聚噁二唑芳亚胺联噻吩的合成及性能

以3,3’-二溴-2,2’-联噻吩和2,5-二(4-氨基苯基)-1,3,4-噁二唑为单体,通过钯催化CAr-N偶联合成了新型功能高分子聚噁二唑芳亚胺联噻吩(POXDIBT)。通过分子模拟、傅里叶变换红外光谱、核磁共振氢谱、热重、紫外可见吸收光谱、荧光光谱等分析技术对聚合物的分子结构、分子链构象、热稳定性及光学性能进行了研究。结果表明,该聚合物呈现锯齿形分子链构象,具有较好的溶解性能,热分解温度Td=323℃,在339nm处具有强吸收,激发波长为340nm时,荧光发射波长为401nm。     

含烷基噻吩与三嗪π-共轭聚合物的合成及性能

以二价镍配合物(Ni(dppp)Cl2)作为催化剂,2-二异丙基氨基-4,6-二氯均三嗪分别与3-丁基-2,5-二溴噻吩格氏(Grignard)试剂、3-辛基2,5-二溴噻吩格氏试剂、3-十二烷基-2,5-二溴噻吩格氏试剂交替共聚合成了3种含2-二异丙基氨基均三嗪的聚合物P1,P2和P3。并经傅里叶变换红外光谱、氢核磁共振谱、紫外-可见光谱、荧光光谱、循环伏安、X射线粉末衍射和凝胶渗透色谱等测试手段对其进行了表征,对聚合物P1在CHCl3溶液中的酸致变色行为进行了研究。结果表明,得到的聚合物在甲苯、氯仿、四氢呋喃(THF)等有机溶剂中溶解性好,3种聚合物的紫外-可见最大吸收波长在372 nm处出现,在CHCl3溶液中聚合物P1,P2,P3最大发射峰分别位于478 nm,549 nm和523 nm。聚合物均在-1.8~0 V出现n-掺杂峰。通过X射线衍射测试聚合物均有一定结晶性但结晶性较差。     

热解柠檬酸制备石墨烯量子点及其光学性质研究

通过热解柠檬酸制备发蓝光的石墨烯量子点(GQDs),并进一步水热处理得到蓝绿色荧光量子点(gGQDs)。通过紫外-可见吸收光谱、荧光光谱、傅里叶变换红外光谱、X射线光电子能谱和X射线衍射对制备的GQDs的结构和光学性质进行了表征和测试;同时,讨论了不同裂解温度和裂解时间及水热处理过程的温度和时间对GQDs荧光性能的影响。     

含2,3-二(5′-辛基噻吩基)喹喔啉单元荧光聚合物的合成及性能EI北大核心CSCD

以二价钯配合物作为催化剂,通过Sonogashira或Suzuki碳碳偶联反应制备了3种含2,3-二(5′-辛基噻吩基)喹喔啉单元的聚苯撑乙炔类(P1)、聚芴类(P2)和聚咔唑类(P3)π-共轭荧光聚合物。经傅里叶变换红外光谱、核磁共振氢谱和X射线粉末衍射对其结构进行了表征。利用紫外-可见光谱、荧光光谱和循环伏安等测试手段对其光学与电化学性能进行了研究,并研究了聚合物在CHCl3-CF3COOH溶液中的酸致变色行为。结果表明,3种聚合物在氯仿溶液和薄膜状态下的长波长处的紫外-可见最大吸收峰分别出现在449nm、420nm、418nm和538nm、425nm和420nm处。3种聚合物在氯仿溶液和薄膜状态下的荧光发射峰分别出现在556nm、529nm、558nm和599nm、556nm、569nm处,其在薄膜状态下分别发深红色、亮黄色和橙红色荧光。聚合物的相对荧光量子效率分别为18.1%、26.6%和16.8%。与P1和P3相比,P2显示较好的酸致变色行为,并在三氟乙酸浓度范围为2.692×10^(-3)~40.38×10^(-3) mol/L之间表现出酸浓度与吸光度之间优良的线性关系。通过循环伏安测试,聚合物均具有一定的空穴传输行为。     

聚3-烷基噻吩系列物的合成与表征

采用Fe(III)催化剂合成法合成聚3-丁基噻吩(P3BT)、聚3-己基噻吩(P3HT)和聚3-十二烷基噻吩(P3DDT)。用GPC和1 H-NMR对所合成的聚合物的相对分子质量和结构进行表征,用SEM对所合成的聚合物的表面形貌进行观察,并用紫外-可见吸收光谱和荧光光谱研究3种聚合物氯仿溶液的光学性能。结果表明,用该方法合成的聚合物以非晶态形式存在;具有较高的相对分子质量;在氯仿溶液中,P3BT、P3HT、P3DDT的最大吸收峰分别为:436nm、437nm和430nm,最大发射峰分别为570.0nm、581.2nm和573.8nm。综合分析发现P3HT更适于用做聚合物太阳能电池材料。     

含2,3-二(5′-辛基噻吩基)喹喔啉单元荧光聚合物的合成及性能

以二价钯配合物作为催化剂,通过Sonogashira或Suzuki碳碳偶联反应制备了3种含2,3-二(5′-辛基噻吩基)喹喔啉单元的聚苯撑乙炔类(P1)、聚芴类(P2)和聚咔唑类(P3)π-共轭荧光聚合物。经傅里叶变换红外光谱、核磁共振氢谱和X射线粉末衍射对其结构进行了表征。利用紫外-可见光谱、荧光光谱和循环伏安等测试手段对其光学与电化学性能进行了研究,并研究了聚合物在CHCl3-CF3COOH溶液中的酸致变色行为。结果表明,3种聚合物在氯仿溶液和薄膜状态下的长波长处的紫外-可见最大吸收峰分别出现在449nm、420nm、418nm和538nm、425nm和420nm处。3种聚合物在氯仿溶液和薄膜状态下的荧光发射峰分别出现在556nm、529nm、558nm和599nm、556nm、569nm处,其在薄膜状态下分别发深红色、亮黄色和橙红色荧光。聚合物的相对荧光量子效率分别为18.1%、26.6%和16.8%。与P1和P3相比,P2显示较好的酸致变色行为,并在三氟乙酸浓度范围为2.692×10~(-3)~40.38×10~(-3) mol/L之间表现出酸浓度与吸光度之间优良的线性关系。通过循环伏安测试,聚合物均具有一定的空穴传输行为。     

利用Heck反应制备3-甲基噻吩与芴的嵌段共聚物及其性能

采用Heck反应合成了3-甲基噻吩齐聚物及3-甲基噻吩与芴的交替和嵌段共聚物。用凝胶渗透色谱（GPC）、核磁共振谱（1H-NMR）、紫外-可见光谱和荧光光谱对所得聚合物进行了表征。结果表明,利用Heck反应成功地制备了上述聚合物。在溶液和薄膜状态下嵌段共聚物与交替共聚物的最大紫外吸收峰分别为414 nm、394 nm和...     

碲化镉量子点/聚(3,4-乙撑二氧噻吩)-聚苯乙烯磺酸复合纳米微球的原位聚合与光学性质

通过原位种子聚合构筑了碲化镉量子点(CdTe QDs)/聚(3,4-乙撑二氧噻吩)-聚苯乙烯磺酸(PEDOT-PSS)复合纳米微球.利用扫描电镜、红外光谱,X射线光电子能谱、紫外可见吸收光谱及荧光发射光谱对其形貌、结构、光学吸收性质及光致发光性能进行了测试分析.研究结果表明,原位聚合的CdTe/PEDOT-PSS复合物...     

发光波长可调的聚吡咯甲烷的制备及光学特性

聚合物发光材料因其拥有诸多优点,在有机发光二极管器件方面的应用前景广阔。然而,对于蓝光聚合物发光材料,由于其发光性能、使用寿命等方面仍然存在不足,难以满足全色显示的需要。以吡咯类单体和4-乙基苯甲醛单体为原料,采用溶液缩聚法制备了3种聚吡咯甲烷(聚{吡咯-[2,5-二(4-乙基苯甲烷)]}(PPE)、聚{N-甲基吡咯-[2,5-二(4-乙基苯甲烷)]}(PNPE)和聚{3-乙酰吡咯-[2,5-二(4-乙基苯甲烷)]}(PAPE)),并利用红外光谱、X射线衍射谱、热分析、紫外-可见光谱和荧光光谱等方法分别对其化学结构、聚集态结构、热性能、紫外-可见吸收行为和发光性能等进行了表征。研究结果表明,PPE、PAPE及PNPE在350 nm左右的紫外光的激发下,分别产生约为474 nm、455 nm及422 nm的可见发射光,对应为蓝色及蓝紫色的发光材料,且聚吡咯甲烷分子中吡咯环上的取代基对其发光性能的影响较大。通过对聚吡咯甲烷进行结构设计可以调节其发光波长,从而开发具有特定蓝色的发光器件材料。     

ZnO/聚噻吩复合材料制备及紫外光激发室温气敏性能

采用两步法制备ZnO/聚噻吩(ZnO/PTh)复合材料,首先制备富含氧空位缺陷的ZnO,然后以此为载体,通过噻吩单体的原位聚合得到最终产物。通过X射线衍射、场发射扫描电镜、高分辨透射电镜、红外光谱、紫外-可见漫反射光谱和荧光光谱对合成材料进行表征,研究了其紫外激发室温气敏性能,分析了紫外激发气敏机理。结果表明:紫外光激发下复合材料室温下对乙醇有较高的灵敏度,对100×10-6乙醇的灵敏度达到12. 6,响应和恢复时间均在40s以内。     

Growth of quantum-confined CdS nanoparticles inside Ti-MCM-41 as a visible light photocatalyst

CdS nanocrystallites have been successfully incorporated into the mesopores of Ti-MCM-41 by a two-step method involving ion-exchange and sulfidation. The X-ray diffraction patterns (XRD), UV-vis absorption spectra (UV-vis), photoluminescence spectra (PL), Raman spectra and N₂ adsorption-desorption isotherms were used to characterize the structure of the composite materials. It is found that most of the CdS nanocrystallites are about 2.6 nm, less than the pore diameter of Ti-MCM-41. The CdS nanocrystallites inside the mesopores of Ti-MCM-41 host show a significant blue shift in the UV-vis absorption spectrum. Under irradiation of visible light (λ > 430 nm), the composite material has greater and more stable photocatalytic activity for hydrogen evolution than bulk CdS, which can be explained by the effective charge separation between the CdS nanocrystallites and mesoporous Ti-MCM-41.     

Aqueous synthesis of luminescent magic sized CdSe nanoclusters

Highly stable water-soluble CdSe nanoclusters (NCs) with magic size were successfully synthesized using homocysteine (HCY) as capping ligands. Their sizes were tunable between 1.2 and 2.0 nm depending on reflux time. The final products were characterized by UV-vis absorption, steady and time-resolved photoluminescence (PL) spectra, X-ray powder diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM). XRD analysis showed that the HCY-capped CdSe NCs were of the cubic structure, UV-vis absorption spectra and HRTEM micrograph exhibited that the NCs were nearly monodisperse and relatively uniform. The as-prepared CdSe NCs had a PL quantum yield of up to 1.4%, almost comparable to the CdSe magic sized clusters prepared by an organometallic route.     

溶剂热制备花状ZnO纳米晶及光性能表征

利用溶剂热法,以乙酸锌（Zn（CH3COO）2·2H2O）和氢氧化钠（NaOH）为源,在乙二醇和水的混合溶剂中制备出了花状氧化锌纳米晶体,用X射线衍射（XRD）、扫描电子显微镜（SEM）、透射电子显微镜（TEM）和选区电子衍射（SAED）测试分析,发现样品为六方纤锌矿结构的ZnO单晶,花状晶体的大小约为600nm,单个花瓣的长、宽分别约为300nm、100nm。对比实验发现,产物形貌对NaOH浓度的依赖性很大。紫外可见吸收光谱（UV—vis spectra）显示,产物除了本征吸收外,在长波方向（600nm处）也有一宽化的、较强的吸收峰。室温荧光光谱（PL spectra）显示,产物在400—480nm有一明显的发光带,且在405nm和472nm处有两个较强的发光峰。     

Synthesis and characterization of thin films of poly(3-methyl thiophene) by rf-plasma polymerization

To facilitate synthesis of poly(3-methyl thiophene) thin film by RF-plasma polymerization process, suitable modifications have been done in a RF-sputtering set up. The deposition rate is found to be 3.33 nm/min. The synthesized films are characterized by FTIR, XRD, Ellipsometry, UV-Visible absorption spectroscopy and SEM. From FTIR, the formation of poly(3-methyl thiophene) has been confirmed. It is found that the synthesized polymer is cross-linked. XRD shows the amorphous nature of the prepared polymer film. The optical band gap has been estimated to be 2.14 eV from UV-visible absorption spectrum. Thickness of the polymer films has been measured to be 2000 Å by ellipsometry.     

Synthesis and characterization of ZnS:Mn2+ nano-particles for white-light emitting

The sol-gel method was used to obtain a kind of white-light emitting ZnS:Mn2+ nanoparticles capped by methacrylic acid with an average particle size of approximately 7 nm. The photoluminescence spectra, X-ray diffraction spectra, Fourier transform infrared reflection spectra and ultraviolet absorption spectra were used to measure their optical properties and crystal structures. The ZnS:Mn2+ nanoparticles with 0.58 wt% Mn2+ concentration emitted white light when excited by 380 nm. The PL spectrum exhibits two emission peaks under irradiation: one at 480 nm generated from the ZnS matrix, and one at 590 nm emitted by the doped Mn2+ ions. The nanoparticles will only emit white light with the optimum Mn2+ concentration (0.58 wt%). X-ray diffraction demonstrates the synthesized ZnS:Mn2+ nanoparticles have zinc blend crystal structure, and the infrared patterns of the capped ZnS:Mn2+ nanoparticles and methacrylic acid are comparable, indicating that the methacrylic polymer has capped or modified ZnS:Mn2+ nanoparticles.     

Sphere-like kesterite Cu2ZnSnS4 nanoparticles synthesized by a facile solvothermal method

In this paper, sphere-like kesterite Cu₂ZnSnS₄ (CZTS) nanoparticles were successfully synthesized by a facile solvothermal method. The CZTS nanoparticles with diameter range of 100-150 nm were agglomerated by CZTS nanocrystals. The as-obtained CZTS nanoparticles were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission election microscopy (TEM), Energy Dispersive Spectrometry (EDS) and UV-vis spectroscopy. Texture structures with kesterite crystallinity were reflected from the X-ray diffraction of 112, 200 and 312 planes of the CZTS nanoparticles. The UV-vis absorption spectra showed that CZTS nanoparticles had strong absorption in the visible light region. The observed band gap of 1.48 eV matched well with the bulk CZTS material that was optimal for solar cells.     

Characterization and photoactivity of TiO2 sols prepared with triethylamine

Using triethylamine as a surface protective agent, a transparent and pale yellowish TiO₂ sol had been prepared at 90 °C. This method was very different from the traditional methods, which produced titanium dioxide nanoparticles with anatase crystalline structure either at high acid condition or high temperature. X-ray diffraction (XRD) and transmission electron spectroscopy (TEM) demonstrated that the as-prepared TiO₂ sol nanoparticles with anatase crystalline structure were uniformly distributed, and the average size was 3 nm. X-ray photoelectron spectroscopy (XPS) and UV-vis absorption spectra showed that triethylamine was adsorbed on TiO₂ sol particles surface. FTIR spectroscopy noted that TiO₂ sol particles had the similar spectra with Degussa P25. Photoactivity of the as-prepared TiO₂ sol was studied by investigating the photodegradation of methyl violet in hydrosol reaction system under visible light irradiation.     

正交结构LiGaS2的合成及表征

为了获得高纯单相LiGaS2多晶原料,采用LiGa与S化合法合成LiGaS2,并与传统的单质直接合成法相对比.利用垂直长石英管作为反应器,采用X射线衍射和Raman光谱对其结构进行表征,同时利用差热–热重分析和紫外光谱对其热性能和光学性能进行研究.研究表明:采用LiGa与S化合法可以获得单相、均一的LiGaS2多晶材料;LiGaS2中的Li–S键平均力常数为fLi-S=16.0 N/m,Ga–S键平均力常数为fGa-S=39.6 N/m;LiGaS2多晶料的熔点为1 020℃,温度低于1 100℃,样品很稳定,没有分解现象;白色样品、黄色样品和灰色样品的紫外吸收边分别为323,435和496 nm.     

TiO2 nanoparticles co-doped with silver and nitrogen for antibacterial application

We have prepared a series of TiO2 nanoparticles for antibacterial applications. These TiO2 nanoparticles were prepared by the hydrolysis precipitation method with Ti(OBu)4, silver nitrate and ammonia. Crystal structure, particle size, interfacial structure and UV-visible light response of the prepared nanoparticles were characterized by X-ray diffraction measurements (XRD), Transmission electron microscopy (TEM), Fourier-transform infrared spectroscopy (FTIR) and UV-Vis diffuse reflectance spectroscopy (UV-Vis-DRs). The XRD spectra showed that all samples were anatase structure calcined at 450 degrees C for 3 hours. The Ag doping made the peak of diffraction wider. The results of TEM showed that the nanoparticles of TiO2, N-TiO2 and 1% Ag-N-TiO2 were all spherical in shape and well distributed with a mean size of 19.8 nm, 39.2 nm and 20.7 nm, respectively. N doping caused the nanoparticle size to increase, while, when the doped amount of Ag+ increased, the TiO2 particle size decreased. The FTIR revealed that Ag and N doping of TiO2 appeared to have strong absorption by -OH group and showed the characteristic absorption band of NH4+ and Ag. The UV-Vis-DRs indicated that the absorption band of Ag-N co-doped TiO2 had red shift and that the optical absorption response (between 400 nm and 700 nm) had obvious enhancement. The antibacterial properties of nanoparticles were investigated by agar diffusion method toward Escherichia coli and Bacillus subtilis. The results indicated that both Ag- and N-doped TiO2 could increase the antibacterial properties of TiO2 nanoparticles under fluorescent light irradiation. A 1% Ag-N-TiO2 had the highest antibacterial activity with a clear antibacterial circle of 33.0 mm toward Escherichia coli and 22.8 mm toward Bacillus subtilis after cultivation for 24 hours.     

Higher visible photocatalytic activities of nitrogen doped In2TiO5 sensitized by carbon nitride

N-doped In(2)TiO(5) modified by carbon nitride (CN) composite (NICN) has been prepared by the pyrogenation of the mixture of urea and In(2)TiO(5) through a polymerizable complex (PC) method. The powder samples were characterized by XRD, FESEM, TEM, UV-vis, and XPS. It is shown by XRD that the precursor sintered at 1000°C is pure and nitrogen dopant does not change the crystal structure of In(2)TiO(5). FESEM and TEM reveal a hole-like morphology of the prepared NICN. With the increase of nitrogen content, the light absorption onset of In(2)TiO(5) shifts from 410 nm to 450 nm, revealing significant narrowing of the band gap. XPS results suggest that only 2.2% of the nitrogen atoms were doped into In(2)TiO(5) through the urea pyrogenation method. Furthermore, the decomposition of Rhodamine B (Rh-B) under visible light reveals that Rh-B can be degraded completely within 20 min and recycling experiments indicate NICN has stable structure and durable photocatalytic activity, suggesting a promising utilization of such photocatalyst under visible light. Finally, an innovative mechanism of N-doped In(2)TiO(5) sensitized by carbon nitride polymer is proposed.