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1.
Food Chem ; 460(Pt 2): 140574, 2024 Jul 29.
Article in English | MEDLINE | ID: mdl-39089028

ABSTRACT

Creating molecules capable of inhibiting ice recrystallization is an active research area aiming to improve the freeze-thaw characteristics of foods and biomedical materials. Peptide mixtures have shown promise in preventing freezing-induced damage, but less is known about the relationship between their amino acid compositions and ice recrystallization inhibition (IRI) activities. In this article, we used Ni2+ immobilized metal affinity chromatography (IMAC) to fractionate pulse protein hydrolysates, created by Alcalase and trypsin, into mixtures lacking and enriched in His, and Cys residues. The aim of this study was to fractionate pulse protein hydrolysates based on their amino acid compositions and evaluate their resulting physicochemical and IRI characteristics. Ni2+ IMAC fractionation induced IRI activity in all of the evaluated soy, chickpea, and pea protein hydrolysates regardless of their amino acid composition. Ni2+ IMAC fractionation produced chemically distinct fractions of peptides, differing by their molecular weights, amino acid composition, and IRI activities. The resulting peptide mixtures' molecular weight, amino acid composition, secondary structure, and sodium ion levels were found to have no correlation with their IRI activities. Thus, we demonstrate for the first time the ability of Ni2+ IMAC fractionation to induce IRI activity in hydrolyzed pulse proteins.

2.
Sci Rep ; 14(1): 17925, 2024 Aug 02.
Article in English | MEDLINE | ID: mdl-39095487

ABSTRACT

This study investigated the role of interfacial deformability in bond integrity and strength, particularly in the production of robust joints between harder austenitic stainless steels (SS) during ultrasonic welding. The specimen without the interlayer experienced limited strength enhancement owing to internal cracking from continuous sliding at interfacial temperatures below 0.6 times the melting point (Tm), which is attributed to the limited deformability of the austenitic SS. In contrast, introducing Fe and Ni interlayers between the substrates resulted in a notable increase in the interfacial strength, surpassing 2500 N in the peak load within a reduced welding duration. The correlation between the interfacial strength and the peak temperature suggests that a substantial decrease in hardness below 0.4 Tm is sufficient for extensive bond formation. Moreover, dynamic recrystallization (DRX) led to grain refinement in the Fe interlayer owing to shorter weld durations, whereas grain growth was observed in the Ni interlayer due to higher peak temperatures. Both the Fe and Ni interlayers significantly improved the bonding integrity by accommodating plasticity through the above phenomena without severe damage to the substrates, leading to increase of interfacial strength by 24% (2050 N to 2500 N) and reduction of weld duration by 40% (1.5 s in Fe interlayer). In addition, the fracture position after the lap shear test shifted from the edge of the weld area to the SS substrate.

3.
Angew Chem Int Ed Engl ; : e202406705, 2024 Jul 24.
Article in English | MEDLINE | ID: mdl-39049163

ABSTRACT

Solution-processed perovskite films generally possess small grain sizes and high density of grain boundaries, which intensify non-radiative recombination of carriers and limits the power conversion efficiency (PCE) of solar cells. In this study, we report the room-temperature ripening enabled by the synergy of hygroscopic salts and moisture in air for efficient hole-conductor-free printable mesoscopic perovskite solar cells (p-MPSCs). Treating perovskite films with proper hygroscopic salts in damp air induces obvious secondary recrystallization, which coarsens the grains size from hundreds of nanometers to several micrometers. It's proposed that the hygroscopic salt at grain boundaries could absorb moisture and form a complex which could not only serve as mass transfer channel but also assist in the dissolution of perovskite grains. This activates mass transfer between small grains and large grains since they possess different solubilities, and thus ripens the perovskite film. Consequently, p-MPSCs treated with the hygroscopic salt of NH4SCN show an improved power conversion efficiency of 20.13% from 17.94%, and maintain >98% of the initial efficiency under maximum power point tracking at 55±5°C for 350 hours.

4.
Int J Biol Macromol ; 276(Pt 2): 134047, 2024 Jul 20.
Article in English | MEDLINE | ID: mdl-39033893

ABSTRACT

The study evaluated the effect of freezing rate on the quality of water-added quick-frozen rice noodles and water-free quick-frozen rice noodles. Results indicated that the retrogradation enthalpy, relative crystallinity, freezable water content, and cooking loss of water-added quick-frozen rice noodles were higher than those of water-free quick-frozen rice noodles with increasing storage time. Furthermore, ice recrystallization accelerated the deterioration of the quality of the rice noodles, resulting in the enlargement of the pores within the rice noodles and the formation of many pores on the surface. This phenomenon was particularly evident in the rice noodles of Y-40 °C (freezing with water at -40 °C) and Y-60 °C (freezing with water at -60 °C). After 28 days of frozen storage, the hardness increased by 83.83 % for rice noodles of Y-20 °C (freezing with water at -20 °C), while the hardness decreased by 51.68 % and 45.80 %, respectively, for rice noodles of Y-40 °C and Y-60 °C. Consequently, the impact of the freezing rate on the quality of water-added quick-frozen rice noodles is more pronounced than that of water-free quick-frozen rice noodles. Moreover, a higher freezing rate can delay the deterioration of the quality of frozen rice noodles by postponing starch retrogradation and inhibiting ice recrystallization.

5.
Sci Rep ; 14(1): 16755, 2024 Jul 20.
Article in English | MEDLINE | ID: mdl-39033237

ABSTRACT

Cryogenic treatment has high potential for improving the deformation behavior through the recrystallization at a low temperature. In this work, true stress-strain curves were obtained via compression tests to understand the deformation behavior of an AA7075 under cryogenic conditions. Results showed a significant improvement in the flow stress of AA7075, increasing from 260 to 560 MPa at the yield point. The strain hardening exponent (n) also increased from 0.25 to 0.35 after deformation at cryogenic temperatures. The presence of Al2CuMg phase influenced the deformation texture of the tested aluminum alloy, resulting in more elongated grains and fine sub-grains after deformation at cryogenic temperatures, due to the hindered recrystallization. Microstructure evolution after deformation at room and cryogenic temperatures was investigated using EBSD technique to characterize texture and recrystallized grains. The results indicated that the spacing of the high-angle grain boundaries (HAGBs) in the sample deformed at room temperature was slightly larger than in the cryogenically treated sample. The alloy deformed at the cryogenic temperature exhibited a higher strain hardening exponent (n = 0.35) compared to room temperature deformation (n = 0.25). Furthermore, finite element analysis supported the experimental findings, showing that the Plastic Equivalent Strain (PEEQ) of the model tested at cryogenic temperature was higher than at room temperature, attributed to grain refinement during low-temperature deformation. The calculated effective stress responses at cryogenic temperatures for the investigated flow stress aligned well with the experimental results. These new aspects and mechanisms of deformation of aluminum alloys at cryogenic temperatures can improve the formability of high-strength alloys in the future production of more complex and integrated lightweight components.

6.
Materials (Basel) ; 17(13)2024 Jun 26.
Article in English | MEDLINE | ID: mdl-38998206

ABSTRACT

The deformation mechanism and static recrystallization (SRX) behavior of an Ni-based single-crystal superalloy are investigated. Indentation tests were performed to investigate the effects of crystal orientation and external stress on SRX behavior. Following solution heat treatment, the depth of the SRX layer below the indentation increases with a deviation angle (ß) from the [001] orientation. The slip analysis indicates that an increased deviation angle leads to an increase in the resolved shear stress on the slip plane and a decrease in the number of active slip systems. In addition, the variation pattern of the SRX layer depth with the deviation angle is consistent for different external stresses. The depth of the SRX layer also increases with external stress. The coarse γ' phases and residual γ/γ' eutectics obviously enhance the pinning effects on the expansion of recrystallized grain boundaries, resulting in slower growth rates of the recrystallized grains in interdendritic regions than those in dendrite core regions.

7.
Materials (Basel) ; 17(13)2024 Jun 27.
Article in English | MEDLINE | ID: mdl-38998235

ABSTRACT

Twin-roll strip casting (TRSC) technology has unique advantages in the production of non-oriented electrical steel. However, the hot deformation behavior of high-grade electrical steel produced by TRSC has hardly been reported. This work systematically studied the hot deformation behavior of free-Al 2.43 wt.% Si electrical steel strip produced by twin-roll strip casting. During the simulated hot rolling test, deformation reduction was set as 30%, and the ranges of deformation temperature and strain rate were 750~950 °C and 0.01~5 s-1, respectively. The obtained true stress-strain curves show that the peak true stress decreased with an increase in the deformation temperature and with a decrease in the strain rate. Then, the effect of hot deformation parameters on microstructure and texture was analyzed using optical microstructure observation, X-ray diffraction, and electron backscattered diffraction examination. In addition, based on the obtained true stress-strain curves of the strip cast during hot deformation, the constitutive equation for the studied silicon steel strip was established, from which it can be found that the deformation activation energy of the studied steel strip is 83.367 kJ/mol. Finally, the kinetics model of dynamic recrystallization for predicting the recrystallization volume percent was established and was verified by a hot rolling experiment conducted on a rolling mill.

8.
Angew Chem Int Ed Engl ; : e202410453, 2024 Jul 22.
Article in English | MEDLINE | ID: mdl-39037423

ABSTRACT

Thorium, a predominant actinide in the Earth's crust, presents significant environmental and health risks due to its radioactive nature. These risks are particularly pronounced during the mining and processing of monazite for rare earth elements (REEs), which contain substantial thorium concentrations. Current instrumental analysis methods for thorium, offer high accuracy but require laborious sample preparation and expensive instruments, making them unsuitable for on-site analysis. Herein, we present a class of color-tunable luminescent lanthanide-based metal-organic frameworks (Ln-MOFs) as fluorochromic sensors for Th4+ cations. Utilizing a heterobimetallic Eu3+/Tb3+ doping strategy, the luminescence colors of EuxTb1-x-BDC-OH can be finely tuned from red, to orange, and to green. More intriguingly, the higher Lewis acidity of Th4+ facilitates the transformation of EuxTb1-x-BDC-OH into a UiO-type Th-MOF via a dissolution-recrystallization mechanism. This process results in a gradual reduction of characteristic Ln3+ emissions and the emergence of blue color ligand-based fluorescence, thereby leading to selective fluorochromic responses with increasing Th4+ concentrations and enabling visible detection of Th4+ cations. Additionally, a custom-built portable optoelectronic device was fabricated, which directly converts luminescence colors into red-green-blue (RGB) values. This device enables easy quantification of Th4+ concentrations without the need for complex instrumentation.

9.
Sci Rep ; 14(1): 15106, 2024 07 02.
Article in English | MEDLINE | ID: mdl-38956156

ABSTRACT

We applied computing-as-a-service to the unattended system-agnostic miscibility prediction of the pharmaceutical surfactants, Vitamin E TPGS and Tween 80, with Copovidone VA64 polymer at temperature relevant for the pharmaceutical hot melt extrusion process. The computations were performed in lieu of running exhaustive hot melt extrusion experiments to identify surfactant-polymer miscibility limits. The computing scheme involved a massively parallelized architecture for molecular dynamics and free energy perturbation from which binodal, spinodal, and mechanical mixture critical points were detected on molar Gibbs free energy profiles at 180 °C. We established tight agreement between the computed stability (miscibility) limits of 9.0 and 10.0 wt% vs. the experimental 7 and 9 wt% for the Vitamin E TPGS and Tween 80 systems, respectively, and identified different destabilizing mechanisms applicable to each system. This paradigm supports that computational stability prediction may serve as a physically meaningful, resource-efficient, and operationally sensible digital twin to experimental screening tests of pharmaceutical systems. This approach is also relevant to amorphous solid dispersion drug delivery systems, as it can identify critical stability points of active pharmaceutical ingredient/excipient mixtures.


Subject(s)
Excipients , Polysorbates , Excipients/chemistry , Polysorbates/chemistry , Vitamin E/chemistry , Surface-Active Agents/chemistry , Pyrrolidines/chemistry , Molecular Dynamics Simulation , Thermodynamics , Hot Melt Extrusion Technology/methods , Vinyl Compounds
10.
Article in English | MEDLINE | ID: mdl-38958684

ABSTRACT

The synthesis of TaSe3 ring-shaped crystals displaying the coffee ring effect is investigated. By recrystallizing TaSe3 microcrystals dissolved in droplets of condensed Se gas, ring-shaped crystals were successfully grown. This novel method for ring formation effectively addressed the issue of connecting the edges of the crystal. Consequently, the synthesis method has the capability to grow MX3 ring-shaped crystals in any location where droplets can condense, can now be grown in specific locations, thus creating opportunities for advancements in electronic component development.

11.
J Sci Food Agric ; 2024 Jun 21.
Article in English | MEDLINE | ID: mdl-39031689

ABSTRACT

BACKGROUND: The cryoprotective effect of xylooligosaccharide (XO) and kappa-carrageenan (KC) mixture on silver carp proteins in fluctuated frozen storage from 4 to -18 °C was analyzed. Positive control as a conventional cryoprotectant mixture of sucrose (4%) and sorbitol (4%), KC (3%) and XO/KC (3%) treatments were incorporated in silver carp surimi and myofibrillar proteins to analyze the water mobility and its influence on structural attributes. RESULTS: The temperature fluctuation significantly increased the structural alteration in samples with no treatments due to oxidative changes, protein denaturation and recrystallization. Meanwhile, the mixture of XO and KC (XO/KC 3%) significantly reduced the tertiary and secondary structural alterations by preventing the oxidative changes in α-helix and tryptophan (Trp) residues. Moreover, XO/KC (3%) inhibited water mobility, hindering the T22 relaxation time, as compared to the samples added with KC (3%) and the positive control. Interestingly, the XO/KC (3%) mixture significantly reduced the formation of extracellular spaces and recrystallization by restricting the partial dehydration of muscles and extracellular solution concentration. CONCLUSION: From the current results, it can be concluded that the XO/KC mixture could be efficient in protecting aquatic food proteins during fluctuating frozen storage by preventing the exposure of Trp residues and α-helix contents. Moreover, XO/KC restricted the water mobility by establishing a bond and making water unavailable for crystallization and recrystallization. Therefore, XO/KC could be used as an effective mixture to prevent fluctuated and frozen storage changes in aquatic foods. © 2024 Society of Chemical Industry.

12.
Materials (Basel) ; 17(11)2024 May 24.
Article in English | MEDLINE | ID: mdl-38893795

ABSTRACT

Through the study of the thermal rheological behavior of Ti6Al4V alloy at different temperatures (500 °C, 600 °C, 700 °C, and 800 °C) and different strain rates (0.1 s-1, 0.05 s-1, 0.01 s-1, and 0.005 s-1), a constitutive model was developed for Ti6Al4V alloy across a wide temperature range in the hot stamping process. The model's correlation coefficient reached 0.9847, indicating its high predictive accuracy. Hot processing maps suitable for the hot stamping process of Ti6Al4V alloy were developed, demonstrating the significant impact of the strain rate on the hot formability of Ti6Al4V alloy. At higher strain rates (>0.05 s-1), the hot processing of Ti6Al4V alloy is less prone to instability. Combining hot processing maps with hot stamping experiments, it was found that the forming quality and thickness uniformity of parts improved significantly with the increase in stamping speed. The phase composition and microstructures of the forming parts under different heating temperature conditions have been investigated using SEM, EBSD, XRD, and TEM, and the maximum heating temperature of hot stamping forming was determined to be 875 °C. The recrystallization mechanism in hot stamping of Ti6Al4V alloys was proposed based on EBSD tests on different sections of a hot stamping formed box-shaped component. With increasing deformation, the effect of dynamic recrystallization (DRX) was enhanced. When the thinning rate reached 15%, DRX surpassed dynamic recovery (DRV) as the dominant softening mechanism. DRX grains at different thinning rates were formed through both discontinuous dynamic recrystallization (DDRX) and continuous dynamic recrystallization (CDRX), with CDRX always being the dominant mechanism.

13.
Materials (Basel) ; 17(11)2024 May 27.
Article in English | MEDLINE | ID: mdl-38893846

ABSTRACT

This paper reports the vapor pressure and enthalpy of vaporization for a promising phase change material (PCM) guanidinium methanesulfonate ([Gdm][OMs]), which is a typical guanidinium organomonosulfonate that displays a lamellar crystalline architecture. [Gdm][OMs] was purified by recrystallization. The elemental analysis and infrared spectrum of [Gdm][OMs] confirmed the purity and composition. Differential scanning calorimetry (DSC) also confirmed its high purity and showed a sharp and symmetrical endothermic melting peak with a melting point (Tm) of 207.6 °C and a specific latent heat of fusion of 183.0 J g-1. Thermogravimetric analysis (TGA) reveals its thermal stability over a wide temperature range, and yet three thermal events at higher temperatures of 351 °C, 447 °C, and 649 °C were associated with vaporization or decomposition. The vapor pressure was measured using the isothermogravimetric method from 220 °C to 300 °C. The Antoine equation was used to describe the temperature dependence of its vapor pressure, and the substance-dependent Antoine constants were obtained by non-linear regression. The enthalpy of vaporization (ΔvapH) was derived from the linear regression of the slopes associated with the linear temperature dependence of the rate of weight loss per unit area of vaporization. Hence, the temperature dependence of vapor pressures ln Pvap (Pa) = 10.99 - 344.58/(T (K) - 493.64) over the temperature range from 493.15 K to 573.15 K and the enthalpy of vaporization ΔvapH = 157.10 ± 20.10 kJ mol-1 at the arithmetic mean temperature of 240 °C were obtained from isothermogravimetric measurements using the Antoine equation and the Clausius-Clapeyron equation, respectively. The flammability test indicates that [Gdm][OMs] is non-flammable. Hence, [Gdm][OMs] enjoys very low volatility, high enthalpy of vaporization, and non-flammability in addition to its known advantages. This work thus offers data support, methodologies, and insights for the application of [Gdm][OMs] and other organic salts as PCMs in thermal energy storage and beyond.

14.
Materials (Basel) ; 17(11)2024 Jun 03.
Article in English | MEDLINE | ID: mdl-38893969

ABSTRACT

The microstructure and texture evolution of Cu-Ni-P alloy after cold rolling and annealing at 500 °C was studied by electron backscattering diffraction (EBSD). The equiaxed grain is elongated and the dislocation density increases gradually after cold rolling. The grain boundaries become blurred and the structure becomes banded when the reduction in cold rolling reaches 95%. A typical rolling texture is formed with the increase in deformation amount in cold rolling. The deformation structure gradually disappeared and recrystallized new grains were formed after annealing at 500 °C. The recrystallization nucleation mechanism of Cu-Ni-P alloy at 60% reduction is mainly a bow nucleation mechanism. A shear band begins to form after annealing at 80% reduction. The shear band becomes the preferred nucleation location with the increase in reduction. Most adjacent recrystallized grains growing in the shear band have a twin relationship.

15.
Acta Pharm Sin B ; 14(6): 2669-2684, 2024 Jun.
Article in English | MEDLINE | ID: mdl-38828156

ABSTRACT

Solid oral controlled release formulations feature numerous clinical advantages for drug candidates with adequate solubility and dissolution rate. However, most new chemical entities exhibit poor water solubility, and hence are exempt from such benefits. Although combining drug amorphization with controlled release formulation is promising to elevate drug solubility, like other supersaturating systems, the problem of drug recrystallization has yet to be resolved, particularly within the dosage form. Here, we explored the potential of an emerging, non-leachable terpolymer nanoparticle (TPN) pore former as an internal recrystallization inhibitor within controlled release amorphous solid dispersion (CRASD) beads comprising a poorly soluble drug (celecoxib) reservoir and insoluble polymer (ethylcellulose) membrane. Compared to conventional pore former, polyvinylpyrrolidone (PVP), TPN-containing membranes exhibited superior structural integrity, less crystal formation at the CRASD bead surface, and greater extent of celecoxib release. All-atom molecular dynamics analyses revealed that in the presence of TPN, intra-molecular bonding, crystal formation tendency, diffusion coefficient, and molecular flexibility of celecoxib were reduced, while intermolecular H-bonding was increased as compared to PVP. This work suggests that selection of a pore former that promotes prolonged molecular separation within a nanoporous controlled release membrane structure may serve as an effective strategy to enhance amorphicity preservation inside CRASD.

16.
Macromol Rapid Commun ; : e2400273, 2024 Jun 14.
Article in English | MEDLINE | ID: mdl-38876477

ABSTRACT

Poly(butylene succinate) (PBS) forms small and imperfect crystals of low melting temperature at high supercooling of the melt. Slow heating allows reorganization of the obtained semicrystalline structure with the changes of the crystallinity and of the size and perfection of crystals analyzed by differential scanning calorimetry (DSC) and temperature-resolved X-ray scattering techniques. Crystals generated at 20 °C begin to melt and reorganize at a few K higher temperature with their initial imperfection and thickness unchanged upon heating to 70-80 °C. Slow heating to temperatures higher than 70-80 °C yields a distinct exothermic peak in the DSC scan, paralleled by detection of crystals of larger size/higher perfection, beginning to melt at ≈100 °C. These observations suggest that below 70-80 °C, reorganization of the semicrystalline morphology is constrained such that only minor and local improvement of the structure of crystals are possible. The formation of both perfect and thicker crystal lamellae at higher temperature proceeds via melting of imperfect crystals followed by melt-recrystallization as for PBS solid-state thickening is impossible. The study shows the limit of low-temperature reorganization processes when not involving both complete melting of crystals and rearrangement of the lamellar-stack structure.

17.
Small ; : e2403648, 2024 Jun 17.
Article in English | MEDLINE | ID: mdl-38881372

ABSTRACT

CsPbBr3@Cs4PbBr6 hexagonal NCs with a bright photoluminescence (PL) peak of 456 nm are created through the dissolution-recrystallization of CsPbBr3 nanoplatelets. Small CsPbBr3 nanocrystals are encapsulated in hexagonal Cs4PbBr6 during recrystallization to form a core-shell structure and keep high brightness and stability. The recrystallization kinetics is systematically investigated to explore the roles of methyl acetate, oleylamine, and n-hexane. Result further indicates that core/shell NCs remained high PL under a variety of harsh conditions (e.g., light irradiation and heat treatment) because of Cs4PbX6 shell and the controlling of recrystallization. Their initial PL intensity is remained after 4 months of storage under ambient conditions and continuous exposure to UV lamp for 180 min. The bright PL is also maintained even treatment at 120 °C. To indicate the universality of this synthesis method, CsPbX3@Cs4PbX6 hexagonal NCs with different emission colors are fabricated by changing temperature, solvent viscosity, and precursors (e,g, oleylamine and halogens). These core-shell samples reveal bright and stable green, orange, and red PL. Because of its high stability, the core/shell NCs are dispersed in flexible films to create diverse patterns. The films also exhibit high brightness and excellent stability. This strategy opens a novel avenue for the application of perovskite nanomaterials in the display field.

18.
J Adv Res ; 2024 Jun 05.
Article in English | MEDLINE | ID: mdl-38844125

ABSTRACT

INTRODUCTION: Magnetostrictive Fe-Ga alloys have garnered extensive attention owing to their excellent magnetic properties and acceptable biocompatibility. Nevertheless, the polycrystalline Fe-Ga alloys currently available tend to display random texture orientations, which constrain their magnetostrictive performance. OBJECTIVES: To regulate the texture orientation of Fe-Ga-NbC alloys and thereby enhancing magnetostriction. METHODS: In this study, a processing route comprising laser powder bed fusion (LPBF) followed by secondary recrystallization annealing (800, 1000, and 1200 °C, respectively) was developed to prepare Fe-Ga-NbC alloys. RESULTS: The results showed that the LPBF-ed (Fe81Ga19)99(NbC)1 alloys exhibited a high content of high energy grain boundaries (HEGBs) due to the repeated melting and solidification. In subsequent annealing process, the migration of HEGBs induced the rearrangement and recrystallization of grains, during which NbC was found to locate at the grain boundaries and influence the migration path of HEGBs via selective pinning, thereby resulting in a strong Goss texture. With the rise in annealing temperature, the content of Goss texture gradually increased from the initial 3.9 % to 71.3 % at 1200 °C, leading to enhanced magnetostriction, lower saturation magnetization and coercivity. Furthermore, in alternating magnetic fields, the alloys annealed at 1200 °C also exhibited higher magnetostriction than the LPBF-ed alloys. And a noteworthy grain coarsening was also observed after annealing, accompanied by a discernible inclination of magnetic domains towards strip domains. Additional, cell tests demonstrated that the prepared alloys had satisfactory biocompatibility and the ability to promote osteogenic differentiation. CONCLUSION: These findings indicated that the LPBF-ed and annealed Fe-Ga-NbC alloys might be a promising alternative as magnetostrictive-driven materials for biomedical applications.

19.
J Pharm Sci ; 2024 Jun 27.
Article in English | MEDLINE | ID: mdl-38944343

ABSTRACT

The incorporation of leucine (Leu), a hydrophobic amino acid, into pharmaceutically relevant particles via spray-drying can improve the physicochemical and particulate properties, stability, and ultimately bioavailability of the final product. More specifically, Leu has been proposed to form a shell on the surface of spray-dried (SD) particles. The aim of this study was to explore the potential of Leu in the SD protein/trehalose (Tre) formulation to control the water uptake and moisture-induced recrystallization of amorphous Tre, using lysozyme (LZM) as a model protein. LZM/Tre (1:1, w/w) was dissolved in water with varied amounts of Leu (0 - 40%, w/w) and processed by spray-drying. The solid form, residual moisture content (RMC), hygroscopicity, and morphology of SD LZM/Tre/Leu powders were evaluated, before and after storage under 22°C/55% RH conditions for 90 and 180 days. The X-ray powder diffraction results showed that Leu was in crystalline form when the amount of Leu in the formulation was at least 20% (w/w). Thermo-gravimetric analysis and scanning electron microscopy results showed that 0%, 5%, and 10% (w/w) Leu formulations led to comparable RMC and raisin-like round particles. In contrast, higher Leu contents resulted in a lower RMC and increased surface corrugation of the SD particles. Dynamic vapor sorption analysis showed that partial recrystallization of amorphous Tre to crystalline Tre·dihydrate occurred in the 0% Leu formulation. However, adding as little as 5% (w/w) Leu inhibited this recrystallization during the water sorption/desorption cycle. In addition, after storage, the formulations with higher Leu contents showed reduced water uptake. Instead of observing recrystallization of amorphous Tre in 0%, 5%, and 10% (w/w) Leu formulations, recrystallization of amorphous Leu was noted in the 5% and 10% (w/w) Leu formulations after storage. In summary, our study demonstrated that the addition of Leu has the potential to reduce water uptake and inhibit moisture-induced recrystallization of amorphous Tre in the SD protein/Tre powder system.

20.
Materials (Basel) ; 17(12)2024 Jun 10.
Article in English | MEDLINE | ID: mdl-38930202

ABSTRACT

In industrial production, the deformation inhomogeneity after metal forging affects the mechanical properties of various parts of the forgings. The question of whether the organization and mechanical properties of ß-titanium alloy can be improved by controlling the amount of forging deformation needs to be answered. Therefore, in this paper, a new sub-stable ß-Ti alloy TB 18 (Ti-5.3Cr-4.9Mo4.9V-4.3Al-0.9Nb-0.3Fe) was subjected to three different levels of deformation, as well as solid solution-aging treatments, and the variation rules of microstructure and mechanical properties were investigated. During the solid solution process, the texture evolution pattern of the TB18 alloy at low deformation (20-40%) is mainly rotational cubic texture deviated into α-fiber texture; at high deformation (60%), the main components of the deformed texture are α-fiber texture with a specific orientation of (114)<113-3>. After subsequent static recrystallization, the α-fiber texture is deviated to an α*-fiber texture, while the specific orientation (114)<113-3> can still be inherited as a major component of the recrystallized texture. The plasticity of the alloy in the normal direction (ND) after the solid solution is influenced by the existence of the <110>//ND texture, and the plasticity of the alloy in the ND direction after aging is determined by a combination of the volume fraction of the <110>//ND texture in the matrix phase and the volume fraction of [112-0]α//ND in the α phase. The results show that it is feasible to change the characteristics of the recrystallization texture of TB18 by controlling the deformation level of hot forging, thus realizing the modulation of the mechanical properties.

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