合成工艺对氮化硅铁物相和结构的影响

以硅铁合金(FeSi75)为原料,分别采用闪速燃烧合成工艺和自蔓延高温合成工艺制备氮化硅铁样品,利用X射线衍射仪和扫描电镜对样品进行了表征,探讨了合成工艺对氮化硅铁物相和显微结构的影响。采用闪速燃烧工艺合成的氮化硅铁相组成为β-Si3N4,α-Si3N4,Fe3Si和少量SiO2;而采用自蔓延高温合成的氮化硅铁由β-Si3N4,α-Si3N4,Fe3Si和Si2N2O组成。闪速燃烧合成的氮化硅铁样品中存在大量长径比较高的柱状氮化硅晶体,Fe3Si位于柱状结晶所包裹材料的内部;自蔓延高温合成的氮化硅铁显微结构为致密的氮化硅块体,在块体表面覆盖有氧氮化硅膜,块体的间隙存在晶形细小的氮化硅晶体,含铁组分镶嵌在致密的块体中。闪速燃烧合成的氮化硅铁结构疏松,活性较强;自蔓延高温合成的氮化硅铁结构致密,性质稳定。     

氮化硅铁在Al2O3-C体系中的高温行为

为了研究高温条件下Al2O3-C体系中氮化硅铁的状态,以闪速燃烧合成氮化硅铁、炭黑、刚玉粉为原料,将试样在高温炉中分别加热至1 450、1 500、1 600℃保温5 h,急速水冷后,对其进行XRD和显微结构分析。结果表明:1 450℃烧后试样的物相包含β-Si3N4、α-Si3N4、α-Al2O3和Fe3Si;1 500℃烧后试样的物相为β-Si3N4、SiC、α-Al2O3和Fe3Si;1 600℃烧后试样中Si3N4大部分转变为SiC,其他物相未发生变化。在升温过程中,氮化硅逐渐转化为碳化硅,材料结构致密。     

硅铁闪速燃烧合成氮化硅铁

利用闪速燃烧合成新技术 ,以粒度≤ 0 .0 88mm的FeSi75硅铁细粉为原料 ,在 0 .2MPa的低氮气压力与 14 0 0℃的燃烧温度条件下 ,制备了细蜂窝状氮化硅铁。XRD和SEM分析结果表明 ,这种氮化硅铁主要由短柱状β Si3N4 相和Si3Fe相组成 ,其结构特征是以Si3Fe形成核心 ,并被Si3N4 包裹。同时 ,还用热力学原理探讨了由硅铁闪速燃烧合成氮化硅铁的工艺条件、形成产物的形式、反应的中间产物和残留金属的形态。热力学研究结论和实验检测结果相一致 ,从而在理论上阐明了闪速燃烧合成是制备氮化硅铁的一种理想工艺     

埋碳条件下氮化硅铁-刚玉复合材料的反应机理

以热固型酚醛树脂为结合剂,在刚玉中分别引入质量分数为0、5%、10%、15%、20%、25%的氮化硅铁,制备出氮化硅铁-刚玉复合材料。结果表明:样品在埋碳气氛下于1 450℃保温24h处理后,常温耐压强度增加;添加氮化硅铁质量分数为15%的样品,耐压强度达到132MPa。氮化硅铁中部分Fe3Si转化成为Fe4N;热固酚醛树脂结合剂中部分残碳与氮气反应生成C3N4;氮化硅与刚玉发生固溶,生成Si5AlON7(Z=1)。氮化硅铁中的氮化硅与刚玉固溶形成Sialon。新形成的物相(Fe4N、C3N4和Si5AlON7)改善了样品的性能。     

闪速燃烧合成氮化硅铁的氮化机理

以硅铁合金Fe Si75为原料,研究了闪速燃烧合成氮化硅铁的氮化机理。结果表明:在氮化过程中,首先是硅的活性氧化,硅被氧化生成气态Si O,使得体系氧分压降低,当氧分压p(O2)≤10–20 MPa(T=1 823 K)时,Si与N2(g)直接反应形成氮化硅,气态Si O最终与N2(g)发生反应生成氮化硅。硅铁合金Fe Si75中的Fe Si2与Fe0.42Si2.67没有促进氮化硅的形成,且与未参与氮化反应的硅反应形成Fe3Si。氮化硅铁的主要物相为氮化硅和Fe3Si,其中存在大量的柱状氮化硅,Fe3Si被柱状Si3N4包裹,呈孤立状态。     

添加剂对Si粉直接氮化工艺中α-Si3 N4含量的影响

通常情况下,Si粉直接氮化法和自蔓延法所制得Si3N4粉体主要以β-Si3N4为主,而为了使Si3N4陶瓷有更好的烧结性能,需要得到高α相含量的Si3N4粉.本研究以Si粉直接氮化法为基础,通过添加NH4Cl、FeCl3来制备高α相含量的Si3N4粉.经XRD和SEM检测分析发现,添加适量NH4Cl、FeCl3可大幅提高Si3N4粉体中α-Si3N4的含量,最高可达88.3%,但FeCl3的含量过高时,则可显著降低α-Si3N4的含量.研究还发现添加NH4Cl、FeCl3还可降低Si粉发生氮化反应的起始温度.     

热力学相图计算技术在闪速燃烧合成氮化硅铁中的应用

将热力学相图计算技术应用于Si-Fe-O-N体系,以评估由FeSi75粉闪速燃烧合成氮化硅铁的条件和目标产物。结果表明:将闪速燃烧温度控制在1200～1500℃之间较为适宜,此时平衡态产物中除主要含有Si3N4以外,还有一定量的Fe与Si间化合物和少量稳定的SiO2存在。此计算结果与实际试验结果吻合良好。     

Al2TiO5-Si3N4复合材料制备工艺研究

以Al2TiO5粉料、α-Si3N4粉料为原料,制备Al2TiO5-Si3N4复合材料。研究了Si3N4加入量、烧成气氛、烧成温度、保温时间对Al2TiO5-Si3N4复合材料性能的影响。研究结果表明,制备Al2TiO5-Si3N4复合材料较佳的工艺条件为Si3N4含量15％、氮化气氛、烧成温度为1550℃,保温时间为2h。     

铁元素在氮化硅铁中的存在状态

用化学分析、XRD，SEM，EDS等检测手段，首次对闪速燃烧工艺制备的新型合成原料——氮化硅铁(Fe-Si3N4)中铁元素的存在状态进行了研究。结果表明：以小于0．074mm的FeSi75颗粒为原料制备氮化硅铁时，FeSi75颗粒表面的硅原子氮化形成氮化硅包覆层，硅铁受热熔化；随着硅的持续氮化减少，铁含量相对增加，硅的氮化难度加大；最后，铁以Fe3Si和α-Fe两种形式保留下来，并且主要分布于氮化硅粉体颗粒的内部，并用热力学进行了分析。     

硅铁含量对反应烧结Fe-Si_3N_4-SiC复合材料性能的影响

以碳化硅、氮化硅、硅铁粉为原料,以热固树脂为结合剂,用1 000 t压砖机机压成型制备了硅铁质量分数分别为0、6%、9%、12%和15%的Fe-Si3N4-SiC试样,研究了硅铁含量对Fe-Si3N4-SiC材料性能的影响。结果表明,经1 300℃氮气气氛下保温8 h制备得到Fe-Si3N4-SiC复合材料,其常温耐压强度和高温抗折强度均优于Si3N4-SiC材料。当硅铁质量分数为12%时,Fe-Si3N4-SiC材料综合性能最佳,而当硅铁质量分数为15%时,Fe的催化作用下降,硅铁合金的氮化程度降低,材料性能下降。     

乙烯酮(双乙烯酮)下游产品废水的治理技术

乙烯酮(双乙烯酮)是十分重要的化工中间体,其下游产品较多。江苏某化工厂开发生产乙烯酮(双乙烯酮)下游产品三十多个,年生产规模三万多吨,是国内以乙烯酮(双乙烯酮)为中间体生产精细化学品的综合骨干企业。针对乙烯酮(双乙烯酮)下游产品废水特点,该厂结合企业实际,开展了产品优化,结构调整,清洁生产,资源循环利用,节水降耗等工作,从源头削减了污染物的生产。同时投资二千多万元新建预处理装置三套,6000m3/d废水生化处理装置一套,使全厂乙烯酮(双乙烯酮)下游产品的废水得到了有效的治理。     

几种乙炔加压设备性能的比较

阐述并比较了几种加压设备在乙炔加压清净过程中的性能和特点。     

三种煤样燃烧热的测定

本文通过三个厂家提供的三种煤样燃烧热的测定,由测定结果综合得出3号煤样燃烧最完全、燃烧热也最大,是三个煤样中最好的一种。     

Semi-empirical equation of state of metals. Equation of state of aluminum

A semi-empirical equation of state for metals is described. Its capabilities are demonstrated by the example of the equation of state for aluminum. New experimental data are presented on the location of the isentrope of aluminum for unloading from the state at p = 229.71 GPa on the shock adiabat to an aerogel (SiO₂) of density 0.08 g/cm³. __________ Translated from Fizika Goreniya i Vzryva, Vol. 44, No. 2, pp. 61–75, March–April, 2008.     

水泥水化热测定方法综述

水泥水化热是中、低热水泥和核电工程用水泥的一项关键的技术指标。全球范围内测定水泥水化热的方法有溶解法、直接法/半绝热法、等温传导量热法三种。本文总结了中、美、欧相关方法标准,对其测试原理、仪器设备、试验过程等方面进行了比对,并对其在领域的应用做了简单的概括。     

小议汽车涂装工艺设计对涂装成本的影响

论述了涂装工艺设计对涂装设备投资、涂装生产成本的影响。     

Measurement of the gradient of viscosity with composition of mixtures of non-ideal gases

A perturbation viscometer is a differential capillary viscometer that measures the logarithmic viscosity gradient of the viscosity-composition curve for gas mixtures. Measurements are made at different gas mixture compositions. Integration of the logarithmic viscosity gradients measured over the full composition range gives the mixture viscosity relative to the viscosity of one of the pure components of the gas mixture. This method is attractive because, for measurements of equal precision, integration of the gradients is potentially an order of magnitude more precise than measurement of the viscosities directly. It can also work at high and low temperatures and perhaps high pressures.The perturbation viscometer has been used to make measurements on ideal gas mixtures at ambient and elevated temperatures. The situation is more complicated when the gas mixtures are non-ideal. Extra effects due to density differences, molar volume change on mixing and differential thermal expansion may be measured in addition to the desired viscosity change producing systematic errors in the results. Thus, a more sophisticated apparatus is required. The standard perturbation viscometer has been modified to separate out the extra effects to permit measurement of the true change in viscosity. In addition, the theoretical operation of the modified apparatus has been revised to account for the design changes to permit calculation of the viscosity-composition profiles from the results.The apparatus has been tested using helium-HFC-125 mixtures and two new viscosity-composition profiles are presented for these mixtures at 23 and . Internal consistency tests have been used to confirm that the data produced are of high quality with an estimated uncertainty in the viscosity ratio data at of 0.9% and at of 1.5%.     

Calorimetric and Computational Study of Enthalpy of Formation of Diperoxide of Cyclohexanone

A thermochemical rather simple experimental technique is applied to determine the enthalpy of formation of Diperoxide of ciclohexanone. The study is complemented with suitable theoretical calculations at the semiempirical and ab initio levels. A particular satisfactory agreement between both ways is found for the ab initio calculation at the 6–311G basis This set level. Some possible extensions of the present procedure are pointed out.     

塔设备改造选型的分析

就当前扩产增容中塔设备设计和改造时板式塔和填料塔的选型问题加以分析。在评述目前国内常用的几种塔板和新型填料之后，着重介绍一种新型塔板（导向梯形浮阀塔板）和一种新型填料（波环填料——乾隆帕克）。     

Effect of degree of deacetylation of chitin on the properties of chitin crystallites

In the present article, chitin from crab shell was systematically deacetylated using a NaOH treatment with control of the reaction time. The degree of deacetylation, monitored using solid-state NMR, revealed that the reaction was pseudo-first order. Based on this, swollen and NaOH-saturated particles are proposed as the reaction system. The weight loss of the partially saponified and neutralized samples after HCl hydrolysis increased linearly with the degree of deacetylation. The crystallinity of the samples was found to increase after acid hydrolysis. According to conductimetric titration, the surface charge density of the crystallites, after acid hydrolysis, was found to increase with base treatment time. The effect of surface charge on the formation of a chiral nematic phase, due to the rodlike nature of the crystallites, was explored. These results show that because the contribution of charged particles to the ionic strength was significant the double layer compression was affected, especially since the surface charge density was close to the Manning limit. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 65:373–380, 1997