Preparation and characterization of free films of high amylose/pectin mixtures cross-linked with sodium trimetaphosphate

High amylose and pectin were mixed at 1:1 mass ratio and cross-linked with sodium trimetaphosphate (STMP) in alkaline medium. Films were prepared from aqueous dispersions of these cross-linked polymer blend at three different concentrations (3, 4 and 5%), by solvent casting method. Characterization of the films included thickness, surface morphology, water uptake, water vapor permeability (WVP), tensile strength measurements and enzymatic digestion. The cross-linking allowed to obtain films with improved mechanical properties and reduced WVP. The high resistance to enzymatic digestion exhibited by these films represents a promising approach to their application in the development of colon drug delivery systems.     

Effect of drying technique on some physical properties of cross-linked high amylose/pectin mixtures

Polymers mixtures as well as cross-linking reactions are approaches that have been used successfully to modulate the polymers characteristics in order to improve the control over drug release rate. High amylose and pectin are polysaccharides frequently used to prepare drug delivery systems. Since the drying technique can strongly influence the properties of such systems, the aim of this work was to characterize high amylose/pectin mixtures cross-linked with sodium trimetaphosphate and dried by different techniques – oven and lyophilization. The results showed that samples dried by lyophilization presented reduced particle size, higher porosity and higher swelling ability than the samples dried in oven. Besides, lower thermal stability and different diffraction patterns showed by the former particles should reflect the structural changes as a function of drying technique.     

明胶/海藻酸钠(京尼平交联)互穿网络膜的制备与性能

为了提高海藻酸钠与明胶各自的性能,首先,以海藻酸钠和明胶为原料,以京尼平、CaCl2为交联剂,采用分步交联法制备了明胶/海藻酸钠互穿网络膜。然后,利用FTIR对明胶/海藻酸钠互穿网络结构进行了表征与分析,根据FTIR结果推测了互穿网络结构形成的机制。最后,探讨了京尼平的加入量和明胶与京尼平的质量比对互穿网络膜力学性能和交联度的影响,及海藻酸钠与明胶的质量比对互穿网络膜力学性能、断面形貌、热稳定性和吸水保水性能的影响。结果表明:当明胶与京尼平的质量比为200∶1、海藻酸钠与明胶的质量比为2∶1时,互穿网络膜具有最佳的力学性能、吸水保水性能和相容性;此外,互穿网络膜的力学性能也优于纯海藻酸钠膜与纯明胶膜的。明胶的加入提高了互穿网络膜在低温区的热稳定性,但降低了高温区的热稳定性。海藻酸钠与明胶之间可能以分子间作用力、氢键及离子键等相互作用,提高了二者各自的初始分解温度与最大热分解温度。研究解决了海藻酸钠与明胶力学性能差的问题,为拓展海藻酸钠在医用领域的应用提供参考。     

Preparation and characterization of plasticized gelatin films cross-linked with low concentrations of Glutaraldehyde

Thermal and mechanical properties as well as moisture resistance and water vapor barrier properties of films from bovine gelatin added with d-sorbitol (30 wt%) as plasticizer and cross-linked with low amounts of glutaraldehyde (GTA, from 0 to 2 wt%) were investigated to determine their suitability as barrier layers for flexible packaging materials. Results revealed that free amino side chain groups of gelatin decreased with GTA, confirming the occurrence of cross-linking between GTA and gelatin. The extent of cross-linking reaction in the presence of d-sorbitol was lower compared with the unplasticized counterpart suggesting that plasticizer hampers GTA to react. The glass transition temperature (T _g) as measured from differential scanning calorimetry (DSC) increased with GTA concentration owing to the formation of more reticulated materials while the incorporation of d-sorbitol led to a small reduction in this parameter due to plasticization. Increasing GTA concentration from 0 to 1 wt% provoked the enhancement of elastic modulus from 3.7 ± 0.2 to 4.9 ± 0.2 GPa. These values reduced significantly by the addition of d-sorbitol, whereas elongation at break improved in about 150%. The optimum formulation for the intended purpose was that containing 1 wt% GTA and 30 wt% d-sorbitol since it exhibited the best set of properties: total soluble mater reduced from 100 to 16%, moisture absorption decreased from 1854.1 ± 85 to 210.4 ± 8%, water vapor permeability at 65% relative humidity improved from 2.42 ± 0.27 to 0.94 ± 0.06 × 10⁻¹⁴ kg m Pa⁻¹ s⁻¹ m⁻², with minor reduction in opacity and with the additional benefit of releasing only 5% of the initial GTA content.     

高导热石墨膜的制备及表征

将不同厚度杜邦聚酰亚胺(PI)薄膜进行压制炭化、石墨化处理得到PI石墨膜。采用扫描电镜、X射线衍射、、拉曼光谱等测试手段分析了PI薄在高温热处理过程中的结构演变。研究结果表明,50μm厚PI膜经3 000℃高温石墨化后能形成三维有序堆积的石墨层状结构和较为完整的石墨晶体,其石墨片层间距为0.336nm,层片堆积高度达到65.94nm,石墨化度高达93%,室温面向电阻率为0.48μ!·m,实测面向热导率达到了994 W/(m·K)。随着热处理温度的提高,PI膜微晶由无定型向有序类石墨结构转变,其结晶度和层片取向程度提高,石墨晶体逐渐完善。PI膜厚度越大,其类石墨晶体生长发育越困难,层片择优取向程度越低。     

无色透明耐高温聚酰亚胺薄膜的制备与性能研究

分别采用两种联苯型二酐单体,对称结构的3,3',4,4'-联苯四甲酸二酐(s-BPDA)以及不对称结构的2,3,3',4'-联苯四甲酸二酐(a-BPDA)与含氟芳香族二胺1,4-双(4'-氨基-2'-三氟甲基苯氧基)联苯(TFDAB)通过两步缩聚法制备了两种聚酰亚胺材料PI-1(s-BPDA/TFDAB)与PI-2(a-BPDA/TFDAB).研究结果表明,不对称结构可以显著增加PI薄膜在可见光区的透明性.25μm厚的PI-2薄膜在450nm处的透光率达到93%,而同样厚度的PI-1薄膜的透光率只有67%.此外,在PI分子结构中引入不对称结构不会牺牲材料的耐热稳定性、力学性能与介电性能.     

Preparation and characterization of transparent/conductive nano-composites films

Polymer-embedding of nano-sized indium tin oxide (SnO·In₂O₃, ITO) produces electrically conductive materials transparent to the visible light at filling factors higher than the percolation threshold. ITO powders are commercially available in an aggregated form and a disaggregation technique was required. Here, aggregated ITO nanoparticles were transformed to colloidal suspension by high-speed stirring. This finely dispersed ceramic suspension was stabilized by addition of poly(vinyl pyrrolidone) and the obtained colloidal system was cast on an optical-grade substrate (PET) to produce electrically conductive-transparent nanocomposite films. Preliminary mechanical and electrical characterization of these films showed good conductivity and interfacial properties.     

Preparation and characterization of polypropylene/sodium propionate (PP/SP) composite films for bread packaging application

To prolong the shelf life of bread, polypropylene/sodium propionate (PP/SP) composite films were prepared via a melt‐extrusion process. To investigate the feasibility of using PP/SP composite films as a bread packaging material, their chemical structure, morphology, mechanical properties, barrier properties against water, surface properties, and antimicrobial properties were investigated. A storage test for bread was also conducted. The mechanical and thermal stability of the PP/SP composite films enhanced with increasing SP content. Compared with pure PP, the PP/SP composites had increased hydrophilicity that increased with increasing SP content. These composite films showed enhanced antimicrobial activity against both Gram‐negative and Gram‐positive microorganisms. This was due to the interaction of SP and water originating from the bread, which modifies the pH of the bread and causes destruction of the cellular structures of fungi and also reduces the growth rate of bacteria. The enhanced thermal, mechanical, antifungal, and antimicrobial properties achieved by the addition of SP can be beneficial for maintaining the freshness of bread and prolonging its shelf life.     

Preparation and properties of cross-linked zirconia nanoparticle films on polycarbonate

Highly-crystalline zirconia (ZrO₂) nanoparticle was functionalized with 3-(N-aminoethyl) aminopropyltrimethoxysilane (AAPTMS) and dispersed in water at primary particle size level under basic condition (pH 13-14). The aqueous ZrO₂ nanoparticle dispersion was cast on a polycarbonate substrate with 1,4-butanediol digylcidyl ether as a cross-linker. Nanoparticle films with as high as 81 wt.% of ZrO₂ were obtained through heating the cast dispersion at 120 °C, which are highly transparent. The refractive index ranges from 1.70 to 1.77 at wavelength of 632 nm with the decrease of the amount of AAPTMS attached to ZrO₂ nanoparticles. Nanoindentation tests show that the hardness of the film reaches 1.7 GPa. In addition, both punched tape abrasion and nanoscratch tests reveal that the films exhibit prominent scratch resistant performance.     

Preparation and characterization of carbon nanotube/polyetherimide nanocomposite films

Multi-walled carbon nanotube (MWCNT)/polyetherimide (PEI) nanocomposite films have been prepared by casting and imidization. A homogeneous dispersion of MWCNTs throughout the PEI matrix is observed by scanning electron microscopy of fracture surfaces, which shows not only a fine dispersion of MWCNTs but also strong interfacial adhesion with the matrix, as evidenced by the presence of many broken but strongly embedded carbon nanotubes (CNTs) in the matrix and by the absence of debonding of CNTs from the matrix. Differential scanning calorimetry and dynamic mechanical analysis show that the glass transition temperature of PEI increases by about 10 °C by the addition of 1 wt% MWCNTs. Mechanical testing shows that for the addition of 1 wt% MWCNTs, the elastic moduli of the nanocomposites are significantly improved by about 250% while the tensile strength is comparable to that of the matrix. This improvement is due to the strong interfacial interaction between the MWCNTs and the PEI matrix which favors stress transfer from the polymer to the CNTs.     

聚乙烯醇/海藻酸钠/碳纳米管复合膜的制备及其吸附性能

通过溶液共混法制备了聚乙烯醇/海藻酸钠/多壁碳纳米管复合膜,对其进行了透光率、力学性能和DSC表征,并研究了对Cr2O27-的吸附性能。结果表明,PVA与SA等质量混合时相容性好;MWNTs的添加有助于提高复合膜力学性能、热性能;在pH值为2、温度为30℃、MWNTs为80mg时,吸附6h后,复合膜对Cr2O27-的去除率达到96.84%。     

Preparation and characterization of PI/PVDF composite films with excellent dielectric property

All-organic polyimide (PI)/poly(vinylidene fluoride) (PVDF) composite materials with high dielectric constant and low dielectric loss were fabricated via solution blending. The dielectric, mechanical, and thermal properties of the PI/PVDF composite films were studied. Results indicated that the dielectric properties of the composites were highly reinforced through the introduction of PVDF, and the composites exhibited excellent thermal stability. When the mass fraction of PVDF was adjusted to 30 wt%, the specimen demonstrated excellent thermal properties, superior mechanical properties, high dielectric constant (5.7, 1 kHz), and low dielectric loss (0.009, 1 kHz). Moreover, the dependence of the dielectric constant and dielectric loss on frequency was investigated. The composite presented stable dielectric constant and dielectric loss that were less than 0.04 within the testing frequency range of 100 Hz–10 MHz. This study demonstrated that the PI/PVDF composites were potential dielectric materials in the field of electronics.     

Preparation and properties of polyimide/LTNO composite films with high dielectric constant

To develop the polymer-based materials with high dielectric constant and thermal stability, Li and Ti doped NiO (LTNO) particles with super high dielectric constant (ε) were dispersed into pyromellitic dianhydride (PMDA) and 4, 4′-oxydianiline (ODA)-based polyimide. Through mixing LTNO particles with the poly(amic acid) precursor solution, casting film and following thermal curing, the polyimide/LTNO composite films were obtained. The thermal stability and structure of the composites were studied by TGA and X-ray diffraction, respectively. Dielectric and conductive measurements were adopted to investigate the properties of the samples. The results revealed that the obtained composites had good morphology stability, but their thermal resistances become a little lower in comparison with pure polyimide. With increasing the content of LTNO particles, ε and conductivity of the composite films increased greatly. For the sample with the LTNO content at 0.4 in volume fraction, ε was as high as 570 at the frequency of 100 Hz. It showed that doping LTNO particles into polyimide would be an efficient route to high ε composites.     

Preparation and characterization of diamond films

Diamond films were deposited by magnetron sputtering of vitreous carbon disc and also by plasma CVD technique using C₂H₂ + H₂ or CO₂ + H₂ gas mixtures. The films were characterized by measuring the electrical, optical and microstructural properties. FTIR and Raman studies were carried out to study the effect ofsp ² andsp ³ bonds present in the films. The films had a high mechanical stress which was determined from the broadening of the optical absorption tail in the films.     

交联PS微球负载纳米Ni颗粒的制备及表征

采用种子聚合法制备出交联聚苯乙烯(PS)微球,经预处理在微球表面引入官能团,采用化学镀法在微球表面负载纳米级Ni颗粒,利用FI-IR、SEM、XRD等测试手段对其进行表征,结果表明:PS微球粒径均匀,平均粒径约为4.3μm,表面光滑;微球负载的纳米Ni颗粒分散性良好、平均晶粒度为9.41nm.利用负载微球对高氯酸铵(AP)进行催化实验,表明负载微球可使AP高温分解峰降低94.2℃左右.研究表明:采用PS微球负载可提高纳米Ni颗粒的分散性,进而提高了Ni颗粒的催化性能.     

SiCN薄膜的制备及其性能研究

利用射频溅射法在Si衬底上制备了SiCN薄膜，并利用X射线衍射（XRD）、红外吸收谱（FTIR）和X射线光电子谱（XPS）对薄膜的结构、成份及化学键合状态进行了分析。结果表明，室温制备的SiCN薄膜为非晶状态，并形成了Si-C、Si-N和C－N键；而在高温下（衬底温度为800℃），薄膜中含有SiCN的晶体成分。此外，还利用原子力显微镜（AFM）对薄膜的表面形貌进行了研究，并进一步研究了样品的场发射性能。在场强为24V／μm时，最大发射电流可达3.3mA/cm^2。     

Preparation of cross-linked sodium alginate microparticles using glutaraldehyde in methanol

Polymeric sodium alginate microparticles were prepared by precipitating sodium alginate in methanol, followed by cross-linking with glutaraldehyde. The extent of cross-linking was controlled by the time of exposure to glutaraldehyde. The topology of microparticles was characterized by scanning electron microscopy (SEM), which indicated smooth surfaces. The equilibrium swelling experiments were carried out in water to observe the effect of cross-linking and drug loading for better utility of microparticles. It was found that swelling decreased, but drug loading increased, with an increase in cross-linking of the matrix.     

氧化海藻酸钠/聚丙烯酰胺水凝胶的制备与表征

通过水-乙醇和水-正丙醇两种不同的溶剂体系制备高分子量和不同氧化度的氧化海藻酸钠(OSA),然后引入聚丙烯酰胺(PAM)交联网络结构,通过二步法获得OSA/PAM复合水凝胶。探讨了不同反应体系下,HCl体积分数对OSA分子量的影响以及氧化剂(高碘酸钠NaIO_4)添加量、反应时间对OSA氧化度的影响规律。结果表明:在水-正丙醇体系下,HCl体积分数为24vol%时,氧化海藻酸钠的分子量达到170 000;调节NaIO_4的添加量和反应时间可以控制OSA的氧化度在10%~85%范围内变化。在此基础上对OSA/PAM复合水凝胶的溶胀率和力学性能进行了探讨,发现氧化度10%的复合水凝胶48h后的溶胀率达1 777%,断裂强度为0.11MPa,随着OSA氧化度的增大,OSA/PAM复合水凝胶的溶胀率增大,而拉伸强度逐渐减小。     

取向碳纳米管/环氧树脂复合薄膜制备及结构与性能表征

碳纳米管(Carbon nanotube, CNT)/环氧树脂(Epoxy resin, EP)纳米复合材料中树脂含量、分布、CNT取向及其与树脂间界面结合是制备高性能纳米复合材料的关键因素。为了探究树脂分布和CNT/EP复合材料性能之间的关系,采用浮动催化化学气相沉积法制备的CNT薄膜和EP为原料,通过浸渍、牵伸、清洗和热压固化工艺制备CNT/EP复合薄膜。利用聚焦离子束结合扫描电子显微镜定性表征树脂在复合膜中的分布状态。结果表明,随着树脂含量增加,树脂在复合薄膜表面富集程度增加。在最优工艺条件下制备的纳米复合材料中CNT含量为66.14wt%, 拉伸强度和拉伸模量达到1405 MPa和46.7 GPa。      

电化学沉积CNx薄膜的摩擦性能研究

以单晶硅片(100)为衬底,尿素-甲醇有机溶液为沉积液,用电化学沉积的方法在阴极制备出CNx薄膜.通过AFM、XPS、Raman光谱和FTIR光谱对得到的CNx薄膜的表面形貌和微观结构进行了表征,并在球-盘摩擦试验机上考察了薄膜的干摩擦性能,用SEM和EDS对摩擦表面进行了分析,研究了摩擦机理.结果表明薄膜表面致密,但粗糙度较大;Raman光谱中出现明显的D峰和G峰,说明薄膜具有无定形的结构特征;薄膜的化学元素组成主要为C,还有少量的N,C、N原子之间主要以共价单键和双键形式结合.CNx薄膜与红宝石球对摩时,摩擦系数随频率的增大而升高,但几乎不随载荷而变化;CNx薄膜在形成转移膜的过程中不仅失去了N,而且发生了石墨化,这与DLC膜的摩擦过程非常相似.