Formation and characterization of core-shell CL-20/TNT composite prepared by spray-drying technique

The core-shell 2,4,6,8,10,12-Hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane/2,4,6-Trinitrotoluene(CL-20/TNT)composite was prepared by spray-drying method in which sensitive high energy explosive(CL-20)was coated with insensitive explosive(TNT).The structure and properties of different formulations of CL-20/TNT composite and CL-20/TNT mixture were characterized by scanning electron microscopy(SEM),Transmission electron microscopy(TEM),Laser particle size analyzer,X-ray photoelectron spectroscopy(XPS),X-ray diffraction(XRD),differential scanning calorimetry(DSC),impact sensitivity test and detonation performance.The results of SEM,TEM,XPS and XRD show that e-CL-20 particles are coated by TNT.When the ratio of CL-20/TNT is 75/25,core-shell structure is well formed,and thickness of the shell is about 20e30 nm.And the analysis of heat and impact show that with the increase of TNT content,the TNT coating on the core-shell composite material can not only catalyze the thermal decomposition of core material(CL-20),but also greatly reduce the impact sensitivity.Compared with the CL-20/TNT mixture(75/25)at the same ratio,the characteristic drop height of core-shell CL-20/TNT composite(75/25)increased by 47.6%and the TNT coating can accelerate the nuclear decomposition in the CL-20/TNT composites.Therefore,the preparation of the core-shell composites can be regarded as a unique means,by which the composites are characterized by controllable decomposition rate,high energy and excellent mechanical sensitivity and could be applied to propellants and other fields.

Spray-drying assisted layer-structured H_(2)TiO_(3) ion sieve synthesis and lithium adsorption performance

A spray-drying assisted solid-state method to prepare spherical layer-structured H_(2)TiO_(3) ion sieve(LSTIS)particles is reported herein.The effects of synthesis parameters(calcination temperature,calcination time,and the lithium-titanium molar ratio)on adsorption-desorption performance(the delithiation ratio,titanium dissolution loss,and the adsorption capacity)were investigated.The as-prepared LSTIS exhibited an equilibrium adsorption capacity of 30.08 mg·g^(-1)(average of 25.85 mg·g^(-1) over 5 cycles)and ultra-low titanium dissolution loss of less than 0.12%(average of 0.086%over 5 cycles).The LSTIS showed excellent selectivity toward Li^(+) in Na^(+),K^(+),Mg^(2+),and Ca^(2+) coexisting saline solutions where its adsorption capacity reached 27.45 mg·g^(-1) and the separation factors of Li^(+) over the coexisting cations exceeded 100.The data suggests that the LSTIS is promising to competitively enrich Li^(+) from saline solutions.

Preparation of Spherical FePO4 by Chemical Co-precipitation Combined with Spray-Drying

Well-shaped spherical agglomerates of FePO4 particles were prepared by a novel method:chemical co-precipitation combined with spray-drying.Tap density analysis,Brunauer-Emmett-Teller analysis,characterizations of X-ray diffraction,scanning electron microscopy,and transmission electron microscopy confirmed that the micron-sized spherical agglomerates with high specific surface area and high tap density were composed of the uniform nano-sized particles.The effects of pH and reaction time on the morphology of the FePO4 particles were investigated by experimental and theoretical analyses.The analyses revealed that amorphous FePO4 was responsible for forming a well-shaped spherical agglomerate,and the ideal spherical particles were obtained at pH 3.The reaction time also played a significant role in controlling the size and surface morphology of the FePO4 particles,and smooth spherical FePO4 particles were obtained at a reaction time of 6 h.By this novel method,poly-porous spherical iron phosphate particles were prepared,which can be used with high efficiency in some special fields,especially as a precursor for synthesizing LiFePO4 and catalysts.

Microencapsulation of nutmeg essential oil by spray-drying with different wall materials

Nutmeg essential oil with volatile components is sensitive to oxygen, light, water and high temperature. Spray-drying is widely used as an encapsulation technique for improving compound stability during processing and storage. In this study, influence of encapsulated matrix on spray-dried nutmeg essential oil microcapsule was investigated using blends of maltodextrin and either gum Arabic(GA-MD), or octenyl succinic acid modified starch(OSA-MD) as wall materials. Characteristics of spray-dried powders from these 2 wall materials were evaluated and compared. Powder property analysis indicated that GA-MD microcapsules presented larger size, higher moisture and poorer flowability compared with OSA-MD microcapsules. Fourier transforms infrared spectroscopy and thermogravimetric analysis showed that both GA-MD and OSA-MD microcapsules improved the stability of nutmeg essential oil. However, GA-MD microcapsules exhibited higher storage stability than OSA-MD microcapsules. This research provided theoretical foundation for wall material choice of microcapsule and nutmeg essential oil utilization in food industry.

Micro-sized nanoaggregates:Spray-drying-assisted fabrication and applications

The applications of nanoparticles suffer from their extremely small size and intrinsic trend of agglom-eration.Rearranging nanoparticles to form micro-sized nanoaggregates(MNAs)with increased size,ordered structure,as well as controllable size,shape,and morphology is a crucial step in various fields of science and technology to maintain the unique characteristics of nanoparticles while obtaining greatly enhanced or new performance at the microscale.The structure of MNAs prominently affects their functionality,which is determined by the arrangement of nanoparticles and the interaction between primary particles.Several methods have been proposed to prepare the MNAs,in which spray-drying technology stands out considering the feasibility,scalability for industry,cost,and efficiency.Forced assembly of nanoparticles through spray-drying under tunable process parameters yields diverse physical properties and structural arrangements of nanoparticles of the MNAs,they therefore exhibit enormous potential in a wide range of application fields.This review presents the construction and applications of spray-dried MNAs.The factors that influence the size,morphology,and structure of the MNAs are discussed in detail.In addition,the outstanding application performance resulting from the tightly packed nanoparticles in regular-shaped MNAs obtained by the spray-drying process is illustrated.

Oil-in-water nanoemulsions loaded with lycopene extracts encapsulated by spray drying:Formulation,characterization and optimization

Lycopene is very susceptible to degradation once released from the protective chromoplast environment.In this study,oil-in-water(O/W)nanoemulsions coupled with spray drying technology were applied for the encapsulation and stabilization of lycopene extracted from tomato waste.Tomato extract was obtained by ultrasound-assisted extraction.Nanoemulsions were prepared by a high-speed rotor stator using isopropyl myristate as the oil phase and Pluronic F-127 as the emulsifier for the aqueous external phase.The effect of emulsification process parameters was investigated.Spray drying of the produced emulsions was attempted to obtain a stabilized dry powder after the addition of a coating agent.The effect of different coating agents(maltodextrin,inulin,gum arabic,pectin,whey and polyvinylpyrrolidone),drying temperature(120-170℃),and feed flow rate(3-9 ml·min^(-1))on the obtained particles was evaluated.Results revealed that the emulsion formulation of 20/80(O/W)with 1.5%(mass fraction)of Pluronic F-127 as stabilizer in the aqueous phase resulted in a stable nanoemulsion with droplet sizes in the range of 259-276 nm with a unimodal and sharp size distribution.The extract in the nanoemulsion was well protected at room temperature with a degradation rate of lycopene of about 50%during a month of storage time.The most stable emulsions were then processed by spray drying to obtain a dry powder.Spray drying was particularly successful when using maltodextrin as a coating agent,obtaining dried spherical particles with mean diameters of(4.87±0.17)μm with a smooth surface.The possibility of dissolving the spray dried powder in order to repristinate.The original emulsion was also successfully verified.

Preparation and characterization of spray-dried valsartan-loaded Eudragit~? EPO solid dispersion microparticles

The purpose of this study was to develop the immediate release stomach-specific spraydried formulation of valsartan(VAL) using Eudragit?E PO(EPO) as the carrier for enhancing dissolution rate in a gastric environment. Enhanced solubility and dissolution in gastric pH was achieved by formulating the solid dispersion using a spray drying technique. Different combinations of drug–polymer–surfactant were dissolved in 10% ethanol solution and spraydried in order to obtain solid dispersion microparticles. Use of the VAL–EPO solid dispersion microparticles resulted in significant improvement of the dissolution rate of the drug at pH 1.2 and pH 4.0, compared to the free drug powder and the commercial product. A hard gelatin capsule was filled with the VAL–EPO solid dispersion powder prior to the dissolution test.The increased dissolution of VAL from solid dispersion microparticles in gastric pH was attributed to the effect of EPO and most importantly the transformation of crystalline drugs to amorphous solid dispersion powder, which was clearly shown by scanning electron microscopy(SEM), differential scanning calorimetry(DSC), and powder X-ray diffraction(PXRD) studies. Thus, VAL, a potential antihypertensive drug in the form of a solid dispersion microparticulate powder, can be effectively delivered in the immediate release dosage form for stomach-specific drug delivery.

Hierarchical coupling effect in hollow Ni/NiFe2O4-CNTs microsphere via spray-drying for enhanced oxygen evolution electrocatalysis

Design and fabrication of cost-effective transition metal and their oxides-based nanocomposites are of paramount significance for metal-air batteries and water-splitting.However,the traditional optimized designs for nanostructure are complicated,low-efficient and underperform for wide-scale applications.Herein,a novel hierarchical framework of hollow Ni/NiFe2O4-CNTs compositemicrosphere forcibly-assembled by zero-dimensional(OD)Ni/NiFo204 nanoparticle(<16 nm)and one-dimensional(1D)self-supporting CNTs was fabricated successfully.Benefitted from the unique nanostructure,such monohybrids can achieve remarkable oxygen evolution reaction(OER)performance in alkaline media with a low overpotential and superior durability,which exceeds most of the commercial catalysts based on IrO/RuO2 or other non-noble metal nanomaterials.The enhanced OER performance of Ni/NiFe2OA-CNTs composite is mainly ascribed to the increased catalytic activity and the optimized conductivity induced by the effects of strong hierarchical coupling and charge transfers between CNTs and Ni/NiFe204 nanoparticles.These effects are greatly boosted by the polarized heterojunction interfaces confirmed by electron holography.The density functional theory(DFT)calculation indicates the epitaxial Ni further enriches the intrinsic electrons contents of NiFe204 and thus accelerates absorption/desorption kinetics of OER intermediates.This work hereby paves a facile route to construct the hollow composite microsphere with excellent OER electrocatalytic activity based on non-noble metal oxide/CNTs.

The influence of amino acids on aztreonam spray-dried powders for inhalation

The dry powder inhalation of antibiotics for the treatment of lung infections has attracted drastically increasing attention as it offers rapid local therapy at lower doses and minimal side effects.In this study,aztreonam(AZT)was used as the model antibiotic and spraydried to prepare powders for inhalation.Amino acids of glycine(GLY),histidine(HIS)and leucine(LEU)were used as excipients to modify the spray-dried particles.It was demonstrated that the GLY-AZT spray-dried powders formed huge agglomerates with the size of 144.51μm,which made it very difficult to be delivered to the lungs(FPF:0.29%w/w only).In comparison with the AZT spray-dried powders,HIS-modified spray-dried powders showed increased compressibility,indicating larger distance and less cohesion between particles;while the LEU-modified spray-dried particles showed a hollow structure with significantly decreased densities.The fine particle fraction for HIS-and LEU-modified powders was 51.4%w/w and 61.7%w/w,respectively,and both were significantly increased(one-way ANOVA,Duncan’s test,P<0.05)compared to that of AZT spray-dried powders(45.4%w/w),showing a great potential to be applied in clinic.

The effects of surface morphology on the aerosol performance of spray-dried particles within HFA 134a based metered dose formulations

The aim of this study was to produce fine particles with different corrugated degree of surface by spray-drying and to investigate the effect of surface morphology on in vitro aerosol performance of the particles within HFA 134a based metered dose formulations.Compositions of rizatriptan and scutellarin were spray-dried using different spray-drying parameters,and particles were suspended within HFA 134a.The surface morphology were determined using scanning electron microscopy(SEM),while the aerodynamic performance of MDIs was evaluated using a next generation pharmaceutical impactor.The surface morphology of spraydried particles could vary from smooth to moderately corrugated,and to raisin-like depending upon spray-drying parameters and preparation compositions.In general,increasing inlet temperature,decreasing feed concentration and/or adding leucine to the feed solution tended to increase the corrugated degree of particle surface.Deposition results indicated that raisinlike particle based MDIs for all compositions of the two drugs produced significantly better aerodynamic performance in terms of fine particle fractions and mass median aerodynamic diameters relative to the formulations of the corresponding smooth or slightly corrugated particles when the particle compositions were the same.The present results demonstrated that wrinkled particles increased fine particle fractions within surfactant-free MDI formulations.

Isothermal Kinetics Modelling of the Fischer-Tropsch Synthesis over the Spray-Dried Fe-Cu-K Catalyst

The isothermal kinetics of the Fischer-Tropsch synthesis （FTS） over Fe-Cu-K spray-dried catalyst was studied in a spinning basket reactor. The experiments were carried out at a constant temperature of 523 K, n（H2）/n（CO） feed ratios of 0.8 2.0, reactor pressures of 1.1 2.5 MPa, and space velocity of 0.556× 10^-3 Nm^3/kgcat·s. Kinetic model for hydrocarbon formation was derived on the basis of simplified carbide mechanism to reduce the number of parameters. Two individual rate constants for methane and ethene were considered. Furthermore, the model was modified empirically by non-intrinsic effect, such as physisorption and fictitious olefin pressures that were taken into account, and the influences of secondary reaction of α-olefins on product distribution. The simulation results showed that the experimental phenomena of FTS and the deviations from ASF distribution, such as the relatively high yield of methane and low yield of ethene observed experimentally could be depicted basically.

Green Microstructural Visualization of Dry-Pressed Spray-Dried Alumina (Al₂O₃)

Slurry parameters were controlled prior to spray-drying to visualize and govern an understanding of which parameters govern hollow coring and granule morphology during spray-drying. An aqueous alumina using a polyvinyl alcohol binder (PVA) system was analyzed and granules were processed by altering the slurry specific gravity and viscosity value prior to spray-drying. Spray-dried granules were uniaxial dry-pressed at varying moisture contents to show the plasticizing effects of moisture during compaction. A novel characterization method using a field emission electron microscope (FESEM) was implemented to image the green microstructures of the granules and compacted samples. Slurries with a higher specific gravity and viscosity resulted in denser granules with spherical shapes. Viscosity affected the binder segregation during the spray-drying process. Granules stored at higher moisture contents resulted in denser compacts with fewer intergranular pores and cracks along granule boundaries. Using a FESEM resulted in higher resolution for green microstructural characterization.

Preparation of neodymium-doped yttrium aluminum garnet powders and fibers

Using nitrate precursors, a novel spray-drying assisted citrate gel process for the preparation of neodymium-doped yttrium alumi- num garnet （YAG） phase was developed. Synthesis of single-phase polycrystalline YAG was achieved at temperatures as low as 800 ℃ using the spray-drying methodology whilst conventional approaches currently available require 1000 ℃. Initially, a solution was prepared by mixing aluminum and yttrium nitrates, citric acid, etilenglycol and neodymium oxide. This solution was dried by pulverization （spray dryer） to obtain aggregated precursor powders of the compound. These aggregates were calcined at 800, 850 and 900 ℃ to determine the phase evolution from amorphous to crystalline by X-ray diffraction （XRD）. The morphology of aggregates was characterized by scanning electron microscopy （SEM） and transmission electron microscopy （TEM）. Moreover, through XRD it was determined that the crystallization of YAG phase started at about 800 ℃ without any intermediate phases. The powders were composed of spherical aggregates with an average diameter of 1 um. From these powders, ceramic fibers with additions of 2at.% and 5at.% Nd, were extracted from the melt with diameters ranging from 30 um to 50 um.

Chitosan and β-cyclodextrin Microspheres as Pulmonary Sustained Delivery Systems

Chitosan and β-cyclodextrin were used to prepare microspheres with theophylline for pulmonary delivery by spray drying method. The characteristics, mucociliotoxicity, permeation rate and drug release were studied. The drug entrapments of microspheres Ⅰ, Ⅱ and Ⅲ were from 35.70% to 21.09% and 13.33%, while yields and encapsulation efficiencies were higher than 45% and about 90% respectively. The microspheres possessed low tap densities （0.34-0.48 g/cm^3）, appropriate diameters （3.35-3.94 μm） and theoretical aerodynamics diameters （2.20-3.04 μm）. SEM images showed the microspheres were spherical with smooth or wrinkled surface surfaces. FT-IR demonstrated theophylline had formed hydrogen bonds with chitosan and fl-cyclodextrin. The microspheres could effectively reduce the ciliotoxicity and easy to penetrate the memberine. The in vitro release of the microspheres was related to the ratio of drug/polymer and microspheres Ⅱ had a prolong release, providing the release of 72.00% in 12 h. The results suggestes that chitosan/β-cyclodextrin microspheres Ⅱ are a promising carrier as sustained release for pulmonary delivery.

High temperature X-ray diffraction study of the formation of Na_(2)Ti_(3)O_(7) from a mixture of sodium carbonate and titanium oxide

Na2Ti3O7 has attracted much attention in the field of anode materials for Na-ion batteries thanks to its non-toxicity and very low working potential of 0.3 V vs Na0/Na+.Building a clearer picture of its formation from cheap Na_(2)CO_(3) and TiO_(2) starting materials is therefore of obvious interest.Here,we report new insights from an in-situ high temperature X-ray diffraction study conducted from room temperature to 800°C,complemented by ex-situ characterizations.We were thereby able to position the previously reported Na_(4)Ti_(5)O_(12) and Na_(2)Ti_(6)O_(13) intermediate phases in a reaction scheme involving three successive steps and temperature ranges.Shifts and/or broadening of a subset of the Na_(2)Ti_(6)O_(13) reflections suggested a combination of intra-layer disorder with the well-established ordering of successive layers.This in-situ study was carried out on reproducible mixtures of Na_(2)CO_(3) and TiO_(2) in 1:3 molar ratio prepared by spraydrying of mixed aqueous suspensions.Single-phase Na_(2)Ti_(3)O_(7) was obtained after only 8 h at 800°C in air,instead of a minimum of 20 h for a conventional solid-state route using the same precursors.Microstructure analysis revealed~15 mm diameter granules made up from rectangular rods of a fewmm length presenting electrochemical properties in line with expectations.In the absence of grinding or formation of intimate composites with conductive carbon,the specific capacity of 137 m Ah/g at C/5 decreased at higher rates.

Formation and Characterization of Plasma Sprayed Photocatalytic TiO2- ZnO Nano- Compounded Coatings

Two kinds of TiO2-ZnO nano-compounded powders aggregated by spray-drying process and evaporation method were used to deposit photocatalytic coatings by atmospheric plasma spraying technique. The phase compositions, morphologies of the agglomerated TiO2-ZnO powders and the as-sprayed coating were characterized using X-ray diffraction (XRD) and field emission scanning electron microscope (FESEM) respectively. Furthermore, roughness measurements were carried out on their surfaces of the plasma sprayed TiO2-ZnO nano-comPounded coatings. Compared with the TiO2ZnO nano-compounded coating deposited from the spray-dried powder, it was found that the TiO2-ZnO nano-compounded coating deposited from the evaporated powder possesses higher anatase phase. It is ascribed to the existing of partially melted or non-melted microstructure in the TiO2-ZnO coating deposited from the evaporated powder. The partially-meltedor non-melted microstructure was retained from the starting agglomerated powder. This microstructure is beneficial to improve the photocatalytic properties of plasma sprayed TiO2-ZnO nano-compounded coatings.

Controllable assembling of highly-doped linked carbon bubbles on graphene microfolds

Carbon-based microassemblies(CMs) have attracted significant attention in numerous applications due to their unique hierarchical structures and delicate building blocks,especially when hollow carbon spheres(HCSs) are reasonably introduced into the construction.Herein,a new design for novel HCSscombined CMs is proposed.Remarkably,the HCSs are linear carbon bubbles linked one-by-one, arranging into necklaces decorating on the graphene microfolds.Detailed thermal analysis confirm that high temperatures straighten the linked carbon bubbles into bamboo-like carbon nanofibers,evidently due to the attenuation of doping degree.Benefiting from the abundant active sites of carbon bubbles,the obtained CMs exhibit satisfactory electrocatalytic activity for oxygen reduction reactions.This work establishes a bridge to precisely control the synthesis of carbon-based hierarchical architectures.

An advanced low-cost cathode composed of graphene-coated Na_(2.4)Fe_(1.8)(SO_(4))_(3) nanograins in a 3D graphene network for ultra-stable sodium storage

Iron-based electrodes have attracted great attention for sodium storage because of the distinct cost effectiveness.However,exploring suitable iron-based electrodes with high power density and long duration remains a big challenge.Herein,a spray-drying strategy is adopted to construct graphene-coated Na_(2.4)Fe_(1.8)(SO_(4))_(3) nanograins in a 3D graphene microsphere network.The unique structural and compositional advantages endow these electrodes to exhibit outstanding electrochemical properties with remarkable rate performance and long cycle life.Mechanism analyses further explain the outstanding electrochemical properties from the structural aspect.

Influences of Sintering Process of Sprayed Precursors on the Struc-ture and Electrochemical Properties of LiMn_2O_4 Cathode Material

Well-defined spinel LiMn2O4 powders were synthesized via sintering a precursor, which was prepared by spraydrying method. The effects of sintering process on the structure and electrochemical properties of LiMn2O4 were discussed. It was found that a single sintering could not synthesize a pure LiMn2O4 compound, while two-step sintering procedure consisting of decomposing sprayed precursors at 350℃ and further sintering at an elevated temperature leads to the formation of a single-phased LiMn2O4 with homogeneous particle size distribution. As compared to that sintered in air, the two-step sintered LiMn2O4 in oxygen shows tighter structure and more uniform particle size, as well as better electrochemical properties. It delivers an initial discharge capacity of 131 mAh·g^-1 （1/10C）, and still has excellent cycling stability at higher rate （1/5C）.

Drying Technology and Formation Process of Naomai Xingshen Capsules

[Objectives]To optimize the drying technology and formation process of Naomai Xingshen Capsules.[Methods]The yield of paste powder and moisture content as evaluation indicators were taken as indicators,the relative density of feed liquid,inlet air temperature and dosage of excipients were selected as investigation factors,the orthogonal experiment method was used to optimize the spray drying process.The moisture absorption rate and angle of repose were taken as evaluation indicators,the types of forming excipient were screened,and the critical relative humidity was determined.[Results]The optimum spray drying process was that the relative density of liquid medicine was 1.05(60℃),the air inlet temperature was 200℃,and the dosage of excipients was 2%.The effect of using dextrin as a forming excipient was better,and the relative humidity of the production environment should be controlled below 65%.[Conclusions]The optimized process is stable,feasible,scientific and reasonable,and can be used for large-scale industrial production.