 nm film thickness. The presence of the 8H ZnS polytype was detected in the low-temperature ZnS:Mn films by TEM selected area electron diffraction and confirmed by X-ray diffraction analysis. Dark field TEM imaging correlated this 8H ring with very small (∼2.5 nm) grains present throughout the low temperature film with a slightly higher density at the film/substrate interface. The 700°C post-deposition annealing was found to initiate a solid state transformation to the cubic (3C) ZnS crystal structure, and resulted in an average grain size of ∼250 nm at the surface of the annealed film.


1961 ◽  
Vol 5 ◽  
pp. 276-284
Author(s):  
E. L. Moore ◽  
J. S. Metcalf

AbstractHigh-temperature X-ray diffraction techniques were employed to study the condensation reactions which occur when sodium orthophosphates are heated to 380°C. Crystalline Na4P2O7 and an amorphous phase were formed first from an equimolar mixture of Na2HPO4·NaH2PO4 and Na2HPO4 at temperatures above 150°C. Further heating resulted in the formation of Na5P3O10-I (high-temperature form) at the expense of the crystalline Na4P4O7 and amorphous phase. Crystalline Na5P3O10-II (low-temperature form) appears after Na5P3O10-I.Conditions which affect the yield of crystalline Na4P2O7 and amorphous phase as intermediates and their effect on the yield of Na5P3O10 are also presented.


Metals ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 645
Author(s):  
Igor Litovchenko ◽  
Sergey Akkuzin ◽  
Nadezhda Polekhina ◽  
Kseniya Almaeva ◽  
Evgeny Moskvichev

The effect of high-temperature thermomechanical treatment on the structural transformations and mechanical properties of metastable austenitic steel of the AISI 321 type is investigated. The features of the grain and defect microstructure of steel were studied by scanning electron microscopy with electron back-scatter diffraction (SEM EBSD) and transmission electron microscopy (TEM). It is shown that in the initial state after solution treatment the average grain size is 18 μm. A high (≈50%) fraction of twin boundaries (annealing twins) was found. In the course of hot (with heating up to 1100 °C) plastic deformation by rolling to moderate strain (e = 1.6, where e is true strain) the grain structure undergoes fragmentation, which gives rise to grain refining (the average grain size is 8 μm). Partial recovery and recrystallization also occur. The fraction of low-angle misorientation boundaries increases up to ≈46%, and that of twin boundaries decreases to ≈25%, compared to the initial state. The yield strength after this treatment reaches up to 477 MPa with elongation-to-failure of 26%. The combination of plastic deformation with heating up to 1100 °C (e = 0.8) and subsequent deformation with heating up to 600 °C (e = 0.7) reduces the average grain size to 1.4 μm and forms submicrocrystalline fragments. The fraction of low-angle misorientation boundaries is ≈60%, and that of twin boundaries is ≈3%. The structural states formed after this treatment provide an increase in the strength properties of steel (yield strength reaches up to 677 MPa) with ductility values of 12%. The mechanisms of plastic deformation and strengthening of metastable austenitic steel under the above high-temperature thermomechanical treatments are discussed.


2010 ◽  
Vol 654-656 ◽  
pp. 1106-1109
Author(s):  
Ya Qiong He ◽  
Chang Hui Mao ◽  
Jian Yang

Nanocrystalline Fe-Co alloy powders, which were prepared by high-energy mechanical milling, were nitrided under the mixing gas of NH3/H2 in the temperature range from 380°C to 510°C. X-ray diffraction (XRD) was used to analyze the grain size and reaction during the processing. The magnetic properties of the nitrided powders were measured by Vibrating Sample Magnetometer (VSM). The results show that with the appearance of Fe4N phase after nitride treatment, and the grain-size of FeCo phase decreases with the increase of nitridation temperature between 380°C to 450°C.The saturation magnetization of nitrided alloy powder treated at 480°C is about 18% higher than that of the initial Fe-Co alloy powder, accompanied by the reduction of the coercivity. Transmission electron microscope (TEM) was used, attempting to further analyze the effect of Fe4N phase on microstructure and magnetic properties of the powder mixtures.


2007 ◽  
Vol 29-30 ◽  
pp. 143-146 ◽  
Author(s):  
Aamir Mukhtar ◽  
De Liang Zhang ◽  
C. Kong ◽  
P. R. Munroe

Cu-(2.5 or 5.0vol.%)Al2O3 nanocomposite balls and granules and Cu-(2.5vol.% or 5.0vol.%)Pb alloy powder were prepared by high energy mechanical milling (HEMM) of mixtures of Cu and either Al2O3 or Pb powders. It was observed that with the increase of the content of Al2O3 nanoparticles from 2.5vol.% to 5vol.% in the powder mixture, the product of HEMM changed from hollow balls into granules and the average grain size and microhardness changed from approximately 130nm and 185HV to 100nm and 224HV, respectively. On the other hand, HEMM of Cu–(2.5 or 5.0vol.%) Pb powder mixtures under the same milling conditions failed to consolidate the powder in-situ. Instead, it led to formation of nanostructured fine powders with an average grain size of less than 50nm. Energy dispersive X-ray mapping showed homogenous distribution of Pb in the powder particles in Cu–5vol.%Pb alloy powder produced after 12 hours of milling. With the increase of the Pb content from 2.5 to 5.0 vol.%, the average microhardness of the Cu-Pb alloy powder particles increases from 270 to 285 HV. The mechanisms of the effects are briefly discussed.


2010 ◽  
Vol 25 (3) ◽  
pp. 471-475 ◽  
Author(s):  
Sea-Hoon Lee ◽  
Byung-Nam Kim ◽  
Hidehiko Tanaka

Al8B4C7 was used as a sintering additive for the densification of nano-SiC powder. The average grain size was approximately 70 nm after sintering SiC-12.5wt% Al8B4C7 at 1550 °C. The densification rate strongly depended on the sintering temperature and the applied pressure. The rearrangement of SiC particles occurred at the initial shrinkage, while viscous flow and liquid phase sintering became important at the middle and final stage of densification.


2019 ◽  
Vol 51 (1) ◽  
pp. 513-530 ◽  
Author(s):  
Zhenbo Zhang ◽  
Éva Ódor ◽  
Diana Farkas ◽  
Bertalan Jóni ◽  
Gábor Ribárik ◽  
...  

Abstract Nanocrystalline materials reveal excellent mechanical properties but the mechanism by which they deform is still debated. X-ray line broadening indicates the presence of large heterogeneous strains even when the average grain size is smaller than 10 nm. Although the primary sources of heterogeneous strains are dislocations, their direct observation in nanocrystalline materials is challenging. In order to identify the source of heterogeneous strains in nanocrystalline materials, we prepared Pd-10 pct Au specimens by inert gas condensation and applied high-pressure torsion (HPT) up to γ ≅ 21. High-resolution transmission electron microscopy (HRTEM) and molecular dynamic (MD) simulations are used to investigate the dislocation structure in the grain interiors and in the grain boundary (GB) regions in the as-prepared and HPT-deformed specimens. Our results show that most of the GBs contain lattice dislocations with high densities. The average dislocation densities determined by HRTEM and MD simulation are in good correlation with the values provided by X-ray line profile analysis. Strain distribution determined by MD simulation is shown to follow the Krivoglaz–Wilkens strain function of dislocations. Experiments, MD simulations, and theoretical analysis all prove that the sources of strain broadening in X-ray diffraction of nanocrystalline materials are lattice dislocations in the GB region. The results are discussed in terms of misfit dislocations emanating in the GB regions reducing elastic strain compatibility. The results provide fundamental new insight for understanding the role of GBs in plastic deformation in both nanograin and coarse grain materials of any grain size.


Nanomaterials ◽  
2019 ◽  
Vol 9 (11) ◽  
pp. 1600 ◽  
Author(s):  
Alexander Tkach ◽  
André Santos ◽  
Sebastian Zlotnik ◽  
Ricardo Serrazina ◽  
Olena Okhay ◽  
...  

If piezoelectric micro-devices based on K0.5Na0.5NbO3 (KNN) thin films are to achieve commercialization, it is critical to optimize the films’ performance using low-cost scalable processing conditions. Here, sol–gel derived KNN thin films are deposited using 0.2 and 0.4 M precursor solutions with 5% solely potassium excess and 20% alkali (both potassium and sodium) excess on platinized sapphire substrates with reduced thermal expansion mismatch in relation to KNN. Being then rapid thermal annealed at 750 °C for 5 min, the films revealed an identical thickness of ~340 nm but different properties. An average grain size of ~100 nm and nearly stoichiometric KNN films are obtained when using 5% potassium excess solution, while 20% alkali excess solutions give the grain size of 500–600 nm and (Na + K)/Nb ratio of 1.07–1.08 in the prepared films. Moreover, the 5% potassium excess solution films have a perovskite structure without clear preferential orientation, whereas a (100) texture appears for 20% alkali excess solutions, being particularly strong for the 0.4 M solution concentration. As a result of the grain size and (100) texturing competition, the highest room-temperature dielectric permittivity and lowest dissipation factor measured in the parallel-plate-capacitor geometry were obtained for KNN films using 0.2 M precursor solutions with 20% alkali excess. These films were also shown to possess more quadratic-like and less coercive local piezoelectric loops, compared to those from 5% potassium excess solution. Furthermore, KNN films with large (100)-textured grains prepared from 0.4 M precursor solution with 20% alkali excess were found to possess superior local piezoresponse attributed to multiscale domain microstructures.


2005 ◽  
Vol 891 ◽  
Author(s):  
Shin-ichiro Uekusa ◽  
Kunitoshi Aoki ◽  
Mohammad Zakir Hossain ◽  
Tomohiro Fukuda ◽  
Noboru Miura

ABSTRACTWe prepared β-FeSi2 thin-films by using a Pulsed Laser Deposition (PLD) method and succeeded to observe photoluminescence (PL) around 1.5 μm corresponding to β-FeSi2 band from the long-time and high-temperature annealed β-FeSi2 thin-films. The β-FeSi2 thin-films were ablated on Si(111) substrates heated at 550°C. After ablation, long-time and high-temperature thermal annealing was performed in order to improve the crystal-quality. Annealing times were 5, 10, 20 and 40 hrs, and annealing temperature was kept at 900 °C. Crystallinity was evaluated by an X-ray diffraction (XRD) measurement. We have observed eminent improvement on crystal-quality of β-FeSi2 thin-films. Annealed samples show (220) or (202) X-ray diffraction signals of β-FeSi2 and the full width at half maximum (FWHM) of these peaks were 0.27° although the thickness of the samples decreased with annealing time. Thermal-diffusion of Si atoms was observed from substrate to thin-films. Fe atoms in the ablated thin-films also diffused into the substrate. The relationship between the thickness of β-FeSi2 thin-films and the thermal-diffusion were investigated with rutherford backscattering (RBS) measurement. Maximum photoluminescence intensity around 1.5 μm was observed from the thickest β-FeSi2 thin-film with only 5 hrs annealing.


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