Phase transformations of aluminium hydroxide in the calcination process

In this paper phase transformations were considered that occur in the process of calcination of aluminium hydroxide, and for qualitative phase analysis low-temperature X-ray analysis was used. Two samples were used, one of chemical purity obtained under laboratory conditions and the other obtained under industrial conditions in the alumina production plant at Kidric?evo, Yugoslavia.It was determined that for both samples in the process of calcination of aluminium hydroxide identical transformations appear, and the sequence of transformations present may be shown in the following way:

     

沉淀铁费托合成催化剂焙烧工艺的优化研究

通过DOE实验设计对沉淀铁费托合成催化剂焙烧过程进行了优化,并给出了焙烧过程的分子模拟与粒子长大模型。结果表明,随着焙烧温度的升高和焙烧时间的延长,催化剂的孔容减小,堆比及骨架密度增加,耐磨性改善。BET表面与磨耗的变化趋势一致,即比表面积越小磨耗越小;磨耗与密度成线性反比关系,密度越高磨耗越小。通过焙烧工艺的优化,可调变Cu、Si通过O原子与Fe原子的键合作用及催化剂的粒子粒径,得到较高F-T活性且稳定性好的沉淀铁催化剂。在该实验中,优化的焙烧温度为560℃。     

富钙生物油煅烧过程中孔结构变化特性的研究

在热重分析仪上进行富钙生物油煅烧实验。结果表明,富钙生物油的煅烧过程分为三个阶段,分别是生物油部分组分的脱CO₂和H₂O阶段、有机酸钙盐分解阶段、碳酸钙分解阶段。其中,有机酸钙盐分解对煅烧产物的孔结构有重要影响。在450℃~600℃,气体析出的气蚀作用与生物油中高分子化合物的碳化沉积现象同时存在,两者共同作用,但后者占主导,高分子化合物的碳化沉积主要发生在500℃~600℃。600℃以后,碳酸钙开始分解,释放出CO₂,气蚀作用使煅烧产物内部形成新的微孔,产物具有发达的孔结构。相同煅烧温度下,富钙生物油煅烧产物的孔隙特性明显优于CaCO₃。     

煤系针状焦煅烧过程中焦炭微晶结构的演变规律

以煤系针状焦的生焦为原料,在2和5℃/min的升温速率下进行煅烧,采用FT-IR、XRD、Raman光谱等分析手段研究煅烧过程中针状焦微晶结构的演变规律。结果表明,随着煅烧温度的升高,针状焦中碳微晶的直径L_a、炭微晶的高度L_c、晶体中的片层含量N以及每层中平均碳原子数n、趋于规整的石墨微晶含量I_g逐渐升高。但是受挥发分逸出和生焦收缩的影响,L_c出现了明显的"拐点"。新增片层与原有片层间存在的随机"层错",导致层间距d₀₀₂的波动。相同温度下升温速率越快,晶格尺寸越小,片层含量N及每层平均碳原子数n越少,L_c出现"拐点"的温度越靠后。理想石墨微晶含量（I_G/I_all）随温度的升高逐渐增加;而具有缺陷的石墨微晶间在煅烧过程中不断相互转化,最终发育为理想石墨微晶。碳网平面上C-C键平均键长α则随着煅烧温度的升高明显增加。     

Influence of yttria addition on the phase transformations of zirconia from zircon ore by carbothermal reduction process

Zircon ore carbothermal reduction with yttria addition has been carried out. The influences of heating temperature and yttria addition on the phase transformations of zirconia from zircon ore by carbothermal reduction have been investigated in detail. The phase transformations of zirconia from zircon ore by carbothermal reduction were monitored by X-ray diffraction. The microstructure and micro-area chemical analysis of the products were characterized by scanning electron microscopy and energy dispersive spectrometer. The chemical states of Zr 3d, Y 3d and O 1s presented in the products of zircon carbothermal reduction with 10 wt% yttria addition were investigated by X-ray photoelectron spectroscopy. The results showed that the optimized heating temperature of zircon carbothermal reduction with no addition was 1600 °C, and the main phase of the products consists of m-ZrO₂, c-ZrO₂, ZrC and β-SiC. Yttria addition could be introduced into zirconia lattice and caused it to form Y₂O₃ stabilized zirconia. Zirconia in the products would be turned into partially stabilized zirconia with yttria addition from 1 wt% to 5 wt% while it would exist in the form of fully stabilized zirconia with over 8 wt% yttria addition.     

Characterization of the self-assembly process of hydrophobically modified dextrin

Hydrophobized dextrin, randomly substituted by long alkyl chain (C₁₆), forms stable hydrogel nanoparticles by self-assembling in water. Hydrophobic chains, distributed along the polymer backbone, promote the formation of hydrophobic microdomains within the nanoparticles. The influence of degree of substitution with hydrophobic chains (DS_C16) on nanoparticles size, colloidal stability, density, aggregation number and nanoparticle weight was studied. Size distribution was also evaluated at different pH, urea concentration and ionic strength conditions. As shown by dynamic light scattering and transmission electron microscopy, the particles are spherical having a diameter of about 20 nm. The more substituted polymer forms more densely packed hydrophobic microdomains, such that the colloidal stability (in water and PBS buffer) of nanoparticles is increased. The knowledge of the aggregate building process and the characteristics of the nanoparticles are crucial for the design of drug delivery systems.     

Some aspects of the hydrothermal calcination of gypsum

Lump-size and powdered gypsum samples were calcined at 135, 150 and 180°C. The products were thoroughly investigated by differential thermal analysis and X-ray diffraction, and their chemically-combined water was determined thermogravimetrically. Results indicated that almost all the treated samples contained gypsum, hemihydrate and anhydrite in varying proportions. Gypsum and anhydrite increased, and the hemihydrate decreased as the heating temperature was increased and the grain size decreased. Such a variation in the phase constitution of the treated samples is discussed.The relative intensity of the main gypsum X-ray diffraction characteristic lines changes upon treatment. In the atmospheric calcination the relative intensities of the lines at 3.059, 2.867, 2.679, 2.59, 2.495, 2.45 and 2.40 Å show a pronounced decrease. Autoclaving, on the other hand, causes a detected decrease in the relative intensity of the line at 7.56 Å and an increase in the 4.27, 3.059, 2.59, 2.495 and 2.45 Å lines. These findings postulate that X-ray diffraction data could hardly be used for the quantitative assessment of the gypsum phase in the dehydration products of any calcined material.     

Characterization and evaluation of the photocatalytic properties of wormhole-like mesoporous silica incorporating TiO2, prepared using different hydrothermal and calcination temperatures

TiO₂?CSiO₂ mesoporous materials were synthesised by deposition of TiO₂ nanoparticles prepared by the sol?Cgel method on to the internal pore surface of wormhole-like mesoporous silica. In this work we synthesised wormhole-like mesoporous silica of different surface area by changing the hydrothermal temperature (70, 100, or 130?°C). Subsequent to this, titania solution was deposited on to the inner surface of the pores and this was followed by calcination at different temperatures (400, 600, or 800?°C). The effect of different hydrothermal and calcination temperature on the photocatalytic properties was evaluated. The samples were characterized by N₂-sorption, X-ray diffraction, X-ray photoelectron spectroscopy, field emission scanning electron microscopy, and transmission electron microscopy. The effect of different hydrothermal and calcination temperatures on the photocatalytic properties was evaluated by measuring the degradation of methylene blue in aqueous solution under UV light irradiation (mercury lamp, 125?W). The results indicated that appropriate surface area and degree of crystallinity are two important factors for obtaining high photocatalytic efficiency. Samples prepared at a hydrothermal temperature of 100?°C and calcined at 800?°C had the best photocatalytic performance, because of the highest surface area and high crystallinity.     

Cu-Mn-Si催化剂在环己醇脱氢和糠醛加氢耦合反应中的研究:沉淀pH值和焙烧温度的影响

采用共沉淀法制备了Cu-Mn-Si催化剂,并将其应用于常压气相环己醇脱氢和糠醛加氢耦合反应中,考察了沉淀pH值和焙烧温度对耦合反应的影响。沉淀pH值对糠醛加氢制2 甲基呋喃反应影响不大,但对环己酮的选择性影响较大。pH值在7.5~10.0制备的催化剂具有优良的反应性能。焙烧温度的提高,导致催化剂的比表面积减小,孔径变大,铜的比表面积下降,还原温度提高。在耦合一体化反应中,环己醇脱氢制备环己酮反应受焙烧温度影响不大,但糠醛转化率和2 甲基呋喃选择性随着焙烧温度的提高而减小。     

Sol-gel synthesis and characterization of yttria stabilized zirconia membranes

Mesoporous yttria stabilized zirconia (YSZ) membranes can be used as supports for ultrathin dense ceramic or metallic membranes, and for ultrafiltration (UF) applications in harsh environments. This paper reports synthesis and characterization of sol-gel derived UF YSZ membranes. 0.25 M zirconia sol was prepared by hydrolysis and condensation of zirconium n-propoxide. A solution-sol mixing method was used to dope 8 mol% yttria in zirconia. Supported YSZ membranes were prepared by dip-coating the yttrium doped zirconia sol on the porous α-alumina substrate, followed by drying and calcining under controlled conditions. The membranes prepared in this study are of cubic fluorite phase. Helium permeation experiments show that the supported membranes are pin-hole (or crack) free. The 5 time dip-coated membrane determined by SEM micrograph is about 3.5 μm in thickness, with an average pore diameter of 3 nm.     

Characterization of the microstructures of copper-based aerogels on the sol–gel process

In this thesis, we will elaborate on the sol–gel process during the preparation of monolithic copper-based aerogel. The microstructure of the copper-based aerogel appears to be various due to the different amounts of raw materials, such as polyacrylic acid, propene oxide, deionized water (H₂O) and copper(II) chloride (CuCl₂) in the sol–gel process. The proper molar ratios between these reactants play a crucial factor in mediating the morphology of the aerogel. The aerogels are characterized by field emission scanning electron microscopy, high-resolution transmission electron microscopy and Brunauer–Emmett–Teller methods. The combined results indicate that the copper-based aerogel shows a typical three-dimensional porous structure with a large surface areas about 568 m²/g, and the skeleton structure of the aerogel is composed of a large number of primary particles with the size about a few nanometers.     

Mixed conductivity, structural and microstructural characterization of titania-doped yttria tetragonal zirconia polycrystalline/titania-doped yttria stabilized zirconia composite anode matrices

Taking advantage of the fact that TiO₂ additions to 8YSZ cause not only the formation of a titania-doped YSZ solid solution but also a titania-doped YTZP solid solution, composite materials based on both solutions were prepared by solid state reaction. In particular, additions of 15 mol% of TiO₂ give rise to composite materials constituted by 0.51 mol fraction titania-doped yttria tetragonal zirconia polycrystalline and 0.49 mol fraction titania-doped yttria stabilized zirconia (0.51TiYTZP/0.49TiYSZ). Furthermore, Y₂(Ti_1−yZr_y)₂O₇ pyrochlore is present as an impurity phase with y close to 1, according to FT-Raman results. Lower and higher additions of titania than that of 15 mol%, i.e., x=0, 5, 10, 20, 25 and 30 mol% were considered to study the evolution of 8YSZ phase as a function of the TiO₂ content. Furthermore, zirconium titanate phase (ZrTiO₄) is detected when the titania content is equal or higher than 20 mol% and this phase admits Y₂O₃ in solid solution according to FE-SEM-EDX.The 0.51TiYTZP/0.49TiYSZ duplex material was selected in this study to establish the mechanism of its electronic conduction under low oxygen partial pressures. In the pO₂ range from 0.21 to 10^−7.5 atm. the conductivity is predominantly ionic and constant over the range and its value is 0.01 S/cm. The ionic plus electronic conductivity is 0.02 S/cm at 1000 °C and 10^−12.3 atm. Furthermore, the onset of electronic conductivity under reducing conditions exhibits a −1/4 pO₂ dependence. Therefore, it is concluded that the n-type electronic conduction in the duplex material can be due to a small polaron-hopping between Ti³⁺ and Ti⁴⁺.     

Effect of BaO on the calcination and hydration characteristic of CA

Phosphoaluminate cement (PAC) clinker had good mechanical properties at early and long-term period. In comparison, the compressive strength of PAC clinker modified by BaO was more prominent. As primary mineral phase for PAC clinker, CA’s mineralogical structure and hydration characteristics were intimately related to the compressive strength of hardened cement paste. In this study, the effects of BaO content on the calcination, mineralogical structure and hydration characteristics of CA were investigated. Experimental results showed that the appropriate calcination temperature of CA was 1400 °C. No more than 11% (the substitution ratio of BaO for CaO) addition of BaO can promote the conversion of C₁₂A₇ to CA and increase the formation ratio of CA. Appropriate content of 7 mol% BaO could endow the hardened paste with excellent compressive strength. In CA mineral phase the high limit addition of BaO was 15 mol%. The addition of BaO decreased and even restrained the formation of C₂AH₈ and C₃AH₆ of CA hydration products and also improved the content of CAH₁₀. The addition of BaO dramatically decreased the hydration velocity and cumulative heat of CA mineral.

     

三氧化铬电催化合成进程监测和表征

为了解决三氧化铬传统生产中存在的问题,进行了以重铬酸钠为原料,在自制电解槽中电催化合成三氧化铬绿色新技术研究.实验表明可用槽电压随反应时间的变化来定量表征三氧化铬电催化合成反应进程,建立了槽电压变化的数学模型及其变化速率方程,所建模型很好地表征了三氧化铬电催化合成进程,并讨论了槽电压的影响因素.     

环己酮氨肟化反应中失活TS-1催化剂上沉积物的物化表征

在液相环己酮氨肟化反应中,有机物在钛硅分子筛催化剂（TS-1）上的沉积是造成失活的原因之一。采用傅里叶变换红外光谱、热重-差热、色谱-质谱联用、X-射线衍射、固体核磁共振、N2物理吸附和扫描电镜等分析手段,对失活TS-1的骨架结构及表面沉积物分子的结构和物化性质进行了表征。结果表明,引起催化剂失活的沉积物富集在分子筛的孔道内,主要有环己酮的氧化或还原产物、环己酮的二聚物、环己酮肟深度反应产物、叔丁基环己酮等可溶性沉积物以及它们缩聚而成的不溶性沉积物,其量可占失活催化剂总质量的5.0%。TPO烧炭时靠近Ti中心处的沉积物可以在较低温度下脱除,而孔道内的其他沉积物需要在较高温度下脱除,650℃沉积的炭可完全脱除。失活催化剂经700℃煅烧再生后,催化活性可恢复到新鲜催化剂的水平。     

Characterization of micro-crystalline lead tungstate with different morphologies produced by the sonochemical process

Micro-crystalline PbWO₄ was sonochemically produced using Pb(CH₃COO)₂ · 3H₂O and Na₂WO₄ · 2H₂O in aqueous solutions with and without anionic surfactant (sodium dodecyl sulphate or sodium lauryl sulphate). The product morphologies were influenced by the pH values and the surfactant. Micro-crystalline PbWO₄ composing of Pb, W and O, and W-O stretching vibration band of WO₄ tetrahedrons were detected using XRD, SEM, EDX, TEM, SAED and FTIR. Photoluminescent intensities, caused by the electronic transition from ¹T₂ to ¹A₁ states, shown to increase with the increase in the pH values of the solutions.     

Protective yttria coatings of melting crucible for metallic fuel slugs

As one of the candidate coating materials for a melting crucible, yttrium oxides were deposited on graphite and niobium substrates using slurry and plasma spraying methods. Thermal cycling tests and interaction studies between U–Zr/U–Zr–RE fuel melt and the Y₂O₃ coatings were carried out to evaluate the performance as reusable coatings for a melting crucible. A multi‐layer coating method was also applied to overcome the issue of a thermal expansion mismatch between the coating and substrate. The results showed that the plasma‐sprayed coatings showed a good consolidation after deposition compared to slurry coating. The plasma‐sprayed Y₂O₃ coating on the niobium substrate showed better thermal cycling resistance than those coated on a graphite substrate. The proposed TaC/Y₂O₃ double‐layer coating which was plasma‐sprayed on the niobium substrate showed improved characteristics with no reaction layer formation and no separation from the substrate after the interaction with the U–Zr–RE melt. Copyright © 2014 John Wiley & Sons, Ltd.     

Characterization of iron-mesoporous molecular sieves obtained by a microwave-hydrothermal process

Fe-SBA-15 materials with different Si/Fe ratios (Si/Fe = 90, 50, 10) have been synthesized by a microwave-hydrothermal (M-H) process and characterized by several spectroscopic techniques. Electrons spin resonance and Mössbauer spectroscopies, along with electron microscopy and X-ray diffraction, allowed differentiation of several iron species. These species correspond to hematite particles, very small “isolated” or oligomeric Fe^III species possibly incorporated in the mesoporous silica wall, and Fe^III oxide clusters either isolated or agglomerated, forming “rafts” at the surface of the silica and exhibiting ferromagnetic ordering. Due to their agglomeration, these clusters appear with a two-peak size distribution, with one peak corresponding to the isolated clusters formed in the mesopores and still embedded in them (ca. 2 nm diameter) and the other corresponding to the agglomerates spread on the surface of the mesoporous silica particles (ca. 9 nm).     

Influence of calcination on the electrical properties of tin-antimony mixed oxide catalysts

The electrical conductivity study of Sn–Sb mixed oxide powders is consistent with an enrichment in Sb (due to calcination) of the surface region where a solid solution of Sb in SnO₂ and a Sb₂O₄ surface phase coexist.

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Sn–Sb Sb- — , Sb SnO₂ Sb₂O₄.