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以对甲氧基苯酚和溴代异戊烷为原料,用脱氯化氢反应制备可溶性聚[2-甲氧基-5-(3'-甲基)丁氧基]对苯乙炔(MMB-PPV),通过核磁氢谱(1HNMR)和红外光谱(FTIR)对产物分子的结构进行表征.用能量为15keV、剂量为3.8×1015~9.6×1016ions/cm2的氮正离子(N+)对MMB-PPV薄膜进行注入改性.紫外-可见吸收光谱(UV-Vis)显示,注入离子在MMB-PPV薄膜内部引入杂质能级,破坏了分子的共轭结构.随着注入剂量增加,吸收边逐渐向长波方向移动,且分子激发态和基态间的光学带隙由2.12eV减小至1.81eV.用简并四波混频(DFWM)技术研究了离子注入MMB-PPV薄膜的三阶非线性光学性能.结果表明,未注入薄膜的三阶非线性极化率(χ(3))值为7.1×10-10esu,随着注入剂量的增加,χ(3)值逐渐增大,当注入剂量达到3.8×1016ions/cm2时,χ(3)值提高到9.3×10-9esu,继续增加注入剂量,χ(3)值开始下降,当注入剂量为9.6×1016ions/cm2时,χ(3)值降低到1.5×10-10esu.对离子注入MMB-PPV薄膜χ(3)值变化的机理进行了探讨. 相似文献
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钛、玻璃碳基体中离子注入5×10~(16)×10~(1(?)Ni~+离子cm~(-2).在30%KOH溶液中测试这些电极对氢析出反应的电催化性能.结果表明,离子注入电极的催化活性优于未注入的钛、玻璃碳基体.由极化测量求得动力学参数j、b和E.这些数据表明,在离子注入电极上,氢析出反应的速度决定步骤与镍电极相似,由电化学放电步骤控制。AES测量表明,镍在钛基体中的深度分布近似高斯分布,在阴极极化过程中,注入的镍没有损失,但明显地移向深处.用XPS研究注入前后Ni_(2p)和Ti_(2(?))电子结合能所产生的位移表明,离子注入可能在基体表面形成合金. 相似文献
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《化学研究与应用》2016,(5)
以硝酸银和聚乙烯醇(PVA)为原料,将不同浓度的硝酸银溶解在PVA水溶液中,通过溶液成膜法制备了含有硝酸银的薄膜。对薄膜加热,硝酸银在聚乙烯醇羟基作用下还原成银粒子,从而使薄膜具有导电性。通过热失重分析仪、差示扫描量热仪、扫描电子显微镜、X射线衍射等方法研究了薄膜热性能和热处理后薄膜表面形貌和结构分析。结果表明,AgNO_3/PVA复合薄膜在150~200℃之间出现一个放热峰,表明硝酸银在此温度区间被还原成银粒子。通过热处理方式制备出纳米银,平均尺寸在100 nm左右。由于银粒子的存在,使薄膜具有导电性,当热处理温度从150℃升至175℃,薄膜表面电导率从3.16×10~(-9)S·cm~(-1)增加至1.76×10~(-4)S·cm~(-1),增加了5个数量级,表明热处理时间和处理温度的提高使银粒子的还原更加充分,粒子之间彼此靠近导致导电性提高。 相似文献
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本文通过等离子体发射光谱研究了高气压介质阻挡放电中压力对于激发态氮的影响。其中压力变化范围是0.1MPa到0.5MPa,不同能级的N_2(C~3Π_u)是典型的活性物质。实验结果显示,随着实验气压增加,等离子体主体活性物质数密度从7×10~(15)cm~(-3)降至1×10~(15)cm~(-3)。电子温度随着气压的增加从5eV降至3eV。电子数密度和气压的关系较为复杂,会受到中性分子和电子温度的影响。氮分子激发过程速率常数则随着压力增加近似线性减少,从6×10~(-16)m~3/s降至3×10~(-16)m~3/s。实验结果显示,介质阻挡放电气压增加会显著减少活性物质数量、电子温度,同时近似线性减少氮分子激发过程速率常数。 相似文献
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《化学通报》2018,(9)
本文通过等离子体发射光谱研究了高气压介质阻挡放电中压力对于激发态氮的影响。其中压力变化范围是0.1MPa到0.5MPa,不同能级的N_2(C~3Π_u)是典型的活性物质。实验结果显示,随着实验气压增加,等离子体主体活性物质数密度从7×10~(15)cm~(-3)降至1×10~(15)cm~(-3)。电子温度随着气压的增加从5eV降至3eV。电子数密度和气压的关系较为复杂,会受到中性分子和电子温度的影响。氮分子激发过程速率常数则随着压力增加近似线性减少,从6×10~(-16)m~3/s降至3×10~(-16)m~3/s。实验结果显示,介质阻挡放电气压增加会显著减少活性物质数量、电子温度,同时近似线性减少氮分子激发过程速率常数。 相似文献
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用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%. 相似文献
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The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula. 相似文献
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Rebecca J. Burton Mandy L. CrowtherNeal J. Fazakerley Shaun M. FilleryBarry M. Hayter Jason G. KettleCaroline A. McMillan Paula PerkinsPeter Robins Peter M. SmithEmma J. Williams Gail L. Wrigley 《Tetrahedron letters》2013
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines. 相似文献
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Regiospecific and direct imidation of the methyl C(sp3)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products. 相似文献
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《Tetrahedron》2014,70(21):3377-3384
The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative. 相似文献
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Scope of the copper catalyzed/mediated selenium-nitrogen coupling reaction has been studied for the synthesis of isoselenazolones. It is noticed that the 2-chloro, 2-bromo-, and 2-iodo-aryl amides substrates can be exploited in the selenium-nitrogen coupling reaction by employing 25-100 mol % of CuI/1,10-phenanthroline (L) and potassium carbonate as a base in DMF. Furthermore, electron rich 2-chloro-arylamides also underwent selenium-nitrogen coupling reaction to give biologically important selenium-nitrogen heterocycles. Also, copper-catalyzed selenium-nitrogen coupling reaction has been meticulously applied for the synthesis of diaryl diselenides having methoxy, amine, and amide functionality from respective aryl iodides in the presence of stoichiometric amount of succinimide as an external Se-N coupling partner. 相似文献
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Hao Xu Liyang Pan Xiaomin Fang Baoying Liu Wenkai Zhang Minghua Lu Yuanqing Xu Tao Ding Haibo Chang 《Tetrahedron letters》2017,58(24):2360-2365
A series of novel N-methyl morpholine (Nmm) based ionic liquids with 1,2-propanediol group were synthesized and used as catalysts for Knoevenagel condensation at room temperature in water. Under the effect of the catalyst, various aldehydes or aliphatic ketones could react with a wide range of activated methylene compounds well, including malononitrile, alkyl cyanoacetate, cyanoacetamide, β-diketone, barbituric acid, 2-arylacetonitrile and thiazolidinedione. Furthermore, most of the products could be separated just by filtrating and washing with water. Additionally, the catalyst is recyclable and applicable for the large-scale synthesis. 相似文献
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A series of polyheterocyclic spirotetrahydrothiophene derivatives were obtained in moderate to excellent yields via a catalyst-free sulfa-Michael/aldol cascade reaction of chalcones 1 and commercially available 1,4-dithiane-2,5-diol 2 under mild conditions. We also present the first asymmetric sulfa-Michael/aldol cascade reaction of chalcones 1 and commercially available 1,4-dithiane-2,5-diol 2 with moderate to good enantioselectivities catalyzed by readily available chiral phase-transfer catalysts (PTCs). 相似文献
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Andrey A. BerezinPanayiotis A. Koutentis 《Tetrahedron》2011,67(22):4069-4078
Both soluble guanylate cyclase (sGC) inhibitors ODQ 1 and NS2028 2 are synthesized via improved protocols. In the former case treating 3,4-dihydroquinoxalin-2(1H)-one oxime 8, which can be prepared in two steps from 1,2-benzenediamine, with 1,1′-carbonyldiimidazole (CDI) gives the dihydro-ODQ 10 that in the presence of KMnO4 oxidises to give ODQ 1 in an overall yield of 46% starting from 1,2-benzenediamine. In the latter case, the synthesis affords NS2028 2 from 2-amino-4-bromophenol 3 in three steps with an overall yield of 85% and avoids the need for chromatography. Furthermore, Suzuki-Miyaura reaction conditions are described that enable the preparation of 8-aryl and 8-heteroaryl derivatives of NS2028 directly from NS2028 2. Finally, demethylation of the 8-(methoxyphenyl) substituted analogues afforded the 8-(hydroxyphenyl) derivatives 40-42. All new products are fully characterised. 相似文献