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1.
采用一种改进的共沉淀法制备了纳米磁铁矿(Fe3O4)及Ni2+掺杂磁铁矿(NixFe3-xO4,x=0.1,0.3,0.6),用X-射线衍射(XRD)、扫描电镜(SEM)、氮气物理性吸附、酸碱滴定等手段对产物进行了表征,用平衡吸附法研究了4种样品对Pb(Ⅱ)离子的吸附容量及吸附模型。结果表明,Fe3O4和3种NixFe3-xO4均为近似球形的单相晶质纳米颗粒;与Fe3O4比较,NixFe3-xO4的颗粒尺寸变小、表面电荷零点和pH=5.0时的表面正电荷量降低;样品的孔体积、比表面积和表面分形度以及表面羟基含量都随产物中Ni2+掺杂量的增加而升高。4种样品对Pb(Ⅱ)的等温吸附数据均适合用Langmuir模型拟合(R2=0.9942~0.9858),其相关系数的大小表现为:Fe3O4>Ni0.1Fe2.9O4>Ni0.3Fe2.7O4=Ni0.6Fe2.4O4;Freundlich模型对样品等温吸附Pb(Ⅱ)的实验数据拟合度较低(R2=0.9813~0.9477),4种样品的Freundlich相关系数的大小关系与Langmuir相关系数相反。初始pH=5.0时,Fe3O4,Ni0.1Fe2.9O4,Ni0.3Fe2.7O4和Ni0.6Fe2.4O4对Pb(Ⅱ)的最大吸附容量分别为6.02,6.68,7.29和8.34mg·g-1。可见,NixFe3-xO4(尤其是Ni2+掺杂量较高的产物)对水环境中重金属Pb(Ⅱ)的去除能力明显高于Fe3O4。  相似文献   

2.
魏世勇  杨小洪 《无机化学学报》2013,29(12):2615-2622
采用一种改进的共沉淀法制备了纳米磁铁矿(Fe3O4)及Ni2+掺杂磁铁矿(NixFe3-xO4x=0.1,0.3,0.6),用X-射线衍射(XRD)、扫描电镜(SEM)、氮气物理性吸附、酸碱滴定等手段对产物进行了表征,用平衡吸附法研究了4种样品对Pb(Ⅱ)离子的吸附容量及吸附模型。结果表明,Fe3O4和3种NixFe3-xO4均为近似球形的单相晶质纳米颗粒;与Fe3O4比较,NixFe3-xO4的颗粒尺寸变小、表面电荷零点和pH=5.0时的表面正电荷量降低;样品的孔体积、比表面积和表面分形度以及表面羟基含量都随产物中Ni2+掺杂量的增加而升高。4种样品对Pb(Ⅱ)的等温吸附数据均适合用Langmuir模型拟合(R2=0.9942~0.9858),其相关系数的大小表现为:Fe3O4>Ni0.1Fe2.9O4>Ni0.3Fe2.7O4=Ni0.6Fe2.4O4;Freundlich模型对样品等温吸附Pb(Ⅱ)的实验数据拟合度较低(R2=0.981 3~0.947 7),4种样品的Freundlich相关系数的大小关系与Langmuir相关系数相反。初始pH=5.0时,Fe3O4,Ni0.1Fe2.9O4,Ni0.3Fe2.7O4和Ni0.6Fe2.4O4对Pb(Ⅱ)的最大吸附容量分别为6.02,6.68,7.29和8.34 mg·g-1。可见,NixFe3-xO4(尤其是Ni2+掺杂量较高的产物)对水环境中重金属Pb(Ⅱ)的去除能力明显高于Fe3O4。  相似文献   

3.
纳米Mn-Zn铁氧体的制备和研究   总被引:10,自引:0,他引:10  
Nanosize manganese zinc ferrites were fabricated by hydrothermal precipitation route using Fe2(SO4)3, ZnSO4·7H2O, MnSO4·H2O as material, then some calcinated at 500 ℃ and studied by XRD, TEM, IR and VSM. The results showed that the products were spinel crystal structure and uniformly sized nanoparticles (15~25 nm) with little aggregation. The analysis of IR showed that the superficial water can be eliminated, but that was embedded in crystal lattice can not be removed by calcinating. The effect Zn content x on the lattice (a) of nanosize Mn1-xZnxFe2O4 was also discussed. The lattice of nanosize Mn1-xZnxFe2O4 decreases with x increasing; and its value deviated the standard lattice (a0) of normal size manganese zinc ferrites. A lot of water was absorbed during the hydrothermal process owing to the large surface of nanosize particles. The change of magnetic properties of MnxZn1-xFe2O4 with x increasing was studied: nanosize MnxZn1-xFe2O4 particles synthesized by us exhibited peculiar magnetic properties curve with Zn content (x) increasing, Superparamagnetic behaviors of the synthesized ZnFe2O4 samples were confirmed by magnetic characterization, which can be explained by the difference between the distribution of the metal ions (Mn2+, Zn2+ and Fe3+) among the tetrahedral (A) and the octahedral (B) sites of nanosize ferrite and that of bulk ferrite.  相似文献   

4.
采用差示扫描量热法(DSC)、热重和微分热重(TG-DTG)及固相原位反应池/快速扫描傅立叶变换红外联用技术(hyphenated in situ thermolysis/RSFTIR)研究了纳米结晶体Ni0.5Zn0.5Fe2O4与高氯酸铵(AP)组成的混合物的热行为和分解反应动力学。结果表明:Ni0.5Zn0.5Fe2O4使得AP的低、高温分解放热峰温分别提前17.44 K和27.74 K,并使得对应的分解热分别增加3.7 J·g-1和193.7 J·g-1。Ni0.5Zn0.5Fe2O4并不影响AP的晶转温度和晶转热。Ni0.5Zn0.5Fe2O4使得AP的TG曲线出现3个阶段,并使得后2个失重阶段的初始和终止温度都有所提前。凝聚相分解产物分析表明Ni0.5Zn0.5Fe2O4加速了凝聚相AP的分解及氨气的释放。含Ni0.5Zn0.5Fe2O4的AP的高温分解反应的动力学参数Ea=238.88 kJ·mol-1A=1018.59 s-1,动力学方程可表示为dα/dt=1018.99(1-α)[-ln(1-α)]3/5e-2.87×104T。始点温度(Te)和峰顶温度(Tp)计算得出AP的热爆炸临界温度值分别为:574.83 K和595.41 K。分解反应的活化熵(ΔS)、活化焓(ΔH)和活化能(ΔG)分别为:109.61 J·mol-1·K-1、236.49 kJ·mol-1及172.58 kJ·mol-1。  相似文献   

5.
(Zn1-xMnx)C2O4·2H2O在空气中的热分解动力学研究   总被引:1,自引:0,他引:1  
用热分析(TG-DTG/DTA)、X射线衍射(XRD)技术和透射电镜(TEM)研究了固态物质Zn1-xMnxC2O4•2H2O在空气中热分解的过程。热分析结果表明,Zn1-xMnxC2O4•2H2O在空气中分两步分解,其失重率与理论计算失重率相吻合。 XRD和TEM结果表明,Zn1-xMnxC2O4•2H2O分解的最终产物为Zn1-xMnxO,其颗粒大小约为10-13 nm。在非等温条件下对Zn1-xMnxC2O4•2H2O的热分解动力学进行了分析。用Friedman法和Flynn-Wall-Ozawa(FWO)法求取了分解过程的活化能E,并用多元线性回归给出了可能的机理函数。Zn1-xMnxC2O4•2H2O两步热分解的活化能分别为155.7513 kJ/mol 和215.9397 kJ/mol。  相似文献   

6.
采用高温固相法在空气中合成了Ba1.97-yZn1-xMgxSi2O7:0.03Eu,yCe3+系列荧光粉。分别采用X-射线衍射和荧光光谱对所合成荧光粉的物相和发光性质进行了表征。在紫外光330~360 nm激发下,固溶体荧光粉Ba1.97-yZn1-xMgxSi2O7:0.03Eu的发射光谱在350~725 nm范围内呈现多谱峰发射,360和500 nm处有强的宽带发射属于Eu2+离子的4f65d1-4f7跃迁,590~725 nm红光区窄带谱源于Eu3+5D0-7FJ (J=1,2,3,4)跃迁,这表明,在空气气氛中,部分Eu3+在Ba1.97-yZn1-xMgxSi2O7基质中被还原成了Eu2+;当x=0.1时,荧光粉Ba1.97Zn0.9Mg0.1Si2O7:0.03Eu的绿色发光最强,表明Eu3+被还原成Eu2+离子的程度最大。当共掺入Ce3+离子后,形成Ba1.97-yZn0.9Mg0.1Si2O7:0.03Eu,yCe3+荧光粉体系,其发光随着Ce3+离子浓度的增大由蓝绿区经白光区到达橙红区;发现名义组成为Ba1.96Zn0.9Mg0.1Si2O7:0.01Ce3+,0.03Eu的荧光粉的色坐标为(0.323,0.311),接近理想白光,是一种有潜在应用价值的白光荧光粉。讨论了稀土离子在Ba2Zn0.9Mg0.1Si2O7基质中的能量传递与发光机理。  相似文献   

7.
嵌入化合物LixMn2O4的水热浸渍合成研究   总被引:6,自引:0,他引:6  
本文用水热浸渍二步法合成了尖晶石型LixMn2O4微粉,并对其采用XRD,SEM, ICP, XPS和IR等进行测试。结果表明产物为单相立方晶体,粒子尺寸范围0.15-0.5 μm, LixMn2O4中X为0.96,其中锰为Mn3+和Mn4+混合价态存在。该液相合成LixMn2O4材料的方法尚未见报道。  相似文献   

8.
采用EDTA-柠檬酸法合成了中温固体氧化物燃料电池阴极材料Sr1.5La0.5Mn1-xCoxO4(SLMCOx),并利用粉末X射线衍射(XRD)、X射线光电子能谱(XPS)以及电化学交流阻抗谱(EIS)进行表征。结果表明,该材料与Ce0.9Gd0.1O1.95(CGO)在1 200℃烧结12 h不发生化学反应。随着Co掺入量的增加,氧化物中Mn3+和Co2+含量增多,晶格氧含量降低,晶格畸变率增大。交流阻抗谱(EIS)测试结果显示,钴的掺杂明显降低电极的极化电阻,其中Sr1.5La0.5Mn0.7Co0.3O4阴极在700℃空气中的极化电阻为0.62 Ω·cm2,明显小于Sr1.5La0.5MnO4阴极在750℃的极化电阻(1.5 Ω·cm2),表明钴掺杂的Sr1.5La0.5Mn1-xCoxO4是一种潜在的IT-SOFC阴极材料。  相似文献   

9.
掺镍型层状LixNiyMn1-yO2正极材料的合成与电性能研究   总被引:6,自引:0,他引:6  
A kind of cathode material of layered LixNiyMn1-yO2 characterized with the O2 type has been synthesized by a simple method. Its precursor NaxNiyMn1-yO2 has been prepared from manganese dioxide, nickel hydroxide and sodium carbonate at high temperature in air and quickly cooled in cold water, then it has been exchanged by the melted LiNO3 at 300~400℃ in air. The effects of calcine-temperature for the precursors and its compositions (the content of Na and Ni) on the electrochemical properties of the material LixNiyMn1-yO2 have been investingated by XRD and electrochemical tests. The results show that the sample Li0.7Ni0.3Mn0.7O2, has the best electrochemical properties which shows only one charge-discharge potential stage of 2.8~3.0V and has a high specific capacity over 180mAh·g-1 cycled between 2.0~4.20V. A significant structure transformation to the spinal-type phase has not been found in the charge-discharge cycling and the discharge specific capacity around 165mAh·g-1 has re-mained after the 20th cyclings for the material.  相似文献   

10.
利用柠檬酸配合物分解法合成了单相的K2NiF4型希土复合氧化物Eu2-xSrxNiO4+δ(0.5≤x≤1.2),粉末X射线衍射分析表明,在x为0.6~0.7的范围内,物相从空间群为Fmmm的正交相转变成空间群为I4/mmm的四方相,随着Sr2+的加入,部分Ni2+转变为Ni3+,其转变量与理论值接近。反映结构稳定性的高温还原峰温与晶胞参数c有对应关系,表明化合物的结构稳定性取决于AO层与ABO3层的层间距离。  相似文献   

11.
基于尖晶石晶体结构信息,本文采用热力学三亚晶格模型,将材料热力学计算和第一性原理计算相结合,研究了Zn_xMn_(1-x) Fe_2O_4和Ni_xMn_(1-x)Fe_2O_4立方相中的Zn~(2+)、Ni~(2+)、Mn~(2+)以及Fe~(3+)在8a和16d亚晶格上的占位有序化行为。结果表明:在锰铁氧体中,室温下Mn~(2+)完全占据在8a亚晶格上,Fe~(3+)完全占据在16d亚晶格上,属于正尖晶石结构;随着热处理温度升高,在1 273 K达到热处理平衡时的占位构型为(Fe~(3+)0.09Mn~(2+)0.91)[Fe~(3+)1.91Mn~(2+)0.09]O_4,在热处理温度升至1 473 K时,达到热处理平衡时的占位构型为(Fe~(3+)0.11Mn~(2+)0.89)[Fe~(3+)1.89Mn~(2+)0.11]O_4,均与实验结果符合较好。在锌铁氧体中,室温下Zn~(2+)完全占据在8a亚晶格上,Fe~(3+)完全占据在16d亚晶格上,属于正尖晶石结构;在热处理温度较高时,Zn~(2+)和Fe~(3+)发生部分置换,符合实验结果。在镍铁氧体中,半数的Fe~(3+)在室温下占据在8a亚晶格上,Ni~(2+)与剩下另一半的Fe~(3+)共同占据在16d亚晶格上,仅在热处理温度较高的时候发生微弱变化,亦与已有的实验结果吻合。在此基础上,本文进一步通过热力学模型研究了立方相尖晶石结构的Zn_xMn_(1-x)Fe_2O_4、Ni_xMn_(1-x)Fe_2O_4复合体系中阳离子占位行为与热处理温度对占位的影响规律。  相似文献   

12.
This work is devoted to a detailed analysis of the interconnection between composition, cation distribution and acidic properties of the surface of nanocrystalline ferrites NixZn1−xFe2O4 obtained by aerosol pyrolysis. The detailed analysis of the Mössbauer spectra allows us to determine the distribution of cations between tetrahedral and octahedral positions in spinel structure. Depending on samples composition, the tetrahedral positions can be occupied by only Fe3+ cations (inverse spinel, x≥0.4) or by Fe3+ and Zn2+ cations (mixed spinel, x=0, 0.2). Increasing the nickel concentration in the ferrite leads to decrease in the number of strong acid centers on the surface. It was found that the decrease in the contribution of strong surface acid sites leads to an increase in sensory sensitivity of the ferrite towards ammonia. For ethanol detection an inverse relationship between sensor signal and surface acidity was observed.  相似文献   

13.
14.
以乙酰丙酮金属盐为前驱体,三乙二醇为溶剂,采用多元醇法制备了镍锌不同配比的Ni_xZn_(1-x)Fe_2O_4(x=0,0.3,0.5,0.7和1.0)铁氧体,并通过X射线衍射仪(XRD),透射电子显微镜(TEM)和振动样品磁强计(VSM)等对样品的结构、形貌、磁性能和磁热性能进行了表征。结果表明:Ni_xZn_(1-x)Fe_2O_4铁氧体分散性较好,尺寸均一,形状近似球形,平均粒径为4~5 nm。Ni_xZn_(1-x)Fe_2O_4纳米颗粒在室温下表现出亚铁磁性,饱和磁化强度随着镍含量的增加先增大后减小,当x=0.5时达到最大值29.38 emu·g~(-1)。在382k Hz交变磁场作用下,Ni_(0.5)Zn_(0.5)Fe_2O_4铁氧体温度可升温至313 K,表现出较好的磁热性能。  相似文献   

15.
 以共沉淀法制备了 LaFexMnyAl12-x-yO19 六铝酸盐催化剂, 并用 X 射线衍射、扫描电镜、N2 吸附-脱附、紫外-可见漫反射光谱和穆斯堡尔谱对催化剂进行了表征, 考察了催化剂上高浓度 N2O 分解反应的性能. 结果表明, 在所考察的条件下, Mn 比 Fe 更有利于促进六铝酸盐晶相的形成. LaFexAl12-xO19 (x = 0.5, 1) 中 Fe 以 Fe3+位于六铝酸盐尖晶石结构中的四面体位和镜面层结构中的三角双锥位, 其中后者为 N2O 分解的主要活性中心. LaMnyAl12-yO19 (y = 0.5, 1) 中 Mn 优先以 Mn2+进入四面体位, 然后以 Mn3+进入尖晶石结构中的八面体位, 并成为 N2O 分解的主要活性中心.  相似文献   

16.
Cation distribution in quenched and furnace-cooled samples of composition NixM1?xFe2O4 (where M is either Mg2+ or Cu2+) has been studied through magnetization measurements. It has been found that cation distribution in these mixed ferrites cannot be predicted by site preference energies. In magnesium-nickel ferrites, cation distribution is controlled by heat treatment up to x = 0.5, beyond which the effect of heat treatment diminishes. Addition of Ni2+ ions in copper ferrite reduces the diffusibility of Cu2+ ions and the distribution tends toward inverse spinel in the high-nickel region.  相似文献   

17.
The non - centrosymmetric tetragonal inverse spinel structure of LiZnNbO4 has been explored with a view to prepare new colored compounds. The substitution of Co2+, Ni2+, Fe2+, Mn2+, and Cu2+ ions were attempted in the place of Zn2+ ions and Sb5+ ions in place of Nb5+ ions. The studies indicated that 0.75 Zn2+ ions in LiZnNbO4 can be replaced by Co2+ ions and 0.5 Zn2+ ions in LiZnNb0.5Sb0.5O4 compound. The substitution of Co2+ ions gives rise to different shades of blue color in Li(Zn1-xCox)NbO4 compounds and from ink blue to blue-green color in Li(Zn1-xCox)(Nb0.5Sb0.5)O4 compounds. The different colors observed in the present study were explained by the traditional allowed d-d transitions as well as the metal-to-metal charge transfer (MMCT) transitions involving Nb5+ (4d0) ions and partially filled 3d electrons. The SHG studies indicate that the prepared compounds are SHG active. All the compounds exhibit reasonable dielectric behavior with low loss. The XPS studies confirm the oxidation states of the different substituted ions. Raman studies indicate variations in the bands due to the substitutions in the parent LiZnNbO4 phase. Magnetic studies on the Co2+ ions substituted compounds suggest antiferromagnetic behavior.  相似文献   

18.
Mössbauer spectra of the Fe1+xV2−xO4 spinel solid solutions are taken to investigate the cation distribution. Room temperature spectra can be interpreted by assuming that the cation distribution is represented approximately as Fe2+[Fe3+xV3+2−x]O4 for 0 x 0.35 and Fe3+[Fe2+Fe3+x−1V3+2−x]O4 for 1 x 2 and the ionic valence arrangement changes from the 2-3-3 type (Fe2+[Fe3+xV3+2−x]O4) to the 3-2-3 one (Fe3+[Fe2+V3+]O4) in the range 0.35 x 1. Fe2VO4 is found to be 3-2-3 spinel, Fe3+[Fe2+V3+]O4. Its paramagnetic spectrum at 473°K is, however, composed of a broad single line with isomer shift value of 0.61 mm/sec relative to stainless steel, in which the line splitting due to the ferric and ferrous ions is rendered indistinguishable.  相似文献   

19.
The oxyfluoride garnets of formula Y3Fe5?xMxO12?xFx and Gd3Fe5?xMxO12?xFx (M = 3d transition element) result from partial substitution of O2? by F? in Y3Fe5O12 and Gd3Fe5O12 oxides. The cationic charge compensation is obtained by replacing the Fe3+ ions by divalent ions as Mn2+, Co2+, Ni2+, Cu2+ or Zn2+ ions. The site occupied by some of these ions (Mn2+, Ni2+, Zn2+) is determined by magnetic or Mössbauer measurements.  相似文献   

20.
The thermodynamic properties of the Fe3O4ZnFe2O4 spinel solid solution were determined at 900°C by the use of the solid electrolyte galvanic cell Fe2O3 + Fe3O4|O2?|Fe2O3 + ZnxFe3?xO4The activity values obtained exhibit slight negative deviation from the ideal solution model. An analysis of the free energy of mixing of the spinel solid solution provided information on the distribution of cations between the tetrahedral and octahedral sites of the spinel lattice. This is the basis for the estimation of the free energy of formation of pure zinc ferrite from oxides. ΔG0ZnFe2O4 = ?2740 ? 1.6 T cal mole?1  相似文献   

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