Silicon Nitride Derived from an Organometallic Polymeric Precursor: Preparation and Characterization

Partially crystalline Si₃N₄, with nanosized crystals and a specific surface area greater than 200 m²/g, is obtained by pyrolysis of a commercially available vinylic polysilane in a stream of anhydrous NH₃ to 1000°C. This polymer does not contain N initially. Crystallization to high-purity α-Si₃N₄ proceeds with additional heating above 1400°C under N₂. The changes in crystallinity, powder morphology, infrared spectra, and elemental compositions, for samples annealed from 1000° to 1600°C under N₂, are consistent with an amorphous-to-crystalline transformation. Although macroscopic consolidation and local densification occur at 1400°C, volatilization and accompanying weight loss limit bulk densification. The effect of temperature on specific surface area is examined and related to the sintering process. These results are applicable to pyrolysis, decomposition, and crystallization studies of ceramics synthesized by polymeric precursor routes.     

SEQUENTIAL LOOP CLOSING IDENTIFICATION OF MULTIVARIABLE PROCESSES USING THE BIASED RELAY FEEDBACK METHOD

Each controller in multiloop control systems for multivariable processes can be tuned sequentially with the ultimate information for the paired input and output while former loops have been closed, and hence, single-input single-output autotuning methods can be applied. In this sequential autotuning for multiloop control systems, several iterations are usually required for better control performances. Especially when pairings are undesirable, the autotuning sequences should be repeated with correct pairings, which result in long field experiments. Here, to avoid this drawback, a simple method to identify process models while loops are being sequentially tuned is proposed. The identified models can be used to correct pairings of multiloop control systems and to improve tuning performances without several field iterations. In addition, they can be used to obtain model-based control systems such as decoupling control systems.     

ON THE UNIMODALITY OF THE EXACT LIKELIHOOD FUNCTION FOR NORMAL AR(2) SERIES

Abstract. For stationary second-order autoregressive normal processes, the conjecture of uniqueness of the solution of the exact likelihood equations is examined. A sufficient condition for uniqueness is given; this condition is satisfied with very high probability if the number of observations is not extremely small. Moreover, it is shown that not more than two maxima may exist. Examples of data which actually produce a likelihood function with two local maxima are given.     

羟胺-环己酮法肟化反应效率的影响因素及改进措施

介绍了羟胺-环己酮法中环己酮肟化反应的原理及工艺流程,讨论了反应温度、环己酮进料的分布、缓冲溶液的pH值、脉冲速度等因素对肟化反应效率的影响,针对各个影响因素提出了改进肟化反应条件的措施并应用于生产实践,提高了肟化反应效率。     

H2O-NH3-CO2体系汽液平衡计算

本文给出计算H2O-NH3-CO2三元体系在温度323.15K～473.15K、压力0.2MPa～8.0MPa、液相NH，摩尔分率≤0.3、富氨区条件下汽液平衡的UNIQUAC模型及其参数，模型的计算结果与试验数据吻合。该模型可用于尿素生产装置中蒸发冷凝、循环吸收以及水解精馏等过程的设备计算。     

Surface Areas of Nitrated Hydrotalcites

Hydrotalcites in the nitrate form were prepared using microwave irradiation in the hydrotreatment step. The surface area (BET) of nitrated hydrotalcites was evaluated. Solids were characterized by atomic absorption, X-ray diffraction and BET analysis. Thermal pretreatment temperature determined the surface area of the hydrotalcites.     

聚硅氧烷-丙烯酸酯共聚物互改性产物的表面特性

通过测定参照液体在固体表面的接触角，计算固体的表面能及固体／液体接触体系的粘附功，考查了聚硅氧烷-丙烯酸酯共聚物互改性产物的表面特性及其对粘接性能影响。     

Zinc Coated Steel/Epoxy Adhesive Systems: Investigation of the Interfacial Zone by FTIR Spectroscopy

The present study takes advantage of the ability of Fourier Transform Infrared Spectroscopy (FTIR) for the analysis of ultrathin organic films on metals. FTIR in the reflection mode (IRRAS) is used in order to study the interaction of ultrathin films of dicyandiamide (hardener of most one-pack epoxy resins) with various substrates, model ones such as gold or zinc and industrial ones such as steel and zinc-coated steels.

Pure zinc surfaces and, to a lesser extent, zinc-coated steels are shown to react with dicyandiamide after heating at 180°C, as evidenced by the frequency shift of the absorption band (at about 2200 cm^-1) characteristic for nitrile groups. As real systems consist of thick layers of a fully formulated adhesive cured onto a metallic substrate, the direct investigation of such a buried interphase is no longer possible by FTIR and by most of the known spectroscopies. Some mechanically tested specimens are then analysed, after failure, by FTIR microspectrometry. The spectra obtained, corresponding to the fracture initiation zone which is about 100 μm in diameter, advocate for the presence of an ultrathin layer of modified polymer still covering the substrate.     

Pervaporation performance analysis and prediction—using a hybrid solution-diffusion and pore-flow model

A hybrid mathematic model for pervaporation is proposed which incorporates the concepts of solution-diffusion model and pore model. The model allows performance prediction as well as the establishment of the internal concentration and pressure profiles within the membrane. The model parameters specific to the particular membrane and mixture system are determined using liquid sorption and pervaporation experimental data. The model is experimentally examined using ethanol–water mixtures and poly(dimethyl siloxane)–poly(vinyldiene fluoride) (PDMS–PVDF) composite membranes. The characteristics of flux and separation factor predicted using the model are in fair agreement with the experimental data under various feed concentrations and downstream pressures for different membrane arrangements, including single-layer, reverse single-layer and double-layer PDMS–PVDF composite membranes. Internal profiles of pressure, concentration and component mole fraction can be established using the model. Concentration polarization phenomena for ethanol and water are located at membrane interfaces and vapor–liquid interfaces, respectively. Performances of several different membrane designs are compared using the model.     

尿素装置液相浓度在线自动检测软件的研究

为了改善尿素装置先进的控制和落后的人工检测物料浓度之间的矛盾，运用化工热力学原理，以及热力学模型组合求解法，研制了液相浓度实时检测软件。并开发了多种软件以适应各类尿素流程（水溶液全循环法、ＣＯ２汽提法、氨汽提法）的需要