Reactive sintering of zinc ferrite

The reactive sintering of zinc ferrite, i.e. firing without previously calcining, has been studied using three types of iron oxide. The conversion into ferrite as well as the simultaneous densification were investigated upon variations in morphology and impurity content. The formation reaction is shown to be accompanied by a strong increase of the median pore size. This phenomenon appears responsible for the generally smaller density of the final material as compared with single-phase sintering. It is shown that reactive sintering is inevitably accompanied by expansion, irrespective of molecular volume variations. A calcining step appears indispensable for the preparation of the highest quality of ferrites.     

Effect of calcining temperature on particle size of hydroxyapatite synthesized by solid-state reaction at room temperature

Using diammonium phosphate, calcium nitrate tetrahydrate and sodium bicarbonate as raw materials, hydroxyapatite (HAP) was facilely synthesized by solid-state reaction at room temperature. The crystallinity, phase, morphology and particle size of the products were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FT-IR), thermogravimetry/differential thermal analysis (TG–DTA) and particle size analyzer. The influence of calcining temperature on the crystallinity and composition of HAP phase was also investigated.     

纳米氧化锌-煅烧高岭土复合材料的制备

以煅烧高岭土和纳米氧化锌为主要原料,用水解沉淀法在煅烧高岭土表面包覆纳米氧化锌,制备一种无机复合型抗紫外材料;采用分光光度计分别测定在波长325、350、375、400nm紫外光下复合材料的紫外光吸光度。结果表明:反应温度、氧化锌包覆量、改性时间、改性剂滴加速度、矿浆浓度、煅烧温度等对纳米氧化锌-煅烧高岭土复合粉体材料的紫外光吸收性能有重要影响。在制备条件为:氧化锌包覆量为8%、反应温度为90℃、改性时间为10min、改性剂滴加速度为3mL/min、矿浆中m(水)∶m(煅烧高岭土)=10∶1、煅烧温度为400℃时,所制备的纳米氧化锌-煅烧高岭土复合粉体材料的紫外光吸收性能较好。     

晶体生长用TiO2纳米晶的改良工艺研究

针对晶体生长的具体应用,分别以硫酸氧钛铵（ATS）和改良硫酸氧钛铵（M－ATS）为原料,采用高温焙烧法制备了TiO2纳米晶,用XRD分析了原料和纳米晶的物相,用SEM分析了纳米晶的形貌,结果表明虽然两种原料具有相似的物相结构,但所得纳米晶的性状不同,M－ATS焙烧所得纳米晶分散性更高,均匀性更好,此外,研究了焙烧温度,保温时间,急烧,缓烧等工艺条件对纳米晶形貌,物相的影响,并给出了批量制备TiO2纳米晶粉体的最佳工艺条件。     

Low-firing binders from magnesium containing carbonate raw materials

This paper presents scientific and experimental data for low-firing hydraulic binders: hydraulic lime and Roman cement based on local mineral raw materials. The binders were prepared by firing representative samples of carbonate–clay magnesian raw materials from Tatarstan. Using X-ray diffraction, we identified the firing products, including a hydraulically active phase, and determined the structural characteristics of its minerals. The compositions of the binders were determined as functions of firing conditions. We examined the influence of the firing temperature and duration of magnesian raw materials in the preparation of binders on MgO activity and demonstrated for the first time the possibility of ensuring an active state of the MgO resulting from firing (up to 21%) and suppressing its negative effect on Roman cement and hydraulic lime hardening processes.     

Preparation and characterization of NiO nanoparticles through calcination of malate gel

NiO nanoparticles have been successfully prepared by calcining malate gel, using basic nickel carbonate (BNC) and malic acid as the raw materials and H₂O as the solvent. The reaction was studied by TG–DTA, XRD and FT-IR. The particle size and morphology of NiO nanoparticles was characterized by TEM. The results show that nickel malate could be formed by the reaction of BNC and malic acid; the gel was composed of nickel malate and residual malic acid; the precursor can translate into NiO nanoparticles completely at 400 °C under the air, and the as-prepared sample has a cubic crystal structure with about 14 nm of average diameter by the Scherrer formula. The NiO calcined at 400 °C for 1 h was of narrow particle size distribution, weak agglomeration and small particle size. The particle size of NiO increased with the increase in temperature. Compared with other methods, the developed method is simple and the raw materials were inexpensive, so that it has the potential for further scale-up application in the industry. Furthermore, the reason for the metallic nickel formation in the course of the preparation was explained.     

低温燃烧合成法制备纳米NiFe_2O_4

以九水硝酸铁、六水硝酸镍、水溶性肼类燃料为原料,添加金属离子络合剂、分散剂等为辅助剂,利用溶液燃烧合成法制备了纳米NiFe2O4粉体。利用XRD、TEM、SEM等测试方法对产物进行了表征,并研究了不同燃料、络合剂用量、分散剂用量、煅烧温度对粉体粒径和形貌的影响。实验结果表明,在以水溶性肼为燃料、络合剂2g、分散剂2g、煅烧温度800℃、煅烧时间2h时,可获得粒径均匀的纳米NiFe2O4粉体。所得产物的粒径范围为40～80nm,结构膨松,分散性良好。     

PbTiO3纳米晶的制备及表征

以硬脂酸、乙酸铅和钛酸丁酯为原料用硬脂酸凝胶法合成ＰｂＴｉＯ３纳米晶原粉，利用改进的烧结设备，同时采用Ｎ２气氛下预烧，通过调节Ｎ２和Ｏ２的流量控制烧结气氛，得到粒径重复性好的ＰｂＴｉＯ３纳米晶，用差热分析，热重分析和Ｘ－射线衍射对合成过程进行了研究，用透射电镜考查纳米晶的粒度和形貌，用５ＤＸ－红外光谱仪对ＰｂＴｉＯ３纳米晶的红外透射谱进行了测试分析。     

工艺参数对醇法制备NiO纳米晶粒尺寸的影响

采用醇法,以Ni(NO)2·6H2O和H2C2O4·2H2O为原料,研究了工艺参数如原料选择、煅烧温度、醇的种类、起始浓度、陈化时间等对NiO纳米粉体晶粒尺寸的影响。用XRD,TEM,BET等方法对粉体进行了表征。结果表明,以乙醇为溶剂,成功地制备了粒径约为10nm、分布范围窄、稳定的NiO粉体。而以异丙醇为溶剂时,所得粉体的晶粒更易长大;起始原料浓度越大,粉体的粒径越大;陈化时间越长,粒径越大。     

溶胶一凝胶法制备钒酸铋及其光催化性能研究

采用溶胶一凝胶法制备钒酸铋颗粒光催化剂,研究银掺杂、煅烧温度、煅烧时间对BiVO4晶型组成和催化活性的影响,用X射线衍射（XRD）、透射电镜进行表征,研究了BiVO4粉体在焙烧过程中的相转变,确定了煅烧温度、煅烧时间及掺杂比例;以甲基橙（MO）的可见光催化降解反应为探针,研究了催化剂的可见光催化性能,研究发现,当煅烧时间为4h,煅烧温度为500℃时,BiV04对甲基橙光催化效率可达约20％。银掺杂的BiVO4对基橙光催化效率可达约40％。     

废玻璃再生利用制备长余辉蓄光釉面砖及其性能的研究

利用传统陶瓷制备方法合成了SrAl2O4:Eu,Dy长余辉发光粉体,该磷光体主发射波长位于520nm,余辉时间长达20h以上,将发光粉掺入适量的低熔点玻璃料,经780℃烧成30min合成了性能较好的低温发光釉料,以废玻璃,粘土为主要原料添加其它少量助剂,经过成型,预烧,将低发光釉料涂覆在其上,在一定温度下烧成,制得长余辉蓄光釉面砖。     

金红石生长用TiO2纳米晶粉体制备及表征

针对金红石晶体生长所需,我们人工合成了硫酸氧钛铵（ATS）晶体。并以其为原料,采用高温焙烧法制备了TiO2纳米晶粉体,用XRD、SEM和TEM分析了纳米晶的物相和形貌。结果表明所得TiO2纳米晶粉体分散性好、流动性好、纯度高且颗粒细小均匀。此外,研究了焙烧温度、保温时间和急烧、缓烧等工艺参数对其形貌、物相的影响,给出了大批是生产TiO2纳米晶粉体的最佳工艺条件。     

Compaction pressure effects in the firing of self-vitrifying ceramic materials

The firing behaviour of two self-vitrifying ceramic materials, coming from a magmatic rock of the aplite type consisting basically of quartz, feldspar and kaolin, both in the raw and purified (iron-free) state, were investigated as a function of the compacting pressure over the range 14 to 280 MN m^–2. The materials exhibit a linear relationship of firing shrinkage versus the logarithm of the cold compacting pressures in the temperature range where vitrification processes occur, while the linearity falls down outside this range. The iron oxide content lowers the vitrification temperature as well as the vitrification range. The observed linear relationship is quite similar to that exhibited by other self-vitrifying ceramic materials for wall and floor tiles previously investigated, and it does not seem to depend on the compacting characteristics of the powders. It has therefore to be related to the gradually growing glassy phases which arise during firing at increasing temperatures. This relationship may thus be considered as a general characteristic of the firing behaviour of strongly self-vitrifying ceramic materials when subjected to green density changes.     

Semiconducting ceramics produced using nanocrystalline barium titanate powder

Positive temperature coefficient of resistance ceramics of composition (Ba_0.89Ca_0.08Pb_0.03)TiO₃ + Y₂O₃ + MnO + SiO₂ have been produced using barium titanate powder with an average crystallite size of 125 nm prepared by calcining barium titanyl oxalate at 900°C. The effect of firing temperature on their microstructure and electrical properties has been studied. The results demonstrate that the ceramics possess semiconducting properties starting at a firing temperature of 1205–1215°C. The room-temperature resistivity of the ceramics has a minimum at t _firing ≈ 1245–1250°C. The samples sintered at 1250–1260°C have the largest positive temperature coefficient of resistance. The highest electric strength (360 V/mm at ρ_25°C = 290 Ω cm) is offered by the thermistor materials sintered at 1260°C, which is 60–70°C below the firing temperature of analogous ceramics produced by solid-state reaction.     

硅藻土微粒负载纳米TiO2的制备

以硫酸氧钛为原料,硅藻土微粒为载体,尿素为沉淀剂,通过改变硫酸氧钛的浓度、硅藻土与二氧化钛质量比、尿素浓度、pH值、水解温度、反应时间和焙烧温度等工艺条件,采用混合均匀沉淀法制备出了硅藻土基负载型纳米二氧化钛．利用SEM和XRD对样品的结构性能进行测定,得出在最佳制备条件下,二氧化钛在硅藻土表面的最大覆盖率为75％,二氧化钛平均粒径为150nm,并初步探讨了二氧化钛粒子和载体之间的结合机理．该产品对模拟室内甲醛的降解实验表明,在可见光范围内本产品对甲醛的处理效果是明显的。     

Preparation and reactivity of lead zirconate-titanate solid solutions produced by precipitation from aqueous solutions

A process for preparation of PZT by precipitation from butoxide precursors is described. The reactivity of the powders during low temperature firing (calcining) has been determined using weight loss, x-ray diffraction, and DTA-TGA techniques.     

碱性条件下介孔三氧化钨的合成与表征

以CTAB为模板剂,钨酸钠为反应物前体,在碱性条件下,用室温法和水热法合成了介孔三氧化钨。X射线衍射分析表明,室温条件下生成的是层状相的介孔材料,而在水热条件下可生成六方相的介孔结构,最适宜的水热时间为2天,水热温度为110℃。400℃煅烧处理后,介孔结构基本坍塌。     

Molten salts synthesis and electrical properties of Sr- and/or Mg-doped perovskite-type LaAlO3 powders

Lanthanum-based LaBO₃ oxides adopting the very stable perovskite structure are currently considered attractive materials for a growing number of applications in the field of solid-state ionics. In particular, LaAlO₃-based perovskites are promising electrolyte materials for solid oxide fuel cells because they show almost pure oxygen ion conductivity at low oxygen partial pressures and high temperatures as well as excellent thermal and chemical stability under the standard operating conditions. This article describes a low-temperature synthesis of pure and acceptor-doped perovskite-type LaAlO₃ nanopowders via a facile and environmental-friendly molten salts method. Using hydrated metal nitrates and sodium hydroxide as raw materials, the proposed methodology consists of two steps: a mechanically induced metathesis reaction and short firing above NaNO₃'s melting point. The purpose of the first is twofold: i.e., to generate in situ the NaNO₃ flux and to obtain a suitable precursor for the synthesis of the target materials in molten nitrates. Accordingly, pure and Mg- and/or Sr-doped LaAlO₃ powders were obtained directly without using any purification step at temperatures ≤500 °C. When preparing the Mg-containing samples, NaNO₂ was also added to the reaction mixture to increase melt reactivity. The formation of the target series in the molten salt is thought to proceed through a “dissolution–precipitation” mechanism with LaAlO₃ particles precipitating during cooling from a solution oversaturated with reactants. Electrical properties of the as-prepared materials were measured as a function of temperature and frequency by means of impedance spectroscopy and found comparable to those shown by similar materials prepared using more complicated routes.     

Fabrication and characterization of porous calcium polyphosphate scaffolds

Porous calcium polyphosphate (CPP) scaffolds with different polymerization degree and crystalline phases were prepared, and then analyzed by scanning electron microscopy (SEM), Thermmogravimetry (TG) and X-ray diffraction (XRD). Number average polymerization degree was calculated by analyzing the calcining process of raw material Ca(H₂PO₄)₂, as a polycondensation reaction. Amorphous CPP were prepared by the quenching from the melt of Ca(H₂PO₄)₂ after calcining, and CPP with different polymerization degree was prepared by controlling the calcining time. Meanwhile, CPP with the same polymerization degree was prepared to amorphous or different crystalline phases CPP which was made from crystallization of amorphous CPP. In vitro degradation studies using 0.1 M of tris-buffered solution were performed to assess the effect of polymerization degree or crystalline phases on mechanical properties and weight loss of the samples. With the increase of polymerization degree, the weight loss during the degradation decreased, contrarily the strength of CPP increased. The degradation velocity of amorphous CPP, α-CPP, β-CPP and γ-CPP with the same polymerization degree decreased in turn at the same period. The full weight loss period of CPP can be controlled between 17 days and more than 1 year. The results of this study suggest that CPP ceramics have potential applications for bone tissue engineering.     

Preparation and mechanism of nanometer Al5O6N via shock wave plasma technique

Cubic Al₅O₆N nanocrystals were successfully synthesized via a novel strategy called shock wave plasma technique, using trinitrotoluene (TNT) and aluminum powder as raw materials and water as protection medium. The precursor including carbon and Al₅O₆N was engendered firstly during the detonation of compound dynamite, and then the pure Al₅O₆N nanoparticles were obtained when the carbon was removed through calcining at high temperature. The precursor and the final as-synthesized Al₅O₆N powder were characterized by X-ray diffraction (XRD), Raman spectrum and high-resolution transmission electron microscope (HRTEM), respectively. The calcining temperature schedule of the precursor was decided through DTA/TG analysis. The results indicate that the precursor consists of 37.7% carbon and 62.3 °C Al₅O₆N. After calcining at 600 °C for 1 h, the average diameter of the as-synthesized Al₅O₆N nanocrystal is 30-40 nm and the morphology micrograph takes on uniform spherical shape. The lattice parameters are consistent completely with the standard cubic Al₅O₆N (JCPDS 48-0686). The well-dispersed Al₅O₆N nanocrystals synthesized by shock wave plasma technique can be attributed to the covering of carbon and fast cooling of water medium. A possible reaction mechanism was also proposed preliminarily based on the experimental results.