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At the core, the quasi- plateau of crystallization appears at 80 s, which corre- sponds to 158 ? C.
These cookies help provide information on metrics the number of visitors, bounce rate, traffic source,
etc. After the end of the crystallization, the polymer is in semi-crystalline phase, pressure is
stabilized, and the specific volume variations are mainly controlled by the temperature evo- lution.
This heat flow difference is plotted against the temperature or time for obtaining a typical
thermogram, as shown in Figure 2. Log in to your Author Panel to purchase a book at the discounted
price. In particular, a drastic reduction of the superstructure reflections attributed to the periodically
spaced VLs becomes apparent. The sample society of this research consisted of 30 participants.
Crystallization in Microemulsions: A Generic Route to Thermodynamic Control and the Estimation
of Critical Nucleus Size By Sharon Cooper, Oliver Cook and Natasha Loines 2,730 6. The thermal
properties were used in the calculation of the free energy difference between amorphous and crystal
forms of indomethacin, which in combination with other measurements provided information for the
theoretical prediction of solubility. Figure 1 shows a schematic representation of these transitions.
This thesis shows that Dynamic Transmission Electron Microscopy (DTEM) is uniquely well suited
to study such fast, complex crystallization dynamics due to the combined 10 nm spatial and 15 ns
temporal resolutions. Advances in Lipids Crystallization Technology By Maria Aliciane Fontenele
Domingues, Ana Paula Badan Ribeiro. All authors have read and agreed to the published version of
the manuscript. A crystalline solid dispersion is the name given to the products containing a
crystalline API dissolved in a crystalline excipient. The specific volume of the crystalline phase was
described by a linear variation, where parameters were adjusted together with the absolute crystallin
ity of the polymer X ?, in order to obtain the best fit of the experimental results: ? ? 44,1.0723.481
103.861 10 c VTPT P ?? ????? 0.477 X ? (8) where T is in. A KrF excimer laser (Coherent Inc., Santa
Clara, CA, USA) with 248-nm wavelength, 20-ns pulse duration and 20-Hz repetition rate was used
to ablate a GST compound target. International Journal of Turbomachinery, Propulsion and Power
(IJTPP). At these conditions, the crystalline structure of inulin and morphology of the particles may
remain intact i.e., amorphous and with a spherical shape. The region a-GST in Figure 7 b reveals an
amorphous GST phase. It is now established that this theory is not consistent. Stability Indicating RP
HPLC Method Development and Validation of Everolimus. Please note that many of the page
functionalities won't work as expected without javascript enabled. They create a supersaturated
solution by evaporating the solvent of a saturated solution. This approach considers that the
solidification process of the polymer in the mold is similar to the quench of a slab, due to sudden
contact between the mold cold su rfaces and the hot polymer. Figures 6 and 7 show comparative
curves of the mea- sured and modeled relative crystallinity evolution, under isothermal and constant
cooling rate conditions. Any additional data relevant to this study are available from the author upon
reasonable request. Of particular interest is the understanding of the structural changes and
underlying mechanisms induced by short optical pulses. The powders obtained were subjected to
different levels of water adsorption, and Tg was identified from MDSC measurements. This
experimental procedure is schematically illustrated in Figure 3. For this study, the PVT experimental
results were ob- tained by using a piston-type dilatometer ( PVT 100) com- merciallized by SWO
HAAKE Polymertechnik GmbH.
Country Loading. Message of recommendation Dear Librarian. The following thermal cycles were
used to measure the heat capacity: first the sample was heated from 20. International Journal of
Turbomachinery, Propulsion and Power (IJTPP). Edited by Sudheer Neralla Chemical Vapor
Deposition. By analyzing the neutral cluster compounds, various influences on the lability of the Nb-
L bond were investigated and, considering intermolecular interactions, the requirements for a
particularly suitable niobium cluster precursor is discussed. Epitaxial GST thin films could, however,
offer the opportunity to follow even small structural changes without initiating a complete
amorphization. Previous Article in Journal White Graphene-Cobalt Oxide Hybrid Filler Reinforced
Polystyrene Nanofibers for Selective Oil Absorption. Dr. Martin Kockerling, University of Rostock
2nd reviewer: Prof. Previous Article in Special Issue Investigation on the Effect of Hyperbranched
Polyester Grafted Graphene Oxide on the Crystallization Behaviors of ? -Nucleated Isotactic
Polypropylene. Journal of Functional Morphology and Kinesiology (JFMK). The agreement between
the modeled evolutions and the experimental ones is fairly good. These interactions are termed as
incompatibilities. Thus, in order to avoid undesired physical changes such as crystallization and
chemical reactivity, it is very important to identify the conditions at which the molecular motion
processes begin. Scraped surface crystallizers are often grouped together in assemblies. Download
Free PDF View PDF See Full PDF Download PDF Loading Preview Sorry, preview is currently
unavailable. The thickness of the GST thin film was approximately 15 nm (estimated from the
Scherrer equation). The decoration was performed by exposing the CNW substrates directly to the
nanoparticles beam, in the MSGA setup. As PhD students, we found it difficult to access the research
we needed, so we decided to create a new Open Access publisher that levels the playing field for
scientists across the world. The processing chamber is part of a horizontal furnace (model CY-
O1200-50ICS from ZHENGHZOU CY SCIENTIFIC INSTRUMENT CO) and consists of a quartz
tube (external diameter 5 cm, length 60 cm) mounted inside a tubular oven. In order to be human-
readable, please install an RSS reader. Please note that many of the page functionalities won't work
as expected without javascript enabled. At initial time t 0, the temperature T 0 is as- sumed to be
homogeneous in the whole system, i.e. me- tallic block and polymer plate, and an initial pressure P 0
is fixed. This mix of phases probably leads to the slightly asymmetric reflections in the
corresponding XRD pattern shown at the bottom of Figure 6 a. Although it is possible to identify the
mentioned complex thermal events with a regular DSC coupled to a supercooling system, it is not
possible to differentiate the reversible from the non-reversible, since only one signal is acquired.
MDSC takes advantage of the modulation of temperature for calculating the heat capacity of the
sample during the same experiment, while it does not require cooling during modulation. Solvent-
Interactive Transformations of Pharmaceutical Compounds By Marique Elizabeth Aucamp, Wilna
Liebenberg and Nicole Stieger 2,255 1 2. Specifically, we want to show the benefits of the so-called
modulated differential scanning calorimetry (MDSC). In this multiphysical coupled model, all the
thermophysical parameters are temperature dependant. Our Authors and Editors We are a community
of more than 103,000 authors and editors from 3,291 institutions spanning 160 countries, including
Nobel Prize winners and some of the world’s most-cited researchers. Although the model geometry is
bidimensional, for the sake of simplicity, the boundary conditions are chosen such that the problem
reduces to a 1D case.
The determination of the crystallinity in the pharmaceutical industry is very important in the quality
control of raw materials, intermediate products, and final products, and to test the effectiveness of
technological procedures for processing control. In detail, the XRD results suggest an intracrystalline
phase transition from vo-GST to c-GST. In this paper, a complete experimental thermal
characterization of a semi-crystalline polymer is performed. The text is divided into four sections and
the conclusions. This technique is preferred over DSC to determine the Tg of solid materials. MDSC
was employed for obtaining the heat capacity changes at the glass transition temperature in order to
get the thermodynamic fragility (mT) of both systems. Additionally, other parameters such as the
dynamic fragility (mD), heating rate dependence of Tg (mDTg), the mean relaxation time, and the
glass-forming ability (GFA) were calculated in order to establish the relevance of these parameters to
the crystallization of amorphous drugs. Since the following stage of the process does not take place
at constant volume but at constant pressure, the pre- sent mathematical model is no longer relevant.
Particularly, this work demonstrates different structural transformations, such as crystalline-to-
amorphous phase changes, interface-assisted epitaxial crystallization, and phase transformations
within crystalline phases. The articles in this book have been contributed by some of the most
respected researchers in this area and cover the frontier areas of research and developments in
crystallization processes. Figure 10 shows temperature evolutions across the polymer thickness ? ? p
YYe. Editors select a small number of articles recently published in the journal that they believe will
be particularly. Gt as a function of time and temperature history is described by means of the
quiescent crystallization kinetics theories. All authors have read and agreed to the published version
of the manuscript. Different transitions may overlap for a single component material, e.g., the
recrystallization and melting of a semicrystalline material. In contrast, the devitrification temperature
(Tdv) corresponds to the temperature at which crystallization in a formerly crystal-free glass solid
occurs. A modification of the Schneider rate crystallization equations is proposed, allowing to
identify in a simple way all the crystallization kinetics parameters, using only DSC measurements.
Feature papers represent the most advanced research with significant potential for high impact in the
field. A Feature. For each experiment, tungsten powder (40 mg) was loaded on an alumina boat and
placed in the center of the quartz tube. These measurements provide qualitative and quantitative in-
formation on physico-chemical transformations such as crystallization, melting or glass transition.
The atomic concentrations of four major zones (O1s, C1s, N1s, W4f) are presented Table 1. Tg is
observed as a slight change in the slope of the curve. The tungsten oxide-carbon hybrid nanomaterial
was obtained through a sequence of processes consisting of oxidation of tungsten nanoparticles
followed by oxide sublimation, vapor transport and condensation on a nano-carbon template. MDSC
was used in combination with X-ray diffraction (XRD) and Fourier transform infrared spectroscopy
(FTIR) to examine the physical properties and find an explanation for the solubility behavior of the
samples. Early Tech Adoption: Foolish or Pragmatic? - 17th ISACA South Florida WOW Con. Paper
should be a substantial original Article that involves several techniques or approaches, provides an
outlook for. Syntheses and X-Ray Crystal Structures of Magnesium- Substituted Polyoxometalates
By Chika Nozaki Kato, Nami Ukai, Daisuke Miyamae, Shunya Arata. Bar diagram of the elemental
composition corresponding with the four major zones (C1s, O1s, N1s, W4f) for all three investigated
samples (CNW control sample, CNW after thermal treatments, respectively nanostructures obtained
after WO 3 decoration) in plasma on condition. Journal of Pharmaceutical and BioTech Industry
(JPBI). This is made possible by the EU reverse charge method. Gout, Urate, and Crystal Deposition
Disease (GUCDD).
You also have the option to opt-out of these cookies. Some Features of Growing Single Crystals of
Refractory Metals from the Melt By Vadim Glebovsky 2,266 12. However, they concluded that
sample preparation was imperative i.e., pellets conformation, since the pore volume and powder
surface area may affect the accuracy of the results. ArF Excimer Laser Annealing of Polycrystalline
Silicon Thin Film By Noriah Bidin and Siti Noraiza Ab Razak 7,938 19. In the food industry, DSC
and MDSC have been widely used in the study of the denaturation of proteins, carbohydrate
stability, and determining first and second-order transitions in lipids. C, for different pressures
ranging from 20 MPa to 160 MPa, and for a 5. Furthermore, all these characteristics change
depending on whether the polymer is in a solid or liquid state. The apparatus was first calibrated in
temperature and heat flow. Crystallization of Ge:Sb:Te Thin Films for Phase Change Memory
Application By J. J. Gervacio Arciniega, E. Therefore, in Figure 16 a is presented the deconvolution
of W4f, while in Figure 16 b the deconvolution for N1s specific region is presented. Herewith, the
experimental setup is represented by a horizontal furnace tube that allows simultaneous heating and
plasma ignition. Concerning the decoration process, it was proved to be very dependent on the
substrate position in the furnace. The correlation between the stability of dispersions and Tg is often
used to make judgments about the probable physical stability of amorphous systems. However, it is
still difficult to predict a relationship between Tg and the stability of dispersions, since for pure
amorphous solids, the Tg is unreliable in relation to the physical stability of the system. Hybrid
Nanostructures Obtained by Transport and Condensation of Tungsten Oxide Vapours onto CNW
Templates. MENGSAYLOEM1 My sample product research idea for you. The cluster source consists
of a water-cooled stainless-steel tube in which a magnetron sputtering plasma gun is mounted.
Multiple requests from the same IP address are counted as one view. XPS deconvolution results for
hybrid nanostructures obtained in plasma off condition in ( a ) W4f region ( b ) N1s region. In this
situation, the oxide nanoparticles totally cover the CNW walls. The determination of the crystallinity
in the pharmaceutical industry is very important in the quality control of raw materials, intermediate
products, and final products, and to test the effectiveness of technological procedures for processing
control. In particular, it is found that crystalline interfaces serve as crystallization templates for
epitaxial formation of metastable cubic GST phase upon phase transitions. By adjusting solution
conditions to decrease the solubility of the product within the metastable zone, the desired molecules
can be pressured to come out of solution and crystallize. After treatment, the samples were then
allowed to cool down back to ambient condition by natural convection, in the horizontal furnace.
XRD patterns in the vicinity of the ( b ) c-GST (111) and ( c ) c-GST (222) reflections. In the non-
reversible flow, the heat flow curve is better defined through the kinetics events Tc, Tm, and Td.
Moreover, each laser pulse increases the crystalline fraction as can be seen by the incremental
increase in peak intensity of the c-GST (111) and c-GST (222) reflections ( Figure 5 b,c). However,
the standard DSC still presents some limitations that may reduce the accuracy and precision of
measurements. The different ways for combining the dispersion are employed to set the conditions
of the solubility and stability of the API. Theo Guenter Kieckbusch, Luiz Antonio Gioielli, Renato
Grimaldi. Open Access is an initiative that aims to make scientific research freely available to all.
Inulin with higher DP showed higher water content, since a large number of hydrogen bonds were
formed. The inset shows FFT pattern, confirming the formation of the c-GST phase. Journal of Low
Power Electronics and Applications (JLPEA). With the simultaneous TGA-DSC, it is possible to
differentiate the melting from the degradation when these events occur in a narrow range of
temperatures (e.g., in sugar-rich systems); the melting and degradation temperatures are largely
affected by the amount of water adsorbed. In this type of product, it is desirable that the initial state
of the drug remains unchanged during the lifetime of the product. Been thinking about
recrystallization recently, so it's a good time to turn back to this graph. I would like to recommend
the following IntechOpen book to be added to our library catalog. This table is completed with a bar
diagram, presented in Figure 9, in which the modifications regarding atomic concentrations, after
each treatment, are presented. From the obtained heat flow curves Figures 4 and 5, the relative
crystallinity was calculated from the partial area method (the area under the crystallization peak at in-
stant t over the total area of the peak), see further in Fig- ures 6 and 7. The method was based on the
linear response of the specific heat determined at the Tg of the amorphous content. The experimental
section involved the compaction of 18 pure small molecule compounds such as acetaminophen,
aspirin, carbamazepine III, ?-indomethacin, and ketoprofen, among others. Visit our dedicated
information section to learn more about MDPI. Thus, the determination of the actual value of these
properties is difficult, because the events may overlap or the signal may be very low to be properly
noticed. The TEM specimen was prepared from the laser irradiated area of GST thin film shown in
Figure 6 a. In the first case ( Figure 3 a), no laser intensity produced by the laser irradiation at low
fluence reaches the substrate, since the laser light is significantly absorbed by the thicker film and the
crystallization is expected to start from the surface of GST thin film. Hence, a simple mixing rule
was used to describe its evolution as a function of temperature and relative crystallinity, Equa- tion
(3): ? ???,1 a TT T. The larger crystals settle between the baffle and draft tube, as shown below, and
are removed in the product slurry, while the fines are recirculated after being redissolved in a heat
exchanger. In other words, the final physical structure is responsible for the thermal and mechanical
characteristics of the obtain- ed parts. However, the presence of an amorphous phase in a ground
material may affect the final shape of the thermogram by modifying its baseline and the occurrence
of other thermal exothermic events of less magnitude such as a devitrification event that contributes
to the overall melting enthalpy. Note that from the first issue of 2016, this journal uses article
numbers instead of page numbers. All articles published by MDPI are made immediately available
worldwide under an open access license. No special. Through the DSC analysis, a single
endothermic peak was observed, which was attributed to the homogeneity of the thermal behavior
despite the heterogeneity in the fibrils’ length. Crystallization kinetics of homopolymers: bulk
crystallization; 10. The specific volume is modeled by a mixture law between the fitted amorphous
specific volume a and the crystal- line specific volume. Previous Article in Journal White Graphene-
Cobalt Oxide Hybrid Filler Reinforced Polystyrene Nanofibers for Selective Oil Absorption. The
W4f spectrum was fitted with Gaussian Lorentz Product (GLP) line shape, best fits of this peak
being obtained with GLP and a very low value of residual fit, where the energy splitting (2.18 eV)
and full width at half maximum (FWHM) fitting parameters were initially constrained and then
allowed to vary. Unlike DSC and TGA, where powders may be analyzed, the conventional DMA
measures the mechanical properties of viscoelastic solids and films subjected to a constant oscillatory
force or deformation. Regarding the CNW samples, before and after thermal treatment, when plasma
was used, the C1s percent decreases from 92.19% up to 51,78%. However, between these two
samples, the O1s percent shows a significant increase in the case of the treated sample (from 4.99%
observed in the control sample, up to 44.21%, the atomic percentage obtained for the CNW sample
after the thermal treatment, without powder source). In contrast with the results obtained without
plasma, the CNW decoration process performed in Ar plasma was effective for all working
temperatures. After the end of the crystallization, the polymer is in semi-crystalline phase, pressure is
stabilized, and the specific volume variations are mainly controlled by the temperature evo- lution.
Notwithstanding its inherently high complexity, the crystallization process is part of our everyday
lives, from ice making in our homes to the most state-of-the-art chemical and electronic industry. But
opting out of some of these cookies may affect your browsing experience. Conflicts of Interest The
authors declare no conflict of interest. In this sense, MDSC was developed to overcome the
disadvantages of conventional DSC. The spe- cific volume evolution is another influencing
parameter which should be taken into account when modeling the cooling of semi-crystalline
polymers. The study of phase transitions has a large impact on different fields such as the food
industry, pharmaceutical industry, and polymers. First, the equations describing pressure evolution,
heat transfer and crystallization in the cavity are introduced. Con- sequently, the viscosity value
(taken here as 10 6 Pa) has no effect on the calculation results. For symmetry reasons, only one half
of the system is modeled. After the end of the crystallization, the polymer is in semi-crystalline
phase, pressure is stabilized, and the specific volume variations are mainly controlled by the
temperature evo- lution. For instance, in the injec- tion molding process (one of the most used in
polymer processing industry), crystallization kinetics directly in- fluences the part behavior regarding
both its dimensional stability and its mechanical and thermal performances. The student conducted
experiments to crystallize bromelain from clarified pineapple juice using different salts like
ammonium sulfate and acetone. Crystals can be organic or inorganic and may be produced from
melts, liquid solutions, vapors or even in solid state. Note that in this work, the pressure history is not
an input data, but a com- putational result. Figure 6 a shows the total heat flow curve for inulin,
while Figure 6 b shows two contributions of the total heat flow curve (reversible and non-reversible).
This experimental procedure is schematically illustrated in Figure 3. Some of the pertinent
fundamental issues and recent results, especially of polymer crystallisation under non-isothermal
conditions and crystallisation of polymer blends, are surveyed. In the reversible heat flow curve, Tg
is clearly observed together with some other molecular rearrangement events. Both polymers are
separately miscible with water in all proportions. The FFT pattern calculated from region t-GST in
Figure 7 a reveals the as-grown t-GST phase, where the phase did not significantly change upon the
laser irradiation. This has recently been accomplished at Lawrence Livermore National Laboratory
(USA), which houses a unique Dynamic Transmission Electron Microscope (DTEM). Feature papers
are submitted upon individual invitation or recommendation by the scientific editors and must
receive. Another variant of the MDSC is the supercooling MDSC (SMDSC). The experimental
section involved the compaction of 18 pure small molecule compounds such as acetaminophen,
aspirin, carbamazepine III, ?-indomethacin, and ketoprofen, among others. On account of this, it has
no strict physical meaning, but it allows the experimental characterization of the crystallization
kinetics by means of differential scanning calorimetry only. Since the molecule’s movement becomes
restrung to only vibrational movements and is not rotational or translational, the Tg is drastically
modified, and the physical properties are modified as well. An example of this is the transition of an
amorphous material passing from the glassy to the rubbery state. The as-grown films were finally
capped with an optically transparent LaAlO 3-x (LAO) protective layer of about 5 nm thickness to
protect the GST thin films against oxidation. Thus, the formation of the a-GST phase strongly
indicates a melting and subsequent quenching process. They are devided into 91 compounds with a
neutral cluster unit (chap. 3.1), 4 neutral network compounds (chap. 3.2), 28 compounds with a
cluster cation (chap. 3.3), 5 compounds with oxidized nitrile-containing cluster units and one
secondary product (chap. 3.4) and 24 compounds with niobium cluster anions (chap. 3.5). One focus
of this work was the analysis of the intermolecular interactions between the cluster units.