Production of composite particles using an innovative continuous dry coating process derived from extrusion

Dry particle coating is used to modify surface properties and monitor the end use properties of powders. These processes are mainly running in batch mode. In certain cases, continuous processes may present interest for specific applications (limitation of investments, stability, versatility…). In this study, the feasibility of dry coating particles by an innovative way derived from the well-known extrusion process was investigated. Adhesion between host and guest particles is induced by mechanical shear stress during processing. A preliminary parametric study on microcrystalline cellulose particles as host particles was carried out in order to determine the operating condition range. Then, coating was successfully performed using talc and a microcrystalline cellulose system, which demonstrates the feasibility of this novel process and led to different morphologies according to the operating conditions.     

Development and characterization of coated-microparticles based on whey protein/alginate using the Encapsulator device

The aim of this study is to prepare whey protein (WP)-based microparticles (MP) using the Encapsulator^® device. The viscosity dependence of the extrusion device required to mix WP with a food-grade and less viscous polymer. Mixed WP/ALG MP were obtained with the optimized WP/alginate (ALG) ratio (62/38). These particles were further coated with WP or ALG using non-traumatic and solvent-free coating process developed in this study. Size and morphology of coated and uncoated MP were determined. Then, swelling and degradation (WP release) of formulations were investigated in pH 1.2 and 7.5 buffers and in simulated gastric and intestinal fluids (SGF, SIF) and compared to pure ALG and pure WP particle behaviours. At pH 1.2, pure ALG shrank and pure WP swelled, whereas the sizes of mixed WP/ALG matrix were stable. In SGF, WP/ALG MP resisted to pepsin degradation compare to pure WP particles due to ALG shrinkage which limited pepsin diffusion within particles. Coating addition with WP or ALG slowed down pepsin degradation. At pH 7.5, WP/ALG particles were rapidly degraded due to ALG sensitivity but the addition of a WP coating limited effectively the swelling and the degradation of MP. In SIF, pancreatin accelerated MP degradation but ALG-coated MP exhibited interesting robustness. These results confirmed the interest and the feasibility to produce coated WP-based MP which could be a potential orally controlled release drug delivery system.     

Solution-Based Particle Formation of Pharmaceutical Powders by Supercritical or Compressed Fluid Co2 and Cryogenic Spray-Freezing Technologies

Micronization is an important procedure used in the pharmaceutical industry to reduce the particle size of active pharmaceutical ingredients (APIs). The spray-drying and milling techniques presently used to micronize drug substances cannot be used to process thermolabile or physically unstable drug substances. Therefore, new micronization techniques, including particle precipitation with supercritical or compressed fluid CO₂ and spray-freezing of drug solutions and suspensions into cryogenic gas to produce solid frozen microparticles, are currently being perfected for future use in the pharmaceutical industry. This review highlights the compressed gas and cryogenic liquid technologies being developed as potential solution-based particle formation technologies for drugs that cannot be processed by conventional micronization techniques.     

Solution-Based Particle Formation of Pharmaceutical Powders by Supercritical or Compressed Fluid Co2 and Cryogenic Spray-Freezing Technologies

Micronization is an important procedure used in the pharmaceutical industry to reduce the particle size of active pharmaceutical ingredients (APIs). The spray-drying and milling techniques presently used to micronize drug substances cannot be used to process thermolabile or physically unstable drug substances. Therefore, new micronization techniques, including particle precipitation with supercritical or compressed fluid CO₂ and spray-freezing of drug solutions and suspensions into cryogenic gas to produce solid frozen microparticles, are currently being perfected for future use in the pharmaceutical industry. This review highlights the compressed gas and cryogenic liquid technologies being developed as potential solution-based particle formation technologies for drugs that cannot be processed by conventional micronization techniques.     

核壳结构型纳米CaCO3-SiO2.nH2O复合粒子的制备

在搅拌槽式反应器中,以用超重力法合成的纳米 ＣａＣＯ３和 Ｎａ２ＳｉＯ３为原料,用溶胶－凝胶技术制备具有核壳结构的纳米 ＣａＣＯ３－ＳｉＯ２·ｎＨ２Ｏ复合粒子　用 ＸＰＳ、 ＴＥＭ、 ＸＲＤ等方法对粒子的化学组成、形貌、晶型等作了分析和表征     

Growth kinetics in particle coating by top-spray fluidized bed systems

The kinetics of growth for the coating of particles in top- spraying fluidized bed systems is reported. The results indicated that only a small amount of particles that visited the spraying region are coated at a time. It was also revealed that different particle sizes are not equally coated during the process. In a polydispersed particle distribution, smaller particles were found to receive more coating than their larger counterparts. This preferential coating, which was associated with a rapid decrease in the distribution variance, is more pronounced in the earlier parts of the process. When a narrower seed distribution was used, the preferential coating was reduced. A segregation factor, f_s, was introduced in the development of a growth kinetics model to represent the chance of each particle size visiting the coating region. The result for the distribution from the model clearly resembled the results obtained experimentally. For the top-spraying process, the segregation factor was found to be an exponentially decaying function of particle weight. For lactose particles coated with hydroxypropyl methyl cellulose, two different rates of growth were observed during the coating process.     

Mathematical modeling of coating time in dry particulate coating using mild vibration field with bead media described by DEM simulation

To theoretically understand the previously reported dry particulate coating process using a mild vibration field with a bead media, a mathematical analysis model of the dry coating system was developed. In this coating process, an ordered mixture with coarse host particles (drug-loaded ion exchange resin, diameter approximately 100 µm) and fine guest particles (acrylic polymer particle, primary particle size of approximately 100 nm) is formed using a vibrating a vessel. Second, the guest particles on the host particulate surface are firmly fixed using the collision of coated particles zirconia beads (diameter 1.5 mm). Our model assumes that the unfixed guest particles are fixed by particle-to-particle collisions (C_c) provided by the apparatus, thereby increasing the coating ratio. C_c was estimated using the discrete element method and some experimental results. The model includes parameters such as the number of C_c, host particles and unfixed guest particles. The coating time simulated by the established model equation in this study fits well with the experimental results of the dry process. It depends on the ratio of the number of collisions contributing to the increased coating ratio to the number of unfixed guest particles on the surface of host particles.     

Feasibility of TEOS coated CoFe2O4 nanoparticles to a GMR biosensor agent for single molecular detection

Magnetic properties of 200 nm ferrimagnetic CoFe2O4 nanoparticles before and after coating with TEOS were explored and compared to soft ferrimagnetic MgFe2O4 nanoparticles (200 nm) to evaluate the feasibility as an in-vitro GMR SV (giant magnetoresistance spin-valve) biosensor agent for single molecular detection (SMD). It was found that the magnetic degradation (or variation) of TEOS coated CoFe2O4 and MgFe2O4 nanoparticles are dominantly affected by the chemical dispersion process, which is carried out in the oleic acid (OA), oleylamine (OL), or OA+OL surfactant, before starting major coating process. In addition, the TEOS coating thickness controlled by TEOS concentration and pH level in the buffer solution prominently influenced on the magnetic degradation of TEOS coated nanoparticles. According to the experimental analysis results, the magnetic degradation of TEOS coated nanoparticles is mainly attributed to the variation of particle dipole interaction caused by the degree of particle aggregation depending on TEOS coating process conditions. The TEOS coated CoFe2O4 nanoparticles exhibited a higher magnetic stability for a GMR biosensor agent, e.g., small variation of remnant magnetization, saturation magnetization and magnetic coercivity, than that of MgFe2O4 nanoparticles at the different coating process conditions. The physical and chemical analysis confirmed that this is primarily due to its higher magnetic anisotropy. The experimentally verified high biocompatibility as well as the stably maintained magnetic properties of TEOS coated CoFe2O4 nanoparticles demonstrate that CoFe2O4 nanoparticles can be considered as one of the promising ferrimagnetic nanoparticle sensor agent for an SMD GMR SV biosensor.     

降低超细高氯酸铵感度的方法研究

为了降低超细高氯酸铵(AP)的机械感度,以十八烷胺为包覆剂,经气流粉碎工艺,制备了超细AP包覆粒子。通过对超细AP包覆粒子进行粒度分析、SEM分析、DSC分析及感度检测,研究了超细AP包覆粒子的包覆效果、热分解特性及感度特性。试验结果表明:超细AP包覆粒子,粒度为D50=5.8μm,表面有包覆层存在;超细AP包覆粒子的感度,与超细AP样品相比,当包覆剂质量分数为1%时,撞击感度降低31.2%,摩擦感度降低12.0%;当包覆剂质量分数为3%时,撞击感度降低34.5%,摩擦感度降低22.0%,且包覆剂用量越大,撞击感度和摩擦感度越低;但包覆剂对AP的热分解会产生一定的负面影响,质量分数应≤1%。     

Biopolymer composites of wheat gluten with silica and alumina

Two composite systems were explored to assess the effect of particle dispersion on the properties of filled wheat gluten composites. Nanosilica particles and micro-alumina particles were combined with several silane coupling agents by various methods to perform a broad brush survey of chemical and physical interactions. Thermo-gravimetric analysis (TGA) was used to assess surface coverage on coated particles. Electron microscopy (scanning and transmission) techniques were used to assess particle dispersion and surface interactions. Producing the silica particles in the wheat gluten matrix led to better physical properties, as measured by 3-point bending, than producing the silica particles first, and then mixing them into the wheat gluten. Similarly, coating the alumina particles with silane coupling agents in the wheat gluten matrix led to better mechanical properties than first coating the alumina with silane and then mixing the coated particles into the wheat gluten.     

超临界撞击流技术制备微胶囊工艺

将超临界流体与撞击流技术相结合,提出了一项新的包覆技术—超临界撞击流技术(SFIT)。以石蜡和玻璃微珠分别作为包覆模型材料的壁材和芯材,考察该技术的可行性和有效性;研究混合器内压力、温度、撞击釜内撞击距离以及膨胀前温度等因素对于微胶囊的表观包覆率和表观形态的影响。结果表明,在混合器内压力20MPa以上、温度75℃,且撞击距离70mm,膨胀前温度140℃时,得到的微胶囊团聚小,包覆均匀且效果较好。实验采用电子扫描电镜、激光粒度分布仪和差式扫描量热仪等检测方法从微胶囊的表观包覆率、粒径分布范围、表面形态等角度进行评价。从结果来看,超临界流体与撞击流技术相结合可以实现微胶囊的包覆且效果良好。     

Effects of discharging vibration conditions and coating structures on improving discharge particle flowability in a smaller particle admixing system

Particle flowability can be improved by admixing particles smaller than the original particles (main particles). However, the effects of coating structures on the improvement of flowability are not yet fully understood. In this study, we focused on vibrating discharge particle flowability and investigated the effect of discharging vibration conditions and coating structures on improving the flowability. Main and admixed particles of 60.8 μm and 8 nm in diameter, respectively, were mixed in various mass ratios, and the discharge particle flow rates of the mixed particles were measured. Scanning electron microscopy and scanning probe microscopy images were used to analyze the coverage diameter, surface coverage ratio, and coverage height of the admixed particles on the main particle surfaces. As a result, the admixing mass ratio that gave maximum flowability was found to depend on the maximum value of the vibration acceleration. This could be explained by the relationship between the coating structures of admixed particles and the coated average surface distances due to the vibration acceleration.     

Construction and characterization of a sputter deposition system for coating granular materials

In many modern ceramic or metal matrix composites the interface between the matrix and the reinforcements (particles or fibres) plays an important role. Either no or only weak mechanical bonding is observed or severe reactions between the matrix and the filler during the manufacturing process take place. A method to promote adhesion or to avoid severe reactions is to use coated reinforcements. A uniform film can act as an adhesion promoter, a compliant layer, a reaction inhibitor or a promoter of thermal transport across the interface.The aim of this work was to construct a particle coating system based on magnetron sputter deposition which allows to keep the particles or the granular material in motion during the deposition process to guarantee a homogenous coating on every single particle. As particles to be coated diamond granulates and carbon fibres were investigated. For transparent diamond particles the uniformity of a metallic coating could be evaluated by transmission optical methods and was found to be quite high. Carbon fibres, on the other hand, could only partially be coated due to agglomeration and shadowing effects. The system presented here can be considered as suitable for coating spherical or close to spherical granular matter.     

温度稳定型Ph(Ni_(1/3)Nb_(2/3))O_3基复相陶瓷的制备及介电性能

选取居里温度不同的两组元，对其中一组元包覆ＰＴ，再与另一组元混合烧结，制备出满足Ｘ７Ｒ 温度稳定特性的复相陶瓷．用ＴＥＭ观察了ＰＴ包覆前后粉末的颗粒形态，结果表明，ＰＴ较好地附着 在颗粒表面ＰＴ包覆层的存在抑制了两相的固溶反应，使材料保持复相结构，改善了材料的介电温度特 性分析了 ＰＴ包覆层的作用     

不同形貌碳酸钙颜料粒子的制备及在喷墨印刷中的应用

目的研究碳酸钙颜料粒子的形貌对喷墨打印涂层性能的影响。方法通过改变分散剂的种类制备不同的碳酸钙颜料粒子,并通过扫描电子显微镜(SEM)、傅里叶变换红外光谱仪(FT-IR)、粒径分析仪对制备的颜料粒子进行表征,研究分散剂种类对颜料形貌和粒径的影响。将4种不同形貌的碳酸钙分别作为颜料,将其应用于喷墨打印纸的表面涂层,并测试涂布纸张的动态渗透性、物理性能、喷墨打印性能。结果 CMC作为分散剂有助于形成粒径分布均匀的球形碳酸钙颜料粒子;纺锤形碳酸钙颜料粒子有助于提高涂布纸的平滑度和光泽度;球状体碳酸钙颜料粒子有助于改善涂布纸的喷墨印刷性能和渗透性;颜料粒子的粒径分布均匀性对涂布纸的动态渗透性影响较大,其影响超过颜料粒子形貌对涂布纸渗透性的影响。结论粒径分布均匀的球状体碳酸钙颜料粒子最适合用于喷墨印刷涂层,可以提高纸张的物理性能、印刷性能和动态渗透性能。     

葡聚糖包覆纳米Fe3O4颗粒的研究

采用化学共沉淀法制备了葡聚糖包覆的纳米Fe3O4颗粒,平均粒径为6nm,包覆层厚度约为3～5nm,纳米Fe3O4粒径分布较窄.红外光谱分析可知,葡聚糖与纳米Fe3O4主要以氢键结合,结合Zeta电位和热重分析,分散作用主要是空间位阻作用,葡聚糖的包覆量约为10%.吸光度测试表明,随着葡聚糖用量的增加,悬浮液的稳定性提高.用量为25%时,悬浮液在室温下静止1周,无分层现象.包覆样的饱和磁化强度为60emu/g,具有良好的超顺磁性.     

Preparation of electrically conductive fibres by new surface coating method

Abstract

In the present research, a new surface coating method (dissolving-coating method) that is on the basis of dissolution mechanism was designed. Substantially transparent antimony doped tin oxide (ATO) particles were used instead of carbon black as conductive particles. ATO coated polyester (PET) fibres and ATO coated polycaprolactam (PA6) fibres were prepared by the traditional coating method and the dissolving–coating method respectively. The electrical conductivity, mechanical property and launderability of the coated fibres were discussed. For the characterisation, a laser particle size distribution analyser was used to analyse the size distribution of ATO. Scanning electron microscopy (SEM) and transmittance electron microscopy (TEM) were used for the observation of ATO particles and fibre surface. Electron probe was carried out to make an elemental analysis of the fibre.     

Characterization and antibacterial properties of nanoboron powders and nanoboron powder coated textiles

The antibacterial properties of boron-containing compounds are well known although there are limited studies available on the pure boron nanoparticles. In this paper, nanoboron particles are characterized in terms of their particle size, shape, stability and surface charge before and after their application onto textile surfaces to study their impact on bacterial activity. It was observed that the boron nanoparticles are effective in limiting the bacterial growth of both Gram-negative and positive species without requiring any stimulation to initiate the antibacterial action. In addition to the antibacterial functionality evaluation of the free boron nanoparticles, nanoboron coated textiles were also characterized and determined to change the wettability and surface charge of the textiles with a variable antimicrobial response to the different species. Consequently, we propose pure nanoboron as a new anti-bacterial agent that can function without external stimulation.     

Synthesis of anode active material particles for lithium-ion batteries by surface modification via chemical vapor deposition and their electrochemical characteristics

The high capacity and optimal cycle characteristics of silicon render it essential in lithium-ion batteries. We have attempted to realize a composite material by coating individual silicon (Si) particles of μm-order diameter with a silicon oxide film to serve as an active material in the anode of a lithium-ion battery and thus improve its charge-discharge characteristics. The particles were coated using an inductively coupled plasma-chemical vapor deposition (ICP-CVD) process that realized a homogeneously coated silicon oxide film on each Si particle. The film was synthesized using tetraethyl orthosilicate (TEOS) with hydrogen (H₂) gas used as a reducing agent to deoxidize the silicon dioxide. This enabled the control of the silicon oxidation number in the layers produced by adjusting the H₂ flow during the silicon oxide deposition by ICP-CVD. The silicon oxide covering the Si particles included both silicon monoxide and suboxide, which served to improve the charge-discharge characteristics. We succeeded in realizing an active material using Si, which is abundant in nature, for the anode of a lithium-ion battery with highly charged, improved cycle properties.     

A New Approach to Assess Gold Nanoparticle Uptake by Mammalian Cells: Combining Optical Dark‐Field and Transmission Electron Microscopy

Toxicological effects of nanoparticles are associated with their internalization into cells. Hence, there is a strong need for techniques revealing the interaction between particles and cells as well as quantifying the uptake at the same time. For that reason, herein optical dark‐field microscopy is used in conjunction with transmission electron microscopy to investigate the uptake of gold nanoparticles into epithelial cells with respect to shape, stabilizing agent, and surface charge. The number of internalized particles is strongly dependent on the stabilizing agent, but not on the particle shape. A test of metabolic activity shows no direct correlation with the number of internalized particles. Therefore, particle properties besides coating and shape are suspected to contribute to the observed toxicity.