红色发光长余辉材料Ca2SnO4:Eu3+的性能研究

利用高温固相法合成了Ca2nO4:Eu3+色发射长余辉发光材料,对样品进行了X射线衍射分析、荧光光谱分析、形貌分析以及发光寿命测量.分析结果表明,在1350℃下烧结3 h的Ca2SnO4:Eu3+为单相产物,所得Ca2SnO4:Eu3+发光材料具有良好的发光性能,在267 nm紫外线激发下发出最强发射位于617 nm的锐线发射,并且具有明显的长余辉发光性能.     

固溶体结构对Ca_(2-x)Sr_xZn_4Ti_(15)O_(36)∶Pr~(3+)发光性质的影响

0引言在绿色和蓝色长余辉发光材料达到应用程度之后,耐候性红色长余辉发光材料成为人们研究的重点。Eu3 、Sm3 激活的硫氧化物[1￣3]、Eu2 铝锶复合硫氧化物[4]和Y2O3∶Eu3 [5]等耐热耐水性红色长余辉材料被相继发现。Pr3 离子掺杂的碱土金属钛酸盐(M TiO3∶Pr,M=M g,Ca,Sr,Ba)是一种新型的红色长余辉发光材料。这种发光材料在615nm附近有很好的单色性红光发射。碱土金属钛酸盐基质化学性能稳定,已开始应用于场发射显示器(FE D)[6,7]。碱土金属钛酸盐是A BO3型化合物,具有钙钛矿结构。B all[8]曾通过在CaTiO3中掺入不同量的Sr2 …     

Yb3+共掺杂对Zn2GeO4:Mn2+绿色长余辉发光性能增强研究

利用高温固相法合成了Zn2GeO4:Mn2+以及Zn2GeO4:Mn2+,Yb3+绿色发射长余辉发光材料,对样品进行了X射线衍射分析、荧光光谱分析、色坐标、热释发光以及发光寿命测量.分析结果表明,在1050℃下烧结3h的Zn2CeO4为单相产物,所得Zn2GeO4:Mn2+发光材料具有良好的发光性能,在紫外灯激发下发出最强发射位于528 nm的宽带发射并具有优良的长余辉发光特性,其色坐标值分别为x=0.145,y=0.773.Yb3+共掺杂对其长余辉发光性能提高明显.余辉发光在暗场环境下肉眼可观察的持续时间超过2h.通过热释光谱对陷阱进行了分析.对Yb3+共掺杂的长余辉发光增强机理进行了讨论.     

钛酸盐红色长余辉陶瓷的制备与表征

以高温熔融法制备了钛酸盐为基质的红色长余辉陶瓷,研究氧化物及稀土氧化物改变对陶瓷发光性能的影响,用荧光光谱仪及X射线衍射仪对所制备的陶瓷试样进行表征.结果表明:添加适当的氧化物可获得均匀的玻璃并显著改善陶瓷的发光性能,共掺杂稀土离子不改变Ca0.8Zn0.2TiO3:Pr3+的发光机制.其发射峰为位于617 nm的窄带峰,对应于Pr3+的1D2→3H4的跃迁发射.添加的氧化物及稀土氧化物不改变基质的晶格,主晶相为CaTiO3.     

乙二醇辅助水热法制备不同形貌的CaTiO_3/CaTiO_3:Pr微晶

对乙二醇存在下水热法制备CaTiO3微晶的形貌进行了研究。对所得样品用X射线衍射、扫描电子显微镜(SEM)、热重分析及红外光谱(FTIR)进行了表征。结果表明,制备的CaTiO3微晶随着乙二醇和水配比的不同,可以形成立方体、三维十字架形及正十二面体等规整的外形。乙二醇在晶粒表面的配位吸附对这些不同形貌的形成有决定的作用。所得样品粒度分布均匀,基本不团聚。掺杂少量Pr3+离子后对样品的微观形貌基本不影响,在200℃低温水热获得的CaTiO3∶Pr样品就有明显的荧光和长余辉发光性能。样品在900℃煅烧后其外形并不发生变化,也不会团聚,但发光性质得到大幅度提高。     

ZnO/Eu~(3+)发光材料的高温固相合成及其发光性能

采用高温固相法制备了ZnO/Eu3+红色长余辉发光材料.应用正交试验设计法(每个因素取3个水平,选用L9(34)正交试验表),以初始亮度为指标,研究了煅烧温度、Eu3+质量分数、敏化剂Li+质量分数、煅烧时间等4个因素对发光性能的影响;利用X射线衍射仪对合成的ZnO/Eu3+发光材料进行了物相分析,应用荧光分光光度计测定了样品的激发光谱和发射光谱,应用照射计测定了样品的发光特性.结果表明,当各个因素在水平范围内变化时,所制备的样品均具有ZnO晶格结构;荧光粉的主激发峰位于365 nm和458 nm处,主发射峰位于480 nm、570 nm和600 nm~640 nm,对应于Eu3+的4f和5d间的激发和发射.所确定的最佳合成条件为:煅烧温度850℃,w(Eu3+)=4%,w(Li+)=2.5%,煅烧时间3 h.     

水热法合成Sr4Al14O25:Eu2+,Dy3+长余辉发光材料及性能研究

采用水热法制备了均匀分散的前驱体,然后通过煅烧获得蓝绿色Sr4 Al14O25:Eu2+,Dy3+长余辉发光材料.在制备前躯体过程中,分别用NH3·H2O和NH4HCO3作为沉淀剂,研究了其对最终发光材料的结构和性能的影响.结果表明,用氨水做沉淀剂最终合成的发光粉为物相较纯的Sr4 Al14O25相,粒径小,分散性好,发光强度高,余辉衰减时间长.     

铝酸盐紫色长时发光材料的研制

采用高温固相法制备了紫色长时发光材料CaAl2O4∶Eu2 , Nd3 . 研究了原料配比、激活剂和助熔剂含量、烧结温度、保温时间、还原气氛等对材料长时发光性能的影响. 当原料中Ca和Al的摩尔比为1.0∶2.3, 激活剂Eu2 含量为0.005 mol/mol, 助熔剂含量为1.6% (质量分数), 烧结温度为1350 ℃, 保温时间为4 h, 在氢气气氛下还原时, 所制得的材料的长时发光性能最佳. 当在原料中掺杂了辅助激活剂Nd3 后, 发光材料的初始发光亮度和发光时间都有了明显的提高.     

燃烧法合成Sr_2Al_3O_6:Eu~(2+),Dy~(3+)发光材料的物相组成研究

提出采用燃烧法合成Sr_3Al_2O_6:Eu~(2+),Dy~(3+)红色长余辉发光材料,旨在通过工艺优化合成出单相的铝酸锶基质,为制备发光性能良好的红色发光材料打下基础。通过对样品进行XRD衍射分析,分别探讨了燃烧温度、尿素添加量以及二次还原工序的引入对样品的物相组成的影响。结果表明:仅调节燃烧温度和尿素添加量不能得到单相Sr_3Al_2O_6基质,产物中往往存在SrAl_2O_4,Sr_4Al_2O_7等杂质相,然而当尿素添加量增加时,虽导致产生大量SrCO_3,但同时也抑制了很难排除的杂质相SrAl_2O_4,Sr_4Al_2O_7的生成。如将该样品在1200℃下还原煅烧则可使SrCO_3分解继而反应生成目标产物Sr_3Al_2O_6,由此获得接近纯相的Sr_3Al_2O_6基质。最终确定较优化的工艺条件为:燃烧温度为850℃,尿素添加量为硝酸盐的2倍,燃烧后在1200℃下进行二次还原煅烧。     

锗酸镉中镨的长余辉发光特性

通过高温固相法在空气条件下制得cd2Ge7016：Pr3’长余辉发光材料。测其结构为一单相。分析了cd2Ge70…cd2Ge7016：Pr3’的激发光谱和发射光谱，指出Cd2Ge7016：Pr3’的发光是Cd2Ge7016本身和Pr3’离子发射产生，基质的发光是Cd2Ge70．6中有陷阱能级，电子从导带跃迁到陷阱能级而产生，Pr3’的发光是该离子的4f一4f跃迁产生的；并把该材料的长余辉性质归结为基质结构中有电子陷阱和空穴陷阱，电子陷阱和空穴陷阱分别能储存电子和空穴，从而产生余辉。并提出余辉机理模型。     

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.