微波均相合成Ce_(0.75)Zr_(0.25)O_2粉体及其烧结性

以Ce(NO3)3.6H2O和ZrOCl2.8H2O为原料,以尿素为沉淀剂,利用微波均相法制备Ce0.75Zr0.25O2粉体,采用热分析仪、X射线衍射仪、扫描电子显微镜表征制备的粉体,对制备的粉体压制成型并烧结,用扫描电子显微镜观察烧结体的微观结构。结果表明,合成Ce0.75Zr0.25O2前驱体时加入2倍于Ce3+物质的量的H2O2可以减小固溶体颗粒粒度,降低固溶温度30℃;所制备的固溶体粉体具有良好的烧结性,在1 550℃得到烧结体的相对密度达99.57%。     

Ce0.6Zr0.35Pr0.05O2纳米固溶体的制备及性能研究

用共沉淀法制备出Ce0.6Zr0.35Pr0.05O2纳米固溶体,并利用TG-DTA-DTG、XRD、TEM和H2-TPR等方法对样品的物相结构、晶粒大小、还原性及高温热稳定性进行表征.结果表明,Ce0.6Zr0.35Pr0.05O2纳米固溶体为物相结构稳定的立方相固溶体,该粉体的平均粒度为10 nm左右,分散性好,而且与Ce0.6Zr0.4O2相比,在Ce0.6Zr0.35Pr0.05O2中,Pr的存在明显提高了其还原性和高温热稳定性.     

水热法制备Ba（ZrTi）O3纳米管的研究

以Ti25Zr合金阳极氧化获得的Ti-Zr-O纳米管为模板,采用Ba(OH)2通过水热反应法制备Ba(ZrTi)O3纳米管,研究了温度、Ba(OH)2·6H2O浓度等工艺参数对Ba(ZrTi)O3纳米管微观组织结构和形貌的影响规律。SEM、TEM及XRD和XPS表征研究表明,获得了管径为(70±5)nm,长度为6μm的BaTi0.75Zr0.25O3纳米管,并且纳米管的结晶性良好;优化出水热法制备BaTi0.75Zr0.25O3纳米管的最佳合成温度为150℃,Ba(OH)2·6H2O的浓度为0.08mol/L。     

稀土Dy和Ce共掺杂La2Zr2O7新型热障涂层用陶瓷材料

用化学沉淀法制备了稀土Dy和Ce共掺杂La2Zr2O7新型热障涂层用陶瓷粉末Lal.7Dy0.3(Zr0.8CeZr0.2)2-O7(LDCZ).通过X射线衍射、扫描电镜、高温膨胀仪、DSC和激光热导仪对粉末相结构、不同煅烧温度下的相组成、微观结构,高温相稳定性,热膨胀系数和导热系数进行了分析.结果表明,稀土共掺杂的La1.7Dy0.3(Zr0.8CeZr0.2)2O7保持了烧绿石结构,120℃时粉末为无定形的混合氧化物,900℃时转化为复合氧化物,1200℃时转变为单一的烧绿石相;高温下LDCZ无明显相变;添加Dy和Ce不仅可提高锆酸镧的热膨胀系数,使其高于8YSZ的热膨胀系数,并可使其导热系数较La2Zr2O7降低25%以上,达到1.28～1.07W/m.K.     

高分子凝胶改进铈锆固溶体的制备及表征

以不同摩尔比的Ce(NO3)4·6H2O和Zr(NO3)4·5H2O为固溶体原料,在其中添加适量的丙烯酰胺(C3H5NO)、N’N亚甲基双丙烯酰胺(C7H10N2O2)和过硫酸铵((NH4)2S2O8)作为高分子凝胶剂,制备出高分子凝胶改进铈锆固溶体,研究了Ce/Zr比对铈锆固溶体性能的影响。结果表明,高分子用单体与网络剂的三维聚合网络,分散固溶体的粉体颗粒,煅烧高分子后形成多孔结构;上述两因素的协同作用促进了多孔纳米铈锆固溶体的形成。当C3H5NO与C7H10N2O2的质量比为5∶1、混合溶质的溶度为0.04 mol/L并经合适的热处理可以得到粒径为10-20 nm的铈锆固溶体。X射线衍射结果表明,Ce/Zr摩尔比为3∶7~5∶5时固溶体为四方相结构;Ce/Zr摩尔比升至6∶4~7∶3时固溶体为立方相结构;晶格常数随着Zr+的增多而减小。N2吸附-脱附实验结果表明,Ce/Zr摩尔比为6:4时固溶体具有优异的比表面积和孔结构数据:比表面积为120.5 m2·g-1;孔径达到8.12 nm;孔容高达0.22 cm3/g。扫描电镜观察结果显示,铈锆固溶体具有蜂窝状的多孔性结构。     

负载磷钼杂多酸/La0.7Ca0.3Fe0.25Co0.75O3/聚吡咯的制备及光催化性能研究

采用甘氨酸-硝酸盐燃烧法成功制备了La0.7Ca0.3Fe0.25Co0.75O3钙钛矿型复合氧化物,以(NH4)2S2O8为氧化剂,运用化学氧化法合成La0.7Ca0.3Fe0.25Co0.75O3/聚吡咯薄膜,然后通过静电自组装方法制备了一种新的表面负载修饰型复合光催化剂La0.7Ca0.3Fe0.25Co0.75O3/PPy/PMO12。采用XRD、SEM、FT-IR对催化剂的物化结构进行了表征。光催化性能测试是以亚甲基蓝染料的水溶液为降解目标,结果表明,PMo12的负载修饰改进了La0.7Ca0.3-Fe0.25Co0.75O3/PPy光催化剂的催化活性。     

共沉淀法制备ZrO2-Al2O3-CeO2的煅烧反应过程及物相表征

以氨水为沉淀剂，采用共沉淀法按一定比例分别制备了ZrO2-Al2O3-CeO2、ZrO2-Al2O3-CeO2、ZrO2-Al2O3-CeO2等4种前驱复合粉体。利用差热-热重分析（DTA/TG）和X射线衍射（XRD）对4种粉体的热转变过程以及不同温度煅烧后的物相组成进行了对比分析，研究了ZrO2-Al2O3-CeO2复合粉体间在煅烧过程中的化学反应及相互影响。结果表明：CeO2与ZrO2优先形成固溶体，CeO2与Al2O3直到1300℃也未发生任何反应；Al2O3的存在明显提高了c-（Ce，Zr）O2的结晶温度，1300℃退火后t-（Ce，Zr）O2仍能保留到室温。     

SPS制备纳米晶Bi_(0.75)Er_(0.25)O_(1.5)固体电解质

以分析纯Bi2O3和Er2O3为原料,采用反向滴定共沉淀法合成Bi和Er的氢氧化物前驱体,并对共沉淀的pH值条件进行了分析。将该前驱体在500℃焙烧3h后得到Bi0.75Er0.25O1.5的纳米粉体,高温XRD结果表明该粉体主要为β相,谢乐公式计算平均晶粒尺寸为10nm,并且随温度升高在650℃转变为δ相。通过热力学计算,确定了SPS下烧结Bi0.75Er0.25O1.5陶瓷适宜的温度和氧分压条件,最后在测试温度为500℃保温1min得到了相对密度达到96%的δ相纳米晶的Bi0.75Er0.25O1.5陶瓷,平均晶粒尺寸为18nm。     

复合溶胶-凝胶法制备锆酸钐涂层的工艺研究

以ZrO(NO3)2·2H2O,Sm2 O3为原料,柠檬酸(C6H8O7·H2O)为整合剂,采用溶胶-凝胶工艺分别制备了Sm2 Zr2O7前驱体溶胶和Sm2Zr2O7粉体,将两者按比例球磨混合制备复合浆料;在ZrB2/SiC基体上铺Al2O3粉高温处理制备过渡层.采用浸渍提拉法在含过渡层的ZrB2/SiC基体上制备出了Sm2Zr2O7涂层.用X射线衍射仪(XRD)分析了Sm2Zr2O7粉体的物相,用场发射扫描电镜(SEM)对粉体、过渡层及涂层的微观形貌进行了表征.结果表明:1150℃保温2h可以制备出具有单一焦绿石结构的Sm2 Zr2O7粉体;采用烧结制度为0～1100℃,8℃/min,1100～1550℃,4℃/min,可以制备出平整均匀的Al2O3过渡层;前驱体Zr离子浓度为1.87mol/L,固含量为45％时,经三次浸涂可以制备出完整的Sm2Zr2O7涂层.     

Ce对Na0.5Bi0.5TiO3粉体的掺杂和扩渗改性研究

为改善Na0.5Bi0.5TiO3材料的电性能,采用溶胶-凝胶法制备了Na0.5Bi0.5TiO3粉体.通过液相Ce掺杂和气相Ce扩渗两种方法,对Na0.5Bi0.5TiO3粉体进行了改性,采用扫描电子显微镜(SEM)、X射线衍射仪(XRD)、阻抗分析仪和电阻仪对改性前后Na0.5Bi0.5TiO3粉体的组成、结构和电性能的变化进行了研究.结果表明:Ce元素的添加有助于Na0.5Bi0.5TiO3粉体电阻率的降低,而扩渗改性使电阻率的降低更为显著,经600℃扩渗的Na0.5Bi0.5TiO3粉体的电阻率由3.71×106Ω.m降至2.39×101Ω.m;稀土Ce掺杂使Na0.5Bi0.5TiO3的介电常数减小,而Ce扩渗使Na0.5Bi0.5TiO3的介电常数显著增大;Ce掺杂使粒径更加均匀,而随着气相扩渗温度的提高,晶粒粒径逐渐变大;Ce掺杂没有改变Na0.5Bi0.5TiO3的主晶相结构,但Na0.5Bi0.5TiO3粉体经Ce扩渗后,出现了单质Bi及Bi2Ti2O7、Na2Ti9O19、Na2Ti6O13的特征峰.     

Bi/WO3复合光催化材料的制备及其抗菌性能

以WO₃为基底,五水硝酸铋(Bi(NO₃)₃·5H₂O)为铋源,通过紫外还原法在WO₃表面沉积具有表面等离子体效应(SPR)的半金属Bi0,制备了具有可见光响应的Bi/WO₃复合光催化材料。以大肠杆菌(E. coli)和金黄色葡萄球菌(S. aureus)为实验对象,考察了所制备复合材料的光催化抗菌性能、结合结构和光电化学性质表征,对Bi的负载量进行了优化。研究发现:优选得到的0.6 mmol Bi/WO₃能够在120 min内灭杀99%以上的细菌。进一步考察了灭菌机制,通过添加不同种类的捕获剂,结合电子顺磁共振(ESR)技术,发现羟基自由基(·OH)和超氧自由基(·O₂?)是导致E. coli失活的主要活性物种。      

活性炭模板法制备锡酸锌掺杂磷化合物及表征

选用磷酸活化后的活性炭为模板,NaSnO₃·3H₂O、ZnSO₄·7H₂O为原料,通过生物质模板法制备了锡酸锌掺杂磷(Zn₂SnO₄/P)化合物。通过X射线粉末衍射(XRD)、扫描电子显微镜(SEM)和N_2吸脱附等温线对制备的Zn₂SnO₄/P的结构、形貌进行表征。结果表明:Zn₂SnO₄/P为尖晶石结构,其形貌基本上和活性炭相匹配。其比表面积、孔体积和平均孔径分别为87m²/g、0.20cm³/g和9.0nm。     

MgCl2对锌在干湿交替环境中腐蚀行为的影响

使用腐蚀失重、X射线衍射(XRD)、扫描电子显微镜与能谱(SEM-EDS)等手段研究了干湿交替环境中MgCl₂对锌腐蚀行为的影响。结果表明,MgCl₂对锌的腐蚀有显著的抑制作用;在沉积NaCl条件下锌表面的腐蚀产物为Zn₅(OH)₈Cl₂·H₂O、Zn₄CO₃(OH)₆·H₂O和Zn(OH)₂,而在沉积MgCl₂条件下锌表面的腐蚀产物只有Zn₅(OH)₈Cl₂·H₂O。在干湿交替环境中MgCl₂对锌腐蚀行为的影响主要是Mg²⁺与氧还原反应产生的OH^-结合使阴极区的pH值降低造成的。     

SiO_2含量对氧化铁基Fe_2O_3-SiO_2二元复合干凝胶性能的影响

以水合氯化铁和正硅酸乙酯为前驱物,通过溶胶-凝胶法制备不同SiO_2含量的氧化铁基Fe_2O_3-SiO_2二元复合凝胶,利用冷冻干燥法对凝胶进行干燥得到复合干凝胶。分别采用BET、IR和SEM对复合凝胶的比表面积、孔结构、红外吸收峰和表面形貌进行分析。结果表明,复合凝胶的比表面积和孔体积随着SiO_2含量的增加而增加...     

Conduction analysis of Li2O doped 0.2[Pb(Mg1/3Nb2/3)]–0.8[PbTiO3–PbZrO3] ceramics fabricated by columbite precursor method

We have fabricated 0.2Pb(Mg_1/3Nb_2/3)O₃–0.8Pb(Zr_0.475Ti_0.525)O₃ [PMN–PZT] ceramics doped with various amounts of Li₂O (0, 0.05, 0.1, 0.2, 0.3 wt.%) using the columbite precursor method. The effects of Li-doping on the conduction behavior of PMN–PZT ceramics are discussed in relation to the low frequency dielectric dispersion and frequency domain measurement. The Li-doped PMN–PZT ceramics sintered at 950 °C showed a sufficient densification with large dielectric constant and low dielectric loss. The incorporation of Li⁺ ion in PMN–PZT ceramics led to an appreciable reduction in electrical conductivity and further enhanced the ferroelectric and piezoelectric properties. The activation energies of PMN–PZT + xLi₂O (x = 0, 0.05, 0.1, 0.2, 0.3 wt.%) ceramics calculated from ac conductivity measurement using the Arrhenius relation were 1.05, 1.25, 1.27, 1.38 and 1.41 eV, respectively. The conduction behavior is examined in the low frequency and high temperature region and the results are discussed in detail through crystal defect mechanism.     

可磁分离ZnFe2O4-TiO2/还原氧化石墨烯复合材料的制备及光催化性能

以TiO2(P25)、 Fe(NO3)3·9H2O、 Zn(NO3)2·6H2O和氧化石墨烯(GO)为原料,通过一步溶剂热法合成可磁分离的ZnFe2O4-TiO2/还原氧化石墨烯(rGO)复合材料。采用UV-Vis、 Raman、 XRD、 SEM和EDS对ZnFe2O4-TiO2/rGO复合材料进行表征,并研究不同rGO比例的ZnFe2O4-TiO2/rGO对模拟染料废水亚甲基蓝(MB)的光催化降解性能。GO在溶剂热反应过程中,被还原成rGO。由于ZnFe2O4和rGO的加入,不仅使ZnFe2O4-TiO2/rGO实现对可见光的吸收,而且使其具有磁性,便于分离和回收利用。当GO质量分数为5wt%时, ZnFe2O4-TiO2/rGO显现出对MB最佳的光催化活性, 60 min光照后的降解率达到99.1%。通过光催化活性物种捕获实验得出ZnFe2O4-TiO2/rGO复合材料降解MB的过程中,活性物种主要为·OH和·O2-, TiO2导带(CB)中的光生电子(e+)转移到ZnFe2O4的价带(VB),遵循Z型转移机制。光催化剂稳定性实验表明, ZnFe2O4-TiO2/rGO复合材料具有优越的稳定性,可作为太阳光照射下降解有机染料的光催化剂。     

Preparation of nanocrystalline SnO2 thin film coated Al2O3 ultrafine particles by fluidized chemical vapor deposition

Fluidized chemical vapor deposition (FCVD) technology was developed for coating SnO₂ thin film on Al₂O₃ ultrafine particles. TEM and HREM analysis found that SnO₂ films with different structures were deposited by controlling the coating temperature, reactant concentration, etc. Nanocrystalline SnO₂ film was coated at 573.15 K by gas phase reaction of SnCl₄ with H₂O. EPMA and EDS studies indicated that the distribution of SnO₂ inner and outer of the agglomerates was uniform. Nucleation and film deposition were coexisted mechanism during the FCVD coating process. The fraction of SnO₂ in the composite particles increased with increasing coating temperature, SnCl₄ concentration, and coating time. The mass fraction of SnO₂ in the composite particles increased strongly with the ratio of P_H2O and P_SnCl4 at low mole ratio of H₂O with SnCl₄, but increased little under the conditions of excess H₂O with respect to SnCl₄.     

Effect of N2O/SiH4 ratio on the properties of low-temperature silicon oxide films from remote plasma chemical vapour deposition

Silicon oxide films have been deposited with remote plasma chemical vapour deposition (RPCVD) at low temperatures (<300 °C) from SiH₄---N₂O. The effect of a gas-phase reaction on the SiO₂ film properties and Si/SiO₂ interface was investigated. As the partial pressure ratio was increased above N₂O/SiH₄ = 4, a gas-phase reaction with powder formation was observed, which degraded film properties, increased surface roughness, and decreased deposition rate. When N₂O/SiH₄ <4, there was no detectable IR absorption in the film associated with hydrogen-related bonds (Si---OH and Si---H) but when N₂O/SiH₄ >4, the incorporation of Si---OH bond became significant and Si¹⁺, intermediate state silicon at the interface, was more abundant. The oxide fixed charge, interface trap density, surface roughness and leakage current were increased when there was powder formation in the gas phase. High plasma power also favoured the powder formation in the gas phase. C---V and I---V characteristics were measured and it was shown that these electrical properties were directly related to the process condition and material properties of the oxide and the Si/SiO₂ interface.     

水蒸气二氧化碳共活化制备聚苯胺基活性碳在离子液体超级电容器中的应用

通过水蒸气二氧化碳(H2 O(gas)-CO2)共活化的物理活化方法制备聚苯胺基活性碳被广泛应用于商业活性碳的规模化生产,相比于化学活化方法,该方法制备的活化产物无活化剂残留、 清洗简单且工艺过程环保.以聚苯胺为原料,探究了H2 O(gas)的量和CO2分压对活化产物的影响.采用氮气吸/脱附、 扫描电镜(SEM)、 透...     

Solution-phase synthesis of smaller cuprous oxide nanocubes

Smaller cuprous oxides (Cu₂O) nanocubes were synthesized by solution-phase method at 160 °C, using ethylene glycol reducing Cu(NO₃)₂·3H₂O with poly(vinylypyrrolidone) (pvp) as capping agent. The Cu₂O nanocubes were characterized by field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED) and X-ray powder diffraction (XRD). SEM showed that most of Cu₂O nanocubes were uniform and monodisperse, with the average edge length about 130 nm. The TEM results were consistent with the SEM results. Selected area electron diffraction (SAED) suggested that as-prepared Cu₂O nanocubes were single crystalline. The geometric shape and size of Cu₂O nanoparticles were greatly affected by the presence of PVP and its molar ratio (in repeating unit) relative to copper nitrate, temperature and the concentration of Cu(NO₃)₂·3H₂O. The mechanism of Cu₂O nanocubes formation was also discussed.