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以六水草酸镨Pr_2(C_2O_4)_3·6H_2O为镨源,通过热分解法制备纳米粒状Pr_6O_(11)。借助热重-差热(TG-DTA)曲线研究了六水草酸镨在空气中的热分解过程。利用X射线衍射仪、扫描电镜以及紫外-可见分光光度计分别表征了六水草酸镨在空气中热分解产物的物相、形貌和光吸收特性。结果表明,六水草酸镨在空气中的热分解过程主要分为两个阶段:第一阶段是室温~300℃,大片状六水草酸镨失去吸附水和结晶水变为小片状Pr_2(C_2O_4)_3;第二阶段是300~800℃,小片状Pr_2(C_2O_4)_3受热分解成小薄片状Pr_6O_(11)。纳米粒状Pr_6O_(11)在900℃下保温10 min获得,其对可见光的吸收能力显著优于小薄片状Pr_6O_(11)。 相似文献
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以四水碳酸镝(Dy_2(CO_3)_3·4H_2O)为镝源,Dy_2(CO_3)_3·4H_2O在空气中热重-热差(TGDTA)分析为依据,利用X射线衍射仪(XRD)、扫描电镜(SEM)和紫外-可见分光光度计(UVVis)分别表征了Dy_2(CO_3)_3·4H_2O在空气中热分解产物的物相、形貌和光学特性。研究结果表明,Dy_2(CO_3)_3·4H_2O在空气中的热分解过程主要分为两个阶段,第一阶段是在室温~285℃之间Dy_2(CO_3)_3·4H_2O失去结晶水变为Dy2(CO3)3,第二阶段是在285~700℃范围内Dy2(CO3)3经过受热分解生产了Dy_2O_3,在700℃下保温15 min获得了Dy_2O_3纳米颗粒。Dy_2O_3纳米颗粒具有较强的光吸收能力。此外,在波长为300~400 nm的范围内,Dy_2O_3纳米颗粒具有较宽的光吸收带。 相似文献
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研究了以碳酸钕(Nd_2(CO_3)_3·H_2O)为钕源,采用热分解法制备纳米氧化钕。根据Nd_2(CO_3)_3·H_2O在空气中的热重-差热(TG-DTA)分析结果,借助X射线衍射仪(XRD)、扫描电镜(SEM)和紫外-可见分光光度计(UV-Vis)分别表征Nd_2(CO_3)_3·H_2O在空气中热分解产物的物相、形貌和光学特性。结果表明,Nd_2(CO_3)_3·H_2O的热分解过程分为3个阶段:第1阶段,室温~300℃,Nd_2(CO_3)_3·H_2O失去结晶水变为Nd_2(CO_3)_3;第2阶段,300~550℃,Nd_2(CO_3)_3受热分解产生中间产物Nd_2O_2CO_3;第3阶段,550~850℃,Nd_2O_2CO_3在850℃下保温15 min,形成纳米Nd_2O_3。第3阶段是控制Nd_2O_3粒径的主要环节。 相似文献
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草酸盐共沉淀前驱体的热分解过程 总被引:2,自引:0,他引:2
研究前驱体热分解过程对制定Ni-Co预合金粉末的制备工艺有一定的指导意义,故采用差热和热重分析法对草酸盐共沉淀前驱体(Ni0.7Co0.3C2O4·2H2O)在氩气和空气中的热分解过程进行研究,并对分解产物进行了物相分析和形貌观察.结果表明: 前驱体在这2种气氛下的热分解机制完全相同; 分解过程分2步进行,第1步脱去结晶水分子(Ni0.7Co0.3C2O4·2H2ONi0.7Co0.3C2O4 2H2O↑),第2步无水前驱体分解成Ni-Co合金粉末和CO2; 但是,最终的固体产物不同,因为在空气中,生成的Ni-Co合金粉末又与氧气反应,最终得到的固体产物是氧化物(NiO和Co3O4),而在氩气中,最终的固体产物仍然是Ni-Co合金粉末. 相似文献
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以碱式碳酸钕(Nd2(C2O4)3·10H2O)为原料,Nd2(C2O4)3·10H2O在空气中热重-热差(TG-DTA)分析结果为依据,采用X射线衍射仪(XRD)、扫描电镜(SEM)和紫外-可见分光光度计(UV-Vis)分别表征了Nd2(C2O4)3·10H2O在空气中热分解产物的物相、形貌和光吸收特性。结果表明,Nd2(C2O4)3·10H2O在空气中的热分解主要分为3个阶段,第一阶段是室温至300℃,Nd2(C2O4)3·10H2O受热失去结晶水变为Nd2(C2O4)3;第二阶段是300~600℃,Nd2(C2O4)3受热分解为中间产物Nd2O2CO3;第三阶段是600~750℃,Nd2O2CO3受热分解为Nd2O3。在950℃时Nd2(C2O4)3·10H2O受热分解并保温15 min获得了Nd2O3纳米颗粒。随着Nd2(C2O4)3·10H2O热分解温度地升高,获得的Nd2O3颗粒越细,对光的吸收能力就越强。特别是Nd2O3纳米颗粒对光的吸收出现了一些较强的吸收峰和较宽的吸收带,可以极大的拓展Nd2O3纳米颗粒的光学特性应用范围。 相似文献
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《稀有金属》2017,(10)
以硝酸、氨水、硝酸铵、商业氧化钇及草酸为初始原料,加入分散剂聚乙二醇(PEG2000)及表面活性剂十二烷基苯磺酸钠(SDBS),采用改进的草酸沉淀工艺成功制备氧化钇前驱体Y(NH_4)(C_2O_4)_2·H_2O及经随后的焙烧工艺获得最终产品Y_2O_3粉体。具体工艺中,将一定浓度的小体积Y(NO_3)_3溶液滴入大体积氨水-硝酸铵混合溶液中形成Y(OH)_3溶胶,整个滴入过程体系pH值保持稳定,然后将85℃温度下的饱和草酸溶液滴加入上述制备的Y(OH)_3溶胶中,进行沉淀转化以制备钇草酸盐前驱体Y(NH_4)(C_2O_4)_2·H_2O,继而经焙烧工艺成功制备Y_2O_3粉体。X射线衍射技术(XRD)和扫描电子显微镜(SEM)表征表明:前驱体Y(NH_4)(C_2O_4)_2·H_2O具有立方晶体结构,有轻微的团聚,经950℃焙烧2 h后,尽管失去了O,C和H,立方相Y_2O_3产品完整地保留了前驱体的形貌特征。进一步,主要通过调整表面活性剂SDBS/分散剂PEG2000质量比及改变草酸沉淀转化终点pH值来考察其对Y_2O_3产品尺寸及形貌的影响。不同条件下制备的Y_2O_3粉体扫描电子显微镜(SEM)表征表明:精确控制实验条件,特别是控制草酸沉淀转化过程终点pH值,可制备出形貌和尺寸可控的Y_2O_3粉体,当草酸沉淀转化过程中终点pH值小于1.8时,制备的Y_2O_3粉体粒径在1μm以下。另外,基于前驱体Y(NH_4)(C_2O_4)_2·H_2O在空气气氛下的差示-热重(TG-DSC)分析结果,其热分解过程应为:Y(NH_4)(C_2O_4)_2·H_2O→Y(NH_4)(C_2O_4)_2→Y_2O_2CO_3→Y_2O_3。 相似文献
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空气中热分解二水草酸镍制备纳米氧化镍 总被引:1,自引:0,他引:1
通过TG-DSC、SEM和TEM对二水草酸镍在空气中热分解过程进行分析,研究结果表明:二水草酸镍在空气中的热分解过程经历了两个阶段,在175~275℃之间二水草酸镍失去结晶水生成NiC2O4;325~400℃之间NiC2O4被热分解为NiO.二水草酸镍空气中热分解制备NiO过程中,在246.5~357.8℃之间热分解产物的形貌变化最大;在357.8~400.0℃之间热分解产物的形貌变化次之.为了有效控制NiO的形貌,可以分段性地控制热分解条件.以10℃/min的升温速率在空气中热分解二水草酸镍,并在400℃时保温10 min,制备出了5 nm左右的球形氧化镍. 相似文献
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水氯镁石复盐法脱水工艺 总被引:2,自引:1,他引:1
用烧瓶蒸馏装置模拟固定床脱水设备,研究用苯胺盐酸盐作脱水剂的复盐法将水氯镁石(MgCl2.6H2O)脱水制备无水氯化镁(MgCl2)的过程,考察复盐配料比例、保护气含水浓度、热解温度、热解时间等因素对所制备无水氯化镁产品中氧化镁和水分含量的影响,优化用固定床脱水工艺条件。结果表明,完全脱水和脱苯胺盐酸盐的最佳温度和时间分别是300℃与25~30 min和320~350℃与10~20min。最佳配料摩尔比C6H5NH2.HCl∶MgCl2.6H2O为1.1∶1.0。在最佳条件下,可得到合格的无水氯化镁产品MgCl298%~98.6%,MgO 0.03%~0.38%,苯胺盐酸盐0.10%~0.12%,水分0.60%~0.81%。 相似文献
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Thesynthesesandcharacterizationofnew typeheteropolycomplexescontainingrareearthelementshavebeenreportedinthepast.Nowmuchattentionhasbeendirectedtowardstheresearchonacidic ,redoxordifunctionalcatalysts[1~ 3] .Vacantheteropolycomplexisanactiveinorganicligan… 相似文献
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用热重-差热(TG-DTA)技术,在不同升温速率条件下,研究了十水草酸镧在空气气氛下的热分解过程.分别采用Ozawa-Flynm-Wall法、Kissinger法、Crane法和同步热分析法确定其热分解动力学参数.TG-DTA曲线表明:十水草酸镧分解为四个阶段,前两个阶段为脱水过程,后两个阶段为La_2(C_2O_4)_3的分解过程.实验计算得出四步反应表观活化能E分别为83.92、76.04、136.26、162.61 k J·mol-1左右;指前因子A分别为4.92×10~(10)、6.1×10~7、2.1×10~9、8.46×10~6s-1左右;反应级数n均为1左右,并用Coats-Redfem积分法得出第三步分解机理受F1控制. 相似文献
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The precursors RE (HSal) 3 ( RE = La, Y, Gd; HSal = C6 H4 (OH) COO) were synthesized by the rheological phase reaction method. The mechanism and products of thermal decomposition of precursors was studied by using TG,DTA, gas chromatography-mass spectrometry (GC-MS). Nano-sized RE2O3 ( RE = La, Y and Gd) power were obtained by thermal decomposition of the precursors in air at 800 ℃. TEM measurement indicates that RE2O3 are spherical particles. The middle level diameter ( d50 ) of the particles are 19.3 ( La2O3 ) , 53.8 ( Y2O3 ) and 28.6 nm( Gd2O3 ) respectively by means of laser particles size analyzer. 相似文献
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Mohammadreza Daroonparvar Muhamad Azizi Mat Yajid Noordin Mohd Yusof Hamid Reza BakhsheshiRad Esah Hamzah Mohsen Nazoktabar 《中国稀土学报(英文版)》2014,32(10):989-1002
Phase transformation of tetragonal ZrO2 to monoclinic phase and also increment of bond coat oxidation kinetic(TGO thickening) can substantially restrict the life time of thermal barrier coating systems(TBCs). So, nanostructured and conventional Y2O3 stabilized ZrO2 coatings were evaluated in fused V2O5-Na2SO4 salts during thermal exposure in air. Microstructural characterization showed lower hot corrosion products(monoclinic zirconia, YVO4 crystals) formation and reduction of TGO thickness in thermal barrier coating system consisting of nanostructured Y2O3 stabilized ZrO2(YSZ) top coat. It was found that inhomogeneities, pores and micro-cracks played a principal role in the molten salts infiltration into the YSZ coating during three steps of hot corrosion process. In the nanostructured YSZ coating with tri-model structure, nano zones which surrounded by fully molten parts could fill the aforementioned defects and could act as barrier for the oxygen and corrosive molten salts penetration into the TBC. 相似文献
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ZHOULAN YIN QINSHENG ZHAO SHAOYI CHEN SIGING WANG GUORONG LIU 《Mineral Processing and Extractive Metallurgy Review》2013,34(1-4)
High temperature X-ray diffraction analysis is employed to study the reduction of three commercial complex ammonium molybdates marked as AM-l, AM-2 and AM-3 which are used as the starting material for the production of molybdenum metal. The compositions of AM-l, AM-2 and AM-3 are (MH4;)6Mo7024-4 H20 (small amount) + (NH4)Mo5O+ (NH.)2Mo40(small amount) + (3 -(NH4)Mo4O13(NH4):Mo40, + β -(NH4)Mo40, + (NH4)Mo40,-2 H6 (small amount) and (NH4(2MoO13 + β - (NH4)2Mo4O13+(NH4)2Mo4O13-2 H2O respectively. It is found that the thermal decomposition of ammonium molybdates into MoO3, proceeds prior to the reduction of MoO3 The intermediary products of the thermal decomposition, (NH4)Mo14041 and identified which arc more stable in hydrogen than in air. MoO.80) and Mo40 are also identified as the intermediary products during the reduction of MoO to MoO. The reduction reaction of Mo4Ois infered from the phase development of AM-l, AM-2 and AM-3 during the reduction course. The thermal decomposition of AM-2 and the subsequent reduction of MoO occur almost at the same time while those of AM-l or AM-3 take place at a larger range of temperatures, which is identical with what is observed in the practical production process. 相似文献
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采用制粒焙烧、碱浸、离子交换、煅烧工艺从某石煤钒矿选矿富集所产钒精矿中提钒。结果表明,V2O5焙烧收率99.50%,浸出率84.49%,净化收率98.15%,树脂吸附—解吸收率99.69%,沉钒—煅烧收率98.85%,全流程总收率81.31%,中间试验指标稳定可靠。所产五氧化二钒产品达到GB3283-87V2O598牌号标准,副产品白炭黑SiO2含量可达96%以上。 相似文献
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The reaction of the mixed rare earth concentrate including monazite ( REPO4 ) and bastnaesite ( REFCO3 )decomposed by CaO and NaCl additives at the temperature range from 100 to 1000 ℃ was studied by means of XRD and TG-DTA.The results show that when CaO and NaCl are not added, only REFCO3 can be decomposed at the temperature of 377 ~ 450 ℃.The decomposition products include REOF, RE2O3 and CeO2.However, REFCO3 can not be decomposed.When CaO is added, the decomposition reactions occur at the temperature range from 660 to 750 ℃.CaO has three decomposition functions: ( 1 ) REPO4 can be decomposed by CaO and the decomposition products include RE2O3 and Ca3 (PO4)2; (2) CaO can decompose REOF, and the decomposition products are RE2O3 and CaF2; (3)CaO can decompose REPO4 with CaF2, and the decomposition products are RE2 O3, Ca5 F( PO4 )3.The decomposition ratio of the mixed rare earth concentrate increased obviously, when CaO and NaC1 were added.NaC1 can supply the liquid for the reaction, improve the mass transfer process and accelerate the reaction.At the same time, NaC1 participated in the reaction that REPO4 was decomposed by CaO. 相似文献
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Hocheol Song Seokheung Chang Kwinam Park Ho-chul Shin Jin-won Park Eung-soo Choi Wan-wook Huh 《Canadian Metallurgical Quarterly》2005,131(2):190-195
Urea and NH4HCO3 were used to control the emission of NO and SO2 from the combustion of coke at high-temperature and low oxygen concentration. Urea and NH4HCO3 could control NO emission only under 1100°C. Their effects disappeared above 1100°C even though the increase of urea and NH4HCO3 content from 10?to?50?wt?%. However, they showed good desulfurization effect on the emission of SO2 at all combustion temperatures and their effects showed remarkable results even at 1500°C. Only 10?wt?% of urea or NH4HCO3 could control the emission of SO2 effectively at 1400 and 1500°C. This effect was caused by ?NH and ?NH2 from the thermal decomposition of reducing agents at high temperature. Low O2 concentration showed little effect on the removal of SO2. Ammonia slip from the thermal decomposition of reducing chemical was not a considerable level. 相似文献