Undercooling and crystallization behaviour of antimony droplets

The level of liquid undercooling below the equilibrium melting point experienced typically in a bulk material is limited by the presence of potent heterogeneous nucleation sites. By subdividing the material into a collection of fine (10 to 150m) droplets the most potent nucleants are isolated into a small fraction of the droplet population, allowing the remainder to reach deep levels of undercooling prior to the onset of solidification. Droplet surface coating characteristics influence both the level and uniformity of the undercooling and, in addition, may alter the nucleation kinetics thereby encouraging the formation of a metastable crystalline phase from the undercooled liquid. An effective means of both creating a stable dispersion of fine droplets and influencing the surface coating is through the droplet emulsion technique. This approach has allowed the level of undercooling for pure antimony to be extended from 0.08 to 0.237T _m through proper control of droplet size, surface coating and applied cooling rate. The formation of a metastable simple cubic phase from the melt has been confirmed using both differential thermal analysis and X-ray diffraction techniques. The simple cubic phase is retained in droplets to temperatures approaching the melting point at a heating rate of 20° C min^–1. Drop tube treatment of emulsified samples has also been successful at producing the metastable simple cubic structure by containerless processing.     

Formation of drug-loaded nanoemulsions in stirred media mills

The feasibility of stirred media mills for the production of nanoemulsions loaded with active pharmaceutical ingredients (API) using plant oils as disperse phase and different types of the non-ionic emulsifier polysorbate is demonstrated. The influence of the emulsion formulation, namely oil type, surfactant and surfactant-to-oil-weight-ratio (SOR) on the product droplet size at constant stressing conditions is studied in detail. At similar stressing conditions and SOR, the type of the used plant oil and surfactant did not influence the product droplet size and the smallest achievable median droplet size was 20 nm. The API saturated oil phases and the pure oil phases exhibit similar viscosities, emulsification kinetics and final product droplet sizes, i.e. no influence of the API on the emulsification process could be identified. However, a strong dependency of the emulsion droplet size on the SOR has been observed. Moreover, very good long-term stabilities could be achieved for the obtained emulsions. A release test with fenofibrate-loaded peanut oil-polysorbate 80-water nanoemulsions showed remarkably fast drug distribution as compared to a formulation containing the same amount of the non-dissolved micronized drug.     

钼网表面MoSi2涂层的制备及其1500℃高温氧化性能

钼网被广泛用作高温催化剂载体,但关于其高温防护涂层的制备及失效机制却鲜有报道.用包埋渗硅方法在钼网表面制备了MoSi2高温抗氧化涂层,并在静态大气环境中开展了1500℃恒温氧化试验.利用X射线衍射仪(XRD)、扫描电镜(SEM)、能谱分析(EDS)等对氧化前后涂层的微观形貌和组织结构进行了表征.结果表明:1500℃氧化2h,MoSi2涂层中的Si元素会发生选择性氧化,在涂层表面形成一层连续的、具有“自愈合”功能的熔融态SiO2保护膜,阻挡氧向基体一侧的扩散,展现出了良好的高温抗氧化性能;高温条件下,涂层中的Si元素会和钼基体发生界面扩散反应生成抗氧化性能差的Mo5Si3,同时MoSi2不断地和氧发生反应生成Mo5Si3和SiO2,当涂层中的MoSi2完全转化为Mo5Si3,涂层将快速氧化失效.     

超声制备微乳化柴油的实验研究

微乳柴油是一种较佳的节能环保材料。采用聚氧乙烯失水山梨醇单油酸酯(Tween80)、失水山梨醇单油酸酯(Span80)和十二烷基苯磺酸钠复配成复配乳化剂,利用超声乳化机理,将超声波用于微乳化,研究了超声参数(声强,作用时间)、乳化剂及乙醇用量对乳液稳定性的影响,并通过正交实验找出了超声制备微乳化柴油的最佳工艺条件。该W/O乳液稳定时间随超声声强的增大而增加,且超声作用时间对乳液稳定时间有个最佳值。超声作用下乳化剂用量为2.5%(wt)时乳液最稳定。乙醇用量跟水油比有关,实验中水油比为0.1(V)时乙醇用量为5%(V),掺水量为10%(V)时的超声柴油微乳化最佳工艺条件为乳化剂用量为2.5%(wt),指示电流为3A(相当于声强为0.15 W/cm2),稳定剂用量为0.158%(wt),超声作用时间为15min,乙醇用量为5%(V)。     

Determination of required hydrophilic–lipophilic balance of citronella oil and development of stable cream formulation

Context: Citronella oil is reported to have excellent mosquito-repellent activity. To develop a stable cream formulation (emulsion), its hydrophilic–lipophilic balance (HLB) value is important.

Objective: To determine required hydrophilic–lipophilic balance (rHLB) value of citronella oil and to develop stable cream formulation.

Materials and Methods: Emulsions of citronella oil were prepared by phase inversion temperature technique using water, Tween 80 and Span 80. A first series of 11 emulsions with HLB values ranging from 5.0 to 15.0 and a second series of eight emulsions with smaller interval in HLB values from 11.0 to 13.8 were prepared. Emulsions were evaluated for creaming index, droplet size and turbidity to determine rHLB. Utilizing determined rHLB, citronella oil cream was formulated and evaluated for different texture parameters. rHLB of light liquid paraffin was also determined for validation of methodology.

Results: rHLB of light liquid paraffin and citronella oil was determined to be 11.80 and 12.60, respectively. Stable citronella oil cream was developed with 10% emulsifier blend. Texture parameters were found to be consistent over the entire storage period.

Discussion: Creaming index, droplet diameter, percent increase in droplet diameter and turbidity are the established parameters to determine rHLB and to develop stable emulsion. Emulsions with optimum emulsifier concentration resulted in less percentage creaming index, smallest droplet, less percentage increase in droplet diameter and highest turbidity. Texture properties evaluation ensures the stability of the developed cream.

Conclusion: rHLB value of citronella oil was found 12.6 and a stable cream was formulated utilizing determined rHLB.     

钛合金微弧氧化膜的性能探讨

钛合金微弧氧化膜具有优良的综合性能,但过去的研究多针对Ti6Al4V及医用纯钛,且电解液常用硅酸盐和磷酸二氢盐体系,不够全面、系统。为此,以磷酸盐溶液体系在船用TA2表面制备了陶瓷微弧涂层。采用SEM、光学显微镜、X射线衍射仪和显微硬度计对陶瓷膜的表面形貌、截面形貌、氧化层厚度、相结构和显微硬度进行了观察测试,用电子万能材料试验机和数字万用表测定了膜层的结合强度和绝缘性,并用盐雾试验机考察了涂层的耐蚀性。结果表明:随氧化时间的延长,膜层厚度不断增加,氧化60min后膜层厚度可达到20μm以上;陶瓷层主要由金红石TiO2相和锐钛矿TiO2相构成,膜基结合强度达到30MPa以上,膜层绝缘性和耐蚀性良好。     

Simultaneous emulsification and interfacial polycondensation for the preparation of colloidal suspensions of nanocapsules

Sub-micrometric particles having an oil core and a polymer shell (nanocapsules) have been prepared by combining in a single stage the emulsification process and an interfacial polymerization reaction. The spontaneous emulsification produced very fast a dispersion of oil droplets of 100–400 nm mean diameter at the surface of which the subsequent polycondensation reaction took place. The process has been optimized with respect to the choice of α-tocopherol as the oil and made robust regarding the presence of monomers in the aqueous and oil phases and their conversion into polymers. The major cause of troubles was the large concentration of diol or diamine monomers in the aqueous phase that made the oil droplets unstable with respect to aggregation immediately after their formation. Once the emulsifier has adsorbed and the polymerization has completed, the final suspensions of nanocapsules were quite stable over long periods. A secondary population of micrometric particles that coexisted with the nanocapsules was present in several cases, which was unfavourable regarding their application as a drug delivery system for cosmetic applications.     

含废机油混装乳化炸药可行性研究

为研究废机油用于制备混装乳化炸药的可行性,采用正交实验的方法制备乳化基质,利用偏光显微镜和扫描电镜记录新制、自然储存和高、低温循环乳化基质的微观形态,并分析了废机油对乳化炸药成乳性、储存性能和爆炸能力的影响。结果表明:废机油和乳化剂在油相中的含量会影响乳化基质的成乳性,废机油与成乳性指数的相关性指数为-0.697,废机油和乳化剂的比值与成乳性指数的相关性指数为-0.674。说明废机油比例越高,废机油与乳化剂的比值越高,越难形成乳化基质。成乳后含废机油乳化基质的储存性与废机油在油相中的含量没有明显的直接关系,含废机油混装乳化炸药爆速与不含废机油混装乳化炸药接近,含废机油乳化炸药可以满足工程爆破对乳化炸药的性能要求。     

Alternate drop coating for forming dual biointerfaces composed of polyelectrolyte multilayers

Two types of polyelectrolyte multilayers were formed on both sides of a quartz crystal microbalance (QCM) substrate by a novel alternate drop coating process. In this study, poly(diallyldimethylammonium chloride) (PDDA) and poly(sodium 4-styrene sulfonate) (PSS) were used as strong-strong polyelectrolytes. On the other hand, PDDA and poly(acrylic acid) (PAA) were used as strong-weak polyelectrolytes. The novel alternate drop coating process can separately fabricate each polyelectrolyte multilayer on both sides of the substrate. The substrate provides dual biointerfaces, both sides of which comprise different multilayers, by employing a combination of polymers. The formation of the multilayer by alternate drop coating was evaluated in terms of changes in the frequency of the QCM and model protein adsorption for proteins such as bovine serum albumin, and their characteristics were investigated with those of the conventional alternate adsorption process by performing dip coating. There was no significant difference between the surface properties resulting from the two formation conditions. This result strongly supported the fact that the multilayers fabricated by alternate drop coating were similar in quality to those fabricated by conventional dip coating. The resulting dual biointerfaces with polyelectrolyte multilayers provide alternative biofunctions in terms of individual protein loading. In summary, the novel alternate drop coating process for substrates is a good candidate for the preparation of dual biointerfaces in the biomedical field.     

含废机油混装乳化炸药可行性研究

为研究废机油用于制备混装乳化炸药的可行性,采用正交实验的方法制备乳化基质,利用偏光显微镜和扫描电镜记录新制、自然储存和高、低温循环乳化基质的微观形态,并分析了废机油对乳化炸药成乳性、储存性能和爆炸能力的影响。结果表明:废机油和乳化剂在油相中的含量会影响乳化基质的成乳性,废机油与成乳性指数的相关性指数为-0.697,废机油和乳化剂的比值与成乳性指数的相关性指数为-0.674。说明废机油比例越高,废机油与乳化剂的比值越高,越难形成乳化基质。成乳后含废机油乳化基质的储存性与废机油在油相中的含量没有明显的直接关系,含废机油混装乳化炸药爆速与不含废机油混装乳化炸药接近,含废机油乳化炸药可以满足工程爆破对乳化炸药的性能要求。     

Development and Oxidation Behavior of Al-Cu-Fe Quasicrystalline Coating on Ti Alloy

An oxidation resistant Al-Cu-Fe quasicrystalline coating was fabricated on substrate of Ti alloy by low pressure plasma spraying (LPPS) method. As-sprayed Al-Cu-Fe coating has a rapidly solidified lamellar microstructure consisting of quasicrystalline phase and crystalline phase. The formation of quasicrystalline coating is related to the annealing. The results from the ox!dat!on experiments showed that Al-Cu-Fe quasicrystalline coating improved the oxidation resistance of Ti-base alloys. During the oxidation period there is no evident spallation of the coating from the substrate. Oxide formed on the surface of Al-Cu-Fe quasicrystalline coating after oxidation consisted of Al2O3. Oxidation occurs Ieading to a change of concentration and phase transformation in the coating surface. Selective oxidation of AI transforms the quasicrystalline phase into the phase.     

Preparation of TiO2 hollow microparticles by spraying water droplets into an organic solution of titanium tetraisopropoxide

Hollow, spherical TiO₂ microparticles several tens of micrometers in diameter were prepared by spraying water into an organic phase containing titanium tetraisopropoxide (TTIP) as a titanium source. The rapid hydrolysis of TTIP at the water-oil interface resulted in the formation of a TiO₂ shell covering the water droplet. Hexane and cyclohexane were better solvents than isopropanol for fabricating hollow spherical microparticles, suggesting the importance of immiscibility of the solvent with water in this synthesis method. The average particle size increased as the distance from the nozzle to the surface of the TTIP solution was increased. The shell thickness was reduced by the addition of ethanol to the sprayed water droplet. These results demonstrate the controllability of the structure of TiO₂ hollow microparticles, including the diameter and the shell thickness.     

Effect of oil phase lipophilicity on in vitro drug release from o/w microemulsions with low surfactant content

In this work we investigated the effects of oil phase lipophilicity on in vitro drug release from topical o/w microemulsions (MEs) containing low percentages of emulsifiers. Three different lipids, isopropyl myristate (IPM), isopropyl palmitate (IPP), and isopropyl stearate (IPS), whose lipophilicity increased in the order IPM < IPP 相似文献   

Effect of Oil Phase Lipophilicity on In Vitro Drug Release from O/W Microemulsions with Low Surfactant Content

ABSTRACT

In this work we investigated the effects of oil phase lipophilicity on in vitro drug release from topical o/w microemulsions (MEs) containing low percentages of emulsifiers. Three different lipids, isopropyl myristate (IPM), isopropyl palmitate (IPP), and isopropyl stearate (IPS), whose lipophilicity increased in the order IPM < IPP <IPS, were used as oil phase to prepare o/w MEs containing low amounts (7.7% w/w) of two surfactant/cosurfactant mixtures, isoceteth-20/glyceryl oleate (5:2) (MEs 1–3) and oleth-20/glyceryl oleate (5:2) (MEs 4–6). All the MEs were prepared using the phase inversion temperature (PIT) method.

Three active compounds (0.5% w/w), Naproxen (NAP), Idebenone (IDE), and Butylmethoxydibenzoylmethane (BMBM), were selected as model drugs and their release rates from PIT MEs were evaluated using Franz-type diffusion cells. All the MEs gave a mean droplet diameter ranging from 28 to 44 nm and showed a single peak in size distribution. The addition of IDE to MEs 1–6 did not significantly change ME droplet size. On the contrary, an increase of the droplet size beyond the ME limit (150 nm) was observed when isoceteth-20 was used as surfactant to prepare MEs containing NAP or MEs containing BMBM and IPS as oil phase. Pseudo-first order release rates were observed only for NAP from MEs 1–3, while MEs containing IDE showed an initial slow release followed by an increased release of the test compound. The release rate constants were found to be dependent on the ME composition and on the active compound incorporated. The highest release rate was observed from ME 1 containing IPM as oil phase and NAP as drug. As regards BMBM, its release rate was not calculated since no release was observed until 6 h from the beginning of the experiment. The cumulative amount of active compound released after 22 h was inversely related to drug lipophilicity (NAP Log P = 2,9; IDE Log P 3,5; BMBM Log P 4,8). These findings could be attributable to a reduced thermodynamic activity of the drugs in the vehicles containing the most lipophilic oil phase due to an increase of drug solubility which could lead to an unfavorable drug partition from the oil phase. The results of this study suggest that the choice of proper combinations of oil phase lipids and emulsifiers may allow achieving drug controlled delivery from topical o/w MEs with low emulsifier content.     

不同增强体对SiC涂层性能的影响

采用3种工艺,以石墨为基体制备SiC抗氧化涂层,通过引入不同组分优化涂层相结构并对其性能进行研究。分别测试了不同制备工艺下的试样在1400℃下的抗氧化性能。通过分析试样氧化前后表面及侧面的SEM图以及涂层XRD衍射结果,研究涂层形貌、相结构及氧化机理。实验结果表明,同时引入SiC晶须及MoSi2的涂层在1400℃下氧化10h,氧化失重不超过1%,表现出良好的抗氧化性能;SiC晶须的存在能够减少涂层微裂纹的产生,减少渗Si过程中Si对基体的腐蚀;MoSi2和Mo的加入均能提高涂层质量并表现出较好的自愈合能力。     

A novel bird-nest-like air superoleophobic/superhydrophilic Cu(OH)2-based composite coating for efficient oil–water separation

An air superoleophobic/superhydrophilic composite coating with a unique structure was fabricated by oxidation and further modification of the copper mesh, and its design principle was clarified. This unique bird-nest-like configuration gives it instant superhydrophilicity due to the high surface roughness and high polar surface free energy components, while air superoleophobicity is caused by its extremely low dispersive surface free energy components. Furthermore, a water-resistance mechanism was proposed whereby a polyelectrolyte plays a critical role in improving the water-resistance of fluorosurfactants. It can separate oil–water mixtures with high efficiency (98.72%) and high flux (25185 L·m⁻²·h⁻¹), and can be reused. In addition, our composite coating had certain anti-acid, anti-alkali, anti-salt and anti-sand impact performance. More importantly, after being soaked in water for a long time or being exposed to the air for a long time, it still retained ultra-high air oil contact angle and showed excellent stability, which provided the possibility for practical applications. Thus, these findings offer the potential for significant practical applications in managing oily wastewater and marine oil spill incidents.     

乳状液制备新工艺——膜乳化过程实验研究

用膜乳化系统制备了Ｏ／Ｗ型乳状液,考察了乳化时间、平均膜孔径、壁面剪应力、膜两侧压差和乳化剂等因素对乳化效果的影响．实验显示,分散相液滴平均直径不随乳化时间而变化;在此条件下,该直径约是膜平均孔径的５～１２倍．随着连续相一侧壁面剪应力的增大液滴平均直径减小,但当壁面剪应力大到一定值后,减小的幅度变得很小．增大膜平均孔径和膜两侧压差都将增加分散相透过膜的通量．此外,乳化剂分子的吸附速度越快,分散相液滴平均直径越小．     

炭/炭复合材料高温抗氧化MoSi2/SiC复合涂层及其抗氧化特性

采用两段式包埋法和封闭处理的复合新工艺制得抗氧化性优良的MoSi₂/SiC复合梯度C/C复合材料高温抗氧化涂层。涂层由内至外结构为:SiC过渡层→SiC致密层→MoSi₂/SiC双相层→以MoSi₂为主的外层。对未封闭处理的涂层,制备过程中高温保温时间长的氧化失重少,1200℃、1300℃空气中氧化失重比1400℃、1500℃氧化失重大。用正硅酸四乙酯对涂层表面进行封闭处理,凝胶形成的SiO₂可充填涂层表面裂纹并覆盖在涂层表面。在1500℃空气中氧化一定时间后,未封闭处理的涂层试样表现为氧化失重;封闭处理后的试样为氧化增重,氧化52h仍然只有1.28%的增重,封闭处理使涂层的抗氧化性能明显改善。      

Effect of Polymerization Coadjuvants on Nanocapsule Elaboration and Triamcinolone Entrapment

The physical and chemical properties of tramcinolone acetonide nanocapsules, prepared by interfacial polymerization of isobutyl-2-cyanoacrylate at the oil/water I interface, have been studied. The joint effect of monomer and oil in organic phase on the size and encapsulation efficiency has been analyzed. Polymer coating around the oil droplets causes an important variation in droplet size and encapsulation efticiency. The release of drug from the nanocapsules was also investigated in vitro.     

Dendritic superstructure formation of polyaniline prepared using a water-soluble polyelectrolyte copolymer as the support matrix

In this letter, we report a dendritic superstructure formation of polyaniline (PANi) via a chemical oxidation approach using ammonium peroxydisulfate (APS) as the oxidant and a water-soluble polyelectrolyte copolymer as the dopant and support matrix. The morphology and the reaction conditions have been correlated, and a possible formation mechanism was proposed. It is suggested that the complex formation between the polyelectrolyte and aniline oligomer functions as nuclei which directs the further growth of polyaniline to dendritic superstructure.