氧化钇纳米粉末的制备

使用草酸作沉淀剂，采用液相沉淀法成功制备了氧化钇纳米级粉末。对该粉末的扫描电镜图以及差热分析图等进行了分析以及对溶液的pH值、浓度、反应方式、分散剂及煅烧温度等因素进行了考察，得出了较为理想的工艺条件。在此工艺条件下制得的氧化钇粉末粒径为20～50m。     

Synthesis of Yttrium Oxide Nanocrystal via Solvothermal Process

Y2O3 nanomaterials have been widely used in transparent ceramics and luminescent devices. Recently there are many studies focusing on controlling the size and morphology of Y2O3 in order to obtain better materials performance. In present study, yttrium oxyhydroxide precursor was synthesized via a facile solvothermal process through the dissolution-recrystallization mechanism of Y2O3 raw powders in the ethylenediamine solvent, then nanosized yttrium oxide crystal was prepared from the precursor through post heat treatment process. The effects of solvothermal treatment temperature, holding time, solvent kinds and post heat treatment parameters on crystalline structure, grain shape and size of nanocrystal were investigated by XRD, TEM and TGA-DTA measurements. TEM images reveal that the morphology of product after post heat treatment at 460 ℃ for 12 h is rice-like nanocrystal. XRD shows that this product is pure cubic Y2O3 cphase. Present study reveals that high purity Y2O3 with rice-like morphology can be easily prepared with average size around 30 nm under suitable post heat treatment parameters. In addition, the effects of solvents such as water and ethanol etc. on the crystal structure and morphology were also investigated. It is suggested that dissolution-recrystallization process may be the main mechanism for the formation of nano-sized YOOH precursors under solvothermal reaction condition, and the ethylenediamine solvent is likely to play an important role in controlling the transformation process of yttria precursors to theY2O3 nanocrystal.     

Studies on the Kinetics of Carbon Tetrachloride Chlorination of Refractory Metal Oxides

Abstract

Studies on the kinetics of chlorination of the oxides of titanium, zirconium, niobium and tantalum by carbon tetrachloride gas in dilution with nitrogen, at low and moderate temperatures, have been carried out. In each case, the effect of time, temperature, partial pressure of carbon tetrachloride and the particle size, on the chlorination of the oxide, has been studied. The influence of some physico-chemical properties of the oxides and their halides on the kinetics process, has been discussed. The chlorination results below and above the dissociation temperature of carbon tetrachloride ( ～ 773 K.) have been examined to find out the difference in the kinetics by CC1₄ and those by elemental carbon and chlorine. From these kinetics results, the mechanism of the chlorination of each of the oxides, has been established and compared. The optimum experimental conditions for preparing the metal chlorides, keeping in view of the maximum utilisation of the carbon tetrachloride, have been established. The merits of carbon tetrachloride as a chlorinating agent, have been highlighted. From these kinetics results, the scope for chlorinating the refractory metal oxides, as well as their mixed oxides, at lower temperatures and lower partial pressures of carbon tetrachloride, with the scope for recycling the reagent, has been briefly discussed. Some preliminary results on the preferential chlorination of these oxides by carbon tetrachloride present in a typical tin slag, have been presented, to further substantiate the merits of carbon tetrachloride as a low temperature chlorinating agent.     

Studies on the Kinetics of Carbon Tetrachloride Chlorination of Refractory Metal Oxides

Studies on the kinetics of chlorination of the oxides of titanium, zirconium, niobium and tantalum by carbon tetrachloride gas in dilution with nitrogen, at low and moderate temperatures, have been carried out. In each case, the effect of time, temperature, partial pressure of carbon tetrachloride and the particle size, on the chlorination of the oxide, has been studied. The influence of some physico-chemical properties of the oxides and their halides on the kinetics process, has been discussed. The chlorination results below and above the dissociation temperature of carbon tetrachloride (～ 773 K) have been examined to find out the difference in the kinetics by CCl₄ and those by elemental carbon and chlorine. From these kinetics results, the mechanism of the chlorination of each of the oxides, has been established and compared. The optimum experimental conditions for preparing the metal chlorides, keeping in view of the maximum utilisation of the carbon tetrachloride, have been established. The merits of carbon tetrachloride as a chlorinating agent, have been highlighted. From these kinetics results, the scope for chlorinating the refractory metal oxides, as well as their mixed oxides, at lower temperatures and lower partial pressures of carbon tetrachloride, with the scope for recycling the reagent, has been briefly discussed. Some preliminary results on the preferential chlorination of these oxides by carbon tetrachloride present in a typical tin slag, have been presented, to further substantiate the merits of carbon tetrachloride as a low temperature chlorinating agent.     

氧化镍在聚氯乙烯热裂解过程中的低温氯化

利用聚氯乙烯(PVC)与氧化亚镍混合物(质量混合比10∶1)中的PVC在氩气气氛低于673K温度条件下释放出的氯化氢作为氯化剂氯化氧化亚镍,并通过氧化焙烧激活氧化亚镍的反应活性促进氯化反应,将氧化亚镍的氯化率由30%提高至95%,表明聚氯乙烯在低温下可以作为氯化剂氯化氧化亚镍。利用TG-DTA测试恒定升温速率(10~40K/min)条件下失重率随温度的变化规律,分析了PVC与氧化亚镍反应动力学。得出PVC+NiO反应体系的表观活化能为96kJ/mol,略小于纯PVC裂解的表观活化能114kJ/mol。     

Sintering of Titanium with Yttrium Oxide Additions for the Scavenging of Chlorine Impurities

Chloride impurities in titanium powders are extremely difficult to remove and present a long-standing problem in titanium powder metallurgy. We show that the detrimental effects of chlorides on the sintering of titanium can be mitigated with trace additions of yttrium oxide, which has a high affinity for the normally volatile species and forms highly stable oxychloride reaction products. Compacts that would otherwise exhibit gross swelling and excessive porosity due to chloride impurities can be now sintered to near full density by liquid phase sintering. The potency of yttrium oxide additions is observable at levels as low as 500?ppm. The scavenging of chlorine by Y₂O₃ appears to be independent of alloy composition and sintering regime. It is effective when used with high-chloride powders such as Kroll sponge fines but ineffective when used with powders containing NaCl impurities or during solid-state sintering. The identification of highly potent chlorine scavengers may enable the future development of chloride-tolerant powder metallurgy (PM) alloys aimed at utilizing low-cost, high-chloride powder feedstocks.     

Influences of Yttrium on Adhesion of Oxide Scale of Fe-Cr-Al Alloy

Ａｄｄｉｔｉｏｎｏｆａｓｍａｌｌａｍｏｕｎｔｏｆｒａｒｅｅａｒｔｈｅｌｅｍｅｎｔｃａｎｉｍｐｒｏｖｅｔｈｅａｄｈｅｒｅｎｃｅｏｆｏｘｉｄｅｓｃａｌｅｓｉｇｎｉｆｉｃａｎｔｌｙ[1] .Ｔｈｅｒｅａｃｔｉｖｅｅｌｅｍｅｎｔｓｍａｙｂｅｉｎｃｏｒｐｏｒａｔｅｄｉｎｔｈｅｂｕｌｋａｌｌｏｙａｓｍｅｔａｌ ｌｉｃｏｒｏｘｉｄｅｄｉｓｐｅｒｓｅｄｃｏｍｐｏｎｅｎｔｓｏｒｂｅａｄｄｅｄａｓｓｕｒｆａｃｅｌａｙｅｒｓｂｙｃｏａｔｉｎｇｏｒｉｏｎｉｍｐｌａｎｔａ ｔｉｏｎ .ＴｈｅＲＥｅｆｆｅｃｔｉｖｅｎｅｓｓｗｉｌｌ…     

高纯氧化钇清洁化生产工艺的研究

阐述了以环烷酸—异辛醇—煤油和环烷酸—石油亚砜—煤油两种组分不同的有机溶剂为萃取剂,在REC l3-HC l-HNO3体系中制取纯度≥99.999%高纯氧化钇清洁化工艺流程及特点。研究解决了工艺过程中各种化工辅料的循环使用和综合利用问题,以较低的运行成本实现了工艺过程中的废物资源化及产品化,同时提高了水的利用率,使提钇萃取分离工艺与环境治理有机结合,降低了工艺生产成本和环境治理成本,实现了清洁化生产。     

沉淀条件对荧光级氧化钇中钙含量的影响

研究了用草酸沉淀钇制备荧光级氧化钇时加料速度、加料比、反应温度、搅拌强度和加料方式对荧光级氧化钇中钙含量的影响。结果表明:温度是影响产品中钙含量的决定性因素,实际生产中应该确保体系温度大于60℃。与此同时,荧光级氧化钇产品中的钙含量与氯化钇料液中的钙含量相关,其Ca/RE建议控制在10×10-6g/g以下。当Ca/RE高于10×10-6g/g时,采用偏正同沉加料方式有利于降低氧化钇产品中的钙含量。     

草酸沉淀法制备大颗粒氧化钇工艺研究

采用草酸沉淀法研究制备了大颗粒氧化钇,并对各制备条件对氧化钇粒度影响进行了分析讨论.同时,结合不同煅烧温度下产物的XRD谱图,对煅烧产物进行物相分析,探讨煅烧过程中产物的晶型转变,并利用SEM观察产物形貌.结果表明:提高酸度、沉淀反应温度、延长陈化时间以及降低加料速度均可以有效增大氧化钇粒度;XRD曲线表明沉淀反应制得前躯体的主要成分为Y2(C2O4)3·10H2O,且当前躯体于400,600,800,1000℃煅烧时,所得产物分别为Y2(C2O4)3·2H2O,YOOH,Y2O3,Y2O3;前躯体形貌与最终的氧化物产品形貌存在一定的相似性,均是由小颗粒形成的团聚体,但颗粒粒度存在较大差异.因此,由实验得出了草酸沉淀法制备大粒度氧化钇的工艺条件,且按此工艺条件制备出粒度大于50μm的氧化钇产品,颗粒分散均匀.此外,本工艺操作简单,产品质量稳定,易于推广,可实现产业化.     

氧化钇弥散强化钨基复合材料的制备及其性能评价

采用高能球磨、通氢烧结和后期热轧处理制备了W-0.5%Y2O3-1%Ti复合材料,对加工变形处理前后的W-0.5%Y2O3-1%Ti的显微组织结构和室温力学性能进行了研究。研究分析表明,采用高能球磨,可使Y2O3和Ti固溶到W中,在高温烧结的过程中,Y2O3和Ti以Y-Ti-O化合物和Ti的形式从钨基体中析出来,弥散分布在钨晶粒的晶界及其晶内。经在1 500℃左右热加工变形处理后,W-0.5%Y2O3-1%Ti的致密度显著提高,与此同时大量体积分数的穿晶断裂赋予了W-0.5%Y2O3-1%Ti复合材料较高的力学性能。实验结果表明经热轧后W-0.5%Y2O3-1%Ti的致密度、抗弯强度、维氏硬度分别可达96.7%,788.0 MPa和HV432.8。     

Electroreduction Kinetics for Molten Oxide Slags

 The oxygen ion conductor, the reducing agent, and the molten oxide slag containing electroactive matter were used as constituent of a galvanic cell. Metal was directly electroreduced from molten slag using a short circuit galvanic cell. The following galvanic cell was assembled in the present experiment: graphite rod, [O]Fe C saturated｜ZrO2(MgO)｜Cu(l)+(FeO)(slag), and molybdenum wire. The FeO electroreduction reaction was studied through measuring short circuit current by controlling factors such as temperature, the FeO content in molten slags, and the external circuit resistance. An overall kinetics model was developed to describe the process of FeO electroreduction. It was found that the modeled curves were in good agreement with the experimental values. The new oxide reduction method in the metallurgy with controlled oxygen flow was proposed and the metallurgical theory with controlled oxygen flow was developed.     

Synthesis and Characterization of Large Surface Area Yttrium Oxide by Precipitation Method

Rareearthoxides(REO)withlargesurfaceareahavehighchemicalreactionactivity ,soitisusedwidelyinthefieldofcatalysis ,SOFC ,advancedce ramicandsoon[1] .Inordertosatisfythedemandofthenewfunctionmaterials ,thepreparationmethodofspecialphysicalpropertyREcompoundneedstobedeveloped .Yttriumoxide ,especiallywithlargesur faceareaisaREOandwidelyusedintheabovefield .Industrially ,yttriumoxideusuallywaspreparedbythermaldecompositionofyttriumoxalateat 80 0～10 0 0℃for 2h .Itssurfaceareaisonly 2～ 4m2 ·…     

Chlorination Kinetics of Titanium Nitride for Production of Titanium Tetrachloride from Nitrided Ilmenite

The kinetics of chlorination of titanium nitride (TiN) was investigated in the temperature range of 523 K to 673 K (250 °C to 400 °C). The results showed that the extent of chlorination slightly increased with increasing temperature and decreasing particle size of titanium nitride at constant flow rate of N₂-Cl₂ gas mixture. At 523 K (250 °C), the extent of chlorination was 85.6 pct in 60 minutes whereas at 673 K (400 °C), it was 97.7 pct investigated by weight loss measurement and confirmed by ICP analyses. The experimental results indicated that a shrinking unreacted core model with mixed-control mechanism governed the chlorination rate. It was observed that the surface chemical reaction of chlorine gas on the surface of TiN particles was rate controlling in the initial stage and, during later stage, internal (pore) diffusion through the intermediate product layer was rate controlling step. Overall the process follows the mixed-control model incorporating both chemical reaction and internal diffusion control. The activation energy for the chlorination of TiN was found to be about 10.97 kJ mol^?1. In processing TiCl₄ from TiN and TiO_0.02C_0.13N_0.85, the solids involved in the chlorination process were characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM) and Energy-dispersive X-ray spectrometer (EDX). The SEM/EDX results demonstrated the consumption of TiN particles with extent of chlorination that showed shrinking core behavior.     

Kinetics of the Carbothermic Reduction of Manganese Oxide from Slag

Metallurgical and Materials Transactions B - Experiments were performed using a range of test conditions to elucidate the rate controlling step during the reaction of liquid iron-carbon droplets...     

Preparation and Characterization of Porous Yttrium Oxide Powders with High Specific Surface Area

Y2O3isoftenusedinthemanufactureofphos phorsandceramics[1～3].However,itisalsousedas selectivecatalysts[1,4,5],suchasforthedehydrationof2alkanols,thedimerizationofmethane,1butene isomerization,hydrogenationof1,3butadieneandac etonealdoladdition,andsupport[6,7]formetalsthat catalyzetheformationofmethanolfromCO2andH2.It iswidelyacceptedthatthecatalysispropertiesofox idesdependstronglyontheirphysicalcharacteristics,especiallyontheirspecificsurfaceareaandporous structure.Agreatdealofattentionhasb…     

Determination of Yttrium in Lanthanum Oxide by PTFE Fluorinating Technique Combined with ETV-ICP-AES

In this study,fluorinating vaporization combined with ETV-ICP-AES technique was used to determineyttrium for which refractory carbide is easily formed.The absolute detection limit is 12 pg,and three-ordermagnitude of improvement is obtained in comparison with the conventional vaporization ETV-ICP-AES.Nomemory effect is observed.The relative standard deviation is better than 5%.Some factors affecting fluorinatingvaporization,including matrix effect are discussed.This technique is applied to determine yttrium in La_2O_3.     

环烷酸-石油亚砜-HCl体系制备荧光级氧化钇

本文研究了用环烷酸—石油亚砜—煤油为萃取剂，以富钇混合稀土氯化物为原料，制备荧光级氧化钇的工艺流程。用３６０升的混合—澄清槽，经两步分离，一步除杂，稳定得到了５Ｎ氧化钇，并制备出了荧光级氧化钇产品