合成了未见报道的标题配合物。通过化学分析、ICP和TG曲线确定了其化学式为K_8H_3[Y(PW_(11)O_(39))_2]·25H_2O;利用IR、UV、XRD、^(183)W-NMR、循环伏安等手段对其结构进行了表征,结果表明杂多阴离子为β_2型Keggin结构。采用稀...合成了未见报道的标题配合物。通过化学分析、ICP和TG曲线确定了其化学式为K_8H_3[Y(PW_(11)O_(39))_2]·25H_2O;利用IR、UV、XRD、^(183)W-NMR、循环伏安等手段对其结构进行了表征,结果表明杂多阴离子为β_2型Keggin结构。采用稀土多元渗的方法对配合物进行了气相热扩渗,经ICP和XPS测试表明:微量的稀土元素La和Ce可以渗入到配合物的体相,并与组份元素存在键合作用。扩渗后化合物的化学式为K_8H_6YLa_(0.11)Ce_(0.18)P_2W_4~ⅤW_(18)~ⅥO_(78)·15H_2O,其晶体属单斜晶系,晶胞参数:a=6.3775nm,b=3.6771nm,c=3.7727nm,β=90.192°,V=88.47326nm^3;导电性的测试结果表明:室温时,扩渗后试样的电导率提高了约10~3倍,且热稳定范围变宽,523K时的电导率为1.33×10^(-2)S·cm^(-1),有望成为实用化的导电材料;~1H MAS NMR测试结果表明其存在三种质子,其导电机理可能是质子导电。展开更多
Potassium tungsten bronze KxLayWO3 (x>0.5 and y<0.01) was synthesized by rare earth co-permeation method using α-K7[SiMg3(OH2)3W9O37] as the precursor. Binding energies of La, W, O and C were determined by XPS....Potassium tungsten bronze KxLayWO3 (x>0.5 and y<0.01) was synthesized by rare earth co-permeation method using α-K7[SiMg3(OH2)3W9O37] as the precursor. Binding energies of La, W, O and C were determined by XPS. From the XPS data, a peak at 34.21 eV indicates that some W6+ turned into W5+ by rare earth co- permeation. The binding energies La3d were the same in the surface and inner of the composite, showing that rare earth element La could diffuse into the body of the composite and the compound of KxLayWO3 was formed at the same time. The binding energies of O1s in KxLayWO3 surface were 531.4 eV and 532.0 eV, respectively, while peak at 531.4 eV disappeared through etching process. The result implies that the binding energy of 531.4 eV was due to the adsorbent O. In addition, the binding energies of C1s in the surface were 283.5 eV, 285.0 eV and 286.7 eV respectively, while the inner had only one peak at 285.0 eV due to standard C1s. This proves that there was no C in the core.展开更多
采用双层辉光离子渗金属技术,在工业纯铁和20钢表面进行W、Mo、Co多元共渗,形成Fe W Mo Co型渗镀复合层.对渗镀层进行了金相组织观察、成分及硬度测量,重点研究了镀层的相组成及镀层与基体间的结合强度.结果表明:纯铁和20钢表面镀层以...采用双层辉光离子渗金属技术,在工业纯铁和20钢表面进行W、Mo、Co多元共渗,形成Fe W Mo Co型渗镀复合层.对渗镀层进行了金相组织观察、成分及硬度测量,重点研究了镀层的相组成及镀层与基体间的结合强度.结果表明:纯铁和20钢表面镀层以金属钨、钼为基体,其上分布大量μ相,并有少量Laves相;镀层硬度高达1000～1400HV,固溶和时效处理对硬度提高影响不大;纯铁表面镀层在渗金属、固溶、时效状态下,持续加载100N未发生镀层剥落现象;20钢表面镀层经固溶处理后,所加载荷在100N内未发生剥落现象,但在渗金属及时效态,当载荷加至80N时,镀层开始剥落.展开更多
文摘合成了未见报道的标题配合物。通过化学分析、ICP和TG曲线确定了其化学式为K_8H_3[Y(PW_(11)O_(39))_2]·25H_2O;利用IR、UV、XRD、^(183)W-NMR、循环伏安等手段对其结构进行了表征,结果表明杂多阴离子为β_2型Keggin结构。采用稀土多元渗的方法对配合物进行了气相热扩渗,经ICP和XPS测试表明:微量的稀土元素La和Ce可以渗入到配合物的体相,并与组份元素存在键合作用。扩渗后化合物的化学式为K_8H_6YLa_(0.11)Ce_(0.18)P_2W_4~ⅤW_(18)~ⅥO_(78)·15H_2O,其晶体属单斜晶系,晶胞参数:a=6.3775nm,b=3.6771nm,c=3.7727nm,β=90.192°,V=88.47326nm^3;导电性的测试结果表明:室温时,扩渗后试样的电导率提高了约10~3倍,且热稳定范围变宽,523K时的电导率为1.33×10^(-2)S·cm^(-1),有望成为实用化的导电材料;~1H MAS NMR测试结果表明其存在三种质子,其导电机理可能是质子导电。
文摘Potassium tungsten bronze KxLayWO3 (x>0.5 and y<0.01) was synthesized by rare earth co-permeation method using α-K7[SiMg3(OH2)3W9O37] as the precursor. Binding energies of La, W, O and C were determined by XPS. From the XPS data, a peak at 34.21 eV indicates that some W6+ turned into W5+ by rare earth co- permeation. The binding energies La3d were the same in the surface and inner of the composite, showing that rare earth element La could diffuse into the body of the composite and the compound of KxLayWO3 was formed at the same time. The binding energies of O1s in KxLayWO3 surface were 531.4 eV and 532.0 eV, respectively, while peak at 531.4 eV disappeared through etching process. The result implies that the binding energy of 531.4 eV was due to the adsorbent O. In addition, the binding energies of C1s in the surface were 283.5 eV, 285.0 eV and 286.7 eV respectively, while the inner had only one peak at 285.0 eV due to standard C1s. This proves that there was no C in the core.
文摘采用双层辉光离子渗金属技术,在工业纯铁和20钢表面进行W、Mo、Co多元共渗,形成Fe W Mo Co型渗镀复合层.对渗镀层进行了金相组织观察、成分及硬度测量,重点研究了镀层的相组成及镀层与基体间的结合强度.结果表明:纯铁和20钢表面镀层以金属钨、钼为基体,其上分布大量μ相,并有少量Laves相;镀层硬度高达1000～1400HV,固溶和时效处理对硬度提高影响不大;纯铁表面镀层在渗金属、固溶、时效状态下,持续加载100N未发生镀层剥落现象;20钢表面镀层经固溶处理后,所加载荷在100N内未发生剥落现象,但在渗金属及时效态,当载荷加至80N时,镀层开始剥落.
