Nanofibre fabrication in a temperature and humidity controlled environment for improved fibre consistency

Fabricating nanofibres with reproducible characteristics is an important demand in the membrane industry in order to establish commercial viability. In this study, the effect of controlled atmospheric conditions on electrospun cellulose acetate (CA) nanofibres was evaluated for temperatures ranging 17.5–32.5 °C and relative humidity ranging 20–70%. CA solution (0.2 g/mL) in a solvent mixture of acetone/dimethylformamide/ethanol (2:2:1) was electrospun into nonwoven fibre mesh with the fibre diameter ranging from 150 nm to 1 μm. The resulting nanofibres were analysed by differential scanning calorimetry, showing a correlation of reducing melt enthalpy with increasing atmospheric temperature. The opposite was seen with increasing atmospheric humidity, which conferred increasing melt enthalpy. Analysis of scanning electron microscopy images provided a correlation of reducing average fibre diameter with increasing atmospheric temperature and increasing fibre diameter with increasing atmospheric humidity. These results correlate with the melt enthalpy results, suggesting that finer CA nanofibres infer a lower melt enthalpy. Together these studies provide strong evidence that the controlled atmospheric conditions affect the fibre diameter of the resulting electrospun nanofibres. A salient observation in this study was that increased humidity reduced the effect of fibre beading yielding a more consistent and therefore better quality of fibre. This has apparent implications for the reproducibility of nanofibre production and offers a new method of controlling fibre morphology. This study has highlighted the requirement to control atmospheric conditions during the electrospinning process to fabricate reproducible fibre mats.     

Effect of the relative humidity on the fibre morphology of polyamide 4.6 and polyamide 6.9 nanofibres

To obtain uniform and reproducible nanofibres, it is important to understand the effect of the different electrospinning parameters on the nanofibre morphology. Even though a lot of literature is available on the electrospinning of nanofibres, only minor research has been performed on the effect of the relative humidity (RH). This paper investigates the influence of this parameter on the electrospinning process and fibre morphology of the hydrophilic polyamide 4.6 and the less hydrophilic polyamide 6.9. First, the electrospinning process and deposition area of the nanofibres is examined at 10, 50 and 70 % RH. Subsequently, the effect of the polyamide concentration and solvent ratio on the fibre morphology is investigated using scanning electron microscopy and differential scanning calorimetry. It was found that the nanofibre diameter decreased with increasing RH. This resulted in less stable crystals for polyamide 4.6 while electrospinning of polyamide 6.9 at higher RH led to slightly more stable crystals. In conclusion, the water affinity of a polymer is an important factor in predicting the nanofibre morphology at different humidities.     

Fabrication and in vitro biomineralization of bioactive glass (BG) nanofibres

Bioactive glass nanofibres have excellent bioactivity and cell compatibility, and are regarded as a promising next-generation biomaterial in the bone-regeneration field. This paper is concentrated on the effect of electrospinning parameters on the diameter and morphology of bioactive glass nanofibres, and the process of in vitro biomineralization. In this work, sol-gel glass nanofibres with high bioactivity were prepared by electrospinning processing in the presence of poly(vinyl pyrrolidone) (PVP) and pluronic P123 (EO(20)-PO(70)-EO(20)) as chain entanglements. The influence of the polymer concentration, types of polymer and electric field strength on the fibre diameter was examined. The average diameter of these BG nanofibres could be controlled in the range from 85 to 400?nm. The addition of PVP resulted in sufficient chain entanglement and the formation of smooth BG nanofibres, and the addition of P123 led to a further decrease of the diameter with appropriate electric field strength, which held the balance between the electrostatic repulsive force and surface tension of the electrospinning solution. Furthermore, the early stage of in vitro biomineralization of the BG nanofibres in the simulated body fluid (SBF) was studied in this work. The behaviour of in vitro biomineralization of bioactive glass nanofibres was different to the conventional ones, and the structure of bioactive glasses contributed to the formation process of hydroxyapatite.     

Electro-active nanofibres electrospun from blends of poly-vinyl cinnamate and a cholesteric liquid crystalline silicone polymer

Electrospinning was used to generate polymer nanofibres from blends of poly-vinyl cinnamate (PVCN) and a cholesteric silicone polymer. Only blends that contained at least 40 % of PVCN produced fibres. Both differential scanning calorimetry and electron dispersion spectroscopy data indicate that the samples are miscible over a wide temperature interval. The variation of fibre diameter with concentration is nonlinear with a well-defined minimum corresponding to an 80 % PVCN blend. The fibres are birefringent with Kerr constants similar to that of cholesteric liquid crystals. Although not significant, the Kerr constant increases with increasing silicone polymer concentration.     

The effect of relative humidity and evaporation rate on electrospinning: fiber diameter and measurement for control implications

This paper presents an experimental study of the influence that relative humidity and evaporation rate have on the electrospinning process in terms of fiber diameter, process measurements, and selection of operating regime (applied voltage and flow rate) for polyethylene oxide/water (aqueous) solutions and poly(vinylpyrrolidone)/alcohol (non-aqueous) solutions. Poly(vinylpyrrolidone) alcohol solutions are studied to understand the separate influence of relative humidity and evaporation rate. Correlations are developed that relate measurable process parameters (jet diameter, charge density) as well as relative humidity and evaporation rate to fiber diameter. In addition, the influence that relative humidity has on selection of operating regime to achieve desired fiber diameter and maximum production rate is presented.     

醋酸羟丙基甲基纤维素琥珀酸酯溶液的高压静电场纺丝

研究了醋酸羟丙基甲基纤维素琥珀酸酯(HPMCAS)溶液高压静电场纺丝过程中高聚物分子量、溶液浓度、静电场强度对成纤性和纤维直径的影响,制备出直径范围为0.43μm～1.0μm的纤维。当溶剂、溶液浓度及静电场强度一定时,重均分子量-Mw分别为2.6万、4.8万和7.2万,HPMCAS溶液中只有7.2万者能纺丝得到光滑纤维。在静电场强度、溶剂组成一定条件下,HPMCAS可纺丝浓度范围为8%～15%(质量分数,下同),且随着纺丝溶液浓度的增大,所得纤维的平均直径逐渐增大。当其它条件保持一定时,随着纺丝电压的增大,所得纤维的平均直径呈下降的趋势,所得纤维结晶度略微增大。     

Experimental Investigation on Flash Evaporation of Saltwater Droplets Released into Vacuum

In this paper, the flash evaporation process of saltwater droplets released into vacuum is experimentally investigated. During the experiment, a saltwater (NaCl) droplet was suspended on a thermocouple junction, which was used to measure the temperature evolution. The droplet surface temperature was captured by an infrared thermal imager, and the shape variation was recorded by a high speed camera. According to the experimental results, the component and solution concentration has great influence on the evaporation process. With a rise of salt concentration in water, the evaporation rate decreases. The shape of temperature transition curve also depends on the salt concentration in solution, no matter whether it is higher or lower than the eutectic point (22.4%). The effects of environmental pressure, initial droplet temperature and initial droplet diameter on the temperature transition of droplets were also summarized based on the experimental data.     

Influence of the liquid layer thickness on the growth of droplets controlled by the thermal action of laser radiation

We have studied the growth of droplets in a thin layer of aqueous ethanol solution under conditions of the solutocapillary convective flow controlled by a laser beam. It is established that, with increasing layer thickness, the time necessary for the formation of a droplet separated from the layer increases, while the time required for the droplet to reach its maximum possible diameter (determined by the criteria of stability) decreases. In the initial stage of droplet formation, the diameter exhibits some decrease related to a short-term increase in the solvent evaporation rate.     

Effect of Surface Evaporation on Steady Thermocapillary Convection in an Annular Pool

In order to understand the effect of surface evaporation on thermocapillary convection in an annular pool, a series of numerical simulation on thermocapillary convection of the fluids with Prandtl number from 0.01 to 50 in the pure vapor environment were carried out. The results show that thermocapillary convection is always coupled with the evaporation process on the free surface. With the increase of evaporation Biot number, the surface temperature decreases, and the evaporation mass flux near the hot wall increases obviously. However, near the cold wall, the evaporation mass flux increases first, and then decreases. When Marangoni number is small, the total evaporation mass rate at free surface increases with the increase of evaporation Biot number; when Marangoni number is larger, it increases first and then approaches a constant value. The aspect ratio of the annular pool has a positive influence on the thermocapillary convection strength and the total evaporation mass rate. With the increase of Prandtl number, the surface temperature rises gradually and the evaporative mass flux increases, and the thermocapillary convection cell moves gradually toward the outer wall and the free surface. This effect decreases with the increase of evaporation Biot number When evaporation Biot number is smaller, the total evaporation mass rate increases with the Prandtl number; when Biot number is larger, Prandtl number has little impact on the total evaporation mass rate.     

反应器长径比对化学气相沉积SiC沉积动力学的影响

以三氯甲基硅烷(MTS)和H2为前驱体,在沉积温度900～1 050℃,H2和MTS摩尔比为4～20和滞留时间0.4～1 s下,采用化学气相沉积(CVD)工艺研究沉积反应器长径比分别为7∶6和7∶2时的碳化硅(SiC)沉积动力学.结果 发现,不同尺寸反应器中SiC沉积速率随工艺参数变化的规律性差异明显.长径比7∶6的反...     

Structure and properties of electrospun PLLA single nanofibres

An electrospinning method was used to spin semi-crystalline poly(L-lactide) (PLLA) nanofibres. Processing parameter effects on the internal molecular structure of electrospun PLLA fibres were investigated by x-ray diffraction (XRD) and differential scanning calorimetry (DSC). Take-up velocity was found as a dominant parameter to induce a highly ordered molecular structure in the electrospun PLLA fibres compared to solution conductivity and polymer concentration, although these two parameters played an important role in controlling the fibre diameter. A collecting method of a single nanofibre by an electrospinning process was developed for the tensile tests to investigate structure-property relationships of the polymer nanofibres. The tensile test results indicated that higher take-up velocity caused higher tensile modulus and strength due to the ordered structure developed through the process.     

Electrospun polyimide/titanium dioxide composite nanofibrous membrane by electrospinning and electrospraying

Fibrous membrane with a fibre diameter of 229 +/- 35 nm was fabricated from polyimide solution by electrospinning. Nanofibrous membrane with a fibre diameter of 251 +/- 37 nm was fabricated by combined electrospinning and electrospraying for polyimide/TiO2. Among the different solvents studied, ethanol was the effective solvent for dispersing the TiO2 nanoparticles in the nanofibrous matrix during electrospraying. The average pore size of polyimide membrane was obtained in the range 0.79-0.89 microm whereas the average pore size of polyimide/TiO2 membrane was found to be in the range 1.23 microm. The tensile stress of polyimide nanofibrous membrane and also polyimide/TiO2 composite fibrous membrane determined to be 0.36 MPa and 0.65 MPa respectively. Nanofibrous membrane containing TiO2 nanoparticles on the surface of the polyimide nanofibres improved the mechanical stability of the membrane.     

溶液静电纺丝制备热塑性聚酰亚胺超细纤维无纺布

为实现热塑性聚酰亚胺(LPI)无纺布的宏量制备奠定基础,以N-N-二甲基乙酰胺(DMAc)为溶剂,采用静电纺丝技术成功制备了平均直径范围为0.36~1.47μm的LPI超细纤维,系统探讨了纺丝液浓度、流速以及纺丝电压等工艺条件对LPI纤维形貌和直径的影响。结果表明:随着浓度从22%(质量分数,下同)增加到30%,LPI纤维的平均直径显著增大,同时直径分布逐渐变宽,并且在纺丝溶液浓度较低时,有纺锤状纤维存在,随着溶液浓度上升,纺锤状纤维消失,随浓度继续上升,纤维开始产生粘连。纺丝电压的改变对纤维的形貌和平均直径变化不显著;随着流速增加,纤维平均直径随之增大,当流速大于1.5mL/h时,开始出现纤维粘连,大于1.8mL/h时,出现纺锤状纤维。通过优化工艺条件,在LPI浓度28%,电压15kV,流速1.2mL/h,温度30℃,接收距离25cm条件下,制备了平均直径为1.18μm的纤维。     

Influence of Aging on the Physical-Mechanical Properties of Acrylic Resin Films Cast from Aqueous Dispersions and Organic Solutions

The physical-mechanical properties of the enteric copolymers, poly(methacrylic acid, ethyl acrylate) Eudragit® L100-55, and Eudragit® L30D have been investigated. Free films of the copolymer containing varying levels of glyceryl triacetate (triacetin) and citrate ester (Citroflex®) plasticizers were prepared by both aqueous and solvent casting techniques. Conditioned films were stored at different humidities and temperatures for predetermined time periods prior to testing. Free films with plasticizer concentration ranging from 0 to 30% by weight of the polymer demonstrated that physical aging at room temperature resulted in physical-mechanical changes as the stress-strain curves indicated a decrease in the percent elongation with increases in the tensile strength. Films prepared from the aqueous latex approached a constant state of equilibrium at a faster rate than films prepared from isopropyl alcohol, where the mechanical properties approach a relatively constant value. Free films containing varying amounts of the plasticizer, triethyl citrate, were stored under different humidity and temperature conditions. In addition, a headspace-gas chromatography (HSGC) method was developed to correlate solvent residues with mechanical properties. The results indicated that an increase in temperature and humidity accelerated the rate of solvent evaporation as a function of time. High vacuum and low humidity conditions were demonstrated to be ineffective conditions for solvent removal. Solvent residues were found in all films after 48 hours of exposure to temperatures up to 60°C and/or exposure to relatively high humidity conditions. A direct relationship between plasticizer content and rate of solvent evaporation from the film was established. Higher concentrations of the plasticizer were found to augment the evaporation of the solvents. This enhanced evaporation was due to the stronger molecular interaction forces between the polymer and the plasticizer than between the polymer and the solvent.     

3003铝合金动态再结晶实验研究

采用Gleeble-1500热模拟试验机对3003铝合金进行变形温度为300～500℃、应变速率为0.01～10.0s-1的高温等温压缩实验,由真应力-真应变曲线计算应变硬化速率,并采用截线法测量热压缩后平均晶粒尺寸,结果表明:3003铝合金动态再结晶临界应变εc随着Z参数的增大而提高,合金发生动态再结晶的临界条件为:...     

溶剂蒸发法制备油核/聚合物壳微胶囊

通过溶剂蒸发法制备了十六烷/聚甲基丙烯酸甲酯核/壳结构微胶囊。SEM和光学显微镜照片显示,微胶囊呈球形,囊壁透明,表面光滑。系统研究表明,在相同条件下,随着PMMA用量的增加,微胶囊粒径增大,粒径分布变宽;随着搅拌速度的增加或/和稳定剂PVA量的增大,微胶囊的粒径减小,粒径分布变窄。     

液滴干燥过程的模拟研究

为更直观地体现液滴蒸发历程,详细分析液滴内部溶剂浓度与液滴比热、液滴表面饱和蒸气压、溶剂扩散系数之间的耦合关系,建立同时考虑液滴内部温度梯度变化及浓度梯度变化的单液滴蒸发模型,并基于网格重构技术解决液滴蒸发过程中的动边界问题,分别以纯水滴和硫酸钠溶液液滴蒸发为例,模拟分析不同操作工况下,液滴滴径、液滴内部温度梯度及溶质浓度梯度的瞬态变化。结果表明:数值模拟的结果与实验结果基本吻合。     

声场强化溶液蒸发的效果及机理

声场效应对溶液蒸发过程实验表明,声场促进溶液的蒸发,不同的声场作用参数和不同的温度,影响效果不同,溶液蒸发效率提高2％-6％,平均效率提高达4％以上。对水．乙醇以及苯．乙醇二组分溶液的超声蒸发动力学过程进行了分析,表明蒸发速率随时间的关系表现出线性的关系,两组分之间的体积百分比越接近,蒸发速率随时间越容易表现出线性的变化关系。通过液气两相平衡、成核和挥发等过程的分析．认为声场强化溶液蒸发的作用机理是声场具有“空化效应”。声场降低溶液的表面张力,从而降低了成核势垒．促进了液体内部的能量交换。增加了汽化成核几率,使溶液蒸发过程得以强化。     

Polyamide 6.9 nanofibres electrospun under steady state conditions from a solvent/non-solvent solution

Nanofibres can be processed into several high-end applications due to their unique characteristics, especially when based on a diversity of polymers with specific properties. This, however, requires that the nanofibrous structures are produced in a highly reproducible way. The article gives focus to polyamide (PA) 6.9, a less exploited PA though with interesting properties such as a very low moisture absorption. To trace and understand the dominant parameters that allow for the aimed reproducible characteristics, the influence of the solution parameters on the steady state behaviour during electrospinning as well as the resultant fibre morphology is followed by scanning electron microscopy and differential scanning calorimetry. Results show a significant effect of the amount of non-solvent acetic acid, added to the solvent formic acid, on the steady state behaviour and the fibre morphology. The non-solvent acetic acid broadens the steady state window by making the electrospin solutions more suitable to obtain uniform and reproducible nanofibrous structures with a narrow nanofibre diameter distribution. The mixture of the solvent formic acid and the non-solvent acetic acid strongly contributes to the future potentials of PA 6.9 nanofibres, with its leading to a smaller fibre distribution and moreover highly reproducible in time.