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The double quench phase separation is a simplified type of continuous cooling process that is widely seen in industrial processes for polymeric membrane formation. Uncommon quenching conditions can lead to the creation of novel membrane microstructures. This study aims to theoretically investigate the impact of nonisothermality on the morphology formation during the double‐quench thermally‐induced phase separation process. First, quench is employed during different stages of phase separation to observe the possibility of secondary morphology formation. Next, two initial quench temperatures are selected, one shallow and the other deep. The initial solution temperature and the secondary quench temperature are kept constant to inspect the impact of the initial quench temperature on the structure formation. Lastly, the results of the secondary quench are compared with and without employing the enthalpy of demixing. Results verified that the stage of phase separation, the initial and secondary quench temperatures, cooling rate, and the secondary quench composition are the most important parameters in the the nonisothermal double quench phase separation process. The morphology should be well‐developed in order for the secondary structure formation. In addition, it is shown that heat generation during demixing in the primary and secondary quenches significantly influences the secondary morphology formation. [ABSTRACT FROM AUTHOR]

In bone, osteoclasts are the primary type of cells responsible for bone resorption. Osteoclasts are mechanosensitive. This paper proposed to apply the shape recovery stress, generated from shape recovery polymers (SMPs), for the in situ modulation of osteoclastogenesis. Three-dimensional PLA/PCL constructs with different mass ratios of poly(lactic acid) (PLA) and polycaprolactone (PCL) at 7∶3, 5∶5, 3∶7 and pure PLA were firstly prepared by thermally induced phase separation (TIPS). The morphology, composition and thermal properties of these constructs were characterized. Then, the selected PLA/PCL (5:5) construct was shape programmed by hot-pressing to the deformation ratios of 0, 50% and 75% at 45 ℃ and shape-fixed at the cooling temperature of 4 ℃, and their shape memory properties were characterized. Finally, the in vitro proof-of-concept experiment was carried out to examine the effect of shape recovery stress on the inhibition of osteoclastogenesis in RAW264.7 macrophages. The shape recovery temperature of the PLA/PCL (5∶5) formulation was found to be close to the human body temperature, thus rendering it a suitable candidate for the fabrication of 3D scaffolds. The shape recovery stress was associated to the shape programming strain. The shape recovery stress generated by the 75% group was 1.7 times that of the 50% group. The in situ applied shape recovery stress effectively inhibited the fusion of macrophages and osteoclastogenesis by suppressing the cells to express relevant markers, and its inhibitory effect on formation of osteoclasts was related to the magnitude of the shape recovery forces applied. [ABSTRACT FROM AUTHOR]

A passive daytime radiative cooling thin film material has been developed to provide the cooling source which requires no input, sustainable, and no pollutants or greenhouse gases emission. The thermally induced phase separation method and simple compression were used to prepare the compressed composite silica dioxide/polyethylene(SiO2/PE) aerogel films. The impact of SiO2 particle sizes and additions on the optical properties of composite films was investigated, and the internal microstructures and optical properties of the films were characterized. The optical properties of the films were enhanced by controlling the degree of compression. The results indicate that the addition of micro SiO2 is more favorable for increasing reflectance and nano SiO2 is more favorable for increasing emissivity, and the densification could result in emissivity enhancement and reflectance reduction. The optimal sample is achieved when the mass ratio of nano SiO2 to micro SiO2 to polyethylene is 0.5∶1∶1 and the compression ratio is one-ninth. This sample has a thickness of 0.5 mm, with 96.4% average reflectance of the solar spectrum and 95% average emissivity of the atmospheric window. The practical application performance of the sample was evaluated by testing its radiative cooling performance, antifouling and mechanical stability abilities. The experimental results show that the optimal sample achieves a significant temperature reduction of up to 6.5 ℃ compared to the sub-environment. This indicates that the SiO2/PE aerogel film has the ability to passively cool the sub-environment during both day and night, and that it has a contact angle with water of 127°, providing water resistance and potential self-cleaning properties in practical applications. [ABSTRACT FROM AUTHOR]

Thermally induced phase separation (TIPS) allows preparation of nano and micro-porous structured materials for various applications. The literature thoroughly examines the impact of initial polymer solution concentration and cooling rate on the products morphology. On the contrary, the influence of the solvent removal methods was so far researched scarcely. Hence, we compare both qualitatively and quantitatively the effects of the solvent removal method on pore size distribution, structure, porosity, and thermal conductivity. Our study was carried out with samples prepared by TIPS from polystyrene/cyclohexane solutions employing either extraction agent or lyophilization at different solvent removal temperatures. Materials exhibited interconnected pore structure, implying good sound insulation properties, and had low thermal conductivity, offering the combination of thermal and sound insulation in one layer of material. Pore sizes after lyophilization were up to two times larger than after solvent removal by an extraction agent. On the other hand, the use of extraction agent led up to 10% porosity decrease with average porosity after lyophilization being above 82%. Our findings demonstrate that the solvent removal method is an important parameter during TIPS and that pros and cons of both methods should be carefully considered to obtain optimal material and TIPS process economy. [ABSTRACT FROM AUTHOR]

This study aims to demonstrate the possibility of incorporating a natural antioxidant biomolecule into polymeric porous scaffolds. To this end, Poly-l-Lactic Acid (PLLA) scaffolds were produced using the Thermally Induced Phase Separation (TIPS) technique and additivated with different amounts of rosmarinic acid (RA). The scaffolds, with a diameter of 4 mm and a thickness of 2 mm, were characterized with a multi-analytical approach. Specifically, Scanning Electron Microscopy analyses demonstrated the presence of an interconnected porous network, characterized by a layer of RA at the level of the pore's surfaces. Moreover, the presence of RA biomolecules increased the hydrophilic nature of the sample, as evidenced by the decrease in the contact angle with water from 128° to 76°. The structure of PLLA and PLLA containing RA molecules has been investigated through DSC and XRD analyses, and the obtained results suggest that the crystallinity decreases when increasing the RA content. This approach is cost-effective, and it can be customized with different biomolecules, offering the possibility of producing porous polymeric structures containing antioxidant molecules. These scaffolds meet the requirements of tissue engineering and could offer a potential solution to reduce inflammation associated with scaffold implantation, thus improving tissue regeneration. [ABSTRACT FROM AUTHOR]

An interconnected sponge structure and porous surface poly (acrylonitrile-co-methyl acrylate) (P(AN-MA)) microfiltration membranes (MF) were fabricated via thermally induced phase separation (TIPS) by using caprolactam (CPL), and acetamide (AC) as the mixed diluent. When the ternary system was composed of 15 wt.% P(AN-MA), 90 wt.% CPL, and 10 wt.% AC and formed in a 25 °C air bath, the membrane exhibited the highest water flux of 8107 L/m2·h. The P(AN-MA) membrane contained hydrophobic groups (-COOCH3) and hydrophilic groups (-CN), leading it to exhibit oleophobic properties underwater and hydrophobic properties in oil. The membrane demonstrates efficient separation of immiscible oil/water mixtures. The pure water flux of the petroleum ether/water mixture measured 870 L/m2·h, and the pure oil flux of the petroleum tetrachloride/water mixture measured 1230 L/m2·h under the influence of gravity. Additionally, the recovery efficiency of diluents through recrystallization was 85.3%, significantly reducing potential pollution and production costs. [ABSTRACT FROM AUTHOR]

Polypropylene-based aerogels with high surface area have been developed for the first time. By chemical crosslinking of polypropylene with oligomeric capped-end amino compounds, followed by dissolution, thermally induced phase separation, and the supercritical CO2 drying process or freeze-drying method, the aerogels exhibit high specific surface areas up to 200 m2/g. Moreover, the silica-cage multi-amino compound was utilized in a similar vein for forming hybrid polypropylene aerogels. According to the SEM, the developed polypropylene-based aerogels exhibit highly porous morphology with micro-nanoscale structural features that can be controlled by processing conditions. Our simple and inexpensive synthetic strategy results in a low-cost, chemically resistant, and highly porous material that can be tailored according to end-use applications. [ABSTRACT FROM AUTHOR]

The escalating prevalence of anterior cruciate ligament (ACL) injuries in sports necessitates innovative strategies for ACL reconstruction. In this study, we propose a multiphasic bone-ligament-bone (BLB) integrated scaffold as a potential solution. The BLB scaffold comprised two polylactic acid (PLA)/deferoxamine (DFO)@mesoporous hydroxyapatite (MHA) thermally induced phase separation (TIPS) scaffolds bridged by silk fibroin (SF)/connective tissue growth factor (CTGF)@Poly(l-lactide-co-ε-caprolactone) (PLCL) nanofiber yarn braided scaffold. This combination mimics the native architecture of the ACL tissue. The mechanical properties of the BLB scaffolds were determined to be compatible with the human ACL. In vitro experiments demonstrated that CTGF induced the expression of ligament-related genes, while TIPS scaffolds loaded with MHA and DFO enhanced the osteogenic-related gene expression of bone marrow stem cells (BMSCs) and promoted the migration and tubular formation of human umbilical vein endothelial cells (HUVECs). In rabbit models, the BLB scaffold efficiently facilitated ligamentization and graft-bone integration processes by providing bioactive substances. The double delivery of DFO and calcium ions by the BLB scaffold synergistically promoted bone regeneration, while CTGF improved collagen formation and ligament healing. Collectively, the findings indicate that the BLB scaffold exhibits substantial promise for ACL reconstruction. Additional investigation and advancement of this scaffold may yield enhanced results in the management of ACL injuries.

In this study, a composite membrane was prepared from recycled low-density polyethylene (R-LDPE), thus helping to lighten plastics' load on the environment, while the powder of alumina was used to enhance the membrane contact angle, its porosity, and its mechanical properties. The membrane preparation was made by means of the thermally induced phase separation method by using the butyl acetate as a solvent, hexane as a non-solvent, and the alumina as an additive. The membrane crystalline property was assessed via the Fourier-transform infrared spectroscopy. The membrane characteristics were then investigated in terms of thickness, contact angle, pore size, porosity, mechanical test, bubble point pressure, atomic force microscopy, and scanning electron microscopy analysis. The results revealed that the addition of alumina had an important role in improving membrane structure, properties and therefore its performance. The evaluation of the R-LDPE-alumina membrane showed that it has a good porosity, good hydrophobicity, and better mechanical properties. The obtained membranes were also applicated to the vacuum membrane distillation to test their performance. [ABSTRACT FROM AUTHOR]

Copyright of Journal of Tiangong University is the property of Journal of Tianjin Polytechnic University and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

This study investigates the effect of the macromolecular architecture of poly(vinylidene fluoride) (PVDF) on its thermally induced phase separation (TIPS) behavior and polymorphic crystallization in the PVDF/γ‐butyrolactone (PVDF/γ‐BL) system. Preparative PVDF fractions with specific macromolecular architecture and phase constitution are generated. The results show that PVDF's macromolecular architecture, particularly the degree of branching and regio‐defects, plays a significant role in its temperature‐dependent crystallization and resulting polymorphic phases. While regio‐defects dominate crystallization in the temperature range between 30 and 25 °C, the degree of branching becomes decisive in the 25–20 °C interval. The developed fractions of PVDF are further analyzed in terms of their molecular weight distribution, revealing that the PVDF fractions crystallized out of solution have similar molecular weight distributions with lower dispersity compared with the feed polymer. These findings are crucial for macromolecular separation and adjustment of PVDF polymorphic properties and hence for the development of tailor‐made PVDF matrix materials for composites and membranes. The findings suggest the possibility of polymorphous phase tailoring of PVDF based on macromolecular architecture due to temperature‐controlled crystallization out of solution and strongly motivate further research to reveal deeper knowledge of regio‐defect and branching influence of PVDF solution crystallization. [ABSTRACT FROM AUTHOR]

Copyright of China Synthetic Fiber Industry is the property of Sinopec Baling Petrochemical Company and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

An interconnected sponge structure and porous surface poly (acrylonitrile-co-methyl acrylate) (P(AN-MA)) microfiltration membranes (MF) were fabricated via thermally induced phase separation (TIPS) by using caprolactam (CPL), and acetamide (AC) as the mixed diluent. When the ternary system was composed of 15 wt.% P(AN-MA), 90 wt.% CPL, and 10 wt.% AC and formed in a 25 °C air bath, the membrane exhibited the highest water flux of 8107 L/m2·h. The P(AN-MA) membrane contained hydrophobic groups (-COOCH3) and hydrophilic groups (-CN), leading it to exhibit oleophobic properties underwater and hydrophobic properties in oil. The membrane demonstrates efficient separation of immiscible oil/water mixtures. The pure water flux of the petroleum ether/water mixture measured 870 L/m2·h, and the pure oil flux of the petroleum tetrachloride/water mixture measured 1230 L/m2·h under the influence of gravity. Additionally, the recovery efficiency of diluents through recrystallization was 85.3%, significantly reducing potential pollution and production costs.

The physical properties of a polymer solution that are composition- and/or temperature-dependent are among the most influential parameters to impact the dynamics and thermodynamics of the phase separation process and, as a result, the morphology formation. In this study, the impact of composition- and temperature-dependent density, heat capacity, and heat conductivity on the membrane structure formation during the thermally induced phase separation process of a high-viscosity polymer solution was investigated via coupling the Cahn–Hilliard equation for phase separation with the Fourier heat transfer equation. The variations of each physical property were also investigated in terms of different boundary conditions and initial solvent volume fractions. It was determined that the physical properties of the polymer solution have a noteworthy impact on the membrane morphology in terms of shorter phase separation time and droplet size. In addition, the influence of enthalpy of demixing in this case is critical because each physical property showed a nonhomogeneous pattern owing to the heat generation during phase separation, which in turn influenced the membrane morphology. Accordingly, it was determined that investigating spinodal decomposition without including heat transfer and the impact of physical properties on the morphology formation would lead to an inadequate understanding of the process, specifically in high-viscosity polymer solutions. [ABSTRACT FROM AUTHOR]

Poly(ether ketone ketone) (PEKK) is a semicrystalline high‐performance polymer with exceptional mechanical properties, high continuous operation temperature, and is insoluble in most common solvents. Porous PEKK, desired for biomedical applications, is produced by a high‐temperature thermally induced phase separation process using PEKK solutions in two high boiling aprotic solvents, 4‐phenylphenol and 9‐fluorenone, with concentrations up to 20 wt.%. It is demonstrated that the solvent choice has a pronounced influence on the phase separation behavior, which determines the foam morphology, physical and mechanical properties of PEKK foams. Porous PEKK with porosities ranging from 70% to 90%, specific surface areas up to 194 m2 g−1 and elastic moduli ranging from 35 to 100 MPa are produced. [ABSTRACT FROM AUTHOR]

Porous films were fabricated from poly(L-lactide) (PLLA)-1,4-dioxane-dimethylacetamide ternary systems via thermally induced phase separation (TIPS) followed by using freeze extraction. The effect of processing parameters including freezing temperature, quenching time, and the film thickness was investigated on the physical, mechanical, and morphological properties of the porous films. The primary objective of increase in the film thickness is to cause a decreased temperature gradient between external layer and internal layers at the same temperature (according to Fourier's law) and to decrease the growth rate of the solvent-rich phase. The results revealed that increasing thickness from 1200 to 1600 µm at − 20 °C for 6 h resulted in producing pore sizes 200 nm and nanofibrous (> 200 nm fiber diameter) instead of 400 nm and nanofibrous (< 100 nm fiber diameter). The nanofibrous (< 100 nm) exhibit higher porosity and water absorption, and lower tensile strength than the nanofibrous (> 200 nm). As a result of the high film thickness, decreasing temperature from − 20 to − 45 °C (increasing temperature gradient), and increasing time from 6 to 24 h, it is indicated that the phase separation happens via the coarsening process and forms nanospindle structure with the pore size 800 nm. [ABSTRACT FROM AUTHOR]

Polyimide (PI) and polystyrene (PS) blend electrospun fibers are prepared by electrospinning method. PI and PS are not completely compatible due to the difference of solubility and surface energy in electrospinning precursor, so PI/PS electrospun fibers have some phase separations along the electric field direction under the high‐voltage electrostatic force. PI with high carbon conversion served as carbon nanofibers, PS with low carbon conversion served as porogenic sacrificial agent, so PI/PS‐based activated carbon nanofibers derived from PI/PS electrospun fibers with well‐controlled opening tubular structure are obtained via thermally induced phase separation process. The morphology and electrochemical performance of activated carbon nanofibers are investigated by structural analysis and electrochemical measurements. The relationships among pores structure, electrolyte character and electrochemical performance of activated carbon fibers are extensively evaluated. Activated carbon nanofibers derived from PI/PS (mass ratio = 1:2) electrospun fibers with nano scale opening tube wall structure show a small charge transfer resistance and the short electric double layers forming time, but also suitable average pore diameter (3.74 nm), high BET specific surface area (952.5 m2 g−1) and average pore volume (0.532 cm3 g−1). Then, a comprehensive electrochemical performance can also be achieved in organic electrolyte: high energy density (31.80 Wh kg−1), good power density (3094.05 W kg−1) and low internal resistance (1.24 Ω). The findings reveal a guideline for the preparation of polymer‐based hierachical porous and opening tubular structure activated carbon nanofibers for electrochemical energy conversion and storage devices. [ABSTRACT FROM AUTHOR]

Constructing and maintaining a three-dimensional network structure with high porosity is critical to the preparation of silica aerogel materials because this structure provides excellent properties. However, due to the pearl-necklace-like structure and narrow interparticle necks, aerogels have poor mechanical strength and a brittle nature. Developing and designing lightweight silica aerogels with distinct mechanical properties is significant to extend their practical applications. In this work, thermally induced phase separation (TIPS) of poly(methyl methacrylate) (PMMA) from a mixture of ethanol and water was used to strengthen the skeletal network of aerogels. Strong and lightweight PMMA-modified silica aerogels were synthesized via the TIPS method and supercritically dried with carbon dioxide. The cloud point temperature of PMMA solutions, physical characteristics, morphological properties, microstructure, thermal conductivities, and mechanical properties were investigated. The resultant composited aerogels not only exhibit a homogenous mesoporous structure but also achieve a significant improvement in mechanical properties. The addition of PMMA increased the flexural strength and compressive strength by as much as 120% and 1400%, respectively, with the greatest amount of PMMA (Mw = 35,000 g/mole), while the density just increased by 28%. Overall, this research suggests that the TIPS method has great efficiency in reinforcing silica aerogels with less sacrifice of low density and large porosity. [ABSTRACT FROM AUTHOR]

Abstract Poly(ether ketone ketone) (PEKK) is a semicrystalline high‐performance polymer with exceptional mechanical properties, high continuous operation temperature, and is insoluble in most common solvents. Porous PEKK, desired for biomedical applications, is produced by a high‐temperature thermally induced phase separation process using PEKK solutions in two high boiling aprotic solvents, 4‐phenylphenol and 9‐fluorenone, with concentrations up to 20 wt.%. It is demonstrated that the solvent choice has a pronounced influence on the phase separation behavior, which determines the foam morphology, physical and mechanical properties of PEKK foams. Porous PEKK with porosities ranging from 70% to 90%, specific surface areas up to 194 m2 g−1 and elastic moduli ranging from 35 to 100 MPa are produced.

[Display omitted] PNIPAM as a stimuli-responsive polymer has generated extreme interests due to its versatile applications. However, there is no research report on whether PNIPAM micro/nano-particles can be extracted from its suspension after phase separation. In the present work, LCST-type phase separation in self-synthesized PNIPAM/water system was investigated in depth by dividing the DLS testing process into four stages. In addition to quenching duration, temperature rise process, quenching temperature and PNIPAM concentration all have a great influence on particle size of the suspension. Meanwhile, the steady-state rheology and dynamic viscoelasticity results show that PNIPAM micro/nano-particles in the suspension are "soft" that can deform. Finally, FE-SEM was used to observe the morphology of dehydrated PNIPAM extracted by sessile droplet evaporation under different conditions. The results indicate that these "soft" particles are easier to fuse together, do not have sufficient mechanical strength to maintain their spherical morphology after dehydration. But the above fusion can be suppressed by adjusting evaporation conditions to acquire smaller PNIPAM particles which have sufficient mechanical properties to keep their basic particle morphology. Further, by changing evaporation pressure to positive or negative pressure, dehydrated PNIPAM micro/nano-particles with excellent uniformity and separation can be obtained. This work will provide guidance for extracting micro/nano-particles from polymer/diluent systems with LCST. [ABSTRACT FROM AUTHOR]

Spherical polyamide 12 (PA12) powder for selective laser sintering (SLS) was prepared by thermally induced phase separation (TIPS) method. It was authenticated that the mixed solvent can regulate the liquid–liquid phase separation (LLPS) process by changing the ratio of diluent to non-diluent. The polymer droplets mainly coalesced in the solution, and then the crystal nucleus of PA12 was formed in the droplets. Finally, high crystallinity PA12 powder was precipitated. The morphology, particle size distribution, thermal properties, the change of crystal structure, and powder spreading performances of the obtained powder were characterized. The powder had a narrow particle size distribution, an average particle size of 55.2 μm, and a broad sintering window of 29°C. The results exhibited that the powders prepared by TIPS had excellent sintering properties, and TIPS method provided more choices for SLS technology.

Polypropylene (PP) is widely used as oxygenation membrane material for extracorporeal membrane oxygenation. However, the microporous pores and poor hemocompatibility of PP oxygenation membrane hamper the efficient applications in blood gas exchange process. This study utilizes fluorinated copolymer poly (ethylene-chlorotrifluoroethylene) (ECTFE) as blending additive to construct PP/ECTFE flat sheet and hollow fiber membranes (HFM) via thermally induced phase separation (TIPS) for blood oxygenation. The PP:ECTFE-3:1 HFMs exhibited high O 2 and CO 2 exchange rates of ∼319.6 ml min−1 m−2 and ∼1532.3 ml min−1 m−2 in blood gas exchange process, respectively. The introduction of fluorinated segments rendered hydrophobic and low-surface-energy membrane surface, as indicated by the water contact angle of ∼119.2° and surface energy of ∼35.1 mN m−1 of PP:ECTFE-3:1 flat sheet membrane, compared with those of ∼96.8° and ∼41.0 mN m−1 for the PP membrane. Consequently, the liquid entry pressure and hemocompatibility were enhanced, affording resistance to plasma leakage for 189 h, which prolonged 30.5 times than 6 h of PP HFM, and was comparable with the level of poly (4-methyl-1-pentene) (PMP) oxygenation membrane. The PP/ECTFE blend oxygenation membranes possess great potential for biomedical application. [Display omitted] • PP/ECTFE flat sheet membranes and hollow fiber membranes were fabricated. • The membranes exhibit prolonged blood oxygenation performance. • Higher liquid entry pressure and improved hemocompatibility were acquired. • The membranes exhibit enhanced gas permeance and long-term stability. [ABSTRACT FROM AUTHOR]

This study aims at characterization of porous poly(ε-caprolactone) (PCL) scaffolds prepared by the methods of thermally induced phase separation (TIPS) and TIPS supported by particulate leaching (PL). Both techniques were combined with freeze-drying. Two PCL grades (with different average molecular weight characterized by MFR 6.1 and 1.2 g/10 min) were employed in the fabrication of scaffolds. Three types of salt (sodium chloride) particles were used in the TIPS-PL preparation of the PCL sample: (i) smaller particles (S) measuring 200–315 μm, (ii) larger particles (B) measuring 500–600 μm, and (iii) mixture of S and B particles (S/B = 1/1 wt/wt). The crystallization behavior of the PCL solutions and the thermal properties of scaffolds were investigated by polarized light microscopy (PLM) and differential scanning calorimetry (DSC), respectively. The structural changes of PCL were studied by attenuated total reflectance infrared spectroscopy (ATR-FTIR). The scaffold structure was visualized by means of scanning electron microscopy (SEM) and X-Ray micro-computed tomography (X-ray micro-CT). Furthermore, the density, porosity, water uptake, contact angle and compressive properties of scaffold were investigated. The molecular weight of PCL had an impact on the crystallization of the PCL solutions and thereby on the crystallinity of scaffolds and the morphology of pore walls formed during TIPS. Sodium chloride grains had an influence on the pore size and overall morphology of foam scaffolds prepared by TIPS-PL. The addition of NaCl decreased significantly the density and compressive properties and increased the porosity and water uptake of scaffolds.

An experimental quasi-equilibrium phase diagram of the polyvinylidene fluoride (PVDF)–camphor mixture is constructed using an original optical method. For the first time, it contains a boundary curve that describes the dependence of camphor solubility in the amorphous regions of PVDF on temperature. It is argued that this diagram cannot be considered a full analogue of the eutectic phase diagrams of two low-molar-mass crystalline substances. The phase diagram is used to interpret the polarized light hot-stage microscopy data on cooling the above mixtures from a homogeneous state to room temperature and scanning electron microscopy data on the morphology of capillary-porous bodies formed upon camphor removal. Based on our calorimetry and X-ray studies, we put in doubt the possibility of incongruent crystalline complex formation between PVDF and camphor previously suggested by Dasgupta et al. (Macromolecules 2005, 38, 5602–5608). We also describe and discuss the high-temperature crystalline structure of racemic camphor, which is not available in the modern literature. [ABSTRACT FROM AUTHOR]

Owing to the fact that heat transfer during the thermally induced phase separation process is limited, a quench rate is inevitably entailed, which leads to the existence of temporal and spatial variations in temperature. Hence, it is of great importance to take into account the nonisothermality during the phase separation process, especially in high viscosity polymer solutions. In this study, the influence of conductive heat transfer on the morphology formation during the thermally induced phase separation process was investigated theoretically in terms of quench depth, boundary conditions, and enthalpy of demixing to elucidate the interaction between temperature and concentration through incorporating the nonlinear Cahn-Hilliard equation and the Fourier heat transfer equation in two dimensions. The Flory-Huggins free energy theory for the thermodynamics of phase separation, slow mode theory, and Rouse law for polymer diffusion without entanglements were taken into account in the model development. The simulation results indicated a strong interaction between heat transfer and phase separation, which impacted the morphology formation significantly. Results confirmed that quench depth had an indispensable impact on phase separation in terms of higher characteristic frequency by increasing the driving force for heat transfer. Applying quench from various boundaries led to a difference in the quench rate due to the high viscosity of the polymer solution. This led to a gradation in pore size and anisotropic morphology formation. The degree and direction of anisotropy depended on quench depth and rate, quench time, heat conduction rate inside the solution, solution viscosity, temperature evolution, and the enthalpy of demixing. It was also verified that the influence of enthalpy of demixing on phase separation could not be neglected as it increased the solution temperature and led to phase separation being accomplished at a higher temperature than the initial quench temperature. [ABSTRACT FROM AUTHOR]

Promoting neovascularization is a prerequisite for many tissue engineering applications and the treatment of cardiovascular disease. Delivery of a pro-angiogenic stimulus via acellular materials offers several benefits over biological therapies but has been hampered by interaction of the implanted material with the innate immune response. However, macrophages, a key component of the innate immune response, release a plurality of soluble factors that can be harnessed to stimulate neovascularization and restore blood flow to damaged tissue. This study investigates the ability of biodegradable poly(D,L-lactic-co-glycolic acid) (PLGA) microspheres to restore tissue perfusion in a hind limb model of ischaemia. Microspheres exhibiting a hierarchical porous structure are associated with an increase in blood flow at day 21 post-implantation compared with solid microspheres composed of the same polymer. This corresponds with an increase in blood vessel density in the surrounding tissue. In vitro simulation of the foreign body response observed demonstrates M2-like macrophages incubated with the porous microspheres secreted increased amounts of vascular endothelial growth factor (VEGF) compared with M1-like macrophages providing a potential mechanism for the increased neovascularization. The results from this study demonstrate implantable biodegradable porous microspheres provide a novel approach for increasing neovascularization that could be exploited for therapeutic applications., (© 2024 The Author(s). Advanced Healthcare Materials published by Wiley‐VCH GmbH.)

A high-performance polypropylene hollow fiber membrane (PP-HFM) was prepared by using a binary environmentally friendly solvent of polypropylene as the raw material, adopting the thermally induced phase separation (TIPS) method, and adjusting the raw material ratio. The binary diluents were soybean oil (SO) and acetyl tributyl citrate (ATBC). The suitable SO/ATBC ratio of 7/3 was based on the size change of the L-L phase separation region in PP-SO/ATBC thermodynamic phase diagram. Through the characterization and comparison of the basic performance of PP-HFMs, it was found that with the increase of the diluent content in the raw materials, the micropores of outer surface of the PP-HFM became larger, and the cross section showed a sponge-like pore structure. The fluoropolymer, Hyflon ADx, was deposited on the outer surface of the hollow fiber membrane using a physical modification method of solution dipping. After modification, the surface pore size of the Hyflon AD40L modified membranes decreased; the contact angle increased to around 107°; the surface energy decreased to 17 mN·m−1; and the surface roughness decreased to 17 nm. Hyflon AD40L/PP-HFMs also had more water resistance properties from the variation of wetting curve. For biocompatibility of the membrane, the adsorption capacity of the modified PP membrane for albumin decreased from approximately 1.2 mg·cm−2 to 1.0 mg·cm−2, and the adsorption of platelets decreased under fluorescence microscopy. The decrease in blood cells and protein adsorption in the blood prolonged the clotting time. In addition, the hemolysis rate of modified PP membrane was reduced to within the standard of 5%, and the cell survival rate of its precipitate was above 100%, which also indicated the excellent biocompatibility of fluoropolymer modified membrane. The improvement of hydrophobicity and blood compatibility makes Hyflon AD/PP-HFMs have the potential for application in membrane oxygenators.

Wide application of chitosan in modern technologies is limited by the lack of reliable and low-cost techniques to prepare size-tuned constructs with a complex surface morphology, improved optical and mechanical properties. We report a new simple method for preparation of transparent thermoreversible chitosan alcogels from chitosan/H 2 O/ethanol ternary systems. This method, termed "low temperature thermally induced phase separation under non-freezing conditions" (LT-TIPS-NF), fine tunes gelation by adjusting only temperature (from 5 to −25 °C) and varying the initial content of chitosan (from 0.5 to 2.0 wt%) and ethanol (from 28.5 to 47.5 vol%). Transparent non-swelling final constructs of complex shape are prepared by fixing the pre-formed alcogels with a base solution. The size of the gel constructs is limited only by the dimensions of the mold and the cooling chamber. The LT-TIPS-NF is applicable both in injection molding and 3D printing techniques. The in vitro and in vivo experiments show the absence of prominent cytotoxicity and well-defined cell adhesion on the obtained hydrogels. Thus, this facile and scalable technique provides the multifunctional chitosan gel preparation with easily controlled properties exploiting inexpensive, renewable, and environmentally friendly source polysaccharide. These materials have prospects for a variety of uses, especially for biomedical applications. [Display omitted] • An approach for thermoreversible chitosan-based alcogel formation by LT-TIPS-NF method was developed. • Nanofibrous hydrogels with high transparency and increased mechanical strength were fabricated by fixation of alcogels. • Molding and 3D-printing of hydrogel constructs with complex structure morphology was performed. • The prepared hydrogels demonstrated good cell viability in vitro and high biocompatibility in vivo. [ABSTRACT FROM AUTHOR]

The work represents a study of structure formation during thermally induced phase separation in low concentrated blends of semicrystalline polymers with thermodynamically poor solvents. According to the phase diagram, cooling of homogeneous blends located to the left of the upper critical solution temperature can cause two phase separation scenarios. The fact that both scenarios are possible is experimentally confirmed by investigating blends of polypropylene with a cosolvent and polyamide-12 with a cosolvent, using polarized light optical microscopy and scanning electron microscopy. The study proves the possibility to develop facile approaches to the formation of porous microspheres from semicrystalline polymers. [ABSTRACT FROM AUTHOR]

Membrane distillation (MD) can treat high-salinity brine. However, the system's efficiency is hindered by obstacles, including salt scaling and temperature polarization. When properly implemented, surface patterns can improve the mass and heat transfer in the boundary layer, which leads to higher MD efficiency. In this work, the performance of direct contact membrane distillation (DCMD) using Sharklet-patterned poly (vinylidene fluoride) (PVDF) membranes is investigated. Both non-patterned and patterned PVDF membranes are prepared by lithographically templated thermally induced phase separation (lt -TIPS) process with optimized conditions. Sharklet patterns on the membranes improve the DCMD performance: up to 17 % higher water flux and 35 % increased brine-side heat transfer coefficient. The scaling resistance of the membranes during DCMD is tested by both saturated CaSO 4 solution and hypersaline NaCl solutions. Patterned PVDF membranes show an average of 30 % higher water flux and up to 45 % lessened flux decline over time compared with non-patterned membranes when treating high-concentration brines. Post-mortem analysis reveals that Sharklet-patterned membranes display less salt-scaling on surfaces with smaller-sized CaSO 4 and NaCl crystals, maintain a relatively cleaner surface, and exhibit better retention of hydrophobicity. [Display omitted] • Sharklet-patterned PVDF membranes were fabricated with patterning fidelity up to 80 %. • The effects of Sharklet patterns on DCMD performances were quantified. • The Sharklet improves flux by 17 % and brine-side heat transfer coefficient by 35 %. • The Sharklet improves membranes' robustness when treating hypersaline feeds. [ABSTRACT FROM AUTHOR]

• High vapor flux UHMWPE composite membranes were prepared by TIPS method. • Membranes prepared by 9.0 million molecular weight of UHMWPE have higher vapor flux. • TA-APTES nanospheres can co-deposit on UHMWPE membranes surface robustly. • TA-APTES nanospheres have abundant secondary reaction sites for fluorination. • Membranes have a high separation efficiency (99.98%) for high salinity anionic dyeing wastewater. Commercial flat sheet membranes have relatively low flux in membrane distillation. Here, a ultra-high molecular weight polyethylene (UHMWPE) composite membrane with high flux was prepared via thermally induced phase separation (TIPS) method for direct contact membrane distillation (DCMD). The UHMWPE membrane has low tortuosity (spherical structure) and low thickness to decrease the vapor mass transfer resistance. In addition, UHMWPE/decalin gel membrane washed in hot decalin (85℃) in order to increase the permeate flux, and the optimum membrane has the highest flux of 43.51 kg/(m2·h). In order to increase the anti-wetting properties of UHMWPE membranes, Tannic acid (TA) − 3-aminopropyltriethoxysilane (APTES) coating composed of abundant nanospheres is co-deposited on the surface of UHMWPE membrane to increase surface roughness. The subsequent fluorination process can decrease the surface energy and improve the anti-surfactant property. The optimum modified membrane has a water contact angle of 152.5°, and the permeate flux is 31.04 kg/(m2·h). Moreover, the membrane has high rejection (99.98 %) and high water recovery (82.87 %) over 60 h testing for high salinity anionic dyeing wastewater. [ABSTRACT FROM AUTHOR]

[Display omitted] • Anti-fouling polyketone membranes were prepared by reduction using NaBH 4. • Reduction altered the chemical composition, while other properties were unaffected. • Reduction significantly reduced attachment of proteins and other foulants. • Dynamic filtration tests showed excellent flux recovery of the modified membranes. This study utilized solvent co-extrusion technology and NaBH 4 reduction to fabricate polyketone (PK) hollow fiber membranes with high water permeance and fouling resistance. Variations in reduction reaction time were explored to assess their impact on chemical composition, morphology, and properties. The results showed that the reduction reaction leads to the conversion of carbonyl groups on the membrane surface to hydroxyl groups, and with prolonged reaction time, the amount of hydroxyl groups on the membrane surface increases to a certain extent. The change in membrane chemical composition enhanced the hydrophilicity, while leaving the membrane morphology, mechanical properties, and separation performance largely unaffected. Static adsorption tests with bovine serum albumin (BSA) and E. coli exhibited distinct fouling behavior. While pristine PK membranes displayed significant BSA adsorption, PK reduction significantly reduced it. Both pristine and reduced PK membranes showed minimal E. coli attachment, likely due to weak interactions. Dynamic filtration tests demonstrated excellent flux recovery for reduced PK membranes, especially after 10 min of reduction, indicating superior fouling resistance with high flux recovery and low irreversible fouling, regardless of foulant type. These findings highlight a straightforward and efficient approach for producing high-performance membranes with exceptional fouling resistance suitable for practical applications. [ABSTRACT FROM AUTHOR]

• Thermal behavior is studied in the UHMWPE – dioctyl adipate mixture. • Increase in polymer molecular weight expectedly promotes LLPS. • Increase in cooling rate unexpectedly disfavors LLPS. • LLPS may be more kinetically dependent process than polymer crystallization. • UHMWPE – dioctyl adipate is a promising system for membrane preparation. The thermal behavior of ultra-high molecular weight polyethylene (UHMWPE) with dioctyl adipate (DOA) was investigated by the differential scanning calorimetry (DSC) method. Capillary-porous bodies were obtained via thermally induced phase separation of DOA mixtures with polyethylenes of different molecular weight at different cooling rates. Analysis of the morphology of the prepared porous bodies together with DSC data and results of cloud point estimation revealed an unexpected effect of a cooling rate on the type of phase separation occurring in the mixture during its cooling from homogeneous state. Particularly it was shown that increase in the cooling rate reduces the probability of realization of liquid – liquid phase separation in the mixture. It was argued that such behavior, different from the standard semicrystalline polymers, is a result of kinetic hindrance of liquid – liquid phase separation in mixtures containing a polymer with such a high molecular weight. [Display omitted] [ABSTRACT FROM AUTHOR]

A new method of fabricating porous membranes based on ultra-high molecular weight polyethylene (UHMWPE) by controlled swelling of the dense film was proposed and successfully utilized. The principle of this method is based on the swelling of non-porous UHMWPE film in organic solvent at elevated temperatures, followed by its cooling and further extraction of organic solvent, resulting in the formation of the porous membrane. In this work, we used commercial UHMWPE film (thickness 155 μm) and o-xylene as a solvent. Either homogeneous mixtures of the polymer melt and solvent or thermoreversible gels with crystallites acting as crosslinks of the inter-macromolecular network (swollen semicrystalline polymer) can be obtained at different soaking times. It was shown that the porous structure and filtration performance of the membranes depended on the swelling degree of the polymer, which can be controlled by the time of polymer soaking in organic solvent at elevated temperature (106 °C was found to be the optimal temperature for UHMWPE). In the case of homogeneous mixtures, the resulting membranes possessed both large and small pores. They were characterized by quite high porosity (45–65% vol.), liquid permeance of 46–134 L m−2 h−1 bar−1, a mean flow pore size of 30–75 nm, and a very high crystallinity degree of 86–89% at a decent tensile strength of 3–9 MPa. For these membranes, rejection of blue dextran dye with a molecular weight of 70 kg/mol was 22–76%. In the case of thermoreversible gels, the resulting membranes had only small pores located in the interlamellar spaces. They were characterized by a lower crystallinity degree of 70–74%, a moderate porosity of 12–28%, liquid permeability of up to 12–26 L m−2 h−1 bar−1, a mean flow pore size of up to 12–17 nm, and a higher tensile strength of 11–20 MPa. These membranes demonstrated blue dextran retention of nearly 100%.

Hybrid porous scaffolds composed of both natural and synthetic biopolymers have demonstrated significant improvements in the tissue engineering field. This study investigates for the first time the fabrication route and characterization of poly-L-lactic acid scaffolds blended with polyhydroxyalkanoate up to 30 wt%. The hybrid scaffolds were prepared by a thermally induced phase separation method starting from ternary solutions. The microstructure of the hybrid porous structures was analyzed by scanning electron microscopy and related to the blend composition. The porosity and the wettability of the scaffolds were evaluated through gravimetric and water contact angle measurements, respectively. The scaffolds were also characterized in terms of the surface chemical properties via Fourier transform infrared spectroscopy in attenuated total reflectance. The mechanical properties were analyzed through tensile tests, while the crystallinity of the PLLA/PHA scaffolds was investigated by differential scanning calorimetry and X-ray diffraction. [ABSTRACT FROM AUTHOR]

A non-toxic and environmentally safe diluent, acetyl tributyl citrate, was employed to prepare poly (vinylidene fluoride)-co-hexafluoropropylene membranes via thermally induced phase separation. Effects of the polymer concentration on the phase diagram, membrane morphology, hydrophobicity, pore size, porosity and mechanical properties (tensile stress and elongation at break) were investigated. The results showed that the pore size and porosity tended to decrease with increasing polymer concentration, whereas the contact angle, liquid entry pressure and mechanical properties showed the opposite trend. In direct contact membrane distillation operation with 3.5 wt-% sodium chloride solution as the feed solution, the prepared membranes performed high salt rejection (> 99.9%). Furthermore, the prepared membranes retained excellent performance in long-term stability tests regarding the permeate flux and salt rejection. [ABSTRACT FROM AUTHOR]

The effect of a N,N-dimethylformamide (DMF)/acetone solvent system (3:7, 4:6, 5:5, 6:4, 7:3) and spinning medium (air and water) on the membrane morphology and the structure-property relationship were investigated. A facile method was optimized to generate a porous, polymer-fiber membrane via the combinative effect of electrospinning and thermally inducing phase separation of the DMF/acetone (4:6) solvent system in a water medium. The attenuated total reflection (ATR) - Fourier transform infrared (FTIR) results showed an increased β-phase compared to the pristine poly(vinylidene fluoride) (PVDF). The XRD and DSC results further confirmed that the co-existing α- and β-phases in the pristine PVDF were converted into a unique β-phase in the electrospun membranes. In addition, the solvent uptake percentage of the DMF/acetone (4:6) solvent system in a water medium (540) is much greater than that in an air medium (320), and over two times better than that of commercial polyethylene (PE) membranes (190). Similarly, the discharge capacity of the PVDF membrane separator prepared with the DMF/acetone (4:6) solvent system in a water medium is higher than that of the air medium. This enhancement of solvent uptake might be due to the interconnected porous morphology present in the water medium.

This article presents a rapid method for selecting solvents suitable for polymer membrane formation by thermally induced phase separation. The method, based on optical microscopy, makes it possible to determine temperatures of liquid-liquid phase separation and polymer crystallization in the blends and to monitor structural changes in the blends during cooling. The proposed method was applied to find out whether a series of disubstituted esters of dicarboxylic acids and their binary mixtures could be used to form polypropylene membranes. The obtained polymer crystallization temperatures and liquid–liquid phase separation temperatures in the different mixtures were used to compare the thermodynamic affinity of the chosen solvents for polypropylene. The results were compared to the data on Hildebrand solubility parameters. It is shown that the thermodynamic affinity of dialkyl phthalate for polypropylene increases as the alkyl-substituent becomes longer, while the comparison of the Hildebrand solubility parameters gives quite unambigiuous results depending on the value chosen for the polymer. [ABSTRACT FROM AUTHOR]

The Hansen solubility parameter (HSP) theory, which includes the Hansen dispersion (D), polar (P), and hydrogen (H) components and a derivative 'solubility parameter distance, Ra' parameter, was adopted to evaluate the interaction between different polymers and their various diluents, so as to obtain a valuable and feasible criterion for the diluent selection of the thermally induced phase separation (TIPS) process for the preparation of polymeric membranes. Firstly, a full-scale database of the four HSP parameters of typical polymer-diluent systems was obtained based on a complete literature review about the phase separation process of all the polymer/diluents systems that have been applied to prepare polymeric membranes via TIPS and our additional exploratory experiments for membrane formation mechanism, in which two different phase separation processes including solid to liquid and liquid to liquid were distinguished. Relationships between the Ra parameter and the phase separation behavior were figured out to get a criterion for selecting the single diluent for the typical polymers. Moreover, the diluent selection was extended by adding a second diluent, and a schematic three-dimensional phase diagram was drawn to provide a feasible understanding of the TIPS process of the polymer-binary diluent system. Taking polypropylene (PP) as the representative example, plenty of exploratory experiments for the membrane formation mechanism based on a literature review were conducted to propose a guide based on the Hansen polar and hydrogen solubility component parameters to help select a proper binary diluent system. [ABSTRACT FROM AUTHOR]

Additive manufacturing (AM) of aerogels increases the achievable geometric complexity, and affords fabrication of hierarchically porous structures. In this work, a custom heated material extrusion (MEX) device prints aerogels of poly(phenylene sulfide) (PPS), an engineering thermoplastic, via in situ thermally induced phase separation (TIPS). First, pre-prepared solid gel inks are dissolved at high temperatures in the heated extruder barrel to form a homogeneous polymer solution. Solutions are then extruded onto a room-temperature substrate, where printed roads maintain their bead shape and rapidly solidify via TIPS, thus enabling layer-wise MEX AM. Printed gels are converted to aerogels via postprocessing solvent exchange and freeze-drying. This work explores the effect of ink composition on printed aerogel morphology and thermomechanical properties. Scanning electron microscopy micrographs reveal complex hierarchical microstructures that are compositionally dependent. Printed aerogels demonstrate tailorable porosities (50.0-74.8%) and densities (0.345-0.684 g cm -3 ), which align well with cast aerogel analogs. Differential scanning calorimetry thermograms indicate printed aerogels are highly crystalline (≈43%), suggesting that printing does not inhibit the solidification process occurring during TIPS (polymer crystallization). Uniaxial compression testing reveals that compositionally dependent microstructure governs aerogel mechanical behavior, with compressive moduli ranging from 33.0 to 106.5 MPa., (© 2023 The Authors. Advanced Materials published by Wiley‐VCH GmbH.)

Recently, solid polymer electrolytes (SPEs) are of great current interest as substitutes to conventional liquid type electrolytes. Although the SPEs significantly alleviate the safety issues of the lithium-ion batteries based on conventional liquid electrolytes, they intrinsically exhibit low ion conductivity. In this study, a bicontinuous solid polymer electrolyte containing polyacrylonitrile (PAN) membrane and a mixture of succinonitrile (SN) and lithium bis(trifluoromethanesulfonyl)imide was prepared with different molarities of the lithium salt. Porous PAN membrane was fabricated via a thermally induced phase separation method (TIPS). The PAN-based SPE exhibited the maximum ionic conductivity of ∼5.0 × 10−3 S/cm at the salt molarity of 1.0 M. [ABSTRACT FROM AUTHOR]

For the first time, we have successfully fabricated microfiltration (MF) hollow fiber membranes by the thermally induced phase separation (TIPS) and non-solvent induced phase separation (NIPS) methods using cellulose acetate benzoate (CBzOH), which is a cellulose derivative with considerable chemical resistance. To obtain an appropriate CBzOH TIPS membrane, a comprehensive solvent screening was performed to choose the appropriate solvent to obtain a membrane with a porous structure. In parallel, the CBzOH membrane was prepared by the NIPS method to compare and evaluate the effect of membrane structure using the same polymer material. Prepared CBzOH membrane by TIPS method showed high porosity, pore size around 100 nm or larger and high pure water permeability (PWP) with slightly low rection performance compared to that by NIPS. On the contrary, CBzOH membranes prepared with the NIPS method showed three times lower PWP with higher rejection. The chemical resistance of the prepared CBzOH membranes was compared with that of cellulose triacetate (CTA) hollow fiber membrane, which is a typical cellulose derivative as a control membrane, using a 2000 ppm sodium hypochlorite (NaClO) solution. CBzOH membranes prepared with TIPS and NIPS methods showed considerable resistance against the NaClO solution regardless of the membrane structure, porosity and pore size. On the other hand, when the CTA membrane, as the control membrane, was subjected to the NaClO solution, membrane mechanical strength sharply decreased over the exposure time to NaClO. It is interesting that although the CBzOH TIPS membrane showed three times higher pure water permeability than other membranes with slightly lower rejection and considerably higher NaClO resistance, the mechanical strength of this membrane is more than two times higher than other membranes. While CBzOH samples showed no change in chemical structure and contact angle, CTA showed considerable change in chemical structure and a sharp decrease in contact angle after treatment with NaClO. Thus, CBzOH TIPS hollow fiber membrane is noticeably interesting considering membrane performance in terms of filtration performance, mechanical strength and chemical resistance on the cost of slightly losing rejection performance.

One of the materials that attracts attention as a potential material for membrane formation is ultrahigh molecular weight polyethylene (UHMWPE). One potential material for membrane formation is ultrahigh molecular weight polyethylene (UHMWPE). The present review summarizes the results of studies carried out over the last 30 years in the field of preparation, modification and structure and property control of membranes made from ultrahigh molecular weight polyethylene. The review also presents a classification of the methods of membrane formation from this polymer and analyzes the conventional (based on the analysis of incomplete phase diagrams) and alternative (based on the analysis of phase diagrams supplemented by a boundary line reflecting the polymer swelling degree dependence on temperature) physicochemical concepts of the thermally induced phase separation (TIPS) method used to prepare UHMWPE membranes. It also considers the main ways to control the structure and properties of UHMWPE membranes obtained by TIPS and the original variations of this method. This review discusses the current challenges in UHMWPE membrane formation, such as the preparation of a homogeneous solution and membrane shrinkage. Finally, the article speculates about the modification and application of UHMWPE membranes and further development prospects. Thus, this paper summarizes the achievements in all aspects of UHMWPE membrane studies.

iPP films with different top and bottom surface parts were prepared via solution cast method. The structure and mechanism of iPP films prepared using this method were analyzed. When the evaporation temperature was not enough to form a homogeneous film, a top surface part was formed due to thermally induced phase separation (TIPS) and the crystallization, a bottom surface part was created due to the adsorption of carrier and both these parts were temperature sensitive. When the evaporation temperature was 60°C, particles with lotus leaf structure appeared in the top surface part, resulting in a quasi superhydrophobic surface. [ABSTRACT FROM AUTHOR]

• Preparation of cellulose monolith with graded porous structure through TIPS. • The graded porous structure of the material improves the mass transfer performance of CM-AO. • Excellent adsorption performance of uranyl ions in radioactive nuclear wastewater. The development and application of new and efficient adsorption materials are key issues in the treatment of nuclear wastewater. This paper introduces a novel hierarchical porous amidoxime cellulose monolith synthesized through thermally induced phase separation (TIPS). The inherent hydrophilicity of cellulose, combined with the graded porous structure achieved through TIPS (with a specific surface area of 10.36 m2/g), endows the material with strong mass transfer ability. The adsorption properties of this amidoxime cellulose monolith for uranyl ions were evaluated in both batch and flow-through column adsorption scenarios. Remarkably, the adsorption saturation was achieved within a concise period of 13 h in batch adsorption. The hierarchical porous structure of the amidoxime cellulose monolith exhibited exceptional adsorption performance for uranyl ion, achieving a removal rate of 99.99 %. Moreover, this removal rate was sustained for 200 min, and the monolith proved recyclable for at least 5 cycles in flow-through column adsorption tests involving nuclear wastewater. When used for adsorption in real wastewater environments, the material achieved the removal of over 99.96 % of total α and β radioactivity. These findings underscore the high efficiency of the newly developed hierarchical porous amidoxime cellulose monolith in uranyl ion adsorption. They emphasize its substantial potential for the efficient adsorption and removal of uranyl ion from nuclear wastewater. [ABSTRACT FROM AUTHOR]

Efforts have been made in thermally induced phase separation (TIPS) process to modify the morphology of polyvinylidene fluoride (PVDF) membranes in order to improve their permeation performance and mechanical properties. Nevertheless, many methods not only altered the outer surface but also impacted the overall membrane structure, resulting in a trade-off between permeability and mechanical properties. In this study, we utilized a modified TIPS process to refine the outer surface morphology without altering the bulk structure. This was achieved by introducing NaCl in the coagulation bath. The PVDF membranes were fabricated using a dope with water insoluble diluent dimethyl phthalate (DMP) as main solvent and water-soluble additives polyethylene glycol 400 (PEG400)/triethylene glycol (TEG) as pore formers. The inclusion of NaCl in the coagulation bath serves to decrease the solubility of PEG within this medium, owing to the salting-out effect. Consequently, the NaCl concentration in the coagulation bath emerges as a crucial factor in regulating the migration of PEG400 toward the membrane surface. This control mechanism facilitates the precise adjustment of the outer surface morphology in the fabrication of membranes. As the NaCl concentration increases in the coagulation bath, the outer surface of the fabricated membrane transited from a mesh-like structure to a spherulite structure. As 0.5 mol L−1 NaCl was added to the coagulation bath, the membranes displayed a pure water permeability of 1073.9 L m−2 h−1 bar−1 while maintaining a narrow pore size distribution. Compared to the membranes fabricated without NaCl addition, the increment of the PWP contributed to the slight increase in mean pore size from 65 nm to 84 nm. Meanwhile, the water-insoluble diluent DMP was not affected by the addition of NaCl, which means that the bulk structure of the membrane could be maintained. Consequently, the increase in permeability did not compromise the mechanical properties of the membranes. All the membranes fabricated in this study maintained a reasonable tensile strength of approximately 3 MPa. This study introduces a simple and environmental method to increase the permeability effectively and fine-tune the pore size of the TIPS membranes while having little effect on the bulk structure. Furthermore, the study provides valuable insights into how changes in outer surface morphology can impact the pore size and permeability of TIPS PVDF membranes. [Display omitted] • Ultrafiltration PVDF membranes was fabricated by a modified TIPS method. • NaCl coagulation bath could control the outflow of PEG toward membrane surface. • The surface of the membranes could be fine-tuned without altering the bulk structure. • The ultrafiltration membranes present a narrow pore size distribution and high permeability. [ABSTRACT FROM AUTHOR]

Objective(s): The present study aimed to prepare polycaprolactone (PCL) scaffolds with high porosity and pore interconnectivity, in order to copy the microstructure of natural bones using the thermally induced phase separation (TIPS) technique. Materials and Methods: The scaffolds were coated with chitosan (CH), bioactive glass (BG), and gelatin nanoparticles (GEL NPs) and assessed using scanning electron microscopy and Fourier-transform infrared spectroscopy (FTIR). Results: The size of the prepared BG and GEL NPs was estimated to be 400 and 234 nanometers, respectively. The porosity and contact angle of PCL/CH/GEL NPs/BG was 74% and 72°, respectively. Weight loss and electron microscopy evaluations indicated the improved degradation rate of the scaffolds and spreading tendency of the cells on the scaffolds when modified as compared to the scaffolds that were purely obtained from PCL. In addition, the in-vitro studies revealed that the MG-63 cells cultured on the PCL/CH/GEL NPs/BG scaffolds showed improved cell proliferation more significantly compared to the scaffolds obtained from PCL, PCL/CH/GEL NPs, PCL/CH, and PCL/GEL NPs. Mechanical examinations also showed that PCL/CH/GEL/BG scaffolds had the highest mechanical strength compared to other groups (i.e., 4.66 Mpa). Cell viability was estimated to be 96.7%, and the alizarin red test indicated the significant improvement of mineralization in the PCL/CH/GEL NP group. Conclusion: According to the results, the PCL scaffolds that were modified by CH/GEL NPs/BG had the high potency to be used as bone tissue engineering scaffolds.

Prostate cancer is a leading cause of death in men and despite improved surgical procedures that aid tumor resection, the risk of recurrence after surgery as a result of positive resection margins remains significant. Adjuvant chemotherapy is often required but this is associated with toxicity. Improved ways of delivering highly toxic chemotherapeutic drugs in a more controlled and targeted manner after the prostate has been removed during surgery could reduce the risk of recurrence and avoid systemic toxicity. The aim of this study was to develop a novel drug-device combination tissue scaffold that can be used to deliver the chemotherapeutic agent, docetaxel, into the tissue cavity that is created following radical prostatectomy. The device component investigated consisted of highly porous, poly(dl-lactide-co-glycolide) microparticles made using thermally induced phase separation. A facile method was established for loading docetaxel with high efficiency within one hour. Sustained drug release was observed from the microparticles when placed into a dynamic system simulating tissue perfusion. The drug released from the microparticles into perfusates collected at regular time intervals inhibited colony formation and exhibited sustained cytotoxicity against 3D spheroids of PC3 prostate cancer cells over 10 days. In conclusion, this study demonstrates the concept of combining docetaxel with the biodegradable microparticles at the point of care is technically feasible for achieving an effective drug-device combination tissue scaffold. This approach could provide an effective new approach for delivering adjuvant chemotherapy following radical prostatectomy.