Crystal Volume Fraction Research Articles

Numerically investigation of particle distribution in industrial-scale DTB crystallizer based on CFD modelling

The suspension state of crystals in the crystallizer is one of the important indicators for evaluating the adaptability of the crystallizer. This study adopted the Euler-Eulerian two-fluid model to simulate and analyze the fluid motion of solid-liquid two-phase flow in the industrial-grade DTB crystallization kettle, as well as the phase suspension distribution of crystal particles. The main influencing factors investigated are: the heat transfer effect, the height of the bottom of the crystallizer, the number and position of the stirring paddle, crystal size and crystal volume fraction. Based on the research of Euler-Eulerian method to simulate fluids, the Euler-Lagrangian method was further used to simulate the motion state of particle phases with different particle sizes in the crystallizer. It was found that the designed DTB crystallizer has good recycle mixing effect. The particles can be mixed evenly during the operation, which can fully realize the solid-liquid mixing and suspension effect of the drug under study.

Mold material and dimension effects on the microstructural gradient in a glass-ceramic

Microstructural gradients can significantly affect the properties of glass-ceramics (GCs). Such spatial variations in glass-ceramic (GC) microstructure may result from a non-uniform cooling rate when the glass-forming liquid is cast into a mold. This study investigates the material and mold size influence on the cooling process, leading to a non-uniform distribution of crystalline nuclei in the parent glass. We used a high-nucleation rate, non-stoichiometric, lithium metasilicate GC as a model. Initially, the glass-forming liquid was cooled in cylindrical molds with diameters of 7 and 14 mm, made from copper and 304 stainless steel – materials with distinct thermal diffusivities. Simulated thermography, validated by thermocouple data, showed contrasting cooling profiles across the samples. Our key findings are: i) cooling rate: faster cooling in the smaller mold resulted in a lower crystal number density and a reduced crystallized volume fraction (αv) as expected; ii) mold material: surprisingly, copper molds led to quicker glass shrinkage, which facilitated the earlier formation of air gaps with reduced heat transfer and slower cooling than steel, favoring incipient crystallization during the cooling path; iii) microstructure: samples cooled in both molds exhibited higher αv in the central and upper (mold contact-free) regions due to slower cooling compared to the mold base and edges. Therefore, this study reveals how mold material and size affect microstructural gradients in GCs, paving the way for tailoring crystallization and microstructure through strategic mold design.

Correlations between selecting crystallization temperature and modulating α-Fe/amorphous complex phase structure in extending frequency characteristic of the Fe-Si-B-Nb-Cu ultra-thin ribbons

Fe-Si-B-Nb-Cu nanocrystalline ribbons, with thicknesses exceeding 20 μm, have been extensively utilized in designing magnetoelectric devices. Recent advancements in automotive electronics and 5 G technology have shifted the focus to higher working frequencies reached to MHz, making ultra-thin ribbons (below 20 μm) more desirable. However, its fully amorphous structure often complicate the adjustment of the α-Fe/amorphous complex phase structure (α-Fe/amor CPS), subsequently affecting frequency characteristics. The study investigated the controllability of α-Fe crystallization behaviors and focused on the relationship between the initial crystallization temperature (Ta2) and the initial crystallization volume fraction (vi). The findings suggest that selecting ultra-thin ribbons and controlling Ta2 to maintain vi below 4 % is effective in adjusting α-Fe crystallization behaviors, achieving a uniform α-Fe/amor CPS with substantial vα-Fe, enhancing the frequency characteristics by technology magnetization process. In a notable example, ribbons with a thickness of 15 ± 1 μm, crystallized at Ta2 = 490 ℃ with a vi of approximately 0.94 %, achieved a uniform α-Fe/amorphous CPS with nano-sized α-Fe grains (average diameter of Dα-Fe = 13.4 nm) and a high grain number density (Nd, α-Fe) of about 3.0 × 1023m−3 and a high volume fraction (vα-Fe) 37.78 %. This resulted in a magnetized permeability (μi) of 5800 at 1 MHz and an impedance (Z) peak of approximately 126 Ω at 40 MHz.

Real-time control of microcrystal formation with inline process microscopy

The control of microcrystal formation during crystallization is necessary to ensure good separation of crystals and molasses without adding excessive wash water. This paper presents an automatic inline process microscope measurement of sugar crystals and how its results are utilized in a real-time process control. The system captures high-precision transilluminated images of sugar crystals flowing through a 10-mm wide gap in the evaporating crystallizer. It automatically analyses the sugar crystals in size range from 10 µm to 4 mm visible in images. System reports the number of detected microcrystals (10–30 µm) and crystals (>30 µm), mean aperture of crystals (MA), co-efficient of variation in size (CV), crystal growth rate and volume fractions of the specified crystal size classes in real time. The performance of the control and monitoring approach is highlighted with the results of example strikes.

Deformation-Induced Crystal Growth or Redissolution, and Crystal-Induced Strengthening or Ductilization in Metallic Glasses Containing Nanocrystals.

It is generally known that the incorporation of crystals in the glass matrix can enhance the ductility of metallic glasses (MGs), at the expense of reduced strength, and that the deformation of MGs, particularly during shear banding, can induce crystal formation/growth. Here, we show that these known trends for the interplay between crystals and deformation of MGs may hold true or become inverted depending on the size of the crystals relative to the shear bands. We performed molecular dynamics simulations of tensile tests on nanocrystal-bearing MGs. When the crystals are relatively small, they bolster the strength rather than the ductility of MGs, and the crystals within a shear band undergo redissolution as the shear band propagates. In contrast, larger crystals tend to enhance ductility at the cost of strength, and the crystal volume fraction increases during deformation. These insights offer a more comprehensive understanding of the intricate relationship between deformation and crystals/crystallization in MGs, useful for fine-tuning the structure and mechanical properties of both MGs and MG-crystal composites.

A simple method for the preparation of cordierite ceramics with high strength and low thermal expansion coefficient

AbstractCordierite ceramics have great application prospects due to their very low coefficient of thermal expansion. However, the low purity of ceramics leads to their unsatisfactory fracture strength, which has always been a research focus. Herein, by applying external pressure to the green body of mixed raw materials and optimizing the synthesis temperature, high‐purity cordierite powder was prepared, and then it was used as the starting material for the fabrication of high‐strength cordierite ceramics. The optimal sample exhibited a flexural strength of 146 MPa, which is about 1.4 times that of the cordierite ceramics reported in the literature. This is attributed to applied external pressure increasing the contact area of raw materials, leading to a more thorough reaction, and the content of the α‐cordierite phase is 98.4 wt% in the sample synthesized at 1275°C. Concurrently, the samples possessed a thermal expansion coefficient of only 1.9 × 10−6°C−1 (room temperature to 800°C). In addition, the increase in columnar crystal volume fraction is also one of the reasons for the high strength and low thermal expansion coefficient of cordierite ceramics.

Effect of 0.5 at. % Cu addition on the crystallization behavior and soft magnetic properties of Fe83B11C1Si2P3 alloy

In order to gain insight into how the addition of Cu element affects the crystallization mechanism of amorphous nanocrystalline alloys and soft magnetic properties, the crystallization behavior of (Fe0.83B0.11Si0.02P0.03C0.01)100-xCux (x = 0 and 0.5) amorphous ribbons was investigated based on kinetic and thermodynamic behavior under non-isothermal and isothermal annealing conditions. The results show that under non-isothermal annealing conditions, the Cu0.5 amorphous ribbon not only favors the formation of the amorphous structure, but also enlarges the temperature window for annealing and improves the thermal stability of the α-Fe(Si) phase. At the same time, the Cu0.5 amorphous ribbon shows slow kinetic and is insensitive to heating rate change during annealing treatment. Under isothermal conditions, the addition of Cu decreases the nucleation activation energy (En) and increases the growth activation energy (Eg). This further indicates that the nucleation of α-Fe(Si) grains is easier than the growth process, which is conducive to the formation of a homogeneous nanostructure and improves the soft magnetic properties of the alloy. Compared to Cu0 amorphous ribbon, it is also shown that the Cu0.5 amorphous ribbon changes the crystallization mechanism from diffusion-controlled one-dimensional to two-dimensional growth when the crystallization volume fraction x is 10–30 vol%. While three-dimensional growth become dominated when x is reaches 60 vol% for both ribbons. Therefore, the kinetics of crystallization as well as microstructure supports that the Cu0.5 ribbon is able to exhibit uniformly fine nanocrystalline structures. Further, the Cu0.5 nanocrystalline ribbon shows a higher Bs of 1.85 T and a lower Hc of 2.55 A/m, respectively, and the favorable (100) orientation of α-Fe(Si) grains formed after annealing is another factor to increase Bs.

The comparative study of crystallization transformation in Zr-Cu-Ag metallic glasses

The crystallization transformation in Zr-Cu-Ag metallic glasses have been comparatively studied. The crystallization enthalpy ΔHx lies in the range of −56.18 ∼ −46.90 J/g for Zr50Cu38Ag12 metallic glass and −55.69 ∼ −44.70 J/g for Zr50Cu36Ag14 metallic glass in their respective isothermal temperatures. The average crystallized volume fraction fmax corresponding to the maximum value of transformation rate [df/d(tIso − τ)]max is about equal to 0.52 and 0.55 for Zr50Cu38Ag12 and Zr50Cu36Ag14 metallic glasses. It is found that at the same isothermal temperature, [df/d(tIso − τ)]max becomes smaller, the time–temperature-transformation (TTT) diagram shifts to the right and time tmax required to reach [df/d(tIso − τ)]max becomes longer when Cu is replaced with Ag, which indicates that the thermal stability will be improved as Ag content rises in these metallic glasses. In addition, the type of growth is interface-controlled growth for Zr50Cu38Ag12 and Zr50Cu36Ag14 metallic glasses.

Tailoring the microstructure and soft magnetic properties of (Fe0.83B0.11Si0.02P0.03C0.01)99.5Cu0.5 nanocrystalline alloy based on the rapid annealing

In this work, the effects of annealing temperatures and time on the microstructure and soft magnetic properties of (Fe0.83B0.11Si0.02P0.03C0.01)99.5Cu0.5 nanocrystalline alloy were investigated using a new rapid annealing process. The results show that at each annealing temperature, there exists an annealing time for optimum soft magnetic properties. The annealing temperature and time were further optimized, and excellent properties with high saturation magnetic induction Bs of 1.79 T and low coercivity Hc of 2.7 A/m were obtained by annealing at 431 °C for 150 s. A microstructure consisting of uniform and fine α-Fe(Si) grains with high number density and high crystallization volume fraction was found to be the key to ensure high Bs and low Hc. However, with increasing annealing time, it was found that α-Fe(Si) grains existed aggregation phenomenon (in the form of high-angle grain boundaries), with the simultaneous precipitation of Fe-B compound precipitated in the residual amorphous matrix. This not only causes the uneven distribution of nanocrystals, but also destroys the competitive effect between nanocrystals and the stability of the structure, thus deteriorating the soft magnetic properties.

Enhancement of the Silicon Nanocrystals’ Electronic Structure within a Silicon Carbide Matrix

Using plasma-enhanced chemical vapor deposition (PECVD), a mixed gas of silane (SiH4) and methane (CH4) was diluted with hydrogen (H2) to produce thin films of silicon nanocrystals embedded in a silicon carbide (SiC) matrix. This method prevents the co-deposition of SiH and SiC from high-temperature annealing procedures. This study experimentally explores the improvement of the electronic structure by adjusting two processing parameters according to classical nucleation theory (ratio of SiH4 to CH4 and working gas pressure). The deposited films were examined using ellipsometry spectroscopy, X-ray diffraction, scanning electron microscopy, atomic force microscopy, and photoluminescence to determine grain size, crystal volume fraction, topography, and bond configurations. The results show that increasing the working gas pressure can increase the density of SiC, while increasing the ratio of SiH4 to CH4 can only produce larger grain sizes. This is consistent with how SiC works and grows. Without using a high-temperature annealing procedure, this technique can improve the electrical structure of SiC contained in the SiC matrix formed by PECVD.

Fibre alignment in fresh concrete with coarse aggregates and its visualization in transparent model concrete

Steel fibres distributed in concrete can greatly improve the mechanical performance of concrete, especially flexural and tensile behavior, if their orientations align to the direction of principal tensile stress. The study attempts to find diversified characters of fibre alignment in fresh concrete with consideration of adding coarse aggregates. A transparent concrete model, consisting of Carbopol gel, glass beads and crystals, is designed for the observation of fibre orientation. It shows good transparency and visibility, and can consider the effect of coarse aggregates since the volume fraction and particle size distribution of crystals are the same as coarse aggregates in real concrete mixture. The rheological properties of the model can be adjusted by the dosage of Carbopol and glass beads. Using this concrete model, the distribution and orientation of fibres can be directly observed and analyzed, considering the effect of aggregate sizes, concrete rheology and vibration time. The results show that coarse aggregates could limit the distribution space of fibres and lead to the decrease of fibre orientation coefficient. Fibre dispersion coefficient also decreases with the increase of aggregate sizes.

Study on flow and heat transfer characteristics of salt solution ice slurry

As a phase change material, ice slurry allows the storage of thermal energy in the form of latent heat. This has great advantages in terms of reducing energy consumption and environmental protection, and is being widely used. In this study, based on the Eulerian-Eulerian CFD model and the Population Balance Model (PBM), the flow and heat transfer characteristic of salt solution ice slurry was simulation studied, which included the pressure drop, friction coefficient, volume fraction, distribution of ice crystals and local heat transfer coefficient during the flow and solidification of salt solution ice slurry in different conditions. And the experimental system is set up to verify the results of the model and analyze the variation rules of these parameters. The results showed that in salt solutions with different concentrations, when the flow rate and solid phase volume fraction increase, the pressure drop and local heat transfer coefficient of the ice slurry will increase. The surface heat transfer coefficient reached to 2.5 × 103 W m-2 K-1, 2.9 × 103 W m-2 K-1, and 3.2 × 103 W m-2 K-1 when ice crystal volume fraction was 5 %, 10 %, and 15 %, respectively. The study will contribute to understanding of the changes in basic characteristics of salt solution slurry during the flow and phase transition processes.

Influence of Ge doping on the magnetic properties and microstructure of Fe-Si-B-P-Cu alloys prepared with industrial raw materials

With the increasing demand for energy efficiency and miniaturization, there is a growing need for magnetic materials with high saturation magnetic flux density (Bs) and low coercivity (Hc). Here, Fe82.3Si4B9P4-xCu0.7Gex (x = 0, 1, 2) nanocrystalline ribbons were prepared using industrial raw materials (IRMs). We found that appropriate Ge doping can optimize Bs by enhancing the crystallization volume fraction of α-Fe phase, and refine grain size by increasing the energy barriers for the growth of α-Fe and Fe(B, P) phases, which ultimately reduces Hc. However, Ge doping can also induce surface crystallization of the ribbons due to the enrichment of Cu elements. Excessive diffusion of Cu into the crystalline layer is not favorable for grain refinement, which deteriorates the soft magnetic properties of the ribbons.

Numerical thermomechanical modelling of lava dome growth during the 2007–2009 dome-building eruption at Volcán de Colima

SUMMARY Lava domes form during effusive eruptions due to an extrusion of highly viscous magmas from volcanic vents. In this paper we present a numerical study of the lava dome growth at Volcán de Colima, Mexico during 2007–2009. The mathematical model treats the lava dome extrusion dynamics as a thermomechanical problem. The equations of motion, continuity and heat transfer are solved with the relevant boundary and initial conditions in the assumption that magma viscosity depends on the volume fraction of crystals and temperature. We perform several sets of numerical experiments to analyse the internal structure of the lava dome (i.e. the distributions of the temperature, crystal content, viscosity and velocity) depending on various heat sources and thermal boundary conditions. Although the lava dome growth at Volcán de Colima during short (a few months) dome-building episodes can be explained by an isothermal model of lava extrusion with the viscosity depending on the volume fraction of crystals, we show here that cooling plays a significant role during long (up to several years) episodes of dome building. A carapace develops as a response to a convective cooling at the lava dome–air interface. The carapace becomes thicker if the radiative heat loss at the interface is also considered. The thick carapace influences the lava dome dynamics preventing its lateral advancement. The release of the latent heat of crystallization leads to an increase of the temperatures in the lava dome interior and to a relative flattening of the dome. Meanwhile, the heat source due to viscous dissipation inside the lava dome is negligible, and it does not influence the lava dome growth. The developed thermomechanical model of the lava dome dynamics at Volcán de Colima can be used elsewhere to analyse effusive eruptions, dome morphology and carapace evolution including its failure potentially leading to pyroclastic flow hazards.

2D X-ray diffraction method for evaluating the local crystallization of Fe-based amorphous alloy ribbon induced by ultrashort pulsed laser local heating

Fe-based amorphous alloys, which exhibit excellent soft magnetic properties, are difficult to machine, owing to their high strength, toughness, and hardness resulting from their unique structures. The authors proposed a novel blanking method that improves the machinability by crystallizing only the local regions involved in machining, thereby reducing the local strength and toughness. Because the micro-region mechanical properties of amorphous alloys vary greatly depending on the precipitated crystal species and volume fraction, it is necessary to nondestructively investigate the type of microstructure achieved by local heat treatment to determine the appropriate blanking conditions. However, an appropriate method for investigating crystals precipitated locally in an amorphous matrix is yet to be established. In this study, we used the 2D X-ray diffraction method to investigate the local crystallization of an Fe-based amorphous alloy ribbon after local heat treatment using an ultrashort pulsed laser. Furthermore, the 2D method was used to investigate the residual stresses in the fully crystallized amorphous alloy ribbons, and the results were compared using the sin2(ψ) method. The 2D method detected the slightly precipitated crystals in a local area with a radius of about 40 µm in the amorphous matrix. The integrated intensity of the diffraction peaks can be used to predict the internal structure after local heat treatment. Furthermore, the 2D method could measure residual stress with smaller error than the sin2(ψ) method. The core-shell crystals precipitated by heat treatment exhibited a compressive residual stress of −82 MPa to −67 MPa in the core Fe3B crystals and tensile residual stress of 39–60 MPa in the shell α-Fe crystals, approximately. The residual stress values of the precipitated crystals depended on the direction of rotation of the quenching roll used in the production of the amorphous alloy ribbons.

Isothermal phase transformation of Zr50Cu43Ag7 amorphous alloy

In the present work, isothermal phase transformation has been studied for Zr50Cu43Ag7 (at%) amorphous alloy. The crystallization enthalpy ΔHx released in phase transformation is calculated. Meanwhile, the incubation time τ and the end time tce of crystallization become shorter with the increasing annealing temperature. The maximum rates of crystallization [df/d(tIso-τ)]max, the crystallization volume fraction fmax and time tmax corresponding to [df/d(tIso-τ)]max are obtained. The local activation energy E(f) decreases firstly for 0 <f< 0.1, then E(f) remains essentially unchanged for 0.1 <f< 0.8 and finally, E(f) sharply decreases with further crystallization transformation. In addition, it is found that the crystallization mechanism for Zr50Cu43Ag7 amorphous alloy is interface-controlled growth.

Evaluation of the non-isothermal crystallization kinetics of the (Zr55Cu30Al10Ni5)99Nb1 bulk metallic glass

Non-isothermal crystallization kinetics of (Zr55Cu30Al10Ni5)99Nb1 bulk metallic glass (BMG) was studied by differential thermal analysis and differential scanning calorimetry. The crystallization pathway was changed by increasing the heating rate. The apparent activation energy at characteristic temperatures was calculated using Kissinger method. Local activation energy variations by crystallized volume fraction (α) (a.u. Ec(α)) was extracted using Ozawa-Flynn-Wall (OFW) method. Crystallization reaction function (f(α)) at different heating rates was extracted by means of Šesták-Berggren (SB) model.

Magnetostriction of Fe-rich FeSiB(P)NbCu amorphous and nanocrystalline soft-magnetic alloys

The compositional effect of magneto-elastic and magnetostriction properties of Fe-rich Fe81B15−xPxSi2Nb1Cu1 (ii) Fe82B14−xPxSi2Nb1Cu1 and (iii) Fe83B13−xPxSi2Nb1Cu1 (x = 0, 4, 8) amorphous and annealed nanocrystalline alloy ribbons were investigated. The present study adds knowledge to the limited magnetostriction literature available for Fe-rich nanocrystalline alloys by systematically varying the Fe and P content. A combination of Becker-Kersten and small angle magnetization rotation (SAMR) techniques has been employed for the magnetostriction (λs) evaluation. Both the as-quenched and nanocrystalline ribbons exhibit large positive magnetostriction and show strong compositional dependence to the P content. In the as-quenched condition, 4 at% P addition shows maximum magneto-elastic response and magnetostriction constant, with Fe81B11P4Si2Nb1Cu1 alloy exhibiting a maximum of + 52 ppm and P-free Fe83B13Si2Nb1Cu1 alloy exhibiting a minimum of + 27 ppm. In the nanocrystalline state, a slight reduction of magnetostriction is seen for all alloys, with a maximum of + 32 ppm (4 at% P) and a minimum of + 22 ppm (P-free) in Fe83 at% alloys. The unusual large magnetostriction of optimally annealed samples is attributed to the relatively low crystal volume fraction (30–45%) of nanocrystalline ribbons. The lowest magnetostriction of Fe83B13Si2Nb1Cu1 alloy in both as-quenched and annealed state is explained based on ribbon structural heterogeneity consisting of crystal nuclei and textured α-Fe surface crystallization. The study reveals a contradictory response of magneto-crystal anisotropy (grain size reduction) and magneto-elastic anisotropy to the P addition and ribbon structural heterogeneity. The study discusses the implications of the large magneto-elastic anisotropy associated with Fe-rich nanocrystalline ribbons and the way forward for improving their magnetic softness.

Effects of Cu and Co additions on the crystallization and magnetic properties of FeNbB alloy

The nanocrystalline-forming element Cu and magnetic element Co are commonly used as additive elements to tune the structure and improve the properties of alloys. In this study, four kinds of amorphous alloys, Fe72Nb12B16, Fe72Nb12B15Cu1, Fe36Co36Nb12B16, and Fe36Co36Nb12B15Cu1, were prepared by melt-spinning and annealed at various temperatures to investigate the effects of Cu and Co additions, individually and in combination, on the crystallization and magnetic properties of Fe72Nb12B16 alloy. The four kinds of alloys exhibited different crystallization behaviors with different primary crystallization phases observed. For the Fe72Nb12B16 alloy, only the α-Mn-type metastable phase formed after annealing. The addition of 1 at.% Cu and 36 at.% Co led to the observation of the α-Mn-type and β-Mn-type metastable phases, respectively, and a reduction in the crystallization volume fraction in the metastable phase. The Fe36Co36Nb12B15Cu1 alloy only exhibited α-Fe(Co) phase as a primary phase, and the addition of both Cu and Co completely inhibited the precipitation of the metastable phase. Cu clusters were found in energy dispersive spectroscopy elemental maps. Compared with other alloys, Fe36Co36Nb12B15Cu1 alloy with both Cu and Co exhibited a lower coercivity (H c) below 973 K.

Crystal entrainment from cool, low-silica rocks into hot, high-silica melts: diverse primary melt compositions at Taranaki volcano, New Zealand

The prevalence of antecrysts in arc volcanic rocks is widely accepted, yet the origin of their carrier melts remains debated. Crystal cargo in lava flows from Taranaki volcano, New Zealand, is dominated by plagioclase, clinopyroxene and amphibole. Except for some crystal rims, mineral phases are in disequilibrium with the melt they are entrained in. Major element chemistry reveals an almost complete compositional overlap between the crystals in the lava and those in xenoliths. The large volume fraction of crystals (35–55 vol%) exerts a strong control on whole-rock compositions, reducing silica by 5–11 wt% compared with the carrier melt. Yet there is no clear relationship between mineral proportion and bulk-rock compositions. Our data are inconsistent with extensive fractional crystallization, commonly invoked as a driver of magma evolution towards silica-rich compositions. Instead, high-temperature, aphyric carrier melts with varied compositions (55–68 wt% SiO 2 ) entrain crystal cargo while ascending through colder, low-silica rocks. Thus, some parental melts at Taranaki volcano are significantly more silica-rich than arc basalts commonly invoked as primary magmas. Further, thermometric and hygrometric constraints preclude a deep crustal hot zone for the source of these melts, which we argue are of subcrustal origin. Supplementary material: Supplementary figures and databases are available at https://doi.org/10.6084/m9.figshare.c.6406813