scholarly journals Induced Crystallization In CW Laser-Irradiated Sol-Gel Deposited Titania Films

1993 ◽  
Vol 321 ◽  
Author(s):  
Gregory J. Exarhos ◽  
Nancy J. Hess

AbstractIsothermal annealing of amorphous TiO2 films deposited from acidic sol-gel precursor solutions results in film densification and concomitant increase in refractive index. Subsequent heating above 300°C leads to irreversible transformation to an anatase crystalline phase. Similar phenomena occur when such amorphous films are subjected to focused cw laser irradiation. Controlled variations in laser fluence are used to density or crystallize selected regions of the film. Low fluence conditioning leads to the evolution of a subtle nanograin-size morphology, evident in AFM images, which appears to retard subsequent film crystallization when such regions are subjected to higher laser fluence. Time-resolved Raman spectroscopy has been used to characterize irradiated regions in order to follow the crystallization kinetics, assess phase homogeneity, and evaluate accompanying changes in residual film stress.

1993 ◽  
Vol 316 ◽  
Author(s):  
Gregory J. Exarhos ◽  
Nancy J. Hess

ABSTRACTIsothermal annealing of amorphous TiO2 films deposited from acidic sol-gel precursor solutions results in film densification and concomitant increase in refractive index. Subsequent heating above 300°C leads to irreversible transformation to an anatase crystalline phase. Similar phenomena occur when such amorphous films are subjected to focused cw laser irradiation. Controlled variations in laser fluence are used to density or crystallize selected regions of the film. Low fluence conditioning leads to the evolution of a subtle nanograin-size morphology, evident in AFM images, which appears to retard subsequent film crystallization when such regions are subjected to higher laser fluence. Time-resolved Raman spectroscopy has been used to characterize irradiated regions in order to follow the crystallization kinetics, assess phase homogeneity, and evaluate accompanying changes in residual film stress.


1991 ◽  
Vol 230 ◽  
Author(s):  
Gregory J. Exarhos ◽  
Nancy J. Hess

AbstractTime-resolved micro-Raman spectroscopy is used to follow the amorphous to crystalline phase transformation in sol-gel deposited titania films induced thermally or through the action of applied hydrostatic pressure in a diamond anvil cell. Time-dependent phonon intensities intrinsic to the growing phase are related to the volume fraction of crystallite present at any time. The sigmoidally generated curves can be modeled in terms of modified Avrami ingrowth kinetics in which diffusion of the amorphous phase to the nucleation center is restricted by the morphology of the evolving phase. Phonon frequency and linewidth measurements during the course of the transformation probe changes in film stress and particle size which are used to understand the mechanistics of the transformation. Raman measurements also are used to derive a phase stability diagram for titania films.


Polymers ◽  
2021 ◽  
Vol 13 (10) ◽  
pp. 1572
Author(s):  
Baku Nagendra ◽  
Paola Rizzo ◽  
Christophe Daniel ◽  
Lucia Baldino ◽  
Gaetano Guerra

Poly(ʟ-lactide) (PLLA) films, even of high thickness, exhibiting co-crystalline and crystalline α phases with their chain axes preferentially perpendicular to the film plane (c⊥ orientation) have been obtained. This c⊥ orientation, unprecedented for PLLA films, can be achieved by the crystallization of amorphous films as induced by low-temperature sorption of molecules being suitable as guests of PLLA co-crystalline forms, such as N,N-dimethylformamide, cyclopentanone or 1,3-dioxolane. This kind of orientation is shown and quantified by two-dimensional wide-angle X-ray diffraction (2D-WAXD) patterns, as taken with the X-ray beam parallel to the film plane (EDGE patterns), which present all the hk0 arcs centered on the meridian. PLLA α-form films, as obtained by low-temperature guest-induced crystallization, also exhibit high transparency, being not far from those of the starting amorphous films.


RSC Advances ◽  
2016 ◽  
Vol 6 (98) ◽  
pp. 95601-95610 ◽  
Author(s):  
Yuko Ikeda ◽  
Preeyanuch Junkong ◽  
Takumi Ohashi ◽  
Treethip Phakkeeree ◽  
Yuta Sakaki ◽  
...  

Guayule and rubber dandelion natural rubbers are useful alternatives forHeveanatural rubber in terms of their strain-induced crystallization behaviours.


2011 ◽  
Vol 61 (2) ◽  
pp. 355-361 ◽  
Author(s):  
P. Karasiński ◽  
E. Gondek ◽  
S. Drewniak ◽  
I. V. Kityk

1987 ◽  
Vol 36 (3) ◽  
pp. 1595-1604 ◽  
Author(s):  
E. Huber ◽  
E. E. Marinero

2018 ◽  
Vol 24 (9) ◽  
pp. 1421-1427 ◽  
Author(s):  
Feng Liu ◽  
Shaoai Xie ◽  
Yan Wang ◽  
Jianjun Yu ◽  
Qinghua Meng

PurposeThe titania (titanium dioxide) is one of the important functional additives in the photosensitive resin and encounters the problem of stabilization in the photosensitive resin for 3D printing. This study aims to achieve enhancement in stabilization by preparation of the polymerizable titania andin situlaser-induced crystallization during 3D printing.Design/methodology/approachA type of polymerizable titania (AAEM@TiO2) was designed and prepared from tetrabutyl titanate (TBT) and 2-(acetoacetoxy)ethyl methacrylate (AAEM) via the sol–gel process, which was characterized by Fourier-transform infrared (FTIR) spectra, ultraviolet–visible (UV-Vis) spectra, surface bonding efficiency (SBE) and settling height (H). AAEM acted on both bonding to the titania and polymerization with the monomer in resin for stabilization. The polymerizable titania could be converted to the pigmented titania by means of laser-induced crystallization. The photosensitive resin was then formulated on the basis of optimization and used in a stereolithography apparatus (SLA) for 3D printing.FindingsThe stabilization effect of AAEM on TiO2was achieved and the mechanism of competition in the light-consuming reactions during photocuring was proposed. The ratio of nAAEM/nTBTin AAEM@TiO2, the concentration of AAEM@TiO2and photoinitiator (PI) used in the photosensitive resin were optimized. The anatase crystal form was indicated by X-ray diffraction (XRD) and clustering of nanocrystals was revealed by scanning electron microscopy (SEM) after SLA 3D printing.Originality/valueThis investigation provides a novel method of pigmentation by preparation of the polymerizable titania andin situlaser-induced crystallization for SLA 3D printing.


1988 ◽  
Vol 143 ◽  
Author(s):  
Dan Q. Wu ◽  
Benjamin Chu

AbstractStructural and dynamical properties of an aqueous gelatin solution (5 wt%, 0.1M NaCi, pH=7) in a sol-gel transition were studied by time-resolved small angle x-ray scattering (SAXS) and dynamic light scattering (DLS) after quenching the gelatin sol at ∼45”C to 11°C. SAXS intensity measurements suggested the presence of gel fibrils which grew initially in cross-section. The average cross-section of the gel fibrils reached a constant value after an initial growth period of ∼800 sec. Further increase in SAXS intensity could be attributed to the increase in the length of the gel fibrils. Photon correlation, on the other hand, clearly showed two relaxation modes in both the sol and the gel (∼1 hr after the quenching process) states: a fast cooperative diffusion mode which remained constant from the sol to the gel state after correction for the temperature dependence of solvent viscosity; and a slow mode that could be attributed to the self-diffusion of the “free” gelatin chains and aggregates. The slow mode contribution to the time correlation function was reduced from ∼40% in sol to ∼20% in gel signaling a decrease but not the elimination of “free” particles in the gel network. The decrease in the intensity contribution by the slow mode is, however, accompanied by a large increase in the characteristic line-width distribution.


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