稀土-吡唑啉酮-2,6-吡啶二羧酸配合物的合成、表征及其性质研究

以稀土氯化物、1-苯基-3-甲基-4-苯甲酰基-5-吡唑啉酮和2,6-吡啶二羧酸为原料,制备了一类新型稀土三元配合物,通过元素分析、红外光谱、紫外光谱、热重-差热分析、光电子能谱分析及X射线粉末衍射等手段对配合物进行了表征,确定了该类配合物的化学组成可能为:Na2[RE(PMBP)3(PDA)]·nH2O(RE=Sm3+,Y3+,Er3+,其中La配合物含有一分子配位水)。抗菌实验结果表明,三元配合物对大肠杆菌、金黄色葡萄球菌具一定的抑制作用,Na2[Er((PMBP)3(PDA)]·5H2O对大肠杆菌作用较好,而Na2[Sm(PMBP)3(PDA)]·5H2O对金黄色葡萄球菌作用较好。采用紫外光谱法和荧光光谱法初步研究了配合物与CT-DNA的作用方式,结果表明配合物是以插入模式与DNA结合的。同时配合物Na2[Sm(PMBP)3(PDA)]·5H2O具有荧光特性,可用作荧光探针等,在生物活性上具有一定的应用前景。     

银掺杂介孔氧化铝抗菌剂的一步合成与表征

以Al(NO_3)_3·9H_2O和AgNO_3为原料,采用水热法制备了介孔氧化铝纳米粒子(Mesoporous Al_2O_3NPs)和银掺杂介孔氧化铝纳米粒子(Mesoporous Ag/Al_2O_3NPs),通过X射线衍射(XRD)、场发射扫描电子显微镜(FE-SEM)、X射线荧光光谱(XRF)、能量分散X射线衍射(EDX)和低温N2吸附-脱附等手段对产物进行了表征,通过最低抑菌浓度和抑菌圈实验研究了材料的抗菌性能.XRD分析表明在介孔Ag/Al_2O_3NPs中Al_2O_3是唯一结晶相,Ag掺杂后,介孔Ag/Al_2O_3NPs晶格常数和半高峰宽增大,晶面间距[(111),(400)和(440)面]减小.FE-SEM形貌分析表明掺杂后的介孔Ag/Al_2O_3NPs颗粒直径减小而孔径增大.EDX和XRF分析表明介孔Ag/Al_2O_3NPs中O/Al摩尔比为1.5,与Al_2O_3NPs中O/Al摩尔比相同.综合XRD和XRF分析结果认为,Ag进入介孔Al_2O_3晶格间隙形成间隙固溶体.低温N2吸附-脱附分析表明掺杂后的介孔Ag/Al_2O_3NPs比表面积、孔体积和孔径增大.曝气抗菌实验结果表明介孔Ag/Al_2O_3NPs的抗菌机理是活性氧和金属银的协同作用.介孔Ag/Al_2O_3NPs对革兰氏阴性菌(大肠杆菌)和革兰氏阳性菌(金黄色葡萄球菌)具有明显的抗菌效果,对大肠杆菌和金黄色葡萄球菌的最低抑菌浓度(MIC)均为80μg/m L,抑菌圈直径分别为26 mm和24 mm.     

M~(2+)(M=Cu、Cd、Ag、Fe)掺杂氧化锌纳米粉晶的抗菌性能

采用柠檬酸溶胶-凝胶法制备了ZnO及M2+掺杂ZnO纳米粉晶(M=Cu、Cd、Ag、Fe),用现代测试技术表征了样品的组成、结构和形貌,以大肠杆菌(Escherichia coli)、金黄色葡萄球菌(Staphylococcus aureus)和白色念珠菌(Candida albicans)为测试菌株,用抑菌圈、最小抑菌浓度和最小杀菌浓度等方法研究了样品在日光照射下的抗菌活性。结果表明,与母体ZnO相比,Cu、Ag、Cd掺杂样品的抗菌性能明显地增强,这可能是由于掺杂金属离子置换Zn2+生成了晶格缺陷和电荷缺陷,阻止了光生电子和光生空穴对的复合从而增强了光催化活性和抗菌活性。     

C12A7-O-纳米材料的制备及抗菌活性

利用溶胶-凝胶法制备了C12A7-O-{[Ca24Al28O64]4+·4(O-)}纳米材料. 采用X射线衍射、电子顺磁共振及透射电子显微镜等手段对制备的材料进行了表征. 结果表明, 在最佳焙烧条件(1150 ℃, 6 h)下制备的材料平均粒径为74 nm, 并具有晶胞参数为(1.199±0.004) nm的C12A7(Ca12Al14O33)笼状结构, 材料内包含浓度高达1.2×1020 cm-3的氧负离子(O-). 初步研究结果表明, 合成的C12A7-O-纳米材料具有良好的广谱抗菌作用.     

低温区CsI掺杂的12CaO·7Al2O3型发射材料负离子的发射特性

本文利用潮湿浸渍法将碘化铯(CsI)掺杂至12CaO·7Al2O3(C12A7)型负离子存储发射材料的表面并对其的结构与存储特性进行了X射线衍射和电子顺磁共振的表征,与此同时还对该材料的发射特性、离子发射分支比以及温度对发射强度的影响等方面进行了研究和分析。将实验和表征结果与未掺杂的C12A7进行对比后发现,C12A7表面上CsI的掺入很大程度上改善了该材料的发射特性。掺杂CsI后,在800 V·cm-1的引出场下,发射温度由570℃降低至470℃,与此同时,在同样的发射条件下,其发射强度也明显增强。低温区(<500℃)氧负离子O-的发射纯度接近100%。以上结果表明掺杂CsI至C12A7表面是一种在低温下获得氧负离子O-源的有效途径。     

纳米氧化鏑/壳聚糖杂化材料的制备和抑菌性研究

用甲苯-2,4-二异氰酸酯(TDI)为功能化试剂,经过一定的物理﹑化学方法处理,使纳米氧化鏑和壳聚糖(CS)以TDI作为桥梁合成新材料DTC(Dy2O3-TDI-CS).重点研究了该材料对金黄色葡萄球菌和大肠杆菌的抑菌性能以及最低抑菌浓度(MIC),并且与壳聚糖的抑菌性进行了对比.实验表明该材料比壳聚糖有更好的抑菌性,...     

SbxZn1-xO1+x/2及其壳聚糖复配物的制备和抗菌性能

采用溶胶-凝胶法制备了SbxZn1-xO1+x/2及其壳聚糖的复配物,通过X-射线衍射仪(XRD)、傅里叶变换红外光谱仪(FTIR)、扫描电子显微镜(SEM)和透射电子显微镜(TEM)等表征了样品的物相结构、组成和微观形貌。以大肠杆菌、白色念珠菌和金黄色葡萄球菌为测试菌种,研究了样品的抗菌性能。结果表明,SbxZn1-xO1+x/2的抗菌活性优于纯ZnO,其中x=0.05的样品活性最好;复配物的抗菌活性明显优于单一组分,当Sb0.05Zn0.95O1.025和壳聚糖质量比mSZ/mCS=2时,样品抗菌性能最佳。     

Bi掺杂NaTaO_3中Bi的化学价态对其光催化性能的影响（英文）

分别采用Na Bi O3和Bi(NO3)3为Bi源制备了Bi掺杂Na Ta O3光催化剂,研究了Bi离子的价态对Na Ta O3光催化分解水制氢性能的影响.采用X射线衍射(XRD)、拉曼光谱、X射线光电子能谱(XPS)和紫外-可见吸收光谱研究了催化剂的晶体结构、Bi离子的化学状态和催化剂的光学吸收性能.以光催化分解水制氢反应研究了Bi离子掺杂Na Ta O3的催化性能.XRD结果表明,对于两个不同Bi源掺杂的Na Ta O3样品,Bi离子的掺杂没有改变催化剂的单斜相结构,但拉曼光谱证实Bi离子的掺杂致使Ta–O–Ta键角偏离了180o.XPS结果表明,以Bi(NO3)3为Bi源时,Bi离子以Bi3+掺杂于Na Ta O3的A位;当以Na Bi O3为原料时,Bi3+和Bi5+共掺杂于Na Ta O3的A位.两种不同Bi源掺杂得到的样品在紫外-可见吸收光谱中给出了相似的光学吸收,但Bi3+的掺杂对Na Ta O3光催化性能影响不大,而Bi3+和Bi5+共掺杂大大提高了Na Ta O3的光解水制氢性能.Bi离子取代Na离子在A位的掺杂,在Na Ta O3结构中引入了能够促进载流子分离的空位和缺陷;与此同时,Bi的掺杂导致Ta–O–Ta键角偏离180o而不利于载流子迁移.对于Bi3+掺杂的Na Ta O3样品,这两种作用相互抵消,使得其催化性能与Na Ta O3相比没有变化;而Bi3+和Bi5+的共掺杂和高价态Bi5+的掺杂引入了更多的空位和缺陷,提高了光生电子-空穴的分离效率,从而提高了光催化产氢性能.研究表明,光催化过程中载流子的迁移是影响催化性能的重要因素,而在ABO3钙钛矿结构的A位引入高价态离子是促进光生载流子分离的有效途径.     

高价银配合物的制备、表征及抗菌性能研究

以亚乙基双胍、吡啶及吡啶衍生物为配体合成了[AgEn(BigH)_2]_2(SO_4)_3·7H_2O(3)、[Ag(Py)_2(N_2)_2](OH)_2(4)和[Ag(2-Apy)_3(OH)](HSO_4)·H_2O(5)三种较稳定的高价银配合物。产物结构经红外光谱、元素分析和XPS进行表征。通过最小抑菌浓度(MIC)和生长抑制曲线来检测配合物的抗菌能力,并对配合物进行光稳定测试。抗菌实验结果显示,所有的配合物在0.5μg/mL浓度下就开始对测试菌产生抑制作用,对大肠杆菌的MIC分别为10、5和5μg/mL,对金黄色葡萄球菌的MIC为40、20和20μg/mL。配合物对大肠杆菌的抗菌活性高于对金黄色葡萄球菌。     

硒化铜纳米晶体的高效抗菌活性研究

制备了十六烷基三甲基溴化铵(CTAB)包被的硒化铜纳米晶体(Cu_(2-x)Se NCs),并对其高效抗菌活性机制进行了研究。革兰氏阴性细菌大肠杆菌(Escherichia coli,E.coli)和革兰氏阳性细菌金黄色葡萄球菌(Staphylococcus aureus,S.aurues)被用作模型菌株,通过探究其最小抑菌浓度(MIC)和最小杀菌浓度(MBC),以及杀菌动力学评估了Cu_(2-x)Se NCs的抗菌性能。实验结果显示,金黄色葡萄球菌对Cu_(2-x)Se NCs更为敏感,这是由于大肠杆菌具有双层膜而金黄色葡萄球菌仅拥有单层膜。此外,当Cu_(2-x)Se NCs浓度为32μg/mL时,不管是革兰氏阳性菌还是革兰氏阴性菌,都会在1 h内全部死亡,证明Cu_(2-x)Se NCs拥有较强的杀菌性能。     

Gelled Na<Subscript>2</Subscript>HPO<Subscript>4</Subscript> · 12H<Subscript>2</Subscript>O with amylose-g-sodium acrylate: heat storage performance,heat capacity and heat of fusion

A novel gelling method was studied to stabilize phase change material Na₂HPO₄ · 12H₂O with amylose grafted sodium acrylate. Gelled Na₂HPO₄ · 12H₂O shows stable heat storage performance prepared at optimized conditions: 2.7mass/mass% sodium acrylate, 0.4 mass/mass% amylose, 0.05–0.09 mass/mass% N, N′-methylenebisacrylamide, 0.05–0.09 mass/mass% K₂S₂O₈ and Na₂SO₃ (mass ratio 1:1), at 50 °C. Na₂HPO₄ · 12H₂O was dispersed in gel network as tiny crystals less than 0.1 mm. Melting points were in the range 35.4 ± 2 °C. Short-term thermal cycling proves the effectiveness of the novel method for eliminating phase separation in the gelled salt. Adiabatic calorimetric measurement of heat capacities shows two phase transitions, which correspond to melting of Na₂HPO₄ · 12H₂O and freezable bond water in gel, respectively. Heat of fusion of pure Na₂HPO₄ · 12H₂O was determined as 260.9 J g⁻¹. Distribution of extra water is: free water:freezable water:nonfreezing water = 0:0.85:0.15.     

Antibacterial glass films prepared on metal surfaces by sol–gel method

This paper describes the preparation and characterization of glass films consisting of SiO₂, Li₂O, Na₂O, K₂O or MgO in varying compositions on stainless steel and aluminum substrates by sol–gel method. Silver phosphate or silver incorporated zeolite was also introduced into the sols for obtaining antibacterial effect. The SiO₂/Li₂O/Na₂O system having the composition of 85:5:10 wt% was found as the optimum for obtaining a stable sol and film formation. The films were investigated by scanning electron microscopy (SEM) and electron dispersive analysis by X-ray (EDX), Fourier transformed infrared (FTIR) spectroscopy, thermo-gravimetric analysis (TGA) and differential thermal analysis (DTA). Homogenous films having 300 ± 20 nm thicknesses were formed by spin coating and then by curing at 500 °C for 1 h. Obtained films had high adherence to the metal substrates and they were also durable in acidic, basic or NaCl environments. They also presented a powerful antibacterial effect against E. coli.     

NaBO2-NaCl-Na2CO3, NaBO2- Na2CO3-NaMoO4, NaBO2- Na2CO3-NaWO4, and NaBO2-NaCl-Na2WO4 ternary systems

The phase diagrams of the NaBO₂-NaCl-Na₂CO₃, NaBO₂-Na₂CO₃-Na₂MoO₄, NaBO₂- Na₂CO₃-Na₂WO₄, and NaBO₂-NaCl-Na₂WO₄ ternary systems were studied by a calculation-experimental method and differential thermal analysis. The coordinates of ternary eutectics were determined: E ₁: 612°C, 16 mol % NaBO₂, 42 mol % NaCl, and 42 mol % Na₂CO₃; E ₂: 568°C, 12 mol % NaBO₂, 28 mol % Na₂CO₃, and 60 mol % Na₂MoO₄; E ₃: 575°C, 12 mol % NaBO₂, 32 mol % Na₂CO₃, and 56 mol % Na₂WO₄; E ₄: 628°C, 8 mol % NaBO₂, 20 mol % NaCl, and 72 mol % Na₂WO₄; and E ₅: 655°C, 9 mol % NaBO₂, 53 mol % NaCl, and 38 mol % Na₂WO₄.     

Efficient oxidative degradation of 2-chlorophenol and 4-chlorophenol over supported CuO-based catalysts

A series of metal oxide catalysts for catalytic oxidative degradation of 2-chlorophenol (2-CP) and 4-chlorophenol (4-CP) were prepared, and the supported CuO catalysts were studied particularly. The supported CuO catalysts were characterized by XRD and NH3-TPD techniques, in which CuO/γ-Al2O3 exhibited high degradation activity. The addition of Na2O or K2O into CuO/γ-Al2O3 improved the oxidative degradation of CPs remarkably, in which Na2O was more efficient than K2O. Over CuO/γ-Al2O3-Na2O, CPs were completely converted and the liberation of the inorganic chloride from 2-CP or 4-CP reached 97% or 100% respectively at 30 ?C for 2 h. The supported CuO catalysts with good dispersion of CuO particles and less acid sites were favorable for the efficient oxidative degradation of CPs. In addition, the initial pH of the reaction solution was found to be an important factor which influenced the catalytic oxidative degradation of CPs and the initial pH of 11.2 and 9.8 was preferred for the oxidative degradation of 2-CP and 4-CP respectively over CuO/γ-Al2O3 catalyst.     

微晶Na0.7MnO2.05的制备及其在水溶液中的充放电特性研究

利用十二核锰簇合物[Mn₁₂O₁₂(CH₃COO)₁₆(H₂O)₄]为前驱物,通过先碱解再灼烧的方法合成了一种钠锰氧化合物Na_0.7MnO_2.05。扫描电子显微镜(SEM)观察结果表明产物由微米级的扁平棒状晶体组成。电化学测试表明,Na_0.7MnO_2.05是一种性能比较优良的超级电容器电极材料。在0.5 mol·L^-1 Na₂SO₄电解质溶液中和0~0.8 V电位窗口范围内,具有良好的循环稳定性能,充放电速率为0.125A·g^-1时单电极比电容达121 F·g^-1。     

NaCl-NaBO2-Na2CO3-NaMoO4 quaternary system

The NaCl-NaBO₂-Na₂CO₃-Na₂MoO₄ quaternary system was studied by a calculation-experimental method and differential thermal analysis. The coordinates of one ternary eutectic and two quaternary eutectics were determined: E ₇: 572°C, 29 mol % NaCl, 10 mol % NaBO₂, 32 mol % Na₂CO₃, and 29 mol % Na₂MoO₄; ɛ₁: 562°C, 36 mol % NaCl, 10 mol % NaBO₂, 30.5 mol % Na₂CO₃, and 23.5 mol % Na₂MoO₄; and ɛ₂: 536°C, 17 mol % NaCl, 10 mol % NaBO₂, 27 mol % Na₂CO₃, and 46 mol % Na₂MoO₄.     

Hydrothermal synthesis of one-dimensional (1D) Na<Subscript>x</Subscript>TiO<Subscript>2</Subscript> nanostructures

Nanorods of sodium titanium dioxide bronze Na_xTiO₂ were synthesized by the hydrothermal treatment of the amorphous TiO₂·nH₂O gel with 10 M NaOH followed by ultrasonication in 0.1 M HCl and thermal treatment (500°C, 10 h). The thermal treatment of the nanorods does not change the morphology of the particles. According to the electron diffraction data, the Na_xTiO₂ nanorods grow along the c axis.__________Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 71–73, January, 2005.     

Thermo-Raman Studies on Dehydration of Na4P2O7⋅10H2O and Phase Transformations of Na4P2O7

In this work, dehydration of sodium diphosphate decahydrate Na₄P₂O₇⋅10H₂O and phase transformations of Na₄P₂O₇ in open air have been studied in detail by thermo-Raman spectroscopy. The spectra were measured continuously in a temperature range from room temperature up to 600°C for the bands of P₂O₇ ^4- and H₂O. The spectral variation showed one step of dehydration and four-phase transformations. The thermo-Raman intensity(TRI) and differential thermo-Raman intensity (DTRI) curves calculated from the characteristic bands of H₂O also showed one step of dehydration with the loss of all hydrated water in the temperature interval from 45 to 69°C. Thermogravimetric measurements supported this result. The thermo-Raman investigation indicated the transformation of Na₄P₂O₇ from low temperature phase to high temperature phase proceed through pre-transitional region from 75 to 410°C before the major orientational disorder at 418°C and minor structural modifications at 511,540 and 560°C. The results from differential scanning calorimetry and differential thermal analysis on Na₄P₂O₇ showed endotherms at 407,517, 523, 548, 557°C and 426, 528, 534, 555, 565°C, respectively. This revised version was published online in July 2006 with corrections to the Cover Date.     

On the mechanism of the P2-Na0.70CoO2→O2-LiCoO2 exchange reaction—Part II: an in situ X-ray diffraction study

A model was proposed to describe the exchange reaction of sodium by lithium in P2 crystals, it was based first on the formation of nucleation centers and then on the growth of O2 domains in P2 crystals from these nucleation centers. This study has shown that depending on the ratio between the growing and nucleation speeds, O2, O6 or faulted structures are obtained and that this model allows a good analysis of the exchange process. XRD patterns simulation and their comparison with that of experimental O2-LiCoO₂ have shown that there was almost no defects in the O2-LiCoO₂ structure obtained by ion exchange in water. Therefore, this study has shown that the growth of the O2 domains in the P2-Na_0.7CoO₂ crystals is faster than the formation of nucleation centers.This P2-Na_0.7CoO₂→O2-LiCoO₂ exchange reaction was also studied in situ by X-ray diffraction; simulations of key XRD patterns by P2-O2 intergrowths were also achieved. It was shown, in good agreement with the simulations, that the growth of O2 domains was faster than the formation of the nucleation centers and kinetically activated by a P2-Na_0.70CoO₂→P2^*-Na_∼0.50CoO₂ phase transition. For those reasons, the P2-Na_0.70CoO₂→O2-LiCoO₂ exchange reaction in water leads to an O2 phase, with an almost ideal packing.