基于双金属MOFs 制备Co3O4/In2O3 复合物及其气敏性能的研究

以硝酸铟(In(NO₃)₃·xH₂O)、对苯二甲酸(H₂BDC)、六水合硝酸钴(Co(NO₃)· 6H₂O) 为原料, 首先采用一锅油浴法合成了含有Co²⁺ 的铟基金属有机框架材料(MOFs) Co²⁺/CPP-3(In) 材料, 然后在450 ℃ 下焙烧制备Co₃O₄/In₂O₃ 复合物气敏材料, 将Co₃O₄/In₂O₃ 复合物的粉体制作成传感器, 并对其气敏性能进行研究。利用扫描电子显微镜和X 射线衍射仪(XRD) 对双金属MOFs Co²⁺/CPP-3(In) 材料和Co₃O₄/In₂O₃ 复合物进行表征, 采用静态配气法测试其气敏性能。结果表明, Co₃O₄/In₂O₃(n_Co : n_In = 0.4 : 1) 样品的形貌保留了其MOFs 前驱体的棒状结构, 棱柱形框架更为突出, 表面呈凹陷状, 棒体中间粗两边细, 六角截面和棒体均布满了孔洞。结合EDX 和XRD 表征结果, Co²⁺/CPP-3(In) MOFs 前驱体完全转化成Co₃O₄/In₂O₃ 复合物; Co₃O₄/In₂O₃(n_Co : n_In = 0.4 : 1) 复合物在 70 ℃ 下对5×10^-6 H₂S 的气敏性能最优, 响应值达到153, 是同条件下纯备In₂O₃对H₂S 响应值的5 倍, 并且有较好的重复性、选择性和稳定性。     

介孔SnO_2纳米材料的制备及酒精气敏特性研究

为了探究新型气敏材料的制备方法,降低普通气敏材料的工作温度及生产能耗与成本,文中采用分子模板法,以非离子表面活性剂十二胺和阳离子表面活性剂十六烷基三甲基溴化铵为模板,结合水热法合成孔径尺寸为5~6nm的介孔SnO2纳米结构材料.通过广角度和小角度X射线衍射及透射电子显微镜等方法对产物进行表征,用CGS-1TP智能分析气敏系统上进行气敏性能各项参数的测定.以所制备的纳米SnO2为气敏材料,对0.1×10-4~2×10-4的酒精进行了气敏测试.测试结果表明:介孔SnO2纳米材料在工作温度为152℃(普通温度为400℃)时,对2×10-1‰酒精的最大灵敏度为312,为普通SnO2纳米材料的5~10倍,响应时间为16s,大大降低了气敏元件的工作温度﹑响应时间和灵敏度.表明所制备的具有介孔形貌的SnO2纳米材料对酒精的气敏性能良好,相比普通的气敏材料具有大规模﹑低成本和低能耗的优势,在酒精的生产与监测方面具有良好的应用前景.     

WO_3纳米粉体的制备及其气敏性能分析

以PEG-400为分散剂制得WO3纳米粉体,用粉末X-射线衍射仪(XRD)和透射电镜(TEM)对产物的物相和形貌进行了表征。结果显示:产物为球形颗粒,600℃下热处理2h颗粒平均粒径为80nm。将粉体制成旁热式气敏元件,气敏性能测试结果表明:该WO3纳米粉体对三甲胺具有较高的灵敏度和选择性。600℃下热处理2h材料气敏性最好,在240℃(最佳工作温度)下对体积分数为1×10-8的三甲胺灵敏度可达到3.2。     

ZnO纳米阵列结构酒精气敏特性研究

为了提高ZnO气敏元件对酒精蒸汽的气敏响应,改善气敏元件的稳定性及耐久性,文中采用化学水热法在预处理后的陶瓷管电极表面生长ZnO纳米阵列材料,通过退火处理后得到薄膜ZnO气敏元件.借助X射线衍射仪和扫描电子显微镜对所得产物的晶体结构和形貌进行表征.采用静态配气法对其进行不同浓度(1×10-4,2×10-4,5×10-4,1×10-3)的酒精蒸汽气敏性能测试.实验结果表明:该结构为分散均匀的ZnO纳米线阵列状结构,该纳米结构薄膜气敏元件具有较好的气敏性能,具有较快的响应及恢复.随环境中酒精蒸汽浓度的增加,其气敏性能逐步提升,在5×10-4酒精蒸汽气敏浓度下气敏性能达到峰值.不同浓度条件下,气敏响应及恢复时间不同,在1×10-4条件下度响应时间最快,1×10-3浓度下恢复时间最快,2×10-4浓度下响应恢复时间最均衡.     

In、Sn共掺杂ZnO纳米线的制备及其气敏性能研究

为了改善纯ZnO纳米线的气敏性能,采用物理蒸发法制备出In、Sn共掺杂的ZnO纳米线,利用XRD、SEM、TEM对产物的形貌、结构进行表征,采用CGS-1TP智能气敏分析系统对其进行酒精气敏性能测试.结果表明,制备出的In、Sn共掺杂ZnO纳米线具有六方纤锌矿结构,平均直径约为80nm,In元素与Sn元素的掺杂量分别为0.12%和1.1%.在最佳工作温度225℃条件下,对气体浓度为400ppm的酒精蒸气的灵敏度S(Ra/Rg)为39.06,响应-恢复时间分别为9s和5s,比同等测试条件下纯ZnO纳米线的灵敏度提高63.9%,响应-恢复时间分别缩短1s和2s.     

贯通大孔SnO_2纳米材料的制备及气敏性能研究

为改善二氧化锡(SnO_2)的气敏性能,以聚苯乙烯(PS)微球为模板,SnO_2纳米晶为骨架,采用颗粒模板法成功制备大孔SnO_2(MP-SnO_2)气敏材料,并对制备的样品进行差热分析(TGDTA)、X射线衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)和氮气吸附脱附分析。结果表明,制备的MP-SnO_2样品具有贯通孔道大孔结构,平均大孔孔径为300 nm,与SnO_2纳米晶相比具有更大的比表面积。通过气敏测试发现MP-SnO_2在280℃工作温度下对体积分数4×10-4的乙醇气体的灵敏度高达138,是SnO_2纳米颗粒的1.6倍,显示出更加优异的气敏性能。     

介孔二氧化锡纳米材料的臭氧气敏性能

以葡萄糖缩合的碳球为模板,由SnCl₄水热反应制备介孔结构的二氧化锡纳米材料,通过X射线衍射、扫描电子显微镜和透射电镜等表征介孔材料的结构和形貌,发现制备的二氧化锡为四方晶系金红石结构,晶粒尺寸13.8 nm. 以二氧化锡为敏感材料制作气敏元件,并测试了气敏元件在100 ℃~420 ℃温度范围内的气敏性能. 结果表明在200 ℃时,介孔结构的二氧化锡气敏元件对体积分数为1×10^-4的臭氧的灵敏度为2 089,最低检测浓度低于3×10^-6（S=28）,气敏响应时间16 s,恢复时间40 s. 在此条件下,该气敏元件具有灵敏度高、检测浓度低、响应恢复快等优点,具有商业应用价值.     

三氧化二铁六角晶体的制备及其气敏性应用

通过化学气相沉积法(CVD)制备了三氧化二铁(α-Fe_2O_3)六角晶体,后对制得的α-Fe_2O_3进行了系列表征,对反应机理进行了分析。同时构建了场效应晶体管(FET)考察了材料电学性能,并测试了器件对一氧化碳(CO)的气敏性能。实验表明:以三氯化铁(FeCl_3)和水蒸汽(H2O)为原料通过CVD方法能够在相对温和的条件下制备准二维α-Fe2O3六角晶体;用制得的材料构建场效应晶体管具有良好的电学性能,并对CO气体具有很好的响应。     

SnO_2-WO_3复合金属氧化物对丙酮的气敏性能

用SnO_2对WO_3纳米片表面进行修饰,制备了SnO_2-WO_3复合材料,并通过扫描电子显微镜和X射线单晶衍射对所制备的材料形貌和晶体结构进行表征。实验结果表明:制备的WO_3具有纳米片状结构,厚度约为20～30 nm。随着SnO_2含量的增加,复合材料逐渐形成表面附着片的球状结构,球的直径约为2.5μm。此外,气敏性能测试研究表明:由复合量为0.2 mmol SnO_2的SnO_2-WO_3复合材料制成的传感器对丙酮具有最佳的气敏性能,其最佳工作温度为300℃,此时的响应值为纯WO_3纳米片的2倍左右,并且对体积分数为2×10-8的丙酮气体有响应。因此,该SnO_2-WO_3复合材料可以作为一种优良的丙酮气敏材料。     

CuO-ZnO花状纳米结构复合材料设计、合成及气敏特性研究

采用一步水热法制备CuO-ZnO花状纳米结构复合材料.采用X射线衍射仪(XRD)、能谱仪(EDX)及扫描电镜(SEM)对制备的材料进行结构及形貌表征,并使用静态配气法测试CuOZnO花状纳米结构复合材料对甲醛的气敏性能.结果表明:适量引入CuO可显著改善ZnO材料的气敏特性.200℃的工作温度下,掺杂摩尔分数为5%CuO的ZnO花状纳米结构材料对体积分数为1×10~(-5)甲醛的灵敏度最高,为8. 1,是未掺杂ZnO的2. 3倍,同时具有良好的循环稳定性和选择性.最后,对CuO掺杂的气敏机理进行了讨论,其气敏性能的提高归因于在ZnO与CuO接触面形成了p-n异质结及CuO的催化特性.     

Electrical conductivity of （Na3AlF6-40%K3AlF6）-AlF3-Al2O3 melts

The effects of contents of AlF3 and Al2O3, and temperature on electrical conductivity of （Na3AlF6-40%K3AlF6）- AlF3-Al2O3 were studied by continuously varying cell censtant （CVCC） technique. The results show that the conductivities of melts increase with the increase of temperature, but by different extents. Every increasing 10 ℃ results in an increase of 1.85 × 10^-2, 1.86× 10^-2, 1.89 × 10^-2 and 2.20 × 10^-2 S/cm in conductivity for the （Na3AlF6-40%K3AlF6）-AlF3 melts containing 0%, 20%, 24%, and 30% AlF3, respectively. An increase of every 10 ℃ in temperature results an increase about 1.89× 10^-2, 1.94 × 10^-2, 1.95 × 10^-2, 1.99× 10^-2 and 2.10× 10^-2 S/cm for （Na3AlF6-40%K3AlF6）-AlF3-Al2O3 melts containing 0%, 1%, 2%, 3% and 4% Al2O3, respectively. The activation energy of conductance was calculated based on Arrhenius equation. Every increasing 1% of AlF3 results in a decrease of 0.019 and 0.020 S/cm in conductivity for （Na3AlF6-40%K3AlF6）-AlF3 melts at 900 and 1 000 ℃, respectively. Every increase of 1% Al2O3 results in a decrease of 0.07 S/cm in conductivity for （Na3AlF6-40%K3AlF6）-AlF3-Al2O3 melts. The activation energy of conductance increases with the increase in content of AlF3 and Al2O3.     

Electrolysis expansion performance of semigraphitic cathode in [K3AlF6/Na3AlF6]-AlF3-Al2O3 bath system

The electrolysis expansion of semigraphitic cathode in [K₃AlF₆/Na₃AlF₆]-AlF₃-Al₂O₃ bath system was tested by self-made modified Rapoport apparatus. A mathematical model was introduced to discuss the effects of α _CR (cryolite ratio) and β _KR (elpasolite content divided by the total amount of elpasolite and sodium cryolite) on performance of cathode electrolysis expansion. The results show that K and Na (potassium and sodium) penetrate into the cathode together and have an obvious influence on the performance of cathode electrolysis expansion. The electrolysis expansion and K/Na penetration rate increase with the increase of α _CR. When α _CR=1.9 and β _KR=0.5, the electrolysis expansion is the highest, which is 3.95%; and when α _CR=1.4 and β _KR=0.1, the electrolysis expansion is the lowest, which is 1.28%. But the effect of β _KR is correlative with α _CR. When α _CR=1.6 and 1.9, with the increase of β _KR, the electrolysis expansion and K/Na penetration rate increase. However, when α _CR=1.4, the electrolysis expansion and K/Na penetration rate firstly increase and then decrease with the increase of β _KR. Foundation item: Project (2005CB623703) supported by the Major State Basic Research and Development Program of China; Project (2008AA030502) supported by the National High-Tech Research and Development Program of China     

Modification of LiCo1/3Ni1/3Mn1/3O2 cathode material by CeO2-coating

LiCo_1/3Ni_1/3Mn_1/3O₂ was coated by a layer of 1.0 wt% CeO₂ via sol-gel method. The bared and coated LiMn_1/3Co_1/3Ni_1/3O₂ was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), cyclic voltammogram (CV) and galvanotactic charge-discharge test. The results show that the coating layer has no effect on the crystal structure, only coating on the surface; the 1.0 wt% CeO₂-coated LiCo_1/3Ni_1/3Mn_1/3O₂ exhibits better discharge capacity and cycling performance than the bared LiCo_1/3Ni_1/3Mn_1/3O₂. The discharge capacity of 1.0 wt% CeO₂-coated cathode is 182.5 mAh·g⁻¹ at a current density of 20 mA·g⁻¹, in contrast to 165.8 mAh·g⁻¹of the bared sample. The discharge capacity retention of 1.0 wt% CeO₂-coated sample after 12 cycles reaches 93.2%, in comparison with 86.6% of the bared sample. CV results show that the CeO₂ coating could suppress phase transitions and prevent the surface of cathode material from direct contact with the electrolyte, thus enhance the electrochemical performance of the coated material.     

Bi2O3和Fe2O3掺杂对BaTiO3陶瓷显微结构的影响

利用扫描电子显微镜(SEM)、透射电子显微镜(TEM)和X射线能量色散谱(EDAX)等结构分析技术,研究了施主(Bi     

Synthesis and characterization of Mg3(PO4)2-coated Li1.05Ni1/3Mn1/3Co1/3O2 cathode material for Li-ion battery

Mg₃(PO₄)₂-coated Li_1.05Ni_1/3Mn_1/3Co_1/3O₂ cathode materials were synthesized via co-precipitation method. The morphology, structure, electrochemical performance and thermal stability were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), cyclic voltammetry(CV), electrochemical impedance spectroscopy(EIS), charge/discharge cycling and differential scanning calorimeter (DSC). SEM analysis shows that Mg₃(PO₄)₂-coating changes the morphologies of their particles and increases the grains size. XRD and CV results show that Mg₃(PO₄)₂-coating powder is homogeneous and has better layered structure than the bare one. Mg₃(PO₄)₂-coating improved high rate discharge capacity and cycle-life performance. The reason why the cycling performance of Mg₃(PO₄)₂-coated sample at 55 °C was better than that of room temperature was the increasing of lithium-ion diffusion rate and charge transfer rate with temperature rising. Mg₃(PO₄)₂-coating improved the cathode thermal stability, and the result was consistent with thermal abuse tests using Li-ion cells: the Mg₃(PO₄)₂ coated Li_1.05Ni_1/3Mn_1/3Co_1/3O₂ cathode did not exhibit thermal runaway with smoke and explosion, in contrast to the cells containing the bare Li_1.05Ni_1/3Mn_1/3Co_1/3O₂. Funded by the National Natural Science Foundation of China (No. 20273047)     

Luminescent properties of BaO-La2O3-B2O3 glasses with dopant

The luminescent properties of glasses synthesized in air atmosphere by conventional high temperature process were stud{ed. The emissions spectra of Eu^2 and Eu^3 were observed in BaO-La2O3-B2O3-Eu2O3 glasses.The results show that the broad emission peaks at 430 nm correspond to 5d→4f emission transition of Eu^2 , the sharp emission peaks at 592, 616, 650 and 250 nm correspond to 5^D0→1Fj(j=1--4) emission transition of Eu^3 ,respectively, which indicates that the BaO-La2O3a-B2O3-Eu2O3 glass can convert ultraviolet and green omponents of sunlight into blue and red light so as to increase the intensity of blue and red light, respectively. The luminescent in--tensity of Eu^2 increases with increasing the molar ratio of Tb^3 in BaO-La2O3-B2O3-Eu2O3a-Tb4O3 glasses, whereas the luminescent intensity of Eua^3 decreases. So the luminescent intensity of Eu(Ⅲ,Ⅱ) is influenced by Tb^3 .These phenomena can be explained by electron transfer mechanism; Eu^3 (4f6) Tb^3 (4f^8)→Eu^2 (4f′) Tb^4 (4f′). Taking advantage of the luminescent properties of BaO-La2O3-B2O3-Eu2O3 glasses, light-conversion glass for agriculture can be produced.     

Structure of Bi2O3-ZnO-B2O3 system low-melting sealing glass

Bi_2O_3-ZnO-B_2O_3 system glass is a kind of lead-free low melting sealing glasses. The structure of Bi_2O_3-ZnO-B_2O_3 system low-melting sealing glass was investigated by DSC, FT-IR, XRD and SEM. The results show that with the increase of B_2O_3 content, the transition temperature Tg and softening temperature T_f of Bi_2O_3-ZnO-B_2O_3 system low-melting sealing glasses increase, which leads to the liquid phase precipitation temperature increasing and promotes the structure stability in the glass. With increasing the heat treatment temperature, a large number of liquid phases appear in samples and the sinter efficiency of the samples increases. The FT-IR spectra of the glasses show the presence of some bands that are assigned to vibrations of Bi-O bond from [BO_3] pyramidal and [BiO_6] octahedral units and B-O from [BO_3] and [BO_4] units. With the decrease of B_2O_3 content, the crystallization tendency of the glass increases. In glass samples B_1 and B_2, crystallization starts at 460 ℃ and 540 ℃, respectively. Both of them precipitate Bi-(24)B_2O_(39) phases.     

Dielectric properties of Pb (Zn1/3 Nb2/3) O3?PbZrO3?PbTiO3 solid solution near morphotropic phase boundary

The dielectric properties of Pb(Zn_1/3Nb_2/3) O₃-PbZrO₃−PbTiO₃ (PZN-PZ-PT) system near the rhombohedral/tetragonal morphotropic phase boundary (MPB) are carefully studied in this paper. It is found that, for all samples, the curves around the temperatures of dielectric permittivity peak show the characteristics of diffuse phase transition. The change in PbZrO₃/PbTiO₃ ratio has much influence on the dielectric properties of the samples. The extent of diffuse phase transition increases with the increasing Zr/Ti ratio. The samples in rhombohedral region have typical diffuse phase transition in the temperature range measured. However, for the samples with tetragonal symmetry, a spontaneous normal ferroelectric-relaxor phase transition exists at temperature lower than that of permittivity peak. This normal ferroelectric-relaxor phase transition is confirmed by the experiment of thermally driven current. The analysis of TEM reveals that the samples in tetragonal region show a 90% macrodomain structure, while the samples in rhombohedral region have the configuration of microdomain structure.     

Research of Lead-free Na0.5Bi0.5TiO3-BaTiO3 System Piezoelectric Ceramics

To reduce the coercive field of Na_0.5Bi_0.5Ti O₃,Ba Ti O₃ were added as dopant materials.Then the(1-x)Na_0.5Bi_0.5Ti O₃-x Ba Ti O₃ ceramic samples were produced in solid synthetic way.The optimum preparation condition and piezoelectric properties of the samples were investigated.The XRD results show that the fabric transites from rhombohedral to tetragonal gradually with the substitution of the Ba²⁺.T...     

Transport Properties of Polycrystalline La2/3Ca1/3Mn1-xCuxO3

The infuence of Cu dopant (x) and sintering temperature(Ts) on the troansport propeties of La2/3Ca1/3Mn1-xCuxO3 series samples prepared by Sol-Gel technique was investigated.X-ray diffraction patterns show that all the samples with different Cu dopant and sintering temperatures (Ts) are of single phase without obvious latice distortion.Experimental results indicate that the insulator-metal transition temperature is diectly related to the sintering temperature and Cu dopant x.It is interesting to observe that a proper amount of Cu dompant can substantially improve magnetoresistance effects.