首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到19条相似文献,搜索用时 125 毫秒
1.
室温下,以聚乙烯醇为保护剂,采用抗坏血酸还原硝酸银,于水相中一步合成出三维多枝雪花状银粉。结合X射线粉末衍射(XRD)、扫描电子显微镜(SEM)等结构表征手段,对三维多枝雪花状银粉的微观结构进行详细分析,在此基础上提出其可能的形成机理。此外,三维多枝雪花状银粉在4-硝基苯酚催化加氢反应中还表现出优异的催化活性。  相似文献   

2.
在H2O和乙二醇(EG)构成的二元体系中,通过Zn AC2与NH4F和H2O的水热反应制备了六角雪花状Zn OHF。Zn OHF在空气中退火,制备出了由单晶Zn O纳米片构建的多孔六角雪花状Zn O。用X射线衍射(XRD),扫描电子显微镜(SEM),透射电子显微镜(TEM)及其热重等多种手段对产物进行结构表征,并提出了可能的化学反应。以甲基橙和酸性大红为例,研究了其光催化性能,结果表明,多孔雪花状Zn O是一种有效的光催化剂。  相似文献   

3.
美国Mobil公司于1972年首先开发的ZSM-5分子筛是一种高硅三维交叉孔道的沸石分子筛,其孔道结构具有良好的择形作用,因此被广泛应用于芳构化、异构化、烷基化和催化裂化等工业催化过程.ZSM-5分子筛的催化性能与其晶粒尺寸、酸性及形貌等密切相关.改变合成方法和制备参数可以合成出不同形貌的ZSM-5分子筛,但目前关于ZSM-5分子筛形貌对其物理化学性质和催化性能的影响报道较少.本文通过改变模板剂类型,采用水热合成法,制备出了类雪花状、椭圆柱状和夹心糖状三种不同形貌的ZSM-5分子筛.通过X射线荧光光谱(XRF)、N_2物理吸脱附(BET)、扫描电镜(SEM)、X射线衍射(XRD)、固体核磁共振(MAS NMR)、NH_3程序升温脱附(NH_3-TPD)及吸附吡啶的红外光谱(Py-IR)等手段对不同形貌分子筛的物理化学性质、形貌、晶体骨架结构和酸性进行了表征.采用浸渍法制备了Ca/HZSM-5催化剂,以甲醇制烯烃(MTO)为探针反应、着重研究了ZSM-5分子筛形貌和晶体结构特性对其酸性和催化性能的影响.合成的三种不同形貌的ZSM-5分子筛具有相近的SiO_2/Al_2O_3比和比表面积.XRD结果表明,通过改变模板剂类型,可制得结晶度较好的ZSM-5分子筛,其中类雪花状分子筛的(101)晶面比例明显多于其它两种分子筛,而椭圆柱状分子筛则暴露更多的(020)晶面.~(27)Al MAS NMR结果表明,绝大部分Al都以四配位形式存在于三种分子筛骨架中,而类雪花状分子筛的峰强度较低,这是由于Al的配位环境不同(偶极作用弱),说明在类雪花状分子筛的交叉晶面中存在大量扭曲、错位和不对称结构;与其它两种分子筛相比,类雪花状分子筛的~(29)Si MAS NMR谱峰宽化、进一步证明该分子筛骨架结构中存在扭曲、错位和不对称性.NH_3-TPD结果表明,类雪花状HZSM-5分子筛的酸量明显高于其它两种分子筛,在SiO_2/Al_2O_3比相近的情况下、类雪花状HZSM-5分子筛晶体骨架结构的错位、扭曲和不对称性造成了该分子筛中酸量增加;但Py-IR结果表明,类雪花状HZSM-5分子筛的酸量低于其它两种分子筛,这与NH_3-TPD结果有差异,主要是由于类雪花状分子筛几何空间结构和晶界处的扭曲、错位对孔道结构的影响,不利于比NH_3分子大的吡啶分子的扩散,进而影响了吡啶分子在酸性位上的吸附.三种不同形貌的ZSM-5分子筛经Ca改性后比表面积和微孔比表面积均明显下降,其中类雪花状和椭圆柱状催化剂的微孔比表面积下降幅度较大,外比表面积下降幅度较小.这是因为各分子筛的晶体结构和晶面的取向差异,导致Ca离子在分子筛上的扩散行为不同.同时,经Ca改性后,三个催化剂的总酸量均有下降,尤其是类雪花状分子筛酸量下降较为明显,表明其中Ca离子更容易扩散到分子筛孔道内,与更多的酸性位作用,而夹心糖状分子筛表面具有更多的Z字形孔道,不利于Ca离子扩散到分子筛孔道内,因而酸量下降较少.Py-IR结果表明,Ca改性后催化剂的总酸量下降,尤其是B酸明显降低,L酸略有增加,其中类雪花状ZSM-5分子筛催化剂的B酸量最低.甲醇制烯烃反应评价结果表明,随着反应温度升高,三个催化剂的总烯选择性和丙烯选择性均呈先升高后降低的趋势.类雪花状ZSM-5分子筛催化剂在甲醇转化率相近时具有最高的烯烃选择性,在反应温度为460℃时,总烯烃选择性为72%,丙烯选择性达39%.  相似文献   

4.
研制一种基于金叉指微电极阵列(IDA)的电流型硝酸根离子(NO-3)微传感电极芯片.基于微机电系统(Micro-Electro-Mechanical Systems,MEMS)工艺制备金IDA微电极,通过电化学沉积技术在IDA微电极表面修饰三维枝状结构纳米银敏感膜,利用敏感膜对硝酸根离子良好的电催化还原性能,采用脉冲方波伏安(SWV)电化学测量方法,实现对硝酸根离子在25~1000μmol/L浓度范围内的快速检测,灵敏度达9.5 nA/(μmol/L),线性度为99.98%,检测下限为10μmol/L.考察水体中常见的NO-2,F-,3PO 4-,SO 42-,2CO3-,NH+4,Na+和K+等离子对该传感芯片的干扰性能,传感芯片表现出较好的抗干扰性能.制备的三维枝状结构纳米银修饰IDA微电极可实现水环境(pH 5.0~9.0)中NO-3的电化学检测,对应用于自然水环境中硝酸根离子的现场检测具有积极意义.  相似文献   

5.
采用一种简单的热蒸发法制备了高度有序的ZnO-SnO2异质外延枝状纳米结构。制备过程分两步进行:首先,在氧化铝片基底上制备SnO2纳米线;然后,以此SnO2纳米线为模板在其上生长ZnO纳米线。用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线衍射(XRD)等手段对产物的形貌、结构进行了表征。XRD表征结果证实第一步和第二步生长的产物分别为SnO2和ZnO。SEM观察结果表明,第一步热蒸发得到直径约100nm、长度达几十微米的SnO2纳米线,第二步热蒸发后得到以第一步SnO2纳米线为主干、沿四个方向有序排列的枝状ZnO纳米结构。TEM观察结果表明,ZnO枝状纳米线沿[001]方向由SnO2纳米线(-101)晶面外延生长。所制备的枝状纳米结构由于具有巨大的比表面积,且外延异质结可以促进电荷的分离和快速转移,因此非常适合于光催化应用。该ZnO-SnO2异质外延枝状纳米结构用于光催化降解甲基橙,表现出优异的性能。  相似文献   

6.
超细银粉在太阳能电池正面电极领域有广阔的应用前景,其粒径分布、分散性、表面态与其性能息息相关。 本文通过在液相还原法合成超细银粉的后期引入氧化石墨烯(GO),利用溶液状态下二者相对活性的表面的相互作用获得了性能优良的银粉。 通过X射线衍射(XRD)、拉曼光谱(Raman)和扫描电子显微镜(SEM)等手段对所得复合超细银粉进行结构及形貌表征,结果显示该法获得的银粉分散性较好、尺寸分布较窄。 进而,利用紫外-可见光谱探讨了GO与银粒子之间的相互作用。 而且研究发现:固定硝酸银溶液的浓度,随着GO含量的增加,银粉的导电性能先升高后降低,当GO的质量分数为2.5%时,导电性能更好。 这为超细银粉在实际中的应用提供重要数据和有益参考。  相似文献   

7.
《高分子学报》2017,(2):155-177
树状分子是指一类结构高度支化的大分子或高分子化合物,其独特的三维纳米球形结构、分子内空腔以及大量富集的表面基团,可产生诸多特殊且有趣的功能及光物理性质,在化学、生物和材料等领域获得了广泛的关注和研究.本文主要综述了我们课题组在具有枝状结构二阶非线性光学高分子方面的研究进展,重点介绍了如何通过合理分子设计,发展不同类型枝状拓扑结构以有效提高材料的综合性能,并展望了该领域的今后发展趋势.  相似文献   

8.
氨基酸等生物大分子作为一种特殊的表面活性剂,在合成特殊形貌纳米材料方面具有很大的应用潜力.本文综述了使用多种氨基酸辅助合成的不同形貌的纳米材料,包括一维纳米材料、雪花状纳米结构、三维纳米球等,并对生物科学和化学学科间的交叉发展进行了展望.  相似文献   

9.
氧化锌微晶的制备和形貌控制   总被引:25,自引:0,他引:25       下载免费PDF全文
本文在溶液体系中合成了多种形貌的氧化锌(ZnO)微晶。所得花状、雪花状、棒状、多刺球状和棱柱状氧化锌微晶用粉末X射线衍射(XRD)和扫描电镜(SEM)进行了鉴定和表征,考察了反应条件如溶剂、温度及pH值对ZnO微粒尺寸和形貌的影响,初步探讨了不同形貌ZnO微粒的生长机理。该文对制备形貌可控的氧化物具有一定的指导意义。  相似文献   

10.
枝状分子因其独特的化学结构,其光化学与光物理研究尤为引人注目。本文重点介绍了近二十年来报道的具有光诱导分子内能量转移的枝状分子的化学结构特点,分析了不同因素对光诱导分子内能量转移效率的影响;阐述了可以根据能量给体与受体的性质,利用化学策略对枝状体的分子内光诱导能量转移进行调控;概括了具有光诱导分子内能量转移性质的枝状分子的目前应用领域;总结了枝状体中分子内能量转移面临的关键科学问题,并展望了具有分子内能量转移的枝状分子的发展方向  相似文献   

11.
A variety of fluoroalkyl end‐capped oligomers/silver nanocomposites were prepared by the reactions of silver ions with poly(methylhydrosiloxane) in the presence of fluoroalkyl end‐capped N,N‐dimethylacrylamide oligomer, N‐(1,1‐dimethyl‐3‐oxobutyl)acrylamide oligomer, N,N‐dimethylacrylamide cooligomer containing poly(dimethylsiloxane) segments in organic media such as toluene and 1,2‐ dichloroethane. These fluorinated oligomers/silver nanocomposites thus obtained were found to exhibit clear plasmon absorption bands around 420 nm related to the formation of silver nanoparticles. In particular, these composites could display narrow plasmon absorptions around 420 nm in toluene by the addition of trioctylamine (TOA). On the other hand, the corresponding non‐fluorinated N‐(1,1‐ dimethyl‐3‐oxobutyl)acrylamide oligomer was not able to afford such a plasmon absorption under similar conditions. These fluorinated oligomers/silver nanocomposites in organic media have been found to be stable for more than 10 days. Transmission electron microscopy (TEM) and dynamic light scattering (DLS) measurements showed that silver nanoparticles could be effectively encapsulated into fluorinated oligomeric aggregate cores to afford colloidal stable fluorinated oligomers/silver nanocomposites. Fluorinated oligomers/silver nanocomposites were also applied to the surface modification of traditional organic polymers such as polystyrene (PSt) and poly(methyl methacrylate) (PMMA) to exhibit not only a good oleophobicity imparted by fluorine but also a higher surface antibacterial activity related to the silver nanoparticles on their surface. Copyright © 2007 John Wiley & Sons, Ltd.  相似文献   

12.
Silver nanoparticles were prepared by UV irradiation from silver salts, such as AgBF4 or AgNO3, when dissolved in an amphiphilic film of poly((oxyethylene)9 methacrylate)‐graft‐poly((dimethyl siloxane)n methacrylate), POEM‐g‐mPDMS. The in situ formation of silver nanoparticles in the graft copolymer film was confirmed by transmission electron microscopy (TEM), UV‐visible spectroscopy, and wide angle X‐ray scattering (WAXS). The results demonstrated that the use of AgBF4 yielded silver nanoparticles with a smaller size (~5 nm) and narrower particle distribution when compared with AgNO3. The formation of silver nanoparticles was explained in terms of the interaction strength of the silver ions with the ether oxygens of POEM, as revealed by differential scanning calorimetry (DSC) and X‐ray photoelectron spectroscopy (XPS). It was thus concluded that a stronger interaction of silver ions with the ether oxygens results in a more stable formation of silver nanoparticles, which produces uniform and small‐sized nanoparticles. DSC and small angle X‐ray scattering (SAXS) data also showed the selective incorporation and in situ reduction of the silver ions within the hydrophilic POEM domains. Excellent mechanical properties of the nanocomposite films (3–5 × 105 dyn/cm2) were observed, mostly because of the confinement of silver nanoparticles in the POEM chains as well as interfaces created by the microphase separation of the graft copolymer film. © 2007 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 45: 1283–1290, 2007  相似文献   

13.
From the reaction of 1H‐imidazole ( 1a ), 4,5‐dichloro‐1H‐imidazole ( 1b ) and 1H‐benzimidazole ( 1c ) with p‐cyanobenzyl bromide ( 2 ), symmetrically substituted N‐heterocyclic carbene (NHC) [( 3a–c )] precursors, 1‐methylimidazole ( 5a ), 4,5‐dichloro‐1‐methylimidazole ( 5b ) and 1‐methylbenzimidazole ( 5c ) with benzyl bromide ( 6 ), non‐symmetrically substituted N‐heterocyclic carbene (NHC) [( 7a–c )] precursors were synthesized. These NHC? precursors were then reacted with silver(I) acetate to yield the NHC‐silver complexes [1,3‐bis(4‐cyanobenzyl)imidazole‐2‐ylidene] silver(I) acetate ( 4a ), [4,5‐dichloro‐1,3‐bis(4‐cyanobenzyl)imidazole‐2‐ylidene] silver(I) acetate ( 4b ), [1,3‐bis(4‐cyanobenzyl)benzimidazole‐2‐ylidene] silver(I) acetate ( 4c ), (1‐methyl‐3‐benzylimidazole‐2‐ylidene) silver(I) acetate ( 8a ), (4,5‐dichloro‐1‐methyl‐3‐benzylimidazole‐2‐ylidene) silver(I) acetate ( 8b ) and (1‐methyl‐3‐benzylbenzimidazole‐2‐ylidene) silver(I) acetate ( 8c ) respectively. The four NHC‐precursors 3a–c, 7c and four NHC–silver complexes 4a–c and 8c were characterized by single crystal X‐ray diffraction. The preliminary antibacterial activity of all the compounds was studied against Gram‐negative bacteria Escherichia coli, and Gram‐positive bacteria Staphylococcus aureus using the qualitative Kirby‐Bauer disc‐diffusion method. All NHC–silver complexes exhibited medium to high antibacterial activity with areas of clearance ranging from 4 to 12 mm at the highest amount used, while the NHC‐precursors showed significantly lower activity. In addition, all NHC–silver complexes underwent preliminary cytotoxicity tests on the human renal‐cancer cell line Caki‐1 and showed medium to high cytotoxicity with IC50 values ranging from 53 ( ± 8) to 3.2 ( ± 0.6) µM. Copyright © 2010 John Wiley & Sons, Ltd.  相似文献   

14.
N‐Heterocyclic carbene (NHC) complexes bromo(1,3‐dibenzyl‐1,3‐dihydro‐2H‐imidazol‐2‐ylidene)silver(I) ( 2a ), bromo[1‐(4‐cyanobenzyl)‐3‐methyl‐1,3‐dihydro‐2H‐imidazol‐2‐ylidene]silver(I) ( 2b ), and bromo[1‐(4‐cyanobenzyl)‐3‐methyl‐1,3‐dihydro‐2H‐benzimidazol‐2‐ylidene]silver(I) ( 2c ) were prepared by the reaction of 1,3‐dibenzyl‐1H‐imidazol‐3‐ium bromide ( 1a ), 3‐(4‐cyanobenzyl)‐1‐methyl‐1H‐imidazol‐3‐ium bromide ( 1b ), and 3‐(4‐cyanobenzyl)‐1‐methyl‐1H‐benzimidazol‐3‐ium bromide ( 1c ), respectively, with silver(I) oxide. NHC Complexes chloro(1,3‐dibenzyl‐1,3‐dihydro‐2H‐imidazol‐2‐ylidene)gold(I) ( 3a ), chloro[1‐(4‐cyanobenzyl)‐3‐methyl‐1,3‐dihydro‐2H‐imidazol‐2‐ylidene]gold(I) ( 3b ), and chloro[1‐(4‐cyanobenzyl)‐3‐methyl‐1,3‐dihydro‐2H‐benzimidazol‐2‐ylidene]gold(I) ( 3c ) were prepared via transmetallation of corresponding (bromo)(NHC)silver(I) complexes with chloro(dimethylsulfido)gold(I). The complex 3a was characterized in two polymorphic forms by single‐crystal X‐ray diffraction showing two rotamers in the solid state. The cytotoxicities of all three bromo(NHC)silver(I) complexes and three (chloro)(NHC)gold(I) complexes were investigated through 3‐(4,5‐dimethylthiazol‐2‐yl)‐2,5‐diphenyl‐2H‐tetrazolium bormide (MTT)‐based preliminary in vitro testing on the Caki‐1 cell line in order to determine their IC50 values. (Bromo)(NHC)silver(I) complexes 2a – 2c and (chloro)(NHC)gold(I) complexes 3a – 3c were found to have IC50 values of 27±2, 28±2, 34±6, 10±1, 12±5, and 12±3 μM , respectively, on the Caki‐1 cell line.  相似文献   

15.
Silver‐loading asymmetric cellulose acetate (CA) hollow fiber membrane was spun via the dry jet‐wet spinning technique. The spinning solution was prepared by dissolving AgNO3 and CA in N,N‐dimethylformamide (DMF). The silver ions were reduced in the spinning dope into silver nano‐particles. The morphology of the resulting hollow fibers was examined using a scanning electron microscope and the silver content in the fiber was measured using an inductively coupled plasma atomic emission spectrometer. The antibacterial activities were evaluated. These hollow fibers had a sponge‐like structure and dense inner and outer surfaces. At a 50 k magnification, the pore on the skin layer was not observable, while the nodule size was smaller than 10 nm. The residual silver content of as‐spun hollow fiber was about 60% of the original silver added in the polymer solution. After immersing in water bath for 180 days, the silver content in the bulk of the hollow fibers decreased to 60% and the silver content on the surface reduced to 10%, yet still showed antibacterial activity against Escherichia coli and Staphylococcus aureus. After permeating with water for 5 days, the silver content in the hollow fibers decreased, and did not show antibacterial activity against E. coli and S. aureus. Thus, silver content must be periodically replenished after permeation. The proper range of AgNO3 in the spinning solution for CA hollow fiber should be about 100–1000 ppm. Copyright © 2005 John Wiley & Sons, Ltd.  相似文献   

16.
A novel silver/poly(carbonate urethane) nanocomposite was prepared through in situ reduction of a silver salt (AgNO3) added to a solution consisting of a commercial poly(carbonate urethane) dissolved in N,N‐dimethylformamide (DMF). In this system, the presence of the poly(carbonate urethane) was proved to protect the silver nanoparticles, whose formation was confirmed by means of UV–vis spectroscopy, from aggregation phenomena. The silver morphology developed in the solid state after DMF casting was imaged by FESEM. Homogeneous dispersion of silver nanoprisms in the poly(carbonate urethane) matrix was clearly observed. The effects of dispersion of silver nanoparticles within the poly(carbonate urethane) matrix were investigated by means of ATR‐FTIR and multifrequency dynamic mechanical thermal analyses. The obtained results revealed that the presence of silver nanoparticles modifies both the phase and the viscoelastic behaviors of poly(carbonate urethane). As a matter of fact, the hydrogen bond formation in the hard and soft segments was found to be hindered and the molecular motions of the soft segments were restricted, because a comparatively higher activation energy was required for the related α‐relaxation process. © 2008 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 46: 344–350, 2008  相似文献   

17.
In the non-magnetic semiconductor silver selenide (Ag2+δSe) with a minor heterogeneous silver excess (0.79 × 10−4 < δ ≤ 1 × 10−2) we measured either a saturating negative magnetoresistance (MR) effect, a linear positive MR effect or a superposition of both. This complex MR behavior depends on the amount of the silver metal excess, but is also strongly influenced by the thermal treatment of the samples. Excess silver that cannot be accommodated homogeneously in the silver selenide lattice creates structural heterogeneities and forms a microstructure which is controlled by the thermal annealing procedure. We suggest that small silver segregations at the grain boundaries of the silver selenide matrix (“nanofilms”) are responsible for the negative MR effect, whereas nanoscale silver particles within the silver selenide matrix (nanoparticles) cause a linear positive effect.  相似文献   

18.
In the present work, a series of eight new imidazole, 4,5–dichloroimidazole, 4,5–diphenylimidazole and benzimidazole based nitro–functionalized mono–N –heterocyclic carbene (NHC)–silver(I) acetate ( 7a–d ) and bis–NHC–silver(I) hexafluorophosphate complexes ( 8a–d ) were synthesised by the reaction of the corresponding azolium hexafluorophosphate salts ( 6a–d ) with silver(I) acetate and silver(I) oxide in methanol and acetonitrile, respectively. All the synthesised compounds were fully characterized by various spectroscopic techniques and elemental analyses. Additionally, the structure of bis–(1–benzyl–3–(p –nitrobenzyl)–4,5–dichloroimidazole–2–ylidene)silver(I) hexafluorophosphate complex ( 8b ) was confirmed by single crystal X–ray diffraction analysis. Preliminary in vitro antibacterial evaluation was conducted for all the compounds ( 6a–d) , ( 7a–d) , and ( 8a–d) by Kirby–Bauer's disc diffusion method followed by the determination of Minimum Inhibitory Concentration (MIC) from broth macrodilution method against five standard bacteria; two Gram–positive bacterial strains (Staphylococcus aureus and Bacillus subtilis) and three Gram–negative bacterial strains ( Escherichia coli , Shigella sonnei, and Salmonella typhi). All the hexafluorophosphate salts ( 6a – d) were found inactive against the tested bacterial strains and their corresponding mono– and bis–NHC–silver(I) complexes ( 7a–d and 8a–d ) exhibited moderate to high antibacterial activity with MIC value in the range 8–128 μg/mL. In addition, preliminary in vitro anticancer potential of all the silver(I) complexes ( 7a–d and 8a–d ) was determined against the human derived breast adenocarcinoma cells (MCF 7) by MTT assay. All the mono– and bis–NHC–silver(I) complexes ( 7a–d and 8a–d ) orchestrated high anticancer potential with IC50 values ranging from 10.39 to 59.56 nM. In comparison, mono– NHC–silver(I) complexes performed better than the bis–NHC–silver(I) complexes.  相似文献   

19.
A microphase‐separated, amphiphilic graft copolymer consisting of a poly (vinyl chloride) (PVC) backbone and poly(oxyethylene methacrylate) (POEM) side chains, (PVC‐g‐POEM at 62:38 wt %) was synthesized via atom transfer radical polymerization (ATRP). Nuclear magnetic resonance (1H NMR), FTIR spectroscopy, and transmission electron microscopy (TEM) clearly revealed that the “grafting from” method using ATRP was successful and that the graft copolymer molecularly self‐assembled into discrete nanophase domains of continuous PVC and isolated POEM regions. The self‐assembled graft copolymer film was used to template the growth of silver nanoparticles in solid state by introducing a AgCF3SO3 precursor and a UV irradiation process. The in situ formation of silver nanoparticles in the graft copolymer template film was confirmed by TEM, UV–visible spectroscopy, and wide angle X‐ray scattering. FTIR spectroscopy and X‐ray photoelectron spectroscopy also demonstrated the selective incorporation and in situ formation of silver nanoparticles within the hydrophilic POEM domains, presumably due to strong interactions between the silver and the ether oxygen in POEM. © 2008 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 46: 3911–3918, 2008  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号