TiO2薄膜/锡掺杂玻璃光波导元件对苯乙烯蒸气的气敏性研究

本文将溶胶-凝胶法制备的溶胶采用浸渍提拉法固定在锡掺杂玻璃光波导元件表面,通过500℃热处理得到TiO2薄膜,且对低浓度的苯乙烯蒸气进行检测。从实验得知,该传感元件在挥发性有机气体浓度(体积分数)低到5.0×10-5时只对苯乙烯有响应,此时其他气体毫无响应,并在1.0×10-6～5.0×10-4范围之内对苯乙烯有较好的响应。响应时间和恢复时间分别为12s和34s。该传感器具有灵敏度高、响应快、可逆性和重复性好、易制作等特点。     

光波导传感元件在检测酸性气体中的应用

采用旋转甩涂法将甲基紫传感薄膜固定在特制的锡(Sn2+,Sn4+)掺杂玻璃光波导(Sn doped glass slide)表面,研究了该传感薄膜与HCl、H2S、以及SO2作用前后的可见吸收光谱的变化,并在此基础上研制了玻璃光波导酸性气体(HCl、H2S、SO2)传感元件。传感薄膜与酸性气体作用时,薄膜的颜色发生变化,从而降低薄膜对倏逝波的吸收,使传感器的输出光强度(信号)增强。本文采用流动注射法对酸性气体进行了检测。实验结果表明,在室温下,该传感元件对硫化氢气体具有明显的响应,而对相同浓度的其他酸性气体的响应相对较小,对浓度在6×10-4～2.5×10-5(V/V)的硫化氢气体具有良好的线性响应(R=0.9979,n=4),相对标准偏差(RSD)为±3.5%,具有响应快、可逆性和重复性好、容易制备、可以在室温下工作等特点。     

ZnFe2O4薄膜/锡掺杂玻璃复合光波导敏感元件的研究

采用浸渍-提拉法,将铁酸锌溶胶固定在锡掺杂玻璃光波导元件表面,通过不同的热处理温度(400℃,500℃,600℃)得到ZnFe2O4薄膜/锡掺杂玻璃复合光波导敏感元件,且对低浓度的苯乙烯蒸汽进行检测。在500℃热处理的传感元件对苯乙烯(相同浓度的挥发性气体中)的响应较大,并在体积比2.0×10-10~2.0×10-6范围内有较好的响应。响应时间和恢复时间分别为17s和60s。     

Y2O3薄膜/锡掺杂玻璃光波导气敏元件及其气敏性

采用溶胶-凝胶法将氧化钇(Y2O3)敏感膜固定在锡掺杂玻璃光波导表面,研制出了Y2O3薄膜/锡掺杂玻璃光波导气敏元件,并对挥发性有机气体进行了检测.通过XRD测试对敏感薄膜的结构及晶粒尺寸进行了表征.实验结果表明,在室温下Y2O3薄膜/锡掺杂玻璃光波导气敏元件对二甲苯、氯苯气体有较好的选择性响应,其响应浓度范围为l×10-3 ～1×10-5(V/V).Y2O3薄膜/锡掺杂玻璃光波导气敏元件具有灵敏度高、成本低、响应速度快、制作工艺简单和可逆性好等优点.     

溶胶-凝胶法制备氧化锌薄膜/锡掺杂玻璃光波导及其气敏性研究

采用溶胶-凝胶法制备出氧化锌薄膜/锡掺杂玻璃光波导气敏元件,并在光波导传感检测系统中对二甲苯气体进行检测.结果表明,室温下该气敏元件对二甲苯气体有较好的响应,而对相同浓度的其它挥发性有机气体的响应相对较小,能检测出的二甲苯气体的响应范围为1×10-3～4×10-6,而对其它挥发性有机物气体的响应相对较小.同时该气敏元件...     

钇掺杂对磷酸亚铁锂薄膜光波导传感元件气敏特性的影响

利用水热法合成出LiFePO4和钇(Y)掺杂的LiFePO4粉体,并作为敏感试剂,用浸渍-提拉法固定在锡掺杂玻璃光波导表面,分别研制了LiFePO4和LiFe0.99 Y0.01 PO4薄膜/锡掺杂玻璃光波导传感元件.用这些薄膜传感元件对挥发性有机气体进行检测,并比较了它们的气敏特性.结果表明,掺杂Y后LiFePO4薄...     

PVA薄膜光波导气敏元件及其应用研究

将纯聚乙烯醇(PVA)和掺有维生素C的PVA作为敏感试剂,通过旋转甩涂法分别研制出了PVA薄膜/锡掺杂玻璃光波导元件和VC-PVA薄膜/锡掺杂玻璃光波导元件并检测其气敏特性.实验结果表明,PVA薄膜/锡掺杂玻璃光波导元件对二甲苯气体有良好的选择性响应,其响应浓度范围为10-4～10-7(体积比);加入VC后,使此敏感元...     

LiFe0.98 Pt0.02 PO4薄膜的光学及气敏性研究

为提高LiFePO_4敏感薄膜元件的灵敏度,以铂(Pt)作为掺杂元素,用水热法一步合成出LiFe_(0.98)Pt_(0.02)PO_4粉末;利用旋涂法将其固定在锡掺杂玻璃光波导表面,制备了LiFe_(0.98)Pt_(0.02)PO_4薄膜/锡掺杂玻璃光波导元件。将敏感薄膜在不同温度下热处理,通过比较各个敏感薄膜元件对苯类挥发性有机气体的响应讨论薄膜处理温度对LiFe_(0.98)Pt_(0.02)PO_4薄膜元件光学特性及气敏性的影响。结果显示,在450℃下处理的薄膜因具有光学透明性好、折射率高、光传播损失小等特点对苯类气体显出较大的响应,能够检测出浓度为1×10~(-7)~1×10~(-3)V/V_0的二甲苯气体。当气体浓度小于1×10~(-6)V/V_0时,其他苯类气体不会对二甲苯的检测产生影响。     

氧化镍-铁酸锌复合薄膜/锡掺杂玻璃光波导传感元件的制备及其对硫化氢气体的气敏性

用溶胶-凝胶法制成了NiO掺杂的ZnFe2O4溶胶,并用浸渍提拉法将其固定在锡掺杂玻璃光波导表面,研制了NiO-ZnFe2O4复合薄膜/锡掺杂玻璃光波导气敏元件,并对无机有毒气体进行了检测。 实验结果表明,在室温下,该传感元件对H2S气体具有一定的选择性响应,而对相同浓度的其它无机气体的响应相对较小,能够检测到1.0×10-9（体积比）的H2S气体,其响应和恢复时间分别是6和8 s。 该元件具有灵敏度高、响应-恢复快、可逆性和重复性好、容易制备,在室温下便于操作等特点。     

热处理对LiFe1-0.01xY0.005xAg0.005xPO4薄膜光波导传感元件气敏性的影响

以FeSO4.7H2O,H3PO4,LiOH.H2O,AgNO3及Y(NO3)3.6H2O为原料,利用水热法一步合成出了LiFe1-0.01xY0.005xAg0.005xPO4粉体(x=0.5,1.0),并将该材料作为敏感试剂,用旋转-甩涂法做成纳米薄膜固定在锡掺杂玻璃光波导表面,在不同温度下进行热处理。采用紫外-可见分光光度计、测厚仪以及自组装的玻璃光波导气敏测试仪研究了热处理对LiFe1-0.01xY0.005xAg0.005xPO4薄膜光学及气敏特性的影响。研究结果表明:在450℃下进行热处理的薄膜元件具有良好的光学透明及较好的气敏特性。相同浓度的不同挥发性有机气体中,该传感元件对二甲苯气体有很好的选择性响应,其检测响应范围为1×10-7～1×10-3(V/V),响应-恢复时间分别小于5和100 s。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

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%.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

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.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

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.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

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.     

Selective syntheses of 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones via temperature-dependent Rh(II)-carbenoid-mediated 2H-azirine-ring expansion

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.     

Copper catalyzed/mediated synthetic methodology for ebselen and related isoselenazolones

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.     

Knoevenagel condensation catalyzed by novel Nmm-based ionic liquids in water

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.     

Construction of polyheterocyclic spirotetrahydrothiophene derivatives via sulfa-Michael/aldol cascade reaction

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).     

Suzuki-Miyaura reactions of the soluble guanylate cyclase inhibitor NS2028: a non-product specific route to C-8 substituted analogues

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.