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Study of nickel precursors in (Ni,M,Ti)O2 (M = Sb, Nb) yellow ceramic pigments (Ni,M,Ti)O2 (M = Sb, Nb)黄色陶瓷颜料中镍前驱体的研究
Pub Date : 2004-02-01 DOI: 10.1179/096797804225012710
S. Šorli, M. A. Tena, J. Badenes, M. Llusar, G. Monrós
Abstract NixTi1 - 3xM2xO2 (M = Sb, Nb; 0·05 ≤ x ≤ 0·10) samples have been synthesised from mixtures of NiO, Nb2O5, Sb2O3, and TiO2. From characterisation of these samples, x = 0·05 was chosen to compare results with different nickel precursors. Thus samples of Ni0·05Ti0·85M0·10O2 (M = Sb, Nb) were also prepared from NiCO3.3Ni(OH)2.4H2O, NiCl2.6H2O, Ni(NO3)2.6H2O, NiSO4.6H2O, and Ni(CH3COO)2.4H2O. A eutectic mixture of alkaline halides (NaF:2NaCl) was used as fluxing agent. Optimal yellow colour was found in the mixture of NiSO4.6H2O, Sb2O5, and TiO2 fired at 1100°C for 2 h.
NixTi1 - 3xM2xO2 (M = Sb, Nb;用NiO、Nb2O5、Sb2O3和TiO2的混合物合成了0.05≤x≤0.10的样品。从这些样品的表征中,选择x = 0·05来比较不同镍前驱体的结果。以NiCO3.3Ni(OH)2.4H2O、NiCl2.6H2O、Ni(NO3)2.6H2O、NiSO4.6H2O、Ni(CH3COO)2.4H2O为原料制备了Ni0·05Ti0·85M0·10O2 (M = Sb, Nb)样品。采用碱性卤化物共晶混合物(NaF:2NaCl)作为助熔剂。在NiSO4.6H2O, Sb2O5和TiO2的混合物中,在1100℃下焙烧2 h,发现最佳的黄色。
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引用次数: 7
Composition of Al2O3-W-WC composite prepared by WO3-Al reaction under coke 焦炭下WO3-Al反应制备的Al2O3-W-WC复合材料的组成
Pub Date : 2004-02-01 DOI: 10.1179/096797804225012684
B. Han, N. Li
Abstract Pellets pressed from WO3, Al, and fused Al2O3 powder mixes according to the stoichiometry 3Al + WO3 + xAl2O3 = (x + 1)Al2O3 + W (x = 0·1-0·5) were heated at 1473, 1623, and 1773 K for 3 h under coke granules. The composition and microstructure of samples were examined by X-ray diffraction analysis, scanning electron microscopy, and energy dispersive X-ray analysis. The products of the Al-WO3 reaction were found to consist of tungsten, corundum, and tungsten carbides. For x ≤ 0·3, temperature had little effect on the X-ray intensity ratios (IWC(101) + IW2C(101)) / IW(101) and IWC(101) / IW2C(101), whereas at x = 0·5 the influence of temperature was significant. Tungsten was converted to tungsten carbides in the samples heated at 1773 K. High temperature improved diffusion in the tungsten carbide layer and promoted the transformations from W to WC and from W2C to WC. Sintering of the corundum and tungsten resulted in cracks that provided rapid diffusion pathways for CO to penetrate and react with W.
根据3Al + WO3 + xAl2O3 = (x + 1)Al2O3 + W (x = 0·1 ~ 0·5)的化学计量量,将WO3、Al和熔融Al2O3粉末混合物压成球,在1473、1623和1773 K下在焦炭颗粒下加热3 h。采用x射线衍射分析、扫描电镜和能量色散x射线分析对样品的组成和微观结构进行了研究。Al-WO3反应的产物由钨、刚玉和碳化钨组成。当x≤0.3时,温度对x射线强度比(IWC(101) + IW2C(101)) / IW(101)和IWC(101) / IW2C(101))影响不大,而在x = 0.5时,温度对x射线强度比的影响显著。在1773 K温度下,钨转化为碳化钨。高温促进了碳化钨层内的扩散,促进了W向WC和W2C向WC的转变。刚玉和钨的烧结产生裂纹,为CO渗透和与W反应提供了快速扩散途径。
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引用次数: 1
Kinetic study of black (Fe,Cr)2O3 pigment synthesis reaction: influence of composition and particle size 黑色(Fe,Cr)2O3颜料合成反应动力学研究:组分和粒度的影响
Pub Date : 2003-12-01 DOI: 10.1179/096797803225009300
A. Escardino, S. Mestre, A. Barba, C. Feliu, A. Blasco, V. Beltrán
Abstract The influence of initial Fe2O3-Cr2O3 mixture particle size and composition on the black (Fe,Cr)2O3 pigment synthesis reaction has been studied. An empirical equation is proposed, based on a mathematical expression derived in a previous study,which relates these variables to resulting pigment mass fraction, synthesis time, and temperature in the studied range of operating conditions.
摘要研究了初始Fe2O3-Cr2O3混合物粒度和组成对黑色(Fe,Cr)2O3颜料合成反应的影响。根据先前研究中导出的数学表达式,提出了一个经验方程,该方程将这些变量与所研究的操作条件范围内产生的颜料质量分数,合成时间和温度联系起来。
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引用次数: 3
Colorimetric study of black (Fe,Cr)2O3 pigment synthesis reaction: relation between chromatic coordinates and synthesis conditions 黑色(Fe,Cr)2O3颜料合成反应的比色法研究:色坐标与合成条件的关系
Pub Date : 2003-12-01 DOI: 10.1179/096797803225009292
A. Escardino, S. Mestre, A. Barba, M. Monzó, A. Blasco, V. Beltrán
Abstract Samples of black (Fe,Cr)2O3 pigment were prepared from a starting mixture of Fe2O3 and Cr2O3 (50:50 by weight) at five temperatures between 1273 and 1423 K, using synthesis times ranging from 0 to 9 h. The influence of synthesis temperature and time on the chromatic coordinates of the pigment samples was established, and their chromatic coordinates were determined. On the basis of the experimental results, a single empirical correlation was obtained between each of the chromatic coordinates and the mass fraction in solid solution of the same composition as the starting oxide mixture present in each pigment sample.
以Fe2O3和Cr2O3(质量比为50:50)的起始混合物为原料,在1273 ~ 1423 K的5种温度下,合成时间0 ~ 9 h,制备了黑色(Fe,Cr)2O3颜料样品。建立了合成温度和合成时间对颜料样品色坐标的影响,并测定了颜料样品的色坐标。在实验结果的基础上,获得了每个色坐标与每个颜料样品中存在的起始氧化物混合物组成相同的固溶体中的质量分数之间的单个经验相关性。
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引用次数: 6
Characterisation of mechanically alloyed Ti–Al–B nanocomposite consolidated by spark plasma sintering 火花等离子烧结固结机械合金Ti-Al-B纳米复合材料的表征
Pub Date : 2003-12-01 DOI: 10.1179/096797803225009319
H. B. Lee, S. Kim, S. Kang, Y. Han
Abstract The microstructure and mechanical properties of TiB2/Al nanocomposites based on the Ti-Al-B system, consolidated by spark plasma sintering of mechanically alloyed activated nanopowders, have been characterised. Mechanical alloying was carried out in a planetary ball mill for 120-180 min at 350 rev min-1. The powders were pressed in vacuum at a pressure of 60 MPa; a dc current of 1800 A was applied for 4 min, generating a maximum temperature in the graphite mould of 1400° C. Analysis of the synthesised nanocomposites by SEM, XRD, and TEM showed them to consist of TiB2 second phase particles, 10-30 nm in size, in a near amorphous Al phase, with unreacted Ti and B on grain boundaries as a ternary phase. Composites consolidated from powders mechanically alloyed from an initial elemental powder mix of 0·3 mol Al, 0·7 mol Ti, and 2·0 mol B achieved the best relative density (98%) and bending strength (847 MPa); the highest Vickers hardness of 19·6 GPa was achieved for the 0·1:0·9:2·0 mol starting composition.
摘要:研究了Ti-Al-B体系的TiB2/Al纳米复合材料的微观结构和力学性能。机械合金化在行星球磨机上进行,转速350 min-1,合金化120 ~ 180 min。粉末在60 MPa的压力下真空压制;通过SEM、XRD和TEM对合成的纳米复合材料进行了分析,结果表明,合成的纳米复合材料由TiB2第二相颗粒组成,尺寸为10 ~ 30 nm,为近无定形Al相,晶界上未反应的Ti和B为三元相。以0.3 mol Al、0.7 mol Ti和2.0 mol B的初始元素粉末混合而成的机械合金粉末固结复合材料的相对密度(98%)和抗弯强度(847 MPa)最佳;当起始组分为0·1:0·9:2·0 mol时,其维氏硬度最高,为19.6 GPa。
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引用次数: 12
Preparation and characterisation of low fusion leucite dental porcelain 低熔合白晶石牙科瓷的制备与表征
Pub Date : 2003-12-01 DOI: 10.1179/096797803225009337
E. El-Meliegy
Abstract Low fusion leucite containing dental porcelain was prepared from Egyptian feldspar and talc raw materials by firing for 6 min at 800-950° C. Porcelain frit was first made through fusion of the respective formulations at temperatures between 1100 and 1300° C and then poured into a cold stream of water. The frit was milled to pass a 75 μm sieve. Thermal expansion was followed using a dilatometer. The crystallisation of leucite was regulated by adjusting the rate of heating and by addition of nucleating agents. The main mineral phase developed is the tetragonal leucite form. The amount of crystallised leucite was monitored to control the translucency of the porcelain. Thermal expansion coefficient was in the range 10·0-14·5 × 10-6 K-1 (20-500° C). Microstructure was investigated using SEM.
以埃及长石和滑石为原料,在800 ~ 950℃下烧制6 min,制备低熔点含牙瓷的白晶石瓷块,分别在1100 ~ 1300℃的温度下熔制瓷块,然后倒入冷水中。将熔块磨成75 μm筛子。用膨胀计跟踪热膨胀。通过调节加热速率和加入成核剂来调节白晶石的结晶。主要发育的矿物相为四方白晶石形态。通过监测白晶石的结晶量来控制瓷器的透明度。热膨胀系数在10·0 ~ 14·5 × 10-6 K-1(20 ~ 500℃)范围内。
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引用次数: 16
Laser dressing of vitrified aluminium oxide grinding wheels 玻璃化氧化铝砂轮的激光修整
Pub Date : 2003-12-01 DOI: 10.1179/096797803225009346
M. Jackson, G. Robinson, N. Dahotre, A. Khangar, R. Moss
Abstract Grinding is a manufacturing process that produces engineering components to a desired surface finish. In continuous grinding operations, the grinding efficiency of vitrified grinding wheels deteriorates as the sharp cutting edges become blunt as a result of the formation of wear flats. Dressing is essentially a sharpening operation which addresses this problem by generating a specific topography on the cutting face of the grinding wheel. High power lasers are being explored as a non-contact dressing technique. In the present study, a high power laser was used to produce a resolidified layer on the surface of vitrified aluminium grinding wheels. The high heat flux intensity produced both solid-solid and solid-liquid phase transformations. Microstructural analysis of the dressed wheel surface showed extensive grain refinement. Microcutting edges are produced on the individual grinding grains. Though a wide grain size distribution was observed, grain shape was more regular (equiaxed), with well defined vertices and edges on each grain. The vertices and edges provide cutting edges for improved grinding at the microscale. Area analysis of surfaces using energy dispersive area analysis (EDAX) revealed the presence of Al, Cr, O, Si, K, and Na. However, X-ray diffractometry on the surface indicated the presence of Al2O3 phase only. The upper resolidified layer contained Si, Na, K, and P, whereas the material below was primarily Al, Cr, and O. This suggests that a glassy phase (with Al, O, Na, K, P, and Si) is formed on the surface. Subsequent laser treatment modified the morphological structure of the vitrified grinding wheel surface, thus creating a dressing effect with locally sculpted microscale cutting edges on each grinding grain. The experimental results indicate that laser modified grinding wheels are comparable in performance to diamond dressed grinding wheels.
磨削是一种制造过程,使工程部件达到所需的表面光洁度。在连续磨削作业中,玻璃化砂轮的磨削效率下降,锋利的切削刃由于形成磨平而变钝。修整本质上是一种锐化操作,它通过在砂轮的切割面上产生特定的地形来解决这个问题。高功率激光作为一种非接触式敷料技术正在被探索。本研究采用高功率激光在玻璃化铝砂轮表面形成再凝固层。高热流密度同时产生固-固相变和固-液相变。修整后的车轮表面的显微组织分析显示出广泛的晶粒细化。在单个磨粒上产生微切削刃。虽然晶粒尺寸分布较宽,但晶粒形状更为规则(等轴),每个晶粒上都有明确的顶点和边缘。顶点和边缘为改善微尺度磨削提供切削刃。使用能量色散面积分析(EDAX)对表面进行面积分析,发现存在Al, Cr, O, Si, K和Na。然而,表面的x射线衍射显示仅存在Al2O3相。上层的再凝固层含有Si、Na、K和P,而下层主要是Al、Cr和O。这表明在表面形成了一个玻璃相(Al、O、Na、K、P和Si)。随后的激光处理改变了玻璃化砂轮表面的形态结构,从而在每个磨粒上产生局部雕刻的微尺度切割边缘的修整效果。实验结果表明,激光修饰砂轮的磨削性能与金刚石修饰砂轮相当。
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引用次数: 37
Vanadium staining in fired clay bricks 烧制粘土砖中的钒染色
Pub Date : 2003-12-01 DOI: 10.1179/096797803225005025
D. Phillips
Abstract This paper reports on a series of efflorescence tests and instrumental techniques that have been used to determine the nature and mechanism of vanadium staining, and the effects of additions of magnesite, calcite, and fluorspar to the brick mix to eliminate the problem. Scanning electron microscopy, electron probe microanalysis, inductively coupled mass spectrometry (with laser ablation attachment), and X-ray photon spectrometry have been used to more fully understand the elemental composition, oxidation states, and formation of vanadium stains in fired clay bricks. It was found that the stains consist of V, K, Na, Mo, S, and O. Vanadium +4 compounds form initially within the brick and are slowly oxidised to vanadium +5 compounds as the water transports the potassium and sodium salts to the brick surface. X-ray diffraction led to a reasonably successful search match for a KVO(SO4)2 phase for the stains. Evolved gas analysis showed loss of vanadium compounds between 700 and 900° C which are most likely VF3 and VCl4. Inductively coupled plasma spectrometry laser ablation studies on thin sections of brick showed areas of glassy phases corresponding to the agglomeration of Mg/V/Al/Si and Mg/Al/Si. The increased alkalinity of magnesia and the comparable sizes of V4+ and Mgions are driving forces for locking vanadium into what is otherwise an acidic glassy phase. The addition of 1 wt-% magnesite to the brick mix led to fired products on a commercial scale that are free from vanadium staining.
摘要:本文报道了用一系列的荧光试验和仪器技术来确定钒染色的性质和机理,以及在混合砖中添加菱镁矿、方解石和萤石来消除钒染色的效果。扫描电子显微镜、电子探针显微分析、电感耦合质谱(激光烧蚀连接)和x射线光子光谱已经被用来更全面地了解烧制粘土砖中钒污点的元素组成、氧化态和形成。发现这些污渍由V、K、Na、Mo、S和o组成。钒+4化合物最初在砖内形成,随着水将钾盐和钠盐运送到砖表面,慢慢氧化成钒+5化合物。x射线衍射导致了对污渍的KVO(SO4)2相相当成功的搜索匹配。演化气体分析表明,在700 ~ 900°C之间,钒化合物的损失最可能是VF3和VCl4。对砖薄片的电感耦合等离子体光谱激光烧蚀研究表明,砖的玻璃相区域对应于Mg/V/Al/Si和Mg/Al/Si的聚集。氧化镁碱度的增加以及V4+和Mgions的大小是将钒锁定在酸性玻璃相中的驱动力。在砖混合物中加入1 wt-%的菱镁矿,可生产出无钒染色的商业规模的烧制产品。
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引用次数: 1
Effect of talc and bauxite on sintering, microstructure, and refractory properties of Egyptian dolomitic magnesite 滑石和铝土矿对埃及白云质菱镁矿烧结、显微结构和耐火性能的影响
Pub Date : 2003-12-01 DOI: 10.1179/096797803225009391
A. Othman
Abstract Refractories produced from mixes of Egyptian dolomitic magnesite with talc and low cost Chinese bauxite have been assessed as potential substitutes for the high temperature basic refractory bricks currently used in steelmaking and other industries. Fifteen batches of different compositions were prepared by firing for 2 h up to 1580° C. Six samples were selected for further investigation on the basis of their phase composition and densification parameters. The mineralogical composition and microstructure, pore size distribution, and mechanical and refractory properties of these samples were investigated. All six samples consisted mainly of MgO and MA spinel refractory phases, plus some calcium silicates and aluminoferrite phases. The latter phases contribute to densification during firing by promoting liquid phase formation. Most samples showed high refractoriness under load, good spalling resistance, better mechanical properties than current refractories, and compact microstructure. It is concluded that these new refractories are good candidate materials for the production of shaped linings for industrial kilns and furnaces.
由埃及白云质菱镁矿与滑石和低成本的中国铝土矿混合制成的耐火材料被认为是目前用于炼钢和其他工业的高温碱性耐火砖的潜在替代品。在1580℃高温下焙烧2 h,制备了15批不同成分的样品,根据其相组成和致密化参数选择了6个样品进行进一步研究。研究了试样的矿物组成、微观结构、孔径分布、力学性能和耐火性能。6个样品主要由MgO和MA尖晶石耐火相组成,外加部分硅酸钙和铁素体铝相。后一相通过促进液相的形成,有助于烧结过程中的致密化。大部分试样在载荷作用下耐火度高,抗剥落性好,力学性能优于现有耐火材料,显微组织致密。结果表明,这些新型耐火材料是生产工业窑炉异形衬里的良好候选材料。
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引用次数: 15
Euphoria and heartbreak: two sides of the coin in the development of structural ceramics 欣快与心碎:结构陶瓷发展的两面
Pub Date : 2003-10-01 DOI: 10.1179/174327613X13789816848661
D. Thompson
Abstract The 1950s saw the emergence of the group of materials originally referred to as 'special ceramics'. These then became 'engineering ceramics', and more recently have been further subdivided into bioceramics, functional ceramics, and structural ceramics. These materials demonstrate excellent properties for the application areas indicated, and share the common feature of not using clay as a starting material. In the early 1960s, it could not have been foreseen that electrical ceramics (including superconductors) would develop much more rapidly than the rest; of course this move was stimulated by concurrent developments in computing and electronic devices. In contrast, the more diverse, scientifically challenging structural ceramics have struggled to find niches in a very competitive marketplace, showing only modest growth over the last 30 years. Silicon carbide has been perhaps the least dramatic in its progress, whereas zirconia, stimulated by the toughening revolution, generated an explosion of interest in the early 1980s, though this has since moderated. In contrast, silicon nitride, with the associated family of sialon ceramics, has maintained an overall upward curve for some 40 years, punctuated by occasional spurts due either to new market opportunities or to materials developments, a good current example of the latter being the recent appearance of a group of ultrahard high pressure derivatives.
20世纪50年代出现了一组最初被称为“特殊陶瓷”的材料。这些后来成为“工程陶瓷”,最近又进一步细分为生物陶瓷、功能陶瓷和结构陶瓷。这些材料在指定的应用领域表现出优异的性能,并具有不使用粘土作为起始材料的共同特点。在20世纪60年代早期,人们无法预见到电陶瓷(包括超导体)的发展会比其他材料快得多;当然,这一举动是由计算机和电子设备的同步发展所刺激的。相比之下,更加多样化,具有科学挑战性的结构陶瓷在竞争激烈的市场中一直在努力寻找利基,在过去的30年里只显示出适度的增长。碳化硅在其发展过程中可能是最不引人注目的,而氧化锆在钢化革命的刺激下,在20世纪80年代初引起了人们的兴趣,尽管后来有所缓和。相比之下,氮化硅,以及相关的硅陶瓷家族,在大约40年的时间里保持了一个整体的上升曲线,由于新的市场机会或材料的发展,偶尔会出现井喷,后者的一个很好的例子是最近出现的一组超硬高压衍生物。
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引用次数: 2
期刊
British Ceramic Transactions
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