Physical vapor transport growth of mercurous chloride crystals

We have carried out experiments to derive a quantitative understanding of the physical vapor transport (PVT) process and to identify convective effects on the crystal growth process. The experimental growth velocity was several orders of magnitude lower than the theoretically predicted value. The effusion holes were used to disturb the impurity boundary layers. We observed a change of 18% (not an order of magnitude) in growth velocities. The Arrhenius behavior of growth rate with temperature was used to derive the sticking coefficient. Experimental result on growth velocity as the aspect ratio was varied showed that with increasing convection, the growth rate increased up to a certain value and then dropped to a constant value. This indicated that a bifurcation had occured with a resulting change in transport behavior.

Growth velocity measurements for the PVT process as a function of orientation of the g-vector were also made. The experimental results clearly showed that the growth velocity varied with g-vector for a particular temperature profile. The effects of convection on crystal quality were studied by varying the thermal conditions (source and crystal temperatures) which affects thermal convection during PVT. The results showed that crystals grown at low Rayleight numbers had better homogeneity. While no microgravity experiments were conducted, computation of mass flux for the horizontal orientation for various gravitational levels showed two distinct regions; above 10^-3 g where the flow was convective and strong circulating cells appeared, and also below 10^-3 g, where the flow was purely diffusive and no circulating cells were predicted. Therefore it is postulated that for the conditions of growth considered, space flight experiments with acceleration less than 10^-3 g could yield crystals grown under diffusive transport.     

A statistical thermodynamic model for oxygen segregation during Czochralski growth of silicon single crystals

A thermodynamic model derived from atomic scale statistics is formulated for the crystal–melt interface where oxygen segregation occurs during silicon crystal growth by the Czochralski method. The model shows that the segregation coefficient is close to but less than unity. Approaches for controlling oxygen concentration in the resulted crystal are discussed.     

Study of the evaporation mechanism in silicon carbide crystals growth from vapour phase

Investigation of the thermal etching (evaporation) of the source material in the process of silicon carbide crystal growth from the vapour phase by the sublimation method has been carried out. It has been established that silicon carbide etching in the temperature interval (2200–2600) °C takes place with the formation of whiskers of evaporation. The mechanism of their formation has been examined and the character of the whisker distribution in the charge of the source silicon carbide has been studied.     

Investigation of the thermal conditions during silicon carbide crystal growth

In the present work an analysis of the thermal conditions during silicon carbide crystal growth from the vapour phase by the sublimation method is carried out. On the basis of the obtained results from the calculation of the temperature distribution along the length of the growing crystal it was drawn a conclusion that in order to decrease the density of dislocations in the growing crystals it is necessary to decrease the temperature gradients in the crucible for growing.     

Processes of vapor phase growth of AIIBVI single crystals and structures based there upon

Results of investigations of semiconductor A^IIB^VI compounds (for example of CdTe and ZnTe) grown by the chemical vapor transport (CVT) method in a closed volume using three transfer agents containing a halogen, compound NH₄X (X = Cl, Br, I) are presented. The processes of vapor phase growth (composition of the vapor phase and mass transfer) in Me(Cd, Zn)Te–NH₄X (X = Cl, Br, I) systems have been calculated theoretically and the results are have been verified in growth experiments. Optoelectronic properties of the grown materials and barrier structures based there upon are discussed.     

Numerical investigation of carbon and silicon carbide contamination during the melting process of the Czochralski silicon crystal growth

Carbon contamination in single crystalline silicon is detrimental to the minority carrier lifetime, one of the critical parameters for electronic wafers. In order to study the generation and accumulation of carbon contamination, transient global modeling of heat and mass transport was performed for the melting process of the Czochralski silicon crystal growth. Carbon contamination, caused by the presence of carbon monoxide in argon gas and silicon carbide in the silicon feedstock, was predicted by the fully coupled chemical model; the model included six reactions taking place in the chamber. A simplified model for silicon carbide generation by the reaction between carbon monoxide and solid silicon was proposed using the closest packing assumption for the blocky silicon feedstock. The accumulation of carbon in the melted silicon feedstock during the melting and stabilization stages was predicted. Owing to this initial carbon content in the melt, controlling carbon contamination before the growth stage becomes crucial for reducing the carbon incorporation in a growing crystal.     

The role of dislocations in the formation of mechanical stresses during annealing of gallium arsenide single crystals

The effect of dislocations on the change of mechanical stresses in undoped semi-insulating gallium arsenide single crystals has been studied during their annealing in vacuum and in the arsenic atmosphere. The phenomena observed are explained by the effect of dislocations playing the role of channels for arsenic diffusion on the concentration of intrinsic point defects in the crystal regions surrounding dislocations. The mechanism of arsenic diffusion over dislocations allows one to consider dislocations as sources and sinks of arsenic without the translational and twinning processes and, thus, makes the well-known data on the reactions of dislocation interaction with point defects and the experimental structural data for single crystals more consistent.     

Crystal growth and structure of KBi(WO4)2 single crystals

Potassium bismuth tungstate [KBi(WO₄)₂] single crystals have been grown by the top‐seeded solution growth technique. Bulk crystal with dimensions up to several centimeters is obtained for the first time. Several self‐flux systems have been used for the growth from the solution and the experiments using K₂W₂O₇ as a solvent are detailed. Powder and single crystal X‐ray diffraction of this crystal are reported. The structure refinement shows that KBi(WO₄)₂ crystallizes in the monoclinic space group C2/c, with a=10.837(3), b=10.586(3), c=7.622(2)Å, β=130.860(3)°, V=661.4(3)ų, and Z=4. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Electrical properties and deep levels spectra of bulk SiC crystals grown by hybrid physical–chemical vapor transport method

Concentrations of nitrogen shallow donors, boron shallow acceptors, charge carriers, and electron traps were measured as a function of position along the growth axis in a series of undoped 6H–SiC boules grown by sublimation method with and without addition of hydrogen to the growth atmosphere. Elemental analysis by secondary ion mass spectrometry and measurements of electrical properties indicate that the addition of hydrogen suppresses nitrogen incorporation and formation of all electron traps. Concentration of boron is not affected by hydrogen presence. The addition of hydrogen to the growth ambient improves the uniformity of nitrogen incorporation and deep trap distribution along the growth axis. The results are interpreted as due to increased carbon transport and corresponding shift of crystal stoichiometry toward carbon-rich side of the SiC existence range.     

Doping behavior of sulfur during growth of GaAs from the vapor phase

A study has been made of sulfur doping from H₂S in the vapor growth of GaAs using the Ga-AsCl₃-H₂ system. In order to separate the effects of the gaseous components the AsH₃-HC1-Ga-H₂ system was also investigated. A linear relationship was found to exist between the measured electron concentrations and PH₂S over a wide range. The $\text{P}{}^{\mathrm{<mtext>-1</mtext><mtext>2</mtext>}}{}_{\mathrm{<mtext>AS</mtext>}}{}_4$ and P^-2_GaCl (or: P^-2_HCl or P^-1_GaCl or P^-1_HCl) dependence of the rate of sulfur uptake combined with the pronounced increase in this uptake upon approaching the exact <100 > orientation suggests that the process is kinetically limited. Some model considerations are presented, based on the hypothesis that the sulphur is competing for adsorption on As sites with the reactive components in the system.     

Epitaxial growth of graphitic carbon on C-face SiC and Sapphire by chemical vapor deposition (CVD)

Epitaxial, graphitic carbon thin films were directly grown on C-face/(0 0 0 1¯) SiC and (0 0 0 1) sapphire by chemical vapor deposition (CVD), using propane as a carbon source and without any catalytic metal on the substrate surface. Raman spectroscopy shows the signature of multilayer graphene/graphite growth on both the SiC and sapphire. Raman 2D-peaks have Lorentzian lineshapes with FWHM of ∼60 cm⁻¹ and the ratio of the D-peak to G-peak intensity (I_D/I_G) linearly decreases (down to 0.06) as growth temperature is increased. The epitaxial relationship between film and substrates were determined by X-ray diffraction. On both substrates, graphitic layers are oriented parallel to the substrate, but exhibit significant rotational disorder about the surface normal, and predominantly rhombohedral stacking. Film thicknesses were determined to be a function of growth time, growth temperature, and propane flow rate.     

Growth of corundum single crystals by the top-seeded solution growth technique (TSSG)

Single crystals of corundum were grown by the top-seeded solution growth technique from a cryolite, Na₃AlF₆, solvent. The relationship between the growth rate (mg/h) of a crystal and the temperature difference (= supersaturation) or the rotation rate of a seed crystal was investigated, and optimum growth conditions for obtaining single crystals with good quality are discussed.     

Influence of reduced working frequencies on the floating‐zone growth of silicon single crystals

Lowering the working frequency in the inductively heated floating zone growth of Si Single crystals will reduce the risk of arcing at the induction coil. This is of particular interest in the growth of large diameter crystals. In the current paper we present results from growth experiments at lower frequencies, 2 MHz and 1.7 MHz. It is found that the growth of dislocation‐free crystals is possible at these frequencies and cause distinct changes in the interface deflection and radial resistivity profiles. Results from numerical simulation of the melt flow at different frequencies are presented. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The Czochralski growth of doped bismuth-germanium oxide (BGO) and bismuth-silicon oxide (BSO) single crystals

Doped single crystals of BGO and BSO with Cr, Mn, Cu, Ni have been grown. The conditions for the growth of doped single crystals by the Czochralski method have been determined, analyses of distributions of dopants in the crystals have been made. For the Mn, Cr, Cu, doped crystals changes of coloration after illumination with visible light have been observed.     

Czochralski growth and constitutional studies on single crystals of potassium lithium niobate (KLN)

The ferroelectric phase of potassium lithium niobate K₃Li_2−xNb_5+xO₁₅ (KLN) is a very promising material for the conversion of infrared light to light in the visible region. However, growing of single crystals is known to be complicated due to the considerable anisotropy of the growth rate and the thermal expansion behaviour. The single crystals of KLN, Mg²⁺‐doped KLN, as well as the mixed crystals of potassium lithium tantalate niobate K₃Li₂(Nb_1−xTa_x)₅O₁₅ (KLTN) were grown by the Czochralski technique. The chemical analyses of the samples were performed by atomic absorption spectroscopy (AAS) and X‐ray fluorescence analysis (XRF). The element concentrations along the single crystals were measured by the electron microprobe analysis (EMPA) to clarify the segregation phenomena in the grown crystals. The elements distribution coefficients were also calculated. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Seeded growth of AlN on N- and Al-polar 〈0001〉 AlN seeds by physical vapor transport

We demonstrated seeded growth of AlN on large-area Al- and N-polar <0 0 0 1>-oriented AlN seeds using the physical vapor transport method (PVT). In both cases, crystals having a diameter of 15 mm were obtained from 5 mm seeds. Based on growth step and terrace width analyses, it was found that the N-polar face was suitable for growth within a large window of growth parameters while the Al-polar seeds yielded high-quality crystals only at low supersaturation.     

Solution growth of single crystals of 4-hydroxycyanobenzene (4HCB) suitable for electronic applications

Squared, platelet-like single crystals of 4-hydroxycyanobenzene (4HCB) have been grown from solutions based on ethylic ether and petroleum ether. Properly modifying the growth conditions, in terms of both solvent used for the growth and concentration of 4HCB in the starting solution, allowed one to tune the planar dimensions of the platelets in the range 2–6 mm, and their thickness in the range 150–600 μm. In this way samples well suited for desired practical manipulation and electronic measurements may be obtained. Moreover, lowering the growth temperature resulted in larger but still thin 4HCB crystals. The ability to tailor crystal thickness has allowed one to study their Space-Charge Limited Current (SCLC) behaviour along that dimension, showing that the so-contacted samples exhibit intrinsic-like bulk conduction behaviour, and are hence well suitable for electronic studies and applications.     

Growth of AlN single crystals on 6H‐SiC (0001) substrates with AlN MOCVD buffer layer

6H‐SiC (0001) deposited 300 nm thick AlN film by MOCVD was used as the substrate to grow AlN crystals by the physical vapour transport (PVT) method. It was confirmed that c‐axis oriented AlN films were grown and this material had a 3D growth mode. The root mean square (RMS) value for the film was measured to be 2.17 nm. Nucleation and further growth of AlN on so prepared substrate was investigated. Colorless and transparent AlN crystal with 1 mm thick and 40 mm in diameter was obtained after 4 h growth on this substrate. The transparent AlN showed strong (0001) texture XRD patterns, only the (0002) reflection was observed in symmetric θ‐2θ scans. The full width at half maximum for a (0002) X‐ray rocking curve was less than 0.1° indicating good crystalline quality. Anisotropic etchings in molten KOH shows that the growth (0001) plane exposed to the AlN source predominately has an aluminum polarity, no N‐polar inversion domains were observed. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)