超细粉体粒度测试方法浅析

介绍了超细粉体粒度测试的几种主要方法(激光衍射散射法、离心沉降法、颗粒图像处理仪和库尔特颗粒计数器)的测试原理及性能特点，并进行了比较。讨论了粒度测试中应注意的几个问题，重点分析了测试条件不同对粒度测定的影响，得出分散介质、分散剂、超声功率及超声时间等是影响粒度测定的最主要的因素；指出了重复性、真实性、易操作性、量程和动态范围是评价粒度仪测试性能的几个重要指标。     

Factors influencing contact angle measurements on wood particles by column wicking

The present work focuses on a capillary rise technique, referred to here as column wicking, for determining contact angles on wood particles. The liquid front rise versus time for different probe liquids has been measured for extracted and non-extracted spruce wood particles packed into glass columns. Wood is a porous, heterogeneous, and hygroscopic material. The sorption process of certain polar liquids in the wood substance, i.e. bulk sorption, is exothermic and causes swelling. This bulk sorption process and the resulting release of heat are observed as a distinct temperature increase within the columns during the wicking of water, formamide, and methanol. No temperature increase is observed for ethylene glycol, diiodomethane, and hexane. In some cases, the increase in temperature is observed in advance of the moving visible liquid front line. This may indicate that vapor is moving in advance of the liquid front, resulting in bulk sorption and the corresponding release of heat. An apparent non-linearity is observed when the square of the capillary rise is plotted versus time, mainly for water, formamide, and methanol. This non-linearity is strongly dependent on the probe liquid used and the variation in wood particle size. For the wicking of water, the bulk sorption, and hence the swelling of the wood particles, seems to appear instantaneously at the wetting front line, but for formamide and methanol a time delay is observed. The bulk sorption and resulting swelling of the wood particles strongly influence the determination of the effective interstitial pore radius between the particles, and thus the determination of contact angles by use of the Washburn equation.     

羧甲基纤维素钠对表面张力和接触角的影响

本文利用各种样品的表面张力和接触角的实验数据,说明羧甲基纤维素钠对洗涤作用的影响。     

Catalytic properties of ultrafine molybdenum-cerium oxide particles prepared by the sol-gel method

The structure and catalytic properties of ultrafine Mo-Ce oxide particles prepared by the sol-gel method have been studied by using X-ray diffraction, transmission electron microscopy, temperature-programmed reduction, laser Raman spectroscopy and microreactor tests. It has been shown that for selective oxidation of toluene to benzaldehyde the ultrafine Mo-Ce oxide particles exhibit higher catalytic activity than the larger oxide particles prepared by a conventional coprecipitation method. The unique catalytic properties of ultrafine Mo-Ce oxide particles may be correlated not only to the interaction between molybdenum oxide and cerium oxide, but also to the higher reactivity of lattice oxygen species in the ultrafine oxide matrix. This revised version was published online in July 2006 with corrections to the Cover Date.     

Preparation of aluminum ultrafine particles by anodizing aluminum foil in acidic electrolyte containing chloride ions

Anodization of aluminum in acidic electrolyte containing chloride ions was used to prepare aluminum ultrafine particles (Al UFPs) for the first time. In addition, the influence of different acid electrolyte was investigated and the mechanism of generating Al UFPs is analyzed. It is found that the pitting corrosion of chloride ions plays an important role in preparing Al UFPs and the acidification of the electrolyte is in favor of the preparation. Al UFPs with different shape and size distribution were obtained via changing the type of acid. Finally, the model of generating Al UFPs via this method is proposed.     

羧甲基纤维素钠对表面张力和接触角的影响

本文利用各种样品的表面张力和接触角的实验数据，说明羧甲基纤维素钠对洗涤作用的影响。     

Contact angle of surfactant solutions on precipitated surfactant surfaces

In this study, the contact angle of a saturated aqueous surfactant solution onto the surface of a precipitate of that surfactant is investigated. Those precipitates include fatty acids (C₁₀, C₁₂, C₁₄, C₁₆, and C₁₈), sodium salts of fatty acids (C₁₄, C₁₆, and C₁₈), calcium salts of fatty acids (C₈, C₁₀, C₁₂, C₁₄, C₁₆, and C₁₈). On virgin surfaces, free fatty acids and calcium salts of fatty acids have advancing contact angles (θ_A) between 77 and 92°, with little dependence on alkyl chain length for C₁₂ and higher alkyl chains. The sodium salt of a fatty acid has a lower θ_A than the free fatty or the calcium salt of the soap. The calcium salt of dodecyl sulfate has a lower θ_A than the calcium salt of dodecanoic acid (θ_A = 46 vs. 82°), but the calcium salt of the 18-carbon hydrophobes showed nearly the same contact angle for the soap and the alkyl sulfate. Greasiness, or slipperyness, or a scummy feel of a precipitated surfactant does not necessarily correspond to a hydrophobic surface.     

Contact angle and wettability of hybrid surface-treated metal adherends

Adhesion performance of adhesively bonded metal joints with aluminum and stainless steel was much dependent on the surface treatment of the adherends. This work was aimed at optimizing hybrid surface treatments to improve wettability of metal surfaces and strength of adhesive metal joints, which was a combination of mechanical, chemical, and energetic surface treatment methods. The surface free energies and wettability of hybrid surface-treated metal adherends were measured for different treatment conditions with abrasion, grit blast, sulfuric acid etching, phosphoric acid anodizing, silane treatment, plasma treatment, and flame treatment. The surface morphology and chemical composition of the metal adherends were investigated by scanning electron microscopy and X-ray photoelectron spectroscopy and the bond strengths of the single-lap joints composed of aluminum and stainless steel adherends were measured with respect to hybrid surface treatment conditions. From the experiments, an effective hybrid surface treatment condition was suggested for metal surfaces with super-hydrophilic characteristics. Also, the failure mode of adhesive metal joints was evaluated by photo-surface analysis method.     

工程相变凝并器内超细颗粒长大与脱除性能分析

传统的除尘系统脱除粗颗粒效率高,而脱除超细颗粒效率非常低,我国燃煤电厂脱除超细颗粒效率无法达到国家标准。湿式相变凝并技术是脱除烟气中超细颗粒的新技术。考虑颗粒性质以及通风因子,改进了超细颗粒凝并长大数学模型。将改进的数学模型写入颗粒群平衡模型中,模拟对比了超细颗粒在管束型相变凝并器和波纹板型相变凝并器内的长大特性及脱除效率。结果表明,两种相变凝并器都能明显提高超细颗粒的脱除效率,但管束型相变凝并器对烟气的冷却效果比波纹板型相变凝并器好。管束型相变凝并器能促进颗粒长大7.71倍,是波纹板型相变凝并器的1.4倍。管束型相变凝并器对颗粒数量浓度脱除效率高达64.7%,而波纹板型相变凝并器对颗粒数量浓度脱除效率为27.2%。     

Flotation behaviour of fine particles with respect to contact angle

The flotation behaviour of methylated quartz particles of different size, but within the size range from 0.2 to 50 μm, and varying contact angle, was probed in a mechanical flotation cell. Results suggest that particles of a given size need to possess a minimum critical contact angle (θ_crit) for flotation to occur. This behaviour is shown not to be solely dependent on fine particles having lower collision efficiency with bubbles, but rather due to a combination of low collision efficiency and particles not having enough kinetic energy at collision with bubbles to form the three phase line of contact and initiate the attachment process. In the particle size range investigated, the critical contact angle increases with a decrease in particle size.     

电沉积法制备钴超细微粒及其表征

用电沉积法制备超细钴粒子,考察反应物浓度、反应电流、反应时间、分散剂添加量等对样品粒径的影响。用XRD、XPS、TEM和激光粒度仪等进行表征。结果表明,所制备的超细钴粒子是平均粒径约500 nm的hcp相单质钴。在实验过程中,发现了外径200 nm,内径40~140 nm的钴环,长度为2μm,直径约75 nm的钴棒。     

低阶煤可浮性及浮选速率模型研究

针对低阶煤浮选困难的问题,采用煤质分析和筛分试验研究了低阶煤的可浮性。在此基础上进行了低阶煤浮选速度试验,并利用试验结果对低阶煤的浮选速率模型进行曲线拟合,经过MATLAB数值计算建立了最终的浮选速率模型。煤泥可浮性试验表明:低阶煤中挥发分、水分和O含量较高,亲水性强,可浮性很差。浮选速度试验表明,随着浮选时间的增加,精煤产率逐渐升高,尾煤产率逐渐降低,当精煤灰分为11.50%时,精煤产率仅为34.46%,尾煤产率高达65.54%,尾煤灰分仅为19.95%;2种浮选速率模型中,一级矩形分布模型计算误差较小,且相关系数平方R2更接近1,达到了很高的拟合精度,因此一级矩形分布模型是低阶煤最合适的浮选速率模型。     

New carbon composites containing ultrafine metal particles. 2. Synthesis by pyrolisis of pitch-organometallic blends

Air-stable new carbon composites containing uniformly dispersed ultrafine Fe, Co, Ni, Ru, Pd, Rh, or Ag particles were obtained by thermal degradation of coal pitches mixed homogeneously with 1–10% of poly(vinyl ferrocene), cobaltocene, nickelocene, (acenaphthylene) Ru₃(CO)₇, PdCl₂(COD), RhCp(COD), and AgC₆H₄CH₂NMe₂, respectively, at 400–1200°C in Ar. Carbonization yields are 45–55% and the size of metal particles varied from 5 to 65 nm depending upon the treatment temperature and identity of the metal. The carbon composites containing Fe particles showed high Vicat hardness and good electrical conductivity. Pd- and Rh-dispersed materials exhibited good catalysis in hydrogenation of 1-hexene. The composite containing ultrafine Ag particles showed excellent bacteriostatic activity forEscherichia coli, Pseudomonas aeruginosa, andBatchillus subtilis.     

Surface modification of silica particles assisted by CO2

This paper reports the synthesis of coating silica particles, in order to design hybrid materials with hydrophobic surface properties. The silica particles were prepared in basic conditions under atmosphere of carbon dioxide (CO₂), using tetraethylorthosilicate (TEOS) as a precursor and octyltriethoxysilane (OTES) as a surface modifying agent. It was demonstrated that the contact angles of silica hybrid films could be changed by varying temperature and pressure of CO₂. The investigation of the prepared hybrid materials by dynamic light scattering (DLS) and environmental scanning electron microscopy (ESEM), respectively, showed that they consisted mainly of particles with a diameter of 100–250 nm. Fourier transform infrared (FT-IR) spectra indicate that the interaction between the coupling reagents, at different conditions, is mainly through chemical bonding.     

超细氧化铈粉体的合成及粒度控制

为了一步合成超细氧化铈粉末，用碳酸氢铵溶液作沉淀剂，使用沉淀法合成氧化铈的前驱体，前驱体经低温烘干、高温煅烧后得到氧化铈超细粉末，同时研究了各种影响因素对氧化铈粉末粒度的影响。结果表明，加入一定量适当的分散剂可以有效控制氧化铈粉末的粒度；同时料液质量浓度、沉淀剂的质量浓度、煅烧温度、保温时间均对氧化铈粉末的粒度有较大影响。通过实验，给出了优化的工艺参数，按此工艺可以直接合成粒度为0．115μm的氧化铈粉末。     

Time dependent wettability of mineral and metal surfaces in the presence of thiol surfactants

The decrease in wettability of mineral and metal surfaces due to the adsorption of surfactants is crucial for flotation recovery and upgrading of these materials in mineral processing. Because of limited residence time in flotation processing, the kinetics of the wettability changes of the mineral surface becomes an important issue. The time dependent wettabilities of silver and galena (PbS) surfaces in aqueous solutions of di-isobutyl dithiophosphinate, a commercial flotation reagent, were determined from in situ measurements of advancing and receding bubble contact angles. Kinetic parameters were calculated from these data. By comparing the in situ measurements with ex situ measurements of water contact angles and external reflection FTIR of the adsorbed organic films on silver, a physical interpretation of the wettability data is given in terms of the evolution of these thin organic films on the mineral surfaces.     

Contact angle behaviour of poly(vinyl chloride)/ epoxidized natural rubber miscible blends

—Contact angle studies of miscible poly(vinyl chloride)/epoxidized natural rubber (PVC/ ENR) blends were carried out in air using water and methylene iodide. The solid surface free energy was calculated from harmonic mean equations. Blending of PVC and ENR decreased their contact angle or increased their solid surface free energy due to the improved chain mobility, and the accumulation of excess polar sites at the surface through conformational alterations resulting from the specific interaction of PVC and ENR. The work of adhesion, interfacial free energy, spreading coefficient, and Girifalco-Good's interaction parameter changed markedly with the blend composition. In blends, PVC and ENR improved hydrophilicity, and wettability with polar and non-polar liquids. The presence of a plasticizer in PVC, in general, further improved the wettability and hydrophilicity in blends.     

Contact angle of surfactant solutions on precipitated surfactant surfaces. II. Effects of surfactant structure,presence of a subsaturated surfactant,pH, and counterion/surfactant ratio

The contact angle of a saturated aqueous surfactant solution on the precipitate of that surfactant was measured by using the sessile drop method. The sodium and calcium salts of alkyl sulfates (C₁₂, C₁₄, and C₁₈) had advancing contact angles higher than those of alkyl trimethylammonium bromides (C₁₄, C₁₆, and C₁₈). The measured advancing contact angles for several surfactant solutions did not substantially change with varying surfactant/counterion ratios; therefore, the precipitating counterion concentration (e.g., water hardness) had little effect on the wettability. The contact angles of fatty acid (C₁₂ and C₁₆) solutions did not show any dependence on pH between a pH of 4 and 10. The contact angles of saturated calcium dodecanoate (CaC₁₂) solutions containing a second subsaturated surfactant (sodium dodecyl sulfate: NaDS) decreased with increasing NaDS concentrations until reaching the critical micelle concentration of the surfactant mixture. These results show that the second suractant can act as a wetting agent in this saturated surfactant system. Application of Young’s equation to contact angles showed that the solid/liquid surface tension can change substantially with surfactant concentration and be important in addition to the liquid/vapor surface tension in reducing contact angles. Application of the Zisman equation results in a “critical” surface tension for the CaC₁₂ or soap scum of 25.5 mN/m, which is comparable to difluoroethene.     

Contact angle measurements to determine the rate of surface oxidation of artists’ alkyd paints during accelerated photo-ageing

The rate of surface photo-oxidation and changes in polarity of the surfaces of artists’ alkyd paint films were studied by a rapid and novel approach using sessile drop contact angle measurements. The contact angles of distilled water and diiodomethane drops on the film surfaces were measured over a period of 25–2000 h of artificial ageing at 40 °C under an indoor light filtered Xenon light source. Chemical changes on the surfaces of the films were also followed using Fourier transform infrared spectroscopy-attenuated total reflectance (FTIR-ATR). Titanium white artists’ paint samples from three different manufacturers were investigated: Winsor & Newton, Ferrario and Da Vinci Paint Co. As the films aged, there was a decrease in the contact angle and an increase in the polar component of the free surface energy of the paint film surfaces indicating the formation of photo-oxidation products. Such changes correspond well to the chemistry of oil paints, and suggested chemistry of long-alkyd paints, because of their relatively high weight percent of fatty acids.     

Formation of monodisperse polyacrylamide particles by dispersion polymerization: particle size and size distribution

Highly monodisperse polyacrylamide microparticles were directly prepared by dispersion polymerization in aqueous alcoholic media initiated by 2,2′‐azobisisobutyronitrile using poly(N‐vinylpyrrolidone) as a steric stabilizer. Monomer conversion was studied dilatometrically and polymer molecular weight was determined viscometrically. The hydrodynamic diameter of polymer particles and its distribution were measured with a dynamic laser light scattering spectrometer. The number of the nuclei produced in the early stage of the polymerization was found to be constant during the remainder of the polymerization. The influences of various polymerization parameters, such as initiator concentration, monomer concentration, stabilizer content, medium polarity, and polymerization temperature on the particle size and size distribution were systematically investigated. Copyright © 2003 Society of Chemical Industry