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。     

Pr6O11对SnO2半导体气敏特性的影响

研究了添加Pr_6O_11的SnO_2半导体气敏元件的气敏特性。在丙酮、乙醇、甲烷、一氧化碳等11种气氛中测量结果表明,元件对丙酮、乙醇具有选择性,Pr_6O_(11)的最佳含量为1.0wt％左右。实验还发现,元件的限定工作温度随着Pr_6O_(11)含量的增加而下降,响应时间和恢复时间缩短,灵敏度随被测气体浓度变化的线性范围相应增大。     

超声喷雾共沉淀法制备纳米氧化锡粉体及其气敏性研究

采用超声波喷雾技术,以SnCl4·5H2O和CO(NH2)2为前驱体原料制备了氧化锡以及Ce稀土离子掺杂纳米粉体.详细地研究了超声喷雾条件、反应时间以及化学组分对纳米SnO2粉体的形貌和尺寸的影响规律,以及前驱体沉淀物脱水化学处理的条件.用XRD,TEM研究了所获纳米粒子的晶相和形貌.结果表明,制备的SnO2纳米粒子呈球状,尺寸在10～20 nm,纳米颗粒均匀,分散性好.以该粉体为基础制备了相应的气敏元件,测定了气体灵敏度与温度和稀土元素掺杂的关系.研究测试表明,纳米SnO2半导体气敏元件对NO2气体有着良好的响应-恢复特性,并且具有较高的灵敏度和较低的工作温度.稀土元素铈的掺杂能明显提高纳米SnO2粉体的气敏性能.     

SmFe_(1-y)Sr_yO_3的制备及其气敏性能

用sol-gel法制备SmFe_(1-y)Sr_yO_3(y=0,0.1,0.2,0.3,0.4,0.5,0.6)粉体.XRD图谱表明SmFe_(1-y)Sr_yO_3为正交钙钛矿结构,粉体的晶胞体积和晶粒尺寸均随Sr~(2+)含量的增大而增大.用SmFe_(1-y)Sr_yO_3纳米粉体制备成气敏元件,测试了其对乙醇气体的气敏特性.结果表明,在同等条件下,以SmFe_(0.7)Sr_(0.3)O_3元件对乙醇的气敏性能最优,在工作温度为240℃时对体积分数为1×10~(-4)的乙醇的灵敏度达到26.14,是SmFeO_3元件的10.80倍.SmFe_(0.7)Sr_(0.3)O_3元件同时还表现出较好的选择性、响应-恢复特性与稳定性,工作温度为240℃时的响应时间和恢复时间分别为28s和83s.     

常温SnO_2-α-Fe_2O_3气敏元件制备

用a-Fe_2O_3研制成的加热式气敏元件功耗大(约1.5W)。常温SnO_2-a-Fe_2O_3气敏元件功耗低(约0.1W),灵敏度高,响应恢复快,稳定,具有一定选择性。 气敏元件制备方法:按62.5％,6.2％和31.3％称取SnO_2,a-Fe_2O_3和硅胶,加水研磨2小时,使其呈浆糊状,点入模具内,放入一对φ0.05mm铂丝电极,晾干,脱模,在860～890℃空气中烧结95分钟。     

PdO,Au, CdO修饰SnO2纳米纤维的制备及其气敏特性

采用静电纺丝的方法制备了SnO₂纳米纤维,并分别用PdO、Au、CdO对该纳米纤维材料进行表面修饰.用X射线衍射(XRD)、扫描电子显微镜(SEM)、X射线能谱(EDX)、X射线光电子能谱(XPS)分析、Brunauer-Emmett-Teller (BET)比表面积测试对材料进行表征.修饰前后, SnO₂纳米纤维都是由约15 nm的纳米颗粒构成的直径约为200 nm的多级结构材料.采用静态测试系统对纯SnO₂及不同物质修饰的SnO₂的气敏特性进行测试,结果表明,未修饰的SnO₂纳米纤维气敏元件对甲醛具有较好的响应.修饰后的SnO₂材料的气敏特性都有明显的改善. CdO修饰的SnO₂气敏元件对甲醛的响应值最高,且响应恢复时间短,选择性好. Au修饰的SnO₂气敏元件对甲醛响应的最佳工作温度从300 ℃降到了200 ℃.经PdO修饰后, SnO₂纳米纤维对甲苯的响应值变得最高.初步分析了经过修饰的SnO₂气敏材料的敏感机理.     

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.     

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。     

MgFe2O4纳米颗粒及其气敏性研究

利用Sol-gel燃烧法合成氧化物MgFe2O4对氯气有很高的灵敏度,并利用XRD对产品的物相进行了分析;用TEM对粉体晶粒和形貌进行检测,将产物粉体制成气敏元件,采用静态配气法在气敏测试仪上进行了灵敏度和响应-恢复曲线的测试,研究证明镁铁复合氧化物对氯气有很好的气敏特性。     

表面气氛处理对气敏元件特性的影响

选择适当气体对气敏元件进行处理是气敏元件表面修饰的重要方法，本文利用ＳＯ２对Ｈ２Ｓ气敏元件进行了不同条件的处理，使得气敏元件的灵敏度和选择性得到了明显的改善。     

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%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

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.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

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.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.