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
ZHOU Bai-Bin *,1,2 WEI Yong-De 1 LI Zhong-Hua 1 ( 1 Department of Applied Chemistry,Ha rbin Institute of Technology ￡?Harbin￡±￡ì￡°￡°￡°￡±￡(c)( 2 Department of Chemistry,Harbin Norm...ZHOU Bai-Bin *,1,2 WEI Yong-De 1 LI Zhong-Hua 1 ( 1 Department of Applied Chemistry,Ha rbin Institute of Technology ￡?Harbin￡±￡ì￡°￡°￡°￡±￡(c)( 2 Department of Chemistry,Harbin Normal University￡?Harbin￡±￡ì￡°￡°￡?￡°￡(c) The air-solid interface reaction of Ce,Lu with K10 H 3[Gd (SiMo 4 W￡*O￡3￡1￡(c) 2]through chemistry-heated permeation is reported for the fi rst time￡(r)The permeated complex is characterized by ICP and the result shows tha t the mini mum Ce,Lu can permeate into the inner sph ere of K 10 H ￡3 ￡?Gd ￡¨SiMo ￡′ W ￡* O ￡3￡1 ￡(c) 2]The IR ,XRD patterns give the eviden ce that after permeation the comple x still keeps the Keggin structure,howe ver,its crystal structure is different from the complex before permeation￡(r)The cond uctivity of the permeated complex has been measured with the four-electr ode method and the data show that the co nductivity of the complex after permeation is 10 6 times higher than that of the sample before permeation and reaches ￡′￡(r)84 6×10 -1 S·cm -1 ￡(r)These indicate that the permeated c omplex is a good solid electrolyte and further appli cations are also expected￡(r)展开更多
The technological condition for the preparation of BaTiO 3 ceramics doped with Nd ￡2O￡3 by Sol￡-Gel was deter￡-mined through orthogonal experimen t￡(r)WhennBa ￡¨Ac ￡(c) ￡2??nTi ￡¨OC ￡′H￡1￡(c)￡...The technological condition for the preparation of BaTiO 3 ceramics doped with Nd ￡2O￡3 by Sol￡-Gel was deter￡-mined through orthogonal experimen t￡(r)WhennBa ￡¨Ac ￡(c) ￡2??nTi ￡¨OC ￡′H￡1￡(c)￡′??n Nd ￡2O￡3??nCH￡3￡¨CH￡2￡(c)2CH 2OH∶n H2 O￡1/2￡±￡(r)￡°￡°??￡±￡(r)￡°￡°??￡°￡(r)￡°￡°￡3??￡*￡(r)￡3￡°??￡3￡*￡(r)￡°￡′￡?pH ￡1/2￡3￡(r)￡μ￡?T￡1/225℃,the light-yellow-transparen t-stable solution and thorough tran sparent gel was generat￡-ed￡?the transforming time of solutio n to gel was ￡2￡μh￡(r)The crystal structur e and particle size of BaTiO3 ceramics doped with Nd 2O3 were studied by SEM and X-ray respectively￡?the type of the crystal was tetragonal￡?the particle size was about ￡2￡′￡(r)7nm￡(r)The dielectric constant ￡¨|?￡(c)and dielectric loss￡¨tan|?￡(c)of BaTiO3 ceramics doped with Nd 2O3 were determined between 10 4 ?10 6 Hz,and the results showed that the di electric constant was increased obviously,the dielectric loss was d ecreased clear and the resistivity(ρ V ￡(c)was also decreased noticeably￡(r)展开更多
BaTiO 3 ceramics doped with Nd 2 O 3 (the additive content was respectively 0.001,0.002,0.003,0.005,0.01,0.03mol)were prepared by Sol-Gel method.Effects of Nd 2 O 3 contents on the dielectric constant (ε),the dielect...BaTiO 3 ceramics doped with Nd 2 O 3 (the additive content was respectively 0.001,0.002,0.003,0.005,0.01,0.03mol)were prepared by Sol-Gel method.Effects of Nd 2 O 3 contents on the dielectric constant (ε),the dielectric loss(tanδ),the Curie-temperature(T C )and the resistivity(ρ)of BaTiO 3 ceramic were studied.When Nd 2 O 3 content was 0.001mol and 0.002mol,t he dielectric constant was increase d obviously,but the dielectric loss was also increased.When Nd 2 O 3 content was 0.003mol,the dielectric constant was increased,and the die lectric loss was decreased,which was suitable fo r application in condenser.The resistivity was decreased obviously with the increasing of Nd 2 O 3 contents,the resistivity was the sm allest when Nd 2 O 3 content was 0.001mol.The Curie-temperature was also decreased with the increasing of Nd 2 O 3 contents.展开更多
在 Li Nb O3 中掺进 3 mol%、5mol%、7mol% Zn O生长 Zn∶ L i Nb O3 晶体 .测试Zn∶ L i Nb O3 晶体的吸收光谱 ,研究 Zn∶ Li Nb O3 晶体吸收边紫移的机制 .测试 Zn∶ Li Nb O3晶体的红外光谱 ,研究 Zn( 7mol% )∶L i Nb O3 晶体 OH-...在 Li Nb O3 中掺进 3 mol%、5mol%、7mol% Zn O生长 Zn∶ L i Nb O3 晶体 .测试Zn∶ L i Nb O3 晶体的吸收光谱 ,研究 Zn∶ Li Nb O3 晶体吸收边紫移的机制 .测试 Zn∶ Li Nb O3晶体的红外光谱 ,研究 Zn( 7mol% )∶L i Nb O3 晶体 OH-吸收峰由 3 484cm- 1移到 3 53 0 cm- 1的机制 .测试 Zn∶ L i Nb O3 晶体倍频转换效率和相位匹配温度 ,研究 Zn∶ Li Nb O3展开更多
Eight new complexes were synthesize d for the first time.The compounds which have the general formula K x H 2 [PM(OH 2 )Mo 7 W 2 V 2 O 39 ]·nH 2 O(M=Cr 3+ ,Mn 2+ ,Fe 3+ ,Co 3+ ,Ni 2+ ,Cu 2+ ,Zn 2+ ,Cd 2+ ;x=4or 5...Eight new complexes were synthesize d for the first time.The compounds which have the general formula K x H 2 [PM(OH 2 )Mo 7 W 2 V 2 O 39 ]·nH 2 O(M=Cr 3+ ,Mn 2+ ,Fe 3+ ,Co 3+ ,Ni 2+ ,Cu 2+ ,Zn 2+ ,Cd 2+ ;x=4or 5)were de-termined by conductance titration a nd elemental analysis.The analysis of IR,UV,XRD and ESR show that the products hold the Keggin structure a nd TG-DTA,IR,XRD at various tempera tures and water solubility test also give the evidences that the range of pyrolysis temperature is 300～350℃.T he study on the substitutional reaction of coordinated water by optical ligand quinine shows that the S N 2nucleophilic substitution occure s when Ni is con-tained in the compound and S N 1nucleophilic substitution occure s when Cu is contained.These also con firmed that the transitional metals are in the in ner sphere of the complexes.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ZHOU Bai-Bin *,1,2 WEI Yong-De 1 LI Zhong-Hua 1 ( 1 Department of Applied Chemistry,Ha rbin Institute of Technology ￡?Harbin￡±￡ì￡°￡°￡°￡±￡(c)( 2 Department of Chemistry,Harbin Normal University￡?Harbin￡±￡ì￡°￡°￡?￡°￡(c) The air-solid interface reaction of Ce,Lu with K10 H 3[Gd (SiMo 4 W￡*O￡3￡1￡(c) 2]through chemistry-heated permeation is reported for the fi rst time￡(r)The permeated complex is characterized by ICP and the result shows tha t the mini mum Ce,Lu can permeate into the inner sph ere of K 10 H ￡3 ￡?Gd ￡¨SiMo ￡′ W ￡* O ￡3￡1 ￡(c) 2]The IR ,XRD patterns give the eviden ce that after permeation the comple x still keeps the Keggin structure,howe ver,its crystal structure is different from the complex before permeation￡(r)The cond uctivity of the permeated complex has been measured with the four-electr ode method and the data show that the co nductivity of the complex after permeation is 10 6 times higher than that of the sample before permeation and reaches ￡′￡(r)84 6×10 -1 S·cm -1 ￡(r)These indicate that the permeated c omplex is a good solid electrolyte and further appli cations are also expected￡(r)
文摘The technological condition for the preparation of BaTiO 3 ceramics doped with Nd ￡2O￡3 by Sol￡-Gel was deter￡-mined through orthogonal experimen t￡(r)WhennBa ￡¨Ac ￡(c) ￡2??nTi ￡¨OC ￡′H￡1￡(c)￡′??n Nd ￡2O￡3??nCH￡3￡¨CH￡2￡(c)2CH 2OH∶n H2 O￡1/2￡±￡(r)￡°￡°??￡±￡(r)￡°￡°??￡°￡(r)￡°￡°￡3??￡*￡(r)￡3￡°??￡3￡*￡(r)￡°￡′￡?pH ￡1/2￡3￡(r)￡μ￡?T￡1/225℃,the light-yellow-transparen t-stable solution and thorough tran sparent gel was generat￡-ed￡?the transforming time of solutio n to gel was ￡2￡μh￡(r)The crystal structur e and particle size of BaTiO3 ceramics doped with Nd 2O3 were studied by SEM and X-ray respectively￡?the type of the crystal was tetragonal￡?the particle size was about ￡2￡′￡(r)7nm￡(r)The dielectric constant ￡¨|?￡(c)and dielectric loss￡¨tan|?￡(c)of BaTiO3 ceramics doped with Nd 2O3 were determined between 10 4 ?10 6 Hz,and the results showed that the di electric constant was increased obviously,the dielectric loss was d ecreased clear and the resistivity(ρ V ￡(c)was also decreased noticeably￡(r)
文摘BaTiO 3 ceramics doped with Nd 2 O 3 (the additive content was respectively 0.001,0.002,0.003,0.005,0.01,0.03mol)were prepared by Sol-Gel method.Effects of Nd 2 O 3 contents on the dielectric constant (ε),the dielectric loss(tanδ),the Curie-temperature(T C )and the resistivity(ρ)of BaTiO 3 ceramic were studied.When Nd 2 O 3 content was 0.001mol and 0.002mol,t he dielectric constant was increase d obviously,but the dielectric loss was also increased.When Nd 2 O 3 content was 0.003mol,the dielectric constant was increased,and the die lectric loss was decreased,which was suitable fo r application in condenser.The resistivity was decreased obviously with the increasing of Nd 2 O 3 contents,the resistivity was the sm allest when Nd 2 O 3 content was 0.001mol.The Curie-temperature was also decreased with the increasing of Nd 2 O 3 contents.
文摘在 Fe∶Li Nb O3 中掺进 3 mol%和 6mol% Mg O,生长了 Mg∶Fe∶L i Nb O3 晶体 .测试了 Mg∶Fe∶Li Nb O3 晶体抗光致散射能力、衍射效率、响应时间和光电导 .推导响应时间与光电导之间的关系 .在 Fe∶Li Nb O3 晶体中掺进 6mol%的 Mg2 + ,它的抗光致散射能力比Fe∶L i Nb O3 晶体提高一个数量级 ,响应速度比 Fe∶Li Nb O3
文摘在 Li Nb O3 中掺进 3 mol%、5mol%、7mol% Zn O生长 Zn∶ L i Nb O3 晶体 .测试Zn∶ L i Nb O3 晶体的吸收光谱 ,研究 Zn∶ Li Nb O3 晶体吸收边紫移的机制 .测试 Zn∶ Li Nb O3晶体的红外光谱 ,研究 Zn( 7mol% )∶L i Nb O3 晶体 OH-吸收峰由 3 484cm- 1移到 3 53 0 cm- 1的机制 .测试 Zn∶ L i Nb O3 晶体倍频转换效率和相位匹配温度 ,研究 Zn∶ Li Nb O3
文摘Eight new complexes were synthesize d for the first time.The compounds which have the general formula K x H 2 [PM(OH 2 )Mo 7 W 2 V 2 O 39 ]·nH 2 O(M=Cr 3+ ,Mn 2+ ,Fe 3+ ,Co 3+ ,Ni 2+ ,Cu 2+ ,Zn 2+ ,Cd 2+ ;x=4or 5)were de-termined by conductance titration a nd elemental analysis.The analysis of IR,UV,XRD and ESR show that the products hold the Keggin structure a nd TG-DTA,IR,XRD at various tempera tures and water solubility test also give the evidences that the range of pyrolysis temperature is 300～350℃.T he study on the substitutional reaction of coordinated water by optical ligand quinine shows that the S N 2nucleophilic substitution occure s when Ni is con-tained in the compound and S N 1nucleophilic substitution occure s when Cu is contained.These also con firmed that the transitional metals are in the in ner sphere of the complexes.
