Fe3 O4@(DS-LDH)合成条件的优化及表征

探究Fe_3O_4@(DS-LDH)的最佳合成方法及合成条件。对比共沉淀法、离子交换法、焙烧还原法制备的Fe_3O_4@(DS-LDH)。通过DLS、Zeta电位、XRD、FT-IR、SEM、VSM等手段对样品表征分析,利用高效液相法测定载药量。采用L_(16)(4~5)正交试验优化共沉淀法合成工艺,并研究Fe_3O_4@(DS-LDH)的体外缓释性能。结果表明,Fe_3O_4@(DS-LDH)的最优合成条件:n(Mg~(2+))/n(Al~(3+))=2,n(Mg~(2+))/n(总Fe)=2,pH=10.5,晶化温度为90℃。最优条件下载药量达27.59%,Fe_3O_4粒径为168.25nm,Fe_3O_4@(DS-LDH)粒径为128.58nm。Fe_3O_4和Fe_3O_4@(DS-LDH)具有较好磁性性能。外加磁场条件下,体外缓释性能良好,12h趋于稳定,达84.65%。表明Fe_3O_4@(DS-LDH)是良好的磁靶向药物传送控制系统。     

Fe3O4@PI催化剂的制备及其费托合成性能

分别采用水热、水热-包覆、球磨法制备了Fe_3O_4、聚酰亚胺(PI)改性的Fe_3O_4@PI和Fe_3O_4-PI催化剂用于费托合成反应,对比研究了PI改性及其含量变化对Fe基催化剂催化CO加氢产物分布的影响规律。结合XRD、SEM、TEM、H_2-TPR、COTPD、FT-IR、XPS、TG和接触角实验等手段对催化剂样品进行了表征。结果表明,Fe_3O_4、Fe_3O_4@PI和Fe_3O_4-PI样品均为球形颗粒; PI改性促进了Fe_3O_4的还原,亲水性增强。Fe_3O_4@PI样品中,PI均匀包覆于Fe_3O_4表面,具有较好的热稳定性;与Fe_3O_4、Fe_3O_4-PI相比,Fe_3O_4@PI样品CO吸附增强。在CO加氢反应中,与Fe_3O_4相比,PI改性的Fe_3O_4@PI和Fe_3O_4-PI样品催化活性下降,二次加氢能力受到抑制,烯烃选择性提高; Fe_3O_4@PI样品烯烃选择性增加明显,烯烷比(O/P)由改性前的0.50提高至2.15;适宜含量的PI改性促进C5+烃生成。     

Fe_3O_4/TiO_2@生物碳骨架复合材料的一步法制备及UV-Fenton催化性能

以玉米秸秆为生物模板,经铁盐和钛盐溶液浸渍后煅烧,制备了新型Fe_3O_4/TiO_2分层介孔玉米秸秆碳骨架复合材料(Fe_3O_4/TiO_2@MSC),并研究了其多相UV-Fenton体系降解四环素的效能.利用X射线衍射(XRD)、X射线光电子能谱(XPS)、N2吸附-脱附、扫描电子显微镜(SEM)和透射电子显微镜(TEM)对合成的催化剂进行了表征.结果表明,Fe_3O_4/TiO_2@MSC保留了玉米秸秆的分级多孔形态,纳米Fe_3O_4和TiO_2在MSC表面生长,秸秆碳作为骨架提高了纳米Fe_3O_4的分散性,防止其团聚,提高了催化剂的稳定性,并且能够增加材料的比表面积和活性点位,进而增强对UV-Fenton体系的催化活性. TiO_2光催化和多相Fenton体系的协同作用促进了Fe(Ⅲ)向Fe(Ⅱ)转化.催化性能研究结果表明,在相同条件下,Fe_3O_4/TiO_2@MSC催化的多相UV-Fenton体系盐酸四环素(TCH)降解效率在反应40 min后达到99. 8%,远高于Fe_3O_4@MSC+H2O_2(30%),UV+H2O_2(73%)、UV+Fe_3O_4@MSC+H2O_2(89. 1%)和UV+Fe_3O_4/TiO_2+H2O_2(89. 2%)体系,并且该体系在中性甚至碱性条件下均能达到满意的TCH去除效果.     

Fe_3O_4/SiO_2-NH_2磁性介孔纳米粒子的制备及其对酸性品红的吸附

采用共沉淀法,合成了由两亲性嵌段共聚物聚(苯乙烯)-b-聚(甲基丙烯酸聚乙二醇酯)(PSt-bPMAPEG)修饰的Fe_3O_4-聚合物复合纳米粒子。以十六烷基三甲基溴化铵(CTAB)为模板剂,正硅酸乙酯(TEOS)为硅源,N-(2-氨乙基)-3-氨丙基三甲氧基硅烷(AAPTS)为功能化试剂,制备了氨基功能化介孔材料Fe_3O_4/SiO_2-NH2。采用X射线衍射(XRD),傅里叶变换红外光谱(FT-IR),透射电子显微镜(TEM),N_2吸附/脱附等手段对Fe_3O_4/SiO_2-NH2进行了表征。结果表明,成功制备粒径约为50nm,孔径分别为3.3nm和42.9nm的Fe_3O_4/SiO_2介孔粒子。将磁性材料对水中酸性品红进行吸附性能研究,探讨了Fe_3O_4/SiO_2-NH2对染料酸性品红的吸附效率。结果表明:Fe_3O_4/SiO_2-NH2的用量为10mg,吸附时间为3.5min,溶液起始浓度为0.25mmol·L-1时吸附率达93.32%。     

棒状CuFe_4O_x的可控合成及其异戊醇脱氢反应的催化性能（英文）

利用液相沉淀法可控合成了均匀的棒状CuFe_4O_x催化剂。通过原位X射线粉末衍射(XRD)、高分辨透射电子显微镜(TEM)及程序升温还原(TPR)等手段表征其晶相结构、形貌和还原性能。通过还原棒状CuFe_4O_x获得Cu~0/Fe_3O_4纳米棒,原位X射线光电子能谱(XPS)用于确定Cu~0/Fe_3O_4表面的相组成。通过液相沉淀法制备棒状CuFe_4O_x,在120℃保持3 h后加入Na2CO3溶液至pH等于9时所得棒状形貌最为规整。以异戊醇脱氢反应作为探针反应,比较了Cu~0/Fe_3O_4纳米棒和Cu~0/Fe_3O_4纳米颗粒的催化反应性能,发现Cu~0/Fe_3O_4纳米棒比Cu~0/Fe_3O_4纳米粒子具有更好的活性和稳定性,表明棒状Fe_3O_4担载的Cu纳米粒子具有更好的结构稳定性。     

以Fe_2P_2O_7为前驱体制备LiFePO_4及其电化学性能（英文）

以磷铁废渣(Fe1.5P)和温室效应气体CO_2为原料,以磷酸为补充磷源合成磷酸铁锂(LiFePO_4)的前驱体Fe_2P_2O_7,并研究了其合成过程对LiFePO_4正极材料储能性能的影响。采用SEM观察了LiFePO_4的表面形貌,采用XRD分析了LiFePO_4和Fe_2P_2O_7的晶体结构。进一步对该方法进行优化,发现Fe1.5P与磷酸混合物(nFe1.5P∶nH3PO4=1∶1)在800℃热处理6 h合成的Fe_2P_2O_7对应的LiFePO_4/C电化学性能最好,在0.1C,0.2C,0.5C和1C倍率下的容量分别可达130,126,117和108 m Ah·g~(-1)。     

基于巯基-烯点击化学法的磁纳米粒子制备及用于螺旋藻中多环芳烃的分析

利用水热法合成了Fe_3O_4纳米粒子,并通过巯基-烯点击化学法合成了Fe_3O_4@DA-IL。通过FT-IR、XRD、SEM、TEM等手段对Fe_3O_4@DA-IL进行表征,并以该复合材料为MSPE的吸附剂用于螺旋藻中的PAHs的富集。实验还优化了吸附剂用量、萃取时间、洗脱剂种类以及洗脱次数,在最佳条件下,方法定量限为0.031~0.49μg/L,回收率为78.4%~107.1%。     

A highly selective magnetic sensor with functionalized Fe/Fe3O4 nanoparticles for detection of Pb2+

A magnetic sensor for detection of Pb~(2+) has been developed based on Fe/Fe_3O_4 nanoparticles modified by3-(3,4-dihydroxyphenyl)propionic acid(DHCA). The carboxyl groups of DHCA have a strong affinity to coordination behavior of Pb~(2+) thus inducing the transformation of Fe/Fe_3O_4 nanoparticles from a dispersed to an aggregated state with a corresponding decrease, then increase in transverse relaxation time(T_2) of the surrounding water protons. Upon addition of the different concentrations of Pb~(2+) to an aq. solution of DHCA functionalized Fe/Fe_3O_4 nanoparticles(DHCA-Fe/Fe_3O_4 NPs)([Fe] = 90 mmol/L), the change of T_2 values display a good linear relationship with the concentration of Pb~(2+) from 40 μmol/L to 100 μmol/L and from 130 μmol/L to 200 μmol/L, respectively. Owing to the especially strong interaction between DHCA and Pb~(2+), DHCA-Fe/Fe_3O_4 NPs exhibited a high selectivity over other metal ions.     

纳米Fe2O3和Fe3O4的制备及其催化高氯酸铵热分解性能的研究——一个仪器分析综合实验

介绍一个仪器分析综合实验——纳米Fe_2O_3和Fe_3O_4的制备及其催化高氯酸铵热分解性能的研究。采用水热法合成纳米Fe_3O_4,进而煅烧得到纳米Fe_2O_3。使用X射线粉末衍射(XRD)对制得的样品结构进行表征,通过透射电镜(TEM)可以发现其为球形颗粒,粒径在10–20 nm范围内。将制得的纳米Fe_2O_3和纳米Fe_3O_4按不同比例加入高氯酸铵(AP)中,通过对混合物进行热分析(TG-DSC),发现纳米Fe_2O_3和纳米Fe_3O_4可以明显促进AP的分解,且Fe_2O_3的催化效果优于Fe_3O_4的催化效果,并对催化机理进行了简单讨论。通过该实验,可以让学生学习水热反应的方法,掌握利用XRD、热分析等多种手段对化合物结构及性能进行表征的技能。     

Fe_3O_4@HKUST-1-C_(18)的制备及用于环境水样中多环芳烃的分析

利用水热法合成Fe_3O_4纳米粒子,并通过层层自组装的方法合成以Fe_3O_4为核、金属-有机骨架(MOFs)为壳的多功能核-壳磁性微球Fe_3O_4@HKUST-1;最后利用Cu2+与-SH之间的配位作用,对磁性微球的壳层进行长链烷基修饰,得到Fe_3O_4@HKUST-1-C_(18)。通过FT-IR,XRD,SEM,TEM等手段对Fe_3O_4@HKUST-1-C_(18)进行表征,并以该复合材料为磁固相萃取吸附剂用于环境水样中的多环芳烃的富集。同时本文还优化了吸附剂用量、萃取时间、离子强度等,在最佳条件下,方法定量限为0.031~0.49μg/L,回收率为68.3%~109.6%。     

The L Spectrum of Fe and Fe3O4

The intensities of the Fe L lines/bands l = L₃M₁, η = L₂M₁, α_1,2 = L₃M_4,5, β₁ = L₂M₄, and β_3,4 = L₁M_2,3 were measured for pure Fe and Fe₃O₄ using a TAP crystal as the dispersing element. The energy of the exciting electrons, E₀, was varied in the range 5 ≤ E₀ ≤ 25 keV. For pure Fe the following results were obtained. The net peak height ratio Ll/Lα remains relatively constant with varying E₀ at approximately 14%. The E₀ dependence of Lη is similar to that of Ll, although Lη is less intense than Ll by a factor of 7. Lβ₁/Lα decreases from 20% for E₀ = 5 keV to about 5% for 25 keV. Lβ_3,4 behaves like Lβ₁ but is weaker by a factor of 15. For Fe₃O₄ a much weaker intensity of Lα was observed which can be partially explained by its stronger absorption. Again, the E₀ dependence of Ll and Lη is similar with Ll/Lα = 19% and Lη/Lα = 4%. Lβ₁ and Lβ_3,4 show a comparable E₀ dependence. Lβ₁/Lα decreases from 50% for E₀ = 5 keV to 34% for 25 keV. Lβ_3,4 is weaker than Lβ₁ by a factor of about 25. The observed E₀ dependence of the different lines was used to estimate a set of mass absorption coefficients. Our value for Lα in Fe agrees well with other data which were deduced from variable E₀ measurements but differs considerably from data given by Heinrich and Henke.     

Electronic behavior of three oxygen non-stoichiometric Fe/Fe oxoperovskites

For comparison with the Mn⁴⁺/Mn³⁺ oxoperovskites at the crossover from localized to itinerant behavior of the σ-bonding e electrons, the electronic properties of three oxygen non-stoichiometric, mixed-valent Fe⁴⁺/Fe³⁺ oxoperovskites were explored by measuring their resistivity ρ(T), thermoelectric power α(T), and magnetic susceptibility χ(T). Oxidation of Ca₂Fe₂O₅ by annealing in ozone progresses by oxygen insertion to give conductive CaFeO₃ perovskite clusters in a localized-electron, weakly oxidized brownmillerite Ca₂Fe₂O_5+δ matrix. Removal of 0.12 oxygen per formula unit from La_1/3Sr_2/3FeO₃ lowers somewhat its cooperative disproportionation reaction, and fivefold-coordinated ions neighboring oxygen vacancies in the more ionically bonded slabs act as donors to the covalently bonded Fe(V)O₆ planes. Single-crystal SrFeO_2.83 exhibited bad-metal behavior with superparamagnetic, electron-rich fluctuations below 240 K that, on cooling below 190 K, become progressively trapped by the oxide-ion vacancies as an immobile second phase; long-range antiferromagnetic order is stabilized below a T_N≈60 K.     

Influence of mechanical activation time,annealing, and Fe/O ratio on Fe3O4/Fe composites formation from Fe2O3 and Fe powders mixture

Commercially, iron (α-Fe) and hematite (α-Fe₂O₃) powders were used for the synthesis of composite powders of Fe₂O₃/Fe type by mechanical milling. Several ratios of Fe₂O₃/Fe were chosen for the composite synthesis; the atomic percent of oxygen in the starting mixtures ranged from 21 to 46 %. The Fe₂O₃/Fe composite samples with various Fe/O ratios were milled for different milling times. The milled composite samples were subjected to the heat treatments in argon up to 900 °C. During the heat treatment at temperatures that do not exceed 550 °C, Fe₃O₄/Fe composite particles are formed by the reaction between the Fe₂O₃ and Fe. Further increase of the heat treatment up to 700 °C leads to the reaction of the Fe₃O₄/Fe composite component phases, resulting thus in the formation of FeO/Fe composite. The heat treatment up to 900 °C of the Fe₂O₃/Fe leads to the formation of a composite of FeO/Fe₃O₄/Fe independent of the milling time and Fe₂O₃/Fe ratios. The onset temperatures of the Fe₃O₄ and FeO formations decrease upon increasing the milling time. Another important aspect is that, in the case of the same milling time but with a large amount of iron into the composite powder the formations temperatures of Fe₃O₄ and FeO are also decreasing. The influence of the mechanical activation time, heat treatment temperature, and Fe/O ratio on the formation of the (Fe₃O₄, FeO)/Fe composite from Fe₂O₃+Fe precursor mixtures was studied by differential scanning calorimetry and X-ray diffraction techniques.     

Structure and properties of iron oxide clusters: From Fe6 to Fe6O20 and from Fe7 to Fe7O24

Geometrical and electronic structures of the neutral and singly negatively charged Fe₆O_n and Fe₇O_m clusters in the range of 1 ≤ n ≤ 20 and 1 ≤ m ≤ 24, respectively, are computed using density functional theory with the generalized gradient approximation. The largest clusters in the two series, Fe₆O₂₀ and Fe₇O₂₄, can be described as Fe(FeO₄)₅ and Fe(FeO₄)₆ or alternatively as [FeO₅](FeO₃)₅ and [FeO₆](FeO₃)₆, respectively. The Fe₆O₂₀ and Fe₇O₂₄ clusters possess adiabatic electron affinities (EA_ad) of 5.64 eV and 5.80 eV and can be attributed to the class of hyperhalogens since FeO₄ is an unique closed‐shell superhalogen with the EA_ad of 3.9 eV. The spin character of the lowest total energy states in both series changes from ferromagnetic to ferrimagnetic or antiferromagnetic when the first Fe? O? Fe bridge is formed. Oxidation decreases substantially the polarizability per atom of the initial bare clusters; namely, from 5.98 ų of Fe₆ to 2.47 ų of Fe₆O₂₀ and from 5.67 ų of Fe₇ to 2.38 ų of Fe₇O₂₄. The results of our computations pertaining to the binding energies of O, Fe, O₂, and FeO in the Fe₇O_m series provide an explanation for the experimentally observed abundance of the iron oxide nanoparticles with stoichiometric compositions. © 2016 Wiley Periodicals, Inc.     

Synthesis and characterisation of Fe6 and Fe12 clusters using bicine

Reaction of bicine {BicH₃, N,N-bis(2-hydroxyethyl)glycine} with an Fe(III) oxo-centered pivalate triangle in MeCN in the presence of Et₂NH yields [Et₂NH₂]₂[Fe₆O₂(OH)₂(Bic)₂(O₂CCMe₃)₈], which possesses an S = 5 ground state.Changing the base to NaOMe produces [Fe₁₂O₄(Bic)₄(HBic)₄(O₂CCMe₃)₈], which contains two Fe₆ units bridged by the carboxylate arms from the bicine ligands. The complex displays strong antiferromagnetic coupling leading to an S = 0 ground state.     

浅谈检验Fe~(2+)与Fe~(3+)的误区

空白试验证明,用浓度大于1mol/L的盐酸溶液做Fe~(3+)的提取液,或用过浓盐酸溶液酸化试液,盐酸中的Fe~(3+)都会给检验试液中的Fe~(3+)带来干扰;检验食品中的铁元素时,若铁是以Fe~(2+)形式存在,如果加入硝酸将其氧化为Fe~(3+),硝酸中Fe~(3+)会对检验试液中的Fe~(3+)带来干扰。     

Application of EDXRF Method in Measurement of Fe Content in Aqueous Fe Sample

介绍了能量色散X荧光分析方法在含水Fe样品测量中的应用.用ANTG -2000型海底X荧光探测系统对含Fe为10％～60％的Fe样进行测量,建立水分对Fe元素特征K α射线影响的校正模型.结果表明,通过该模型校正,对含饱和水情况下Fe样品的分析相对误差小于4％,具有良好的分析效果.     

EDXRF方法在测量含水Fe样中Fe含量的应用

介绍了能量色散X荧光分析方法在含水Fe样品测量中的应用。用ANTG 2000型海底X荧光探测系统对含Fe为10%～60%的Fe样进行测量,建立水分对Fe元素特征Kα射线影响的校正模型。结果表明,通过该模型校正,对含饱和水情况下Fe样品的分析相对误差小于4%,具有良好的分析效果。     

Fe L-edge X-ray absorption spectroscopy of low-spin heme relative to non-heme Fe complexes: delocalization of Fe d-electrons into the porphyrin ligand

Hemes (iron porphyrins) are involved in a range of functions in biology, including electron transfer, small-molecule binding and transport, and O2 activation. The delocalization of the Fe d-electrons into the porphyrin ring and its effect on the redox chemistry and reactivity of these systems has been difficult to study by optical spectroscopies due to the dominant porphyrin pi-->pi(*) transitions, which obscure the metal center. Recently, we have developed a methodology that allows for the interpretation of the multiplet structure of Fe L-edges in terms of differential orbital covalency (i.e., differences in mixing of the d-orbitals with ligand orbitals) using a valence bond configuration interaction (VBCI) model. Applied to low-spin heme systems, this methodology allows experimental determination of the delocalization of the Fe d-electrons into the porphyrin (P) ring in terms of both P-->Fe sigma and pi-donation and Fe-->P pi back-bonding. We find that pi-donation to Fe(III) is much larger than pi back-bonding from Fe(II), indicating that a hole superexchange pathway dominates electron transfer. The implications of the results are also discussed in terms of the differences between heme and non-heme oxygen activation chemistry.