Chemische Zusammensetzung und Mikrostruktur polymerabgeleiteter Gläser und Keramiken im System Si–C–O. Teil 2: Charakterisierung der Gefügeausbildung mittels hochauflösender Durchstrahlungselektronenmikroskopie und Feinbereichsbeugung

Chemical Composition and Microstructure of Polymer‐Derived Glasses and Ceramics in the Si–C–O System. Part 2: Characterization of microstructure formation by means of high‐resolution transmission electron microscopy and selected area diffraction Liquid or solid silicone resins represent the economically most interesting class of organic precursors for the pyrolytic production of glass and ceramics materials on silicon basis. As dense, dimensionally stable components can be cost‐effectively achieved by admixing reactive filler powders, chemical composition and microstructure development of the polymer‐derived residues must be exactly known during thermal decomposition. Thus, in the present work, glasses and ceramics produced by pyrolysis of the model precursor polymethylsiloxane at temperatures from 525 to 1550 °C are investigated. In part 1, by means of analytical electron microscopy, the bonding state of silicon was determined on a nanometre scale and the phase separation of the metastable Si–C–O matrix into SiO₂, C and SiC was proved. The in‐situ crystallization could be considerably accelerated by adding fine‐grained powder of inert fillers, such as Al₂O₃ or SiC, which permits effective process control. In part 2, the microstructure is characterized by high‐resolution transmission electron microscopy and selected area diffraction. Turbostratic carbon and cubic β‐SiC precipitate as crystallization products. Theses phases are embedded in an amorphous matrix. Inert fillers reduce the crystallization temperature by several hundred °C. In this case, the polymer‐derived Si–C–O material acts as a binding agent between the powder particles. Reaction layer formation does not occur. On the investigated pyrolysis conditions, no crystallization of SiO₂ was observed.     

Laser scanning path generation considering photopolymer solidification in micro-stereolithography

It is essential to automate the scanning path generation process to effectively implement the micro-stereolithography. However, a scanning path that is generated based only on a 3D CAD model introduces dimensional inaccuracies. In micro-stereolithography, the photopolymer solidification is affected by fabrication conditions, such as the optical properties (laser power, laser scanning speed, laser scanning pitch focusing condition, etc.) and material properties of the photopolymer. Thus, the photopolymer solidification phenomena must be considered when generating a laser scanning path. In this paper, a scanning path generation algorithm that uses 3D CAD data and considers the photopolymer solidification phenomena is proposed to improve the dimensional accuracy in micro-stereolithography. Multi-line photopolymer solidification experiments were performed for various laser scanning conditions to examine the photopolymer solidification phenomena. From these experiments, linear relations between the solidification length (width) and scanning length (width) were acquired and stored in a database. Subsequently, these data were utilized to compensate the scanning path of the laser beam. In addition, experiments for determining the layer thickness in the z-direction were performed and these results were also used in the scanning path generation algorithm.This research was supported by the Highly Advanced National Project (http://www.most.go.kr), which performs some of the National R&D Program, and sponsored by the Korean Ministry of Science and Technology under the contract project code M10214000116-02B1500-02010.     

Phenol novolac/poly(4- hydroxyphenylmaleimide) blend hardeners for DGEBA-type epoxy resin

Phenol novolac/poly (4-hydroxyphenylmaleimide) (PHPMI) blends were used as an epoxy resin hardener. The curing behavior of the above system and the thermal and mechanical properties of the cured epoxy resin were studied. It was not necessary to use a curing accelerator for this system, because PHPMI caused acceleration of the curing reaction. The curing mechanism of this system was investigated by using model compounds. Test pieces from the neat resins and the glass fiber reinforced resins were evaluated in terms of thermal and mechanical properties, respectively. It was found that heat resistance and mechanical properties were improved by increasing the amount of PHPMI in the hardener.     

Use of inverse gas chromatography to quantify interactions in amine cured epoxy resins

Flory–Huggins interaction parameters, λ, were determined for a series of probes in an amine cured epoxy resin matrix (433–493 K) and its precursors (324–363 K) by inverse gas chromatography (IGC). Hildebrand–Scatchard theory was combined with Flory–Huggins theory in order to estimate infinte dilution solubility parameters (δ₂) for the matrix and its precursors at 298 K. It was shown that the value of the solubility parameter for the cured resin matrix lies between those of its precursors. Compared to the majority of published work, an unusual aspect of this application of IGC is that solubility parameters have been determined when the stationery phases are (i) small molecules and (ii) a highly crosslinked polymer. Moreover, all possible attempts have been made to ensure equilibrium conditions between probe and stationary phase, and compensation for asymmetry of peak profile has been applied in determining δ₂. The solubility parameters estimated by IGC are in good agreement with those calculated by other methods.     

Synthetic resins: XV. Chelation ion exchange properties of 2,4- dinitrophenylhydrazone of resacetophenone-formaldehyde resin

A number of copolymers were synthesised by condensing the 2,4-dinitrophenylhydrazone of resacetophenone with substituted benzoic acids/ phenols and formaldehyde in the presence of sodium hydroxide or hydrochloric acid. The decomposition temperature, solubility and viscosity of the polymers have been determined. The ion-exchange properties have been studied by using a batch equilibrium method. The distribution of a number of metal ions between an aqueous solution and the resin have been measured. A wide range of pH and variable ionic strengths have been investigated.     

Microstructure-related fracture toughness and fatigue crack growth behaviour in toughened, anhydride-cured epoxy resins

Fracture toughness and fatigue crack propagation (FCP) of plain and modified anhydride-cured epoxy resin (EP) were studied at ambient temperature. Liquid carboxyl-terminated acrylonitrile-butadiene (CTBN) and silicon (SI) rubber dispersions were used as tougheners for the EP. The morphology of the modified EP was characterized by dynamic mechanical analysis (DMA) and by scanning electron microscopy (SEM). The fracture toughness, K_c, of the compositions decreased with increasing deformation rate. K_c of the EP was slightly improved by CTBN addition and practically unaffected by incorporation of the SI dispersion when tests were performed at low cross-head speed, v. Both modifiers improved K_c at high v, and also the resistance to FCP, by shifting the curves to higher stress intensity factor ranges, ΔK, by comparison with the plain EP. It was established that both fracture and fatigue performance rely on the compliance, J_R, at the rubbery plateau, and thus on the apparent molecular mass between crosslinks, M_c. The failure mechanisms were less dependent upon the loading mode (fracture, fatigue), but differed basically for the various modifiers. Rubber-induced cavitation and shear yielding of the EP were dominant for CTBN, whereas crack bifurcation and branching controlled the cracking in SI-modified EP. The simultaneous use of both modifiers resulted in a synergistic effect for both the fracture toughness at high deformation rate and the FCP behavior.     

多元酚——甲醛树脂中游离酚,游离醛含量的测定

多元酚－－甲醛树脂是本院开发的热固粘接剂新产品，本文给出了这一产品技术指标中游离酚、游离醛含量的测定方法，并对方法进行了讨论。     

Kynar—500涂装工艺与涂层性能研究

介绍了Kynar－500涂料的涂装工艺，并对涂层的性能作了试验与分析。     

集成电路密封用高纯邻甲酚醛环氧树脂的制备

ECN树脂中的可水解氯含量是决定树脂质量的—个重要指标。本文研究了反应温度、ECH/OCN配比、反应时间和碱用量等因素的影响,取得了规律性的认识,并获得最佳配方,制备出高纯度的ECN树脂系列产品。     

国外聚甲醛生产技术现状与发展

综述了国外主要甲醛生产厂商的工艺技术，树脂生产技术的发展和品种开发情况。