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1.
利用纳米晶的催化性质合成二联苯   总被引:7,自引:0,他引:7       下载免费PDF全文
利用GaP纳米晶的表面催化作用, 从苯直接合成了二联苯, 并研究了合成反应过程中GaP纳米晶含量的影响. 结果表明:在没有GaP纳米晶时, 直到480℃也没有观察到苯的明显聚合; 而当有GaP纳米晶存在时, 参与聚合反应的苯的数量与GaP纳米晶的含量成正比, 在足够高的GaP纳米晶含量情况下, 高温(450~480℃)时苯几乎完全发生聚合, 而且二联苯的相对产率较高; 与之相反, 在低温条件(250~300℃)下, 即使有足够的GaP纳米晶存在, 苯也只有少量发生聚合, 二联苯的相对产率迅速降低. 对样品所做的红外、核磁共振、以及元素分析证实了样品是二联苯.  相似文献   

2.
反应时间对GaP纳米材料粒度的影响   总被引:2,自引:0,他引:2  
以GaCl3和Na3P为原料,利用苯热合成方法,在相同的温度、不同的反应时间下制备GaP纳米粒子。由分散在苯中的GaP纳米粒子的吸收光谱和透射电子显微镜测试结果可知,反应时间延长时GaP苯溶液的光吸收谱发生明显的蓝移。本文分析了出现这一现象的原因,并从实验上进行了验证。  相似文献   

3.
分别以磷和GaCl~3的乙醚溶液、GaCl~3的苯溶液为原料,用苯热合成法制备了GaP纳米微晶。初步探讨了反应过程中介质中的水和氧对生成物的影响,并利用化学键的解离能数据对生成物的稳定性进行了分析。结果表明:介质中的水和氧可以在很大程度上影响反应过程,甚至改变反应进行的方向。  相似文献   

4.
苯热GaP纳米微晶介质中水氧对反应过程的影响   总被引:1,自引:0,他引:1  
分别以磷和GaCl~3的乙醚溶液、GaCl~3的苯溶液为原料,用苯热合成法制备了GaP纳米微晶。初步探讨了反应过程中介质中的水和氧对生成物的影响,并利用化学键的解离能数据对生成物的稳定性进行了分析。结果表明:介质中的水和氧可以在很大程度上影响反应过程,甚至改变反应进行的方向。  相似文献   

5.
胶溶法制备NiO纳米晶热敏材料   总被引:17,自引:2,他引:17  
本文用胶溶法合成了NiO纳米晶超微粒.初步探讨了合成的最佳实验条件.研究了不同灼烧温度及同一温度不同灼烧时间对NiO超微粒子微晶的晶化过程的影响.用X射线衍射、红外光谱、热重、差热、透射电镜研究了样品的性能.结果表明,用胶溶法制得的NiO纳米晶的粒度均小于6nm,属立方晶系,形状为球形.电导率随着温度的升高而迅速增大,是一个有应用前景的热敏材料.  相似文献   

6.
溶剂热合成单分散硫化镉纳米晶   总被引:3,自引:1,他引:2  
汤嘉立  吴访升  陈铭 《化学学报》2008,66(14):1647-1650
在双表面活性剂十八胺和油酸存在条件下, 以氯化镉和硫粉作为反应前驱物, 通过简单的溶剂热方法合成单分散性闪锌矿硫化镉纳米晶, 粒径大小在13 nm. 用X射线衍射(XRD)、透射电子显微镜(TEM)对产物的结构和形貌进行了表征, 同时对硫化镉纳米晶的紫外吸收谱和光致发光谱(PL)性能进行了表征. 实验结果表明合成的样品具有很好的发光性能, 此外溶剂热反应的温度对纳米晶的单分散性有重要影响. 并对硫化镉纳米晶的形成机理做了初步的研究.  相似文献   

7.
BaTiO3纳米晶的合成与表征   总被引:12,自引:2,他引:12  
以硬脂酸、硬脂酸钡和钛酸丁酯为原料合成了BaTiO3纳米晶,粒度为10~20nm,烧成温度为650℃,低于传统的合成温度。用红外光谱、差热分析、热重分析和X射线衍射对合成过程进行了研究,用透射电镜考察纳米晶的粒度和形貌。用发射光谱和X射线荧光光谱对样品纯度进行了分析。结果表明,此法合成的纳米晶BaTiO3纯度高、粒度小且较均匀,在常温下属立方钙钛矿型。  相似文献   

8.
线团式纳米NaY分子筛复合材料的制备及形成机理   总被引:1,自引:0,他引:1  
通过在偏高岭土水热合成NaY分子筛的晶化过程中加入乙醇的方法,制备了线团式纳米NaY分子筛复合材料,用XRD、SEM、ICP OES研究了晶化过程中固液相结构和组成的变化,初步探讨了其形成机理,提出了制备纳米NaY分子筛复合材料的条件.  相似文献   

9.
以二硫化四甲基秋兰姆((TMTD)作为有机硫源,分别在苯、水-苯溶剂中于不同温度、不同时间溶剂热法合成了CdS纳米晶体。采用FE-SEM、XRD和FTIR对晶体的结构和成形机理进行了研究。结果表明,溶剂热温度比反应时间对晶体形貌的形成影响更大。CdS纳米晶体是立方与六角的混合晶型。此外,溶剂的种类也是影响CdS纳米晶体结构和成形的重要因素,并且对花形CdS纳米晶体进行了阴极发光(CL)光谱的研究。  相似文献   

10.
以巯基乙醇为修饰剂,在水溶液中合成了稳定的CdSe/CdS纳米晶,应用单因素法和多目标单纯形法探索合成条件。通过透射电镜观察所合成的纳米晶的形貌和大小,用紫外-可见吸收光谱和荧光光谱对其光学特性进行了表征。并且以L-色氨酸荧光量子产率0.14为标准,测量了合成的CdSe/CdS纳米晶的荧光量子产率为0.37。  相似文献   

11.
Diphenylene was synthesized directly from benzene under the catalytic effect of GaP nanocrystals, and the effect of GaP nanocrystals content was studied. The experimental results showed that no reactions took place without GaP nanocrystals. The more the GaP nanocrystals added, the more the reaction complete. Furthermore, at high temperatures (450-480℃), when the content of GaP nanocrystals was high enough, almost all benzene polymerized and the yield of diphenylene was rather high. On the contrast, even if there are enough GaP nanocrystals in the reaction mixture, almost no polymerization reaction took place at low temperature (for example, 250-300℃), and the yield of diphenylene was very poor. The analytical results of XRD, IR, elemental analysis and NMR proved that the sample was truly diphenylene.  相似文献   

12.
A mild aqueous synthesis route was successfully established to synthesize well crystallized and monodisperse GaP and InP nanocrystals, which were proved to exhibit pronounced quantum confinement by room-temperature UV/Vis adsorption and photoluminescence (PL) spectra.  相似文献   

13.
With GaP nanocrystals being used in a close reaction system, 6-phenylfulvene is successfully obtained via a high yield thermic conversion from benzene, which provides the possibility of applying nanocrystals to mediate organic reactions.  相似文献   

14.
Sterically induced shape and crystalline phase control of GaP nanocrystals   总被引:3,自引:0,他引:3  
We demonstrate a novel synthetic scheme that can be used to control the crystalline phase and shape of GaP semiconductor nanocrystals. Our study shows that steric effects of surfactant ligands can modulate the crystalline phases and control the shapes of nanocrystals. The shape of the nanocrystals obtained varies from zero-dimensional spheres to one-dimensional rods via controlling the ratio between primary and tertiary alkylamines. III-V semiconductors (in our case: GaP) under 10 nm in width are first reported, and unique optical properties due to shape anisotropy are also observed.  相似文献   

15.
Gao S  Xie Y  Zhu L  Tian X 《Inorganic chemistry》2003,42(17):5442-5447
The thermostability and reactivity of GaP nanocrystals in O(2) were investigated using the thermogravimetric analysis (TGA), differential thermal analysis (DTA), powder X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS) analysis techniques. alpha-Ga(2)O(3) nanoparticles, nano-hollow-particles, or nanorods and nanotubes can be separately obtained from the oxidation of nanocrystalline GaP at 400 degrees C for 30 min in dry O(2) atmosphere via manipulating different heating rates. Transmission electron microscopy (TEM) and energy-dispersive X-ray spectrometry (EDX) analysis showed that the products were all alpha-Ga(2)O(3) but with different morphologies when different heating rates were applied. The formation mechanisms of the different morphological alpha-Ga(2)O(3) nanocrystals were discussed.  相似文献   

16.
In this paper, we present a new procedure for the rapid synthesis of luminescent ZnSe nanocrystals in aqueous phase by microwave irradiation with controllable temperature. The effects of microwave irradiation and experimental conditions on the synthesis of nanocrystals were investigated systematically. It was found that there were significant effects of pH value of reaction solutions, molar ratio of precursors, and heating time of microwave irradiation on the optical properties of the ZnSe nanocrystals. A series of nanocrystals with different size was prepared in 1 h, and the photoluminescence quantum yield reached up to 17% at the optimal reaction condition. The results of HRTEM and XRD showed that the as-prepared nanocrystals had high crystallinity. The characterizations of EDS spectra and elemental analysis showed that the sulfur content of nanocrystals increased with the growth of nanocrystals. We speculated that the structure of nanocrystals was an alloy ZnSe(S) shell on the surface of the ZnSe particles core. Furthermore, we found that the oxygen from air in the reaction vessel played an important role in the decomposition of the thiol group under microwave irradiation.  相似文献   

17.
Hydrophilic Ce, Tb doped BaYF(5) nanocrystals with uniform size were synthesized by a microwave-assisted route. The synthesized nanocrystals can be well dispersed in hydrophilic solutions (DMSO, DMF, EG, H(2)O). This synthesis procedure represents a less time consuming method, with high product yield and without using any assistant or/and template reagents, which may be expected to be a general method for rapid synthesis of other hydrophilic RE doped fluoride fluorescent nanocrystals. The Ce(3+), Tb(3+) codoped BaYF(5) nanocrystals show bright green fluorescence emission. The Ce(3+) acts as an effective energy transfer medium and the emission at the high (5)D(3) energy level of Tb is enhanced in this host material.  相似文献   

18.
Highly photoluminescent glass was prepared by embedding water-soluble nanocrystals in a glass matrix using a novel sol-gel process. Thiol-stabilized CdTe nanocrystals and aminopropyltrimethoxysilane were found to be the best combination in the preparation. The synthesis process had to be optimized to avoid nanocrystal agglomeration. The nanocrystals thus embedded in the glass matrix did not show any deterioration of the surface condition. The obtained glass combines excellent optical properties of nanocrystals with the high stability of glass; it emits light of various colors with narrow emission spectra and high photoluminescent efficiency (41%).  相似文献   

19.
Platinum nanocrystals with different shapes are generally produced by wet-chemical synthesis in colloidal solutions. In this study, we shaped electrochemically Pt nanocrystals on highly boron doped diamond electrodes without adding surfactants or additives. Their shapes were controlled by varying deposition potential during electrodeposition process, as confirmed with high resolution scanning electron microscope. Their crystallography of Pt nanocrystals was analyzed through hydrogen adsorption/desorption behavior in acidic solutions. Oxygen reduction reactions on these nanocrystals were investigated, indicating shape dependence. The discussion on shaping mechanism reveals that hydrogen evolution reaction is deemed to be responsible.  相似文献   

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