两步沉淀法合成Bi3.25La0.75Ti3O12(BLT)粉体及其表征

以五水硝酸铋(Bi(NO3)3·5H2O)、水合硝酸镧(La(NO3)3·nH2O)和钛酸四丁酯((C4H9O)4Ti)为原料,氨水为沉淀剂,分两步沉淀Ti离子和Bi、La离子,利用沉淀法合成了Bi3.25La0.75Ti3O12(BLT)粉体.利用差热分析(DTA)和热失重(TG)对两步沉淀法制备的前驱体粉体的热行为进行了分析,用X射线衍射(XRD)研究了其晶相演化过程,利用场发射扫描电子显微镜(FESEM)对BLT粉体粒度和形貌进行了观察.结果显示两步法制备的前驱体粉体经低温煅烧直接转化为单一的铋层状钙钛矿相BLT粉体,在700℃煅烧2 h合成的BLT粉体颗粒不大于100nm,颗粒间结合疏松,具有良好的分散性.     

沉淀法制备纳米Eu：Y2O3荧光粉

试验分别以微米级Y2O3、Eu2O3粉体为原料，碳酸氢铵为沉淀剂，三乙醇胺为络合剂，采用三乙醇胺络合沉淀法制备了化学组成为NC6H12（NH4）Y2（CO3）（NO3）2·nH2O的前驱体。研究了前驱体在不同的煅烧温度下的物相变化，结果表明，前驱体在500℃保温2h即可直接生成立方相的Eu：Y2O3，在1000℃保温2h的条件下得到了结晶度高、分散性好、平均粒径为50～60nm、近球形的纳米Eu：Y2O3荧光粉。     

水热合成法制备纳米级CuWO_4·2H_2O粉体及其合成机理(英文)

选用Cu(NO3)2·3H2O和Na2WO4·2H2O分析纯作为反应原材料,通过水热合成法制备了纳米级的Cu WO4·2H2O粉体。讨论了前驱体Cu2WO4(OH)2的生成过程,并且建立了在水热合成过程中前驱体Cu2WO4(OH)2向Cu WO4·2H2O转变的机理。利用HRTEM以及XRD分析了前驱体和水热反应产物的物相及微观结构和形貌。结果表明:水热反应产物Cu WO4·2H2O粉体呈球形,粒径分布范围为20~30 nm。Cu WO4·2H2O粉体的生成过程符合原位结晶机制。在长时间的高热高压的水热环境中,WO42-离子在前驱体Cu2WO4(OH)2表面吸附扩散,通过脱水和原子重排,Cu WO4·2H2O在Cu2WO4(OH)2表面异相形核。WO42-离子通过Cu WO4·2H2O层与Cu2WO4(OH)2发生反应,直到WO42-离子被耗尽。     

负热膨胀材料立方ZrMo2O8的制备研究

以ZrO(NO3)2和N6H24Mo7O24·4H2O等为原料,采用湿化学法制备出立方相ZrMo2O8粉体.对前驱体在室温～800℃进行了TG-DSC测试,采用XRD、SEM对立方相ZrMo2O8粉体进行了分析观测.结果表明:亚稳相立方ZrMo2O8的制备对热处理工艺十分敏感,采用湿化学法在450℃制各出单一立方相ZrMo2O8粉体,在室温～400℃热膨胀系数为-4.337×10-6K-1.     

Hydrothermal Synthesis of Nano-sized Cupric Tungstate (Ⅵ) Dihydrate and Its Synthesis Mechanism

选用Cu(NO3)2·3H2O和Na2WO4·2H2O分析纯作为反应原材料,通过水热合成法制备了纳米级的Cu WO4·2H2O粉体。讨论了前驱体Cu2WO4(OH)2的生成过程,并且建立了在水热合成过程中前驱体Cu2WO4(OH)2向Cu WO4·2H2O转变的机理。利用HRTEM以及XRD分析了前驱体和水热反应产物的物相及微观结构和形貌。结果表明:水热反应产物Cu WO4·2H2O粉体呈球形,粒径分布范围为20~30 nm。Cu WO4·2H2O粉体的生成过程符合原位结晶机制。在长时间的高热高压的水热环境中,WO42-离子在前驱体Cu2WO4(OH)2表面吸附扩散,通过脱水和原子重排,Cu WO4·2H2O在Cu2WO4(OH)2表面异相形核。WO42-离子通过Cu WO4·2H2O层与Cu2WO4(OH)2发生反应,直到WO42-离子被耗尽。     

室温固相反应法制备Ni0.66Mn2.34-xCoxO4(x=0.15,0.30,0.45,0.60)负温度系数热敏电阻

以Mn(CH3COO)2·4H2O,Ni(CH3COO)2·4H2O,Co(CH3COO)2·4H2O和H2C2O4·2H2O为原料,采用室温固相反应法制备出镍锰钴草酸盐前驱体,将该前驱体在850℃煅烧2 h得到尖晶石相Ni0 66Mn2.34xCoxO4(x=0.15,0.30,0.45,0.60)超细粉体.用XRD,TGA,SEM,沉降式粒度分析仪和热膨胀仪对镍锰钴草酸盐前驱体与Ni0.66Mn2.34-xCoxO4(x=0.15,0.30,0.45,0.60)超细粉体进行了表征.结果表明,由室温固相反应法得到的草酸盐前驱体是单相的镍锰钴复合草酸盐在850℃煅烧2 h得到镍锰钴氧化物为纯尖晶石相,粉体颗粒为球形,团聚较少,粒径均匀,平均粒径约为0.2μm,有较好的烧结活性,是制备热敏陶瓷材料的理想粉体.     

两步无机盐-凝胶法制备PMN-PT弛豫铁电陶瓷粉体

0．65Pb（Mg1／3Nb2／3）O3—0．35PbTiO3（简称：PMN-PT）弛豫铁电粉体采用两步无机盐-凝胶法制备。以氧化镁，醋酸铅，钛酸丁脂为原料，柠檬酸为螫合剂，乙二醇为溶剂，分别合成稳定的Mg，Pb-Ti的有机化合物先驱体溶液。Nb2O5粉体与Mg先驱体溶液均匀混合，并采用溶胶-凝胶工艺制备MgNb2O6（MN）先驱体粉体；MN粉体与Pb-Ti先驱体溶液均匀混合，并制备PMN-PT粉体。通过XRD和SEM分析PMN-PT钙钛矿相形成的影响因素和微观形貌，研究全钙钛矿相PMN-PT铁电粉体的制备。结果表明：过量3％MgO前驱体经1050℃，4h煅烧可以得到纯相MgNb2O6先驱体粉体：过量5％PbO前驱体经900℃，4h煅烧可以得到全钙钛矿相PMN-PT粉体。     

MgCO3·3H2O晶体生长及晶形的影响因素

提出一种新的反应结晶过程,即采用Na2CO3溶液为沉淀剂,选择合适条件与MgCl2溶液进行均相(不加晶种)结晶反应,实现从卤水中沉淀镁,制得MgCO3·3H2O晶体.研究温度、反应液初始浓度及滴加速率对MgCO3·3H2O晶体生长及晶形的影响,采用XRD和SEM对得到的晶体进行表征.结果表明:MgCO3·3H2O晶体的收率为98.1%,纯度为99.9%,所得到的晶体为MgCO3·3H2O,且温度、反应液初始浓度及滴加速率对MgCO3·3H2O晶体的生长、形态及颗粒大小都有着显著的影响.     

尿素均相沉淀法制备纳米粉体Ce0.8Sm0.2O1.9的烧结性能

以尿素为沉淀剂,Sm2O3和Ce(NO3)3.6H2O为起始原料,采用均相沉淀法制备Sm3+掺杂CeO2基纳米固溶体Ce0.8Sm0.2O1.9(SDC)。利用TG-DTA、XRD、SEM和BET等手段对前驱体的热分解行为和SDC粉体的性能进行表征,研究焙烧温度对SDC粉体粒径和烧结性能的影响。结果表明:随焙烧温度的升高,晶粒尺寸逐渐增大;700℃焙烧的前驱体是具有良好结晶性能的类球形萤石型结构固溶体,晶粒尺寸为15 nm,粒子间仅有较弱的软团聚;该粉体具有较好的成型和烧结性能,将素坯在1 400℃保温2 h,得到相对密度高于95%、平均粒径约为0.6μm的固体电解质陶瓷体。     

制备过程pH值对FePO4·xH2O及LiFePO4性能的影响

以FeSO4·7H2O,H3PO4,H2O2和NH3·H2O为原料合成FePO4·xH2O前驱体,考察制备过程溶液pH值对合成FePO4·xH2O前驱体性能的影响;将Li2CO3,FePO4·xH2O和乙炔黑球磨混合,通过低温固相反应合成LiFePO4.用X射线衍射和扫描电镜对FePO4·xH2O和LiFePO4进行结构和表面形貌表征,研究不同pH值条件下合成的FePO4·xH2O前驱体为原料对制备的LiFePO4电化学性能的影响.结果表明溶液pH值1.5时制备的FePO4·xH2O中含有少量Fe(PO4)2(OH)2杂质.当pH分别为2、3、4和5时,合成的FePO4·xH2O均为纯相.pH值为2左右合成的FePO4·xH2O前驱体制备出的LiFePO4具有良好的电化学性能;其振实密度达1.11 g/cm3.     

Fe-15Ce合金在H2-CO2、H2-H2S及H2-H2S-CO2气氛下的腐蚀

研究了600℃时Fe-15Ce合金在H2-CO2、H2-H2S及H2-H2S-CO2 3种气氛中的腐蚀行为，Fe-15Ce合金腐蚀后发生了Ce的内氧化或形成了复杂的腐蚀产物膜，而未出现Ce的选择性氧化或硫化，这主要是合金中存在着两相及Ce在Fe中极低的溶解度的结果。Fe-15Ce合金在本实验条件下的氧化-硫化腐蚀速度低于相同温度、压力下的纯硫化。     

用氢-氧取代氧-乙炔作焊接切割的必要性及可行性

阐述了用氢代乙炔的必要性．通过时HGQU2000／315火焰电孤焊割机的考察和试用证实了用氢代乙炔的可行性，比较了两种气体的性质并提出了使用特性差异和注意事项．提出了进一步探索的问题。     

Thermodynamics and phase diagrams in the binary systems Na2O-SiO2, Na2O-GeO2, Na2O-B2O3, Li2O-B2O3, CaO-B2O3, SrO-B2O3, and BaO-B2O3

We applied our model to the enthalpy of mixing data of the binary systems Na₂O-SiO₂, Na₂O-GeO₂, Na₂O-B₂O₃, Li₂O-B₂O₃, CaO-B₂O₃, SrO-B₂O₃, and BaO-B₂O₃. The most stable composition in the liquid, that is where the enthalpy of mixing is most negative, is with a metal-oxygen ratio of 4 to 3, for monovalent metals (Na and Li) and 3 to 4 for divalent metals (Ba and Ca) in liquid silicates or borates. The same applies to the CaO-SiO₂, CaO-Al₂O₃, PbO-B₂O₃, PbO-SiO₂, ZnO-B₂O₃, and ZnO-SiO₂ systems. The oxygen to metal ratio, its constant value in various types of systems, reflects and describes the structure of the liquid. Using the analyzed enthalpies of mixing data and the available phase diagrams, we calculated the enthalpies of formation of the various binary compounds. The results are in excellent agreement with data in the literature that were obtained from direct solid-solid calorimetry.     

IrO2-MnO2中间层Ti/RuO2-TiO2-SnO2电极制备及性能

通过热分解法制备了含IrO2-MnO2中间层Ti/RuO2-TiO2-SnO2电极,采用SEM、EDX、XRD、CV等检测方法对中间层进行表征,同时采用强化加速寿命试验对电极电化学稳定性进行表征。结果表明:450℃时前躯体完全氧化并形成固溶体,制备的中间层晶粒细小,表面结构致密,电化学孔隙率小。添加中间层使Ti/RuO2-TiO2-SnO2电极强化寿命由未加中间层的7.5h提高到995.8h,远高于国家标准20h。     

ACTIVITY OF La_2O_3 IN LIQUID La_2O_3-CaF_2 AND La_2O_3-CaF_2-CaO-SiO_2 SLAGS

用石墨为还原剂,将渣中La_2O_3还原入液态Sn,以测定1500℃下La_2O_3-CaF_2和La_2O_3-CaF_2-CaO-SiO_2渣中La_2O_3的活度.对La_2O_3-CaF_2系,并用Gibbs-Duhem积分法求得CaF_2的活度. 根据液态渣的离子结构模型,对上述二渣系中La_2O_3的活度数据进行了简单的讨论.     

Mechanoluminescence in BaSi2O2N2:Eu

Mechanoluminescence (ML), a general term for the phenomenon in which light emission occurs during any mechanical action on a solid, can be divided roughly into two classes: destructive ML and non-destructive ML. For practical use in high-end applications (e.g. pressure sensors), materials with non-destructive ML properties are preferred. This paper reports on the strong non-destructive ML in BaSi₂O₂N₂:Eu. When irradiated in advance with ultraviolet or blue light, this phosphor shows intense blue-green light emission upon mechanical stimulation such as friction or pressure. The ML has an emission band peaking at 498 nm, which is ～4 nm red-shifted compared to the steady-state photoluminescence. The origin of the ML is discussed and related to the persistent luminescence of BaSi₂O₂N₂:Eu. The same traps are responsible for both phenomena. Based on the occurrence of ML in this phosphor, we were able to show that the predominant crystallographic structure of BaSi₂O₂N₂:Eu belongs to space group Cmc2₁.     

氢分子在贮氢材料Li2MgN2H2表面的吸附与解离

采用第一性原理计算方法研究了Li-Mg-N-H体系贮氢材料的放氢产物Li2MgN2H2的吸氢反应过程中的过渡态、表面电子态密度和表面能。结果表明:氢分子在Li2MgN2H2低指数表面中最低能量(100)表面的Mg-Mg-Li穴位吸附位置能够形成最稳定的吸附结构并发生解离,氢分子吸附能为-0.1898eV,解离能约为0.84eV(81kJ/mol),表明该反应所需的反应活化能仍较高,吸氢反应速度缓慢。     

The Quasi-Ternary System Cu2Se-Ga2Se3-GeSe2

The quasi-ternary system Cu₂Se-Ga₂Se₃-GeSe₂ was investigated using the methods of differential thermal and x-ray analysis. An isothermal section at 770 K and a liquidus surface projection of the phase diagram were constructed. The existence of the quaternary phase CuGaGeSe₄, the boundaries of solid solutions ranges of the system compounds were established.     

High temperature corrosion of Fe-Cr-Mn-alloys in H2-H2S and H2-H2O-H2S gas mixtures

The sulfidation of Fe-20% Cr-30% Mn, Fe-25%Cr-20%Mn and Fe-25% Cr was studied at 700°C in H₂-H₂S and the oxidation and sulfidation in H₂-H₂O-H₂S after preoxidation in H₂-H₂O. The sulfidation rate is strongly increased for the Mn-containing alloys, layers of (Mn,Cr)S and (Mn,Fe)Cr₂S₄ are formed. Also the oxidation rate is enhanced compared to Fe-25% Cr by formation of MnCr₂O₄ instead of Cr₂O₃. The sulfidation after preoxidation leads to internal and external sulfidation of the Mn-containing alloys. With increasing oxygen pressure p(O₂) = 10^?26…10^?22 atm. of the H₂-H₂O-H₂S mixtures the sulfidation is suppressed, for the higher oxygen pressure 10^?23 and 10^?22 atm. fast oxidation prevails under formation of MnCr₂O₄. Manganese cannot increase the sulfidation resistance of alloys, in spite of the stability and low degree of disorder of its sulfide, since the mixed sulfide (Mn,Cr)S is formed which has a high degree of disorder, high diffusivities and high growth rate according to the doping effect of trivalent Cr³⁺.     

34Cr2Ni2Mo

正34Cr2Ni2Mo结构钢具有高的强度、韧度和良好的淬透性和抗过热的稳定性,但白点敏感性高,有回火脆性。焊接性较差,焊前需经高温预热,焊后需消除应力,经调质后使用。一般制作强度高、塑性好的重要零部件,渗氮处理后制作特殊性能要求的重要零件,如轴类、齿轮、紧固件等。