锌-钬共掺杂无机抗菌材料的制备及性能研究

采用溶胶-凝胶法制备了一种新型无机抗菌材料--锌-钬抗菌白炭黑。通过单因素实验和响应曲面法优化,得到了最优制备条件为:锌浓度0.711 mol·L^-1,钬浓度0.5 mmol·L^-1及反应时间65 min。获得了分散性好、粒度较小、抗菌性能良好的复合抗菌材料。通过SEM,EDS,FTIR,粒径检测和抗菌检测等手段对锌-钬抗菌白炭黑进行了表征。结果表明:锌-钬抗菌白炭黑结构蓬松,平均粒径为28.948μm,且锌离子和钬离子的添加对载体白炭黑的结构基本没有影响,其抗菌率可达83.41%。     

Precipitation of Zinc Sulfide Particles from Homogeneous Solutions

Zinc sulfide particles were homogeneously precipitated by thermal decomposition of thioacetamide in acidic aqueous solutions in a one-step process. The influence of the operating conditions (initial concentration of zinc ion and TAA) on the nucleation time and number concentration of the generated particles was investigated. The experimental results show that the model of homogeneous nucleation previously developed and successfully tested for silver particle generation by a chemical reduction method can also be applied to the formation of zinc sulfide particles by homogeneous precipitation. Furthermore, in the particle formation method in which the nucleation time t* can be measured, the particle number concentration n* can be predicted by the simple relation n*=1/(4pir*Dt*) (r* is the critical nucleus radius, and D the monomer diffusion coefficient). Thus the particle number concentration can be easily predicted even if the rate expression and the critical supersaturation concentration are unknown. Copyright 2000 Academic Press.     

Spectroscopic study on the zinc-contaminated soils for the determination of zinc speciation

The purpose of this paper reported the zinc species in the highly contaminated soils from metallurgical area around Erh-Jen River in the southern of Taiwan. FTIR and XPS were used to investigate the zinc species in the contaminated soils. Through a FTIR analysis, appreciable of zinc bound by organic matter was found and their bonding structure consisted of antisymmetric and symmetric stretchings, Zn-HSsym and Zn-HSasym. With XPS analysis, the Angstrom scale depth scan was surveyed for investigation the zinc speciation. No signal of zinc was detected in the depth of 900A for the larger particle contaminated soils whereas the detectable signal of zinc was determined in the XPS experiment. With further regression and fitting results, the major zinc species presented in the surface of larger and fine particle contaminated soils consisted of reductive and oxidative zinc species. In the deeper depth of contaminated soils, an inverse spinel zinc ferrite was found in the case of larger particle soil. No inverse spinel zinc ferrite was detected in the case of fine particle soil and could be attributed to the relatively small particle size.     

壳聚糖对Zn2+的吸附性能研究

本文用壳聚糖对Ｚｎ＾２＋的吸附条件进行了研究,探讨了脱乙酰度,分子量,粒度大小,溶液的ｐＨ值,温度,Ｚｎ＾２＋起始浓度和不同锌盐等方面对壳聚糖吸附性能的影响。结果表明：壳聚糖对Ｚｎ＾２＋的吸附具有Ｌａｎｇｍｕｉｒ吸附特征,其吸附最佳条件是壳聚糖脱乙酰度为１００％,锌盐为硫酸锌,Ｚｎ＾２＋溶液ｐＨ值为６．０,起始浓度４－５ｍｇ／ｍｌ。     

Bioleaching of Zinc and Iron from Steel Plant Waste using <Emphasis Type="Italic">Acidithiobacillus Ferrooxidans</Emphasis>

The bacterial leaching of zinc and iron from solid wastes at the Isdemir iron and steel plant has been investigated using Acidithiobacillus ferrooxidans as the bacterial agent. The effects of a range of operational parameters, including particle size, solids concentration and pH, on the efficiency of the bioleaching process were investigated. In each test, several variables were determined to assess the efficiency of leaching, including slurry pH and redox potential, temperature, bacteria population and concentrations of zinc and iron in solution. Experimental results demonstrated that pulp solids concentration, slurry pH and solids particle size were all important parameters in the bacterial leaching process. Maximum extraction was achieved at pH values around 1.3 and a solids concentration of 1% w/v, with 35% of the Zn content and 37% of the Fe being dissolved.     

基于单颗粒电感耦合等离子体质谱法测定环境基质水样中纳米银颗粒

采用单颗粒电感耦合等离子体质谱法(SP-ICP-MS)同时测定环境水样中纳米银颗粒(AgNPs)的颗粒浓度、质量浓度和粒径分布,并考察了溶液的pH值、溶解性有机质(DOM)浓度以及离子强度等对AgNPs测定的影响。结果表明:SP-ICP-MS方法对60 nm AgNPs标准溶液的测定结果与标准值一致,准确性较好;pH值(5.0～7.0)、离子强度(≤1 mmol/L)和DOM浓度(≤30 mg/L)对测定结果影响较小;当溶液的pH值≤5.0或离子强度1 mmol/L时,AgNPs的颗粒浓度和粒径随pH值的下降或离子强度的增强而减小。采用SP-ICP-MS方法测定河水、染料废水、养殖废水3种水样中AgNPs的加标回收率分别为98.1%、83.3%和93.3%,表明该方法在合适的基质条件下可用于快速准确测定环境水样中AgNPs的颗粒浓度、质量浓度和粒径分布。     

Aqueous pathways for the formation of zinc oxide nanoparticles

We examine the effect of reactant concentrations, temperatures and feeding methods on the morphology of ZnO formed when reacting solutions of ZnSO(4) and NaOH. The catalytic effect of hydroxide in excess relative to the stoichiometric ratio is considered. It is shown that, having fixed other reaction conditions, the end-products, particle structures and size strongly depend on the mole ratio of the precursors. The presence of zinc salt hydroxide species was confirmed at sub-stoichiometric ratios in slightly acidic conditions. At the stoichiometric ratio both zinc hydroxide and zinc oxide are formed, while only zinc oxide forms in an excess of hydroxide. The method of feeding the reactants into the reaction vessel also has a strong influence on the end-product properties, as does the reaction temperature. By control of these parameters the specific surface area could be varied from 10 to 33 m(2) g(-1), the particle shape could be varied from equiaxed, through to star-like and needle-like, and the particle size may be varied from 50 to over 300 nm.     

Adsorption mechanism and dispersion efficiency of three anionic additives [poly(acrylic acid), poly(styrene sulfonate) and HEDP] on zinc oxide

Adsorption on ZnO of sodium poly(acrylate) (PAA), sodium poly(styrene sulfonate) (PSS) and a monomer surfactant [hydroxyethylidene diphosphonate (HEDP)] was investigated in suspensions initially equilibrated at pH 7. Results demonstrate interplay in the adsorption mechanism between zinc complexation, salt precipitation, and ZnO dissolution. In the case of PAA, the adsorption isotherm exhibits a maximum attributed to the precipitation of zinc polyacrylate. PSS and HEDP formed high-affinity adsorption isotherms, but the plateau adsorption of HEDP was significantly lower than that of PSS. The adsorption isotherm of each additive is divided into two areas. At low additive concentration (high zinc/additive ratio), the total zinc concentration in the solution decreased and the pH increased upon addition. At a higher additive ratio, zinc concentration and pH increased with the organic concentration. The increase in pH is due to the displacement of hydroxyl ions from the surface and the increase in zinc concentration results from the dissolution of ZnO due to the complexation of zinc ions by the organics. The stability of the ZnO dispersions was investigated by measurement of the particle size distribution after addition of various amounts of polymers. The three additives stabilized the ZnO dispersions efficiently once full surface coverage was reached.     

一维有序ZnO纳米棒阵列的制备和优化

以氧化铟锡透明导电膜玻璃(ITO)做载体,先在室温下采用浸渍-提拉法制备出ZnO纳米晶作为种子层,再结合低成本的水热生长法合成了一维有序的ZnO纳米棒阵列.结合X射线衍射(XRD)、扫描电子显微镜(SEM)和能量色散谱仪(EDS)表征,研究了前驱液浓度、溶胶陈化时间、种子层提拉次数、水热生长时间和次数等5种因素对ZnO纳米棒的结构及形貌的影响.研究结果表明, ZnO纳米棒阵列的长度和直径会随着前驱液的浓度和溶胶陈化时间以及水热生长时间的延长而增加.当前驱液浓度为0.5 mol·L^-1时,陈化时间为24 h,浸渍-提拉3次,水热反应3次,每次反应时间为150 min时,可得到一维有序的ZnO纳米棒阵列.     

Production of Zinc-Doped Yttrium Ferrite Nanopowders by the Sol–Gel Method

Zinc-doped yttrium orthoferrite nanocrystals having the perovskite structure were prepared by coprecipitation of yttrium, zinc, and iron hydroxides. The limiting zinc doping level of the yttrium ferrite to yield a ZnFe₂O₄ spinel second phase was determined. The yttrium orthoferrite particle size was found to be a nonmonotone function of dopant concentration. The specific magnetization of yttrium ferrite nanocrystals increases with increasing zinc doping level from 0.242 A m²/kg (in undoped YFeO₃) to 1.327 A m²/kg (the ratio (1–x)YFeO₃: xZn (x = 0.4)) at Т = 300 K in 1250-kA/m field. A zinc ferrite impurity in samples enhances the ferromagnetism of the material.     

Extraction and determination of zinc in pharmaceutical samples

A systematic study of extraction of zinc salicylate is reported. Optimum conditions for the extraction and determination of zinc are evaluated from a critical study of the effect of pH, sodium salicylate concentration and triphenylphosphine oxide concentration. The effect of foreign ions on the extraction is also discussed. The probable composition of the species has been deduced from the extraction data. The method has been used to separate zinc from cadmium and mercury in binary mixtures and for the determination of zinc in various pharmaceutical products.     

Spherical Zinc Oxide Nano Particles from Zinc Acetate in the Precipitation Method

The liquid precipitation method using zinc acetate dihydrate was applied for the synthesis of uniform and spherical ZnO nanoparticles. The ultrafine zinc oxid was prepared in a water‐ethanol mixture solution. The solution containing zinc cation was soluble in water. The surface‐active agent triethanolamine (TEA) was soluble in ethanol. Then alkali precipitated by adding n‐propylamine. The spherical zinc oxide particle morphology was found to be highly dependent on the zinc salt concentration, ethanol‐water ratio, and the surface‐active agent additive. The process can produce white ZnO powder of 50–90 nm in size. The morphology of zinc oxide showed a powder shape by transmission electron microscopy (TEM), the crystallization phase structure of zinc oxide by X‐ray diffraction (XRD), and the zinc oxide remaining by using an organic analysis by infrared spectroscopy (IR).     

原子捕集-导数火焰原子吸收光谱法测定中草药中的微量锌

提出了原子捕集－导数火焰原子吸收光谱法，考察了捕集管位置，火焰状态、冷却水流量、捕集时间、导数测量系统灵敏度档等实验条件对灵敏度的影响。在测量系统20mV/min灵敏度档下，捕集5min，特征浓度为0．037ng/mL，较常规火焰原子吸收光谱法提高了1243倍。     

Early stages of ZnS growth studied by stopped-flow UV absorption spectroscopy: effects of educt concentrations on the nanoparticle formation

The growth of ZnS nanoparticles by precipitation from supersaturated aqueous solution is studied by stopped-flow UV absorption spectroscopy. The average size, size distribution, and concentration of the particles are monitored within the sub-second time regime with a resolution of 1.28 ms. Particle growth at these early stages is governed by pronounced ripening. The UV absorption data strongly suggest that growth occurs by preferential adsorption of HS- anions relative to Zn(2+) or ZnOH(+) cations. Correspondingly, the initial sulfide concentration has a much more pronounced influence on the growth kinetics than the initial zinc concentration. These findings are verified by zeta-potential measurements which confirm that the particle surfaces are negatively charged under near-neutral pH conditions.     

Detailed investigations of ZnO photoelectrodes preparation for dye sensitized solar cells

Wurtzite ZnO hexagonal nanopyramids were successfully synthesized in the liquid phase from homogeneous methanolic solutions of zinc acetate and tetramethylammonium hydroxide at an excess of zinc ions. The formation and properties of the nanocrystals were examined as a function of synthesis conditions. No significant influence of the [Zn(2+)]/[OH(-)] ratio was noticed on the final particle size, in spite of increased amounts of OH(-) ions, which tend to accelerate the particle nucleation and growth. Nevertheless, the reactant concentration ratio influences the surface properties of the ZnO nanocrystals. Mesoporous ZnO films were prepared by doctor blading ethanolic pastes containing ZnO nanoparticles and ethyl cellulose onto FTO conductive glass substrate followed by calcination. Additionally, the influence of a plasticizer (triacetin)-used during the paste preparation-on the film quality was investigated. A higher content of ZnO nanoparticles and plasticizer in the pastes improved the film quality. Four different temperatures (i.e., 400, 425, 450, and 475 °C) were used for the film calcination and their influence on the structural properties of the films was characterized. In principle, increasing the calcination temperature goes hand in hand with an increase of particle size, as well as the pore diameter and reduction of the surface area. Suitable mesoporous films were employed as photoanodes in dye sensitized solar cells (DSSCs). In order to assess the effect of the varied parameters on complete DSSC devices-using cis-diisothiocyanato-bis(2,2'-bipyridyl-4,4'-dicarboxylato) ruthenium(II)bis(tetrabutylammonium (N719) as a sensitizer-incident photon to current efficiency (IPCE) and current voltage measurements were carried out. The IPCE measurements confirmed photoinduced electron injection from the dye, reaching IPCE values up to 76%. Furthermore, current-voltage characteristics of complete cells emphasized the importance of the proper preparation methods and temperatures. These features are important assets for the preparation of nanocrystalline ZnO based photoelectrodes and for improving the DSSC performance.     

Surface and capillary forces encountered by zinc sulfide microspheres in aqueous electrolyte

The colloid probe technique was used to investigate the interactions between individual zinc sulfide (ZnS) microspheres and an air bubble in electrolyte solution. Incorporation of zinc ions into the electrolyte solution overcomes the disproportionate zinc ion dissolution and mimics high-volume-fraction conditions common in flotation. Determined interaction forces revealed a distinct lack of long-ranged hydrophobic forces, indicated by the presence of a DLVO repulsion prior to particle engulfment. Single microsphere contact angles were determined from particle-bubble interactions. Contact angles increased with decreasing radii and with surface oxidation. Surface modification by the absorption of copper and subsequently potassium O-ethyldithiocarbonate (KED) reduced repulsive forces and strongly increased contact angles.     

Facile chemical approach to ZnO submicrometer particles with controllable morphologies

We have developed a simple wet-chemistry approach to fabricating ZnO submicrometer particles with unique morphologies including rings, bowls, hemispheres, and disks. The size and morphology of the particles can be conveniently tailored by varying the concentrations of the zinc precursor. The reaction temperature, pH, and concentration of ammonia are also found to play critical roles in directing the formation of these particle morphologies. These submicrometer particles exhibit strong white-light emission upon UV excitation as a result of the presence of surface defect states resulting from the fabrication method and synthesis conditions.     

BDIE·[Zn-Al]催化二氧化碳与氧化环己烯的共聚反应

用α二亚胺型BDIE配体(N,N′(2,6二异丙基苯基)乙二亚胺)与氧联锌铝醇盐([ZnAl])以配位的方式制备了高位阻催化体系BDIE·[ZnAl],并催化二氧化碳与氧化环己烯共聚.研究了各种因素对该反应的影响,发现最适宜的反应条件为BDIE[ZnAl]的摩尔比为0.5、反应温度为80℃、催化剂浓度为0.1gmL、二氧化碳压力为2MPa.在此条件下反应24h其催化效率达到31.6gg与其它高位阻体系相比,该催化剂用成本低的异丙醇铝和无水醋酸锌代替二乙锌,聚合操作过程简单,是一种有发展前景的催化体系.     

Zinc sulfide nanoparticles: a mechanism of formation in aqueous solutions and optical properties

The formation of sols and precipitates of zinc sulfide as a result of the exchange reaction in an aqueous solution was studied. The precipitates consist of aggregates of primary particles about 3 nm in size. The primary ZnS particle size in aqueous sols increases with an increase in the concentration of zinc sulfate and sodium sulfide, with the accumulation of the final reaction product, and with temperature. This effect does not exceed an 1.5-fold increase. At the first step, the particles with a considerable fraction of the amorphous phase are formed and undergo intragrain crystallization. The photoluminescence properties of aqueous sols of zinc sulfide were studied. They are caused by defects in the ZnS lattice and by the presence of the lattice oxygen.     

Particle Emission from Welding of Painted Steel

The particulate emission caused by welding of steel plates covered with 29 diversified shop primers has been investigated. The investigation includes the determination of particle mass, particle size distribution, and of the contents of heavy metals such as lead and cadmium. The results show that all investigated primers except those with high concentration of zinc pigment produce mass emissions which are very low in comparison to manual arc welding with covered electrode and CO₂-welding on uncoated steel. The emitted particles of the primers are smaller than 1 μm particle diameter and therefore respirable. Lead and cadmium was found in particles emitted during the welding process of all investigated primers. The highest amount was found in particles of primers with high contents of zinc and ferric oxide.