磷酸二氢钾插层改性高岭土复合物的制备与表征

实验制备了磷酸二氢钾插层改性高岭土用于新型复合阻燃材料。首先以二甲基亚砜(DMSO)为前驱体,采用超声法制备了高岭土-二甲基亚砜(K-DMSO)插层物,再将醋酸钾(KAc)取代DMSO,制备预插层体高岭土-醋酸钾(K-KAc)。最后通过第三步插层取代法,将磷酸二氢钾(KDP)引入,制备了高岭土-磷酸二氢钾(K-KDP)插层复合物,产物的插层率达到81.3%。通过红外光谱(FTIR)、X射线衍射(XRD)和扫描电子显微镜(SEM)对各步反应产物进行了表征。FTIR谱图显示,K-KDP在1 201 cm-1出现PO的振动峰;XRD显示各步插层反应中高岭土(001)晶面特征衍射峰依次向低角度方向移动,层间距相应从0.716 nm增加到1.59 nm;SEM显示插层后的高岭土粒子分散更为均匀。     

阳极界面修饰对钙钛矿太阳能电池性能的影响

采用在聚(3,4-乙撑二氧噻吩)∶聚苯乙烯磺酸(Poly(3,4-ethylenedioxythiophene)∶Poly(styrenesulfonate),PEDOT∶PSS)阳极界面层上直接旋涂二甲基亚砜(Dimethyl Sulfoxide,DMSO)的方法,对PEDOT∶PSS薄膜进行修饰,以提高所制得的钙钛矿太阳能电池器件性能.在5000rpm转速条件下旋涂DMSO后,器件的能量转换效率达到11.43%,与PEDOT∶PSS阳极界面层未做任何修饰的器件相比,效率提高了29.15%.测试表征了修饰前后PEDOT∶PSS薄膜的透光性、表面形貌、电导率、器件的外量子效率曲线以及器件在光照和暗态下的J-V特性曲线,分析了器件性能提高的原因.结果表明:经过修饰的PEDOT∶PSS薄膜导电性显著增强,从而更加有利于器件阳极对空穴的抽取和收集;较未修饰时,器件的短路电流密度得到了大幅度提升,进而使得器件获得更高的能量转换效率.     

云母/交联聚苯乙烯复合材料制备及沿面闪络性能

交联聚苯乙烯具有优异的电气性能、力学性能和可加工性能,已作为高压绝缘材料得到了重要应用。随着脉冲功率技术向小型化方向发展,对交联聚苯乙烯真空沿面闪络性能提出了更高要求。以苯乙烯为单体,二乙烯基苯为交联剂,偶氮二异丁腈为引发剂,采用超声波分散技术将不同质量分数的云母均匀分散于溶液体系中,通过原位自由基聚合制备出云母/交联聚苯乙烯复合材料。采用红外光谱、电子扫描显微镜等对材料组成和形貌进行了表征,采用短脉冲高压测试平台研究了云母对交联聚苯乙烯真空沿面闪络性能的影响。结果表明,当云母质量分数低于5%时,复合材料中云母为均匀分散状态,随着掺杂量进一步提升,出现了明显的团聚现象;当云母质量分数为3.5%~5%之间时,真空沿面闪络击穿电压和耐电寿命较交联聚苯乙烯得到了明显提升。     

优化反式平面钙钛矿太阳电池性能的简便方法——利用PEDOT:PSS与DMSO共混空穴传输层

优化界面接触、增强界面处载流子传输对于提高钙钛矿电池性能具有重要意义。本研究将适量二甲基亚砜（DMSO）添加到聚（3,4-乙烯二氧噻吩）-聚（苯乙烯磺酸盐）(PEDOT∶PSS)空穴传输层中,改善了空穴传输层的导电性和空穴传输特性,有效提高了反式平面钙钛矿太阳能电池光伏性能。短路电流(J_sc)从21.29 mA/cm²提高到22.15 mA/cm²,填充因子（FF）从76.35%提高到80.09%,转换效率（PCE）从16.02%提高到17.01%。薄膜与器件性能综合测试结果表明,DMSO的掺入使PEDOT∶PSS发生适度相分离,形成更好的PEDOT导电通道,增强了PEDOT∶PSS的导电特性。稳态光致发光光谱呈现出显著的荧光猝灭效应,也表明掺杂DMSO后PEDOT∶PSS的空穴提取能力得到提高,钙钛矿活性层与阳极之间的空穴传输更加顺畅,有助于实现高达80%以上的填充因子。本研究为改善反式平面钙钛矿太阳电池或有机太阳电池光伏性能提供了一种高效、简便的方法,具有很好的现实意义。     

二甲基亚砜添加剂对聚合物太阳能电池性能的影响

研究了二甲基亚砜(DMSO)掺杂浓度对基于聚(3-己基噻吩)(P3HT)和(6,6)-苯基碳60丁酸甲酯(PCBM)为有源层的聚合物太阳能电池性能影响。结果表明,掺杂DMSO可以提高聚合物太阳能电池短路电流密度和填充因子。DMSO掺杂质量比为3%时,电池短路电流密度提高到7.88 mA·cm-2,填充因子为55.5%。能量转换效率达到2.54％,相比没有掺杂DMSO的电池,能量转换效率提高了17%。傅里叶变换红外光谱被用于鉴定和分析掺杂DMSO对材料P3HT∶PCBM化学性质的影响。傅里叶变换红外光谱表明,掺杂后P3HT和PCBM的化学性质都没有改变。为分析掺杂DMSO改善器件能量转换效率的原因,通过紫外-可见光谱和电流密度-电压特性曲线分别表征器件的光吸收能力以及电致发光器件的载流子迁移率。与P3HT∶PCBM薄膜相比,P3HT∶PCBM∶DMSO薄膜在可见光范围内的吸收峰有明显红移且吸收强度增强。可见光吸收的改善是实现短路电流密度提高的有力保障。太阳能电池性能的增强是因为DMSO的掺杂提高了P3HT∶PCBM的载流子迁移率和吸收光谱宽度。     

二甲基亚砜添加剂对聚合物太阳能电池性能的影响（英文）

研究了二甲基亚砜(DMSO)掺杂浓度对基于聚(3-己基噻吩)(P3HT)和(6,6)-苯基碳60丁酸甲酯(PCBM)为有源层的聚合物太阳能电池性能影响。结果表明,掺杂DMSO可以提高聚合物太阳能电池短路电流密度和填充因子。DMSO掺杂质量比为3%时,电池短路电流密度提高到7.88mA·cm-2,填充因子为55.5%。能量转换效率达到2.54%,相比没有掺杂DMSO的电池,能量转换效率提高了17%。傅里叶变换红外光谱被用于鉴定和分析掺杂DMSO对材料P3HT∶PCBM化学性质的影响。傅里叶变换红外光谱表明,掺杂后P3HT和PCBM的化学性质都没有改变。为分析掺杂DMSO改善器件能量转换效率的原因,通过紫外-可见光谱和电流密度-电压特性曲线分别表征器件的光吸收能力以及电致发光器件的载流子迁移率。与P3HT∶PCBM薄膜相比,P3HT∶PCBM∶DMSO薄膜在可见光范围内的吸收峰有明显红移且吸收强度增强。可见光吸收的改善是实现短路电流密度提高的有力保障。太阳能电池性能的增强是因为DMSO的掺杂提高了P3HT∶PCBM的载流子迁移率和吸收光谱宽度。     

多孔塑料光纤氨传感探头的制备与应用

基于交联共聚技术,以藻红为荧光指示剂,苯乙烯为聚合单体、双甲基丙烯酸一缩二乙二醇酯为交联剂,研制了苯乙烯聚合多孔塑料光纤,用于微量氨的传感分析。研究了荧光指示剂在共聚体中的固定技术,考察了传感探头在不同聚合交联度、惰性致孔剂、荧光指示剂浓度条件下对氨的响应性能的影响。在最优条件下,聚苯乙烯多孔塑料光纤探头透明、刚性、耐水和耐化学性能好,透光率为88%—92%,对氨的检测线性浓度范围为2×10~(-4)—9.1×10~(-3)mol/L,并具有较好的稳定性和可逆性。     

超声引发苯乙烯微乳液聚合转化率的紫外光谱法分析

研究了苯乙烯微乳液聚合体系中苯乙烯浓度和转化率的测定方法,探讨了紫外光谱法分析测定苯乙烯浓度的影响因素。实验结果表明：以95%乙醇为溶剂和参比液,紫外吸收波长为247 nm时,苯乙烯浓度的范围在9.70×10-6 mol·L-1～6.95×10-5mol·L-1内,其吸光度与浓度呈良好的线性关系,其最大摩尔吸光系数ε 为1.384×104 L·mol-1·cm-1。微乳液聚合体系中十二烷基硫酸钠、正戊醇的存在对苯乙烯浓度的分析测定没有影响。苯乙烯微乳液聚合体系中的聚苯乙烯可以通过加95%乙醇进行沉淀分离,残余的微量聚苯乙烯对分析结果无影响。将紫外光谱法与化学法和重量法比较,表明紫外光谱法测定苯乙烯的转化率是可行的,该方法操作简便,灵敏度高。     

负载碘催化剂聚苯乙烯微粒子的制备

利用聚乙烯吡咯烷酮共聚对聚苯乙烯微球的表面改性进行碘催化剂的固定化,制备粒径均一、可循环使用的催化剂微粒.红外光谱研究表明,聚乙烯吡咯烷酮和苯乙烯的共聚,进入聚苯乙烯聚合链中,碘的负载主要通过与聚合链中吡咯烷酮基团的配位进行,由此对吡咯烷酮相关的特征振动产生较大影响.     

苯甲酰胺对高岭石插层的FTIR和XRD研究

苯甲酰胺在熔融状态下取代前驱体中的DMSO分子插层高岭石,产物经丙酮洗涤,得到纯净的高岭石/苯甲酰胺插层复合物。XRD结果显示高岭石层间距从0.717 nm膨胀到1.437 nm。插层作用使高岭石内表面羟基红外伸缩振动峰由3 696和3 657 cm-1移动至3 701和3 651 cm-1处;苯甲酰胺3 368和3 172 cm-1处NH₂基伸缩振动峰红移至3 474和3 184 cm-1处,1 659 cm-1处羰基峰移至1 640 cm-1处,这些表明原高岭石层间氢键的损失及与苯甲酰胺分子之间氢键的形成。插层反应于30 min迅速达到平衡,插层率随反应温度的增加先增加后减小,180 ℃时有最大插层率;以丙酮作为洗涤剂可以消除表面吸附和残余的苯甲酰胺晶体而不影响复合物的结构。     

Preparation and characterization of a magneto-polymeric nanocomposite: Fe3O4 nanoparticles in a grafted, cross-linked and plasticized poly(vinyl chloride) matrix

In this work two kind of materials: (1) grafted, cross-linked and plasticized poly(vinyl chloride) (PVC) “plastic films” and (2) magnetic plastic films “magneto-polymeric nanocomposites” were prepared. Precursor solutions or “plastisols” used to obtain the plastic films were obtained by mixing PVC (emulsion grade) as polymeric matrix, di(2-ethylhexyl)phthalate (DOP) as plasticizer, a thermal stabilizer based in Ca/Zn salts, and a cross-linking agent, 3-mercaptopropyltrimethoxysilane (MTMS) or 3-aminopropyltriethoxysilane (ATES), at several concentrations. Flexible films were obtained from the plastisols using static casting. The stress–strain behavior and the gel content (determined by Soxhlet extraction with boiling THF) of the flexible films were measured in order to evaluate the effect of the cross-linking agent and their content on the degree of cross-linking. The magneto-polymeric nanocomposites were obtained by mixing the optimum composition of the plastisols (analyzed previously) with magnetite (Fe₃O₄)-based ferrofluid and DOP. Later, flexible films were obtained by static casting of the plastisol/ferrofluid systems. The magnetic films were characterized by the above-mentioned techniques and X-ray diffraction, vibrating sample magnetometry and thermogravimetrical analysis.     

ICP-AES测定苦瓜籽矿质元素及GC-MS鉴定其油脂脂肪酸

苦瓜籽中活性成分的研究逐渐引起人们注意,但其矿质元素组成未见报道,其油脂脂肪酸主要成分也说法不一。文章选取海南产大苦瓜籽用电感耦合等离子体原子发射光谱仪(ICP-AES)法测定矿质元素,发现其中K,Mg和P含量最高;Cr和Zn的含量分别高达5.165和45.45μg.g-1,在植物性食品中较为罕见。以超临界CO2萃取其中油脂,得率为36.89%,碱法衍生为脂肪酸甲酯后,气相色谱-质谱联用法(GC-MS)鉴定苦瓜籽油脂中脂肪酸组成,发现其饱和脂肪酸(SFA)占36.71%,主要为硬脂酸;单不饱和脂肪酸(MUFA)仅占3.33%,主要为油酸(LA);多不饱和脂肪酸(PUFA)占59.96%,主要为α-桐酸,含量高达54.26%。明确苦瓜籽微量元素与脂肪酸组成,对进一步挖掘其药、食用价值具有重要的理论指导意义。     

Effect of plasticizer on electrical conductivity and cell parameters of (PVC+KBrO<Subscript>3</Subscript>) polymer electrolyte system

The effect of a plasticizer dimethyl formamide (DMF) on the properties of a potassium ion conducting electrolyte based on polyvinyl chloride (PVC) complexed with potassium bromate (KBrO₃) prepared using solution-cast technique was investigated. Various experimental techniques, such as electrical conductivity (composition and temperature dependence) and transport number measurements, were used to characterize these polymer electrolyte films. It was found that the addition of plasticizer (DMF) significantly improved the ionic conductivity. Transport number for K⁺ ion ranged from 0.95 to 0.97 depending on the composition and temperature. Electrochemical cells of configuration K/PVC+KBrO₃/(I₂+C+electrolyte) and K/PVC+KBrO₃+plasticizer/(I₂+C+electrolyte) were fabricated. The discharge characteristics of the cells were studied under a constant load of 100 kΩ. The open-circuit voltage, short-circuit current, and discharge time for the plateau region were measured. The PVC+KBrO₃ polymer electrolyte system with added plasticizer showed an increased discharge time with respect to pure PVC+KBrO₃ electrolyte system. The features of complexation of the electrolytes were studied by X-ray diffraction.     

硬脂酸稀土对PVC热稳定性的作用机理研究

采用FTIR及XRD对硬脂酸稀土稳定剂进行结构表征 ,可知硬脂酸稀土中硬脂酸酸根与稀土离子间的作用主要是离子键性质的 ,且硬脂酸稀土具有层状晶体结构 ,晶层中稀土离子倾斜于基面。刚果红法测定结果表明 ,随着硬脂酸稀土用量增加 ,PVC的热稳定时间呈现增加的趋势 ,4种不同稀土硬脂酸盐稳定能力大小顺序为Last>Ndst>Yst>Dyst。通过FTIR对PVC稀土稳定体系稳定机理进行预测 ,结果表明Last和Ndst两种稀土稳定剂能取代不稳定的Cl原子 ,阻止PVC分子链上脱HCl反应 ,改变构象使其达到稳定的效果。Yst和Dyst在改变构象方面贡献较不明显。     

直接沉淀法中不同晶型钛酸锌的X射线粉末衍射研究

以Ti(SO₄)₂和Zn(NO₃)₂·6H₂O为原料,碳酸铵为沉淀剂,采用直接沉淀法制备了钛酸锌的粉体。探讨了反应条件对所得钛酸锌晶体结构的影响,并对样品进行了XRD和TG-DTA等分析。钛酸与碳酸锌分子生成的先后顺序影响得到的钛酸锌的结构。在钛酸优先生成的体系中,碳酸锌分子生成之后与周围足量的钛酸分子发生碰撞反应,由于钛酸优先生成且沉淀剂足量,碰撞反应充分且在碰撞反应中钛酸保持过量,反应生成了亚钛酸锌(Zn₂Ti₃O₈)。在碳酸锌优先生成的体系中,钛酸分子生成之后与周围足量的碳酸锌分子发生碰撞反应,由于碳酸锌优先生成且沉淀剂足量,碰撞反应充分且在碰撞反应中碳酸锌保持过量,反应生成了正钛酸锌(Zn₂TiO₄)。另外,沉淀剂用量和反应温度都影响着最终产物的种类和晶型。沉淀剂用量越多、反应温度越高,越易于生成Zn₂Ti3O₈或Zn₂TiO₄。只有在沉淀剂不足、反应温度较低的情况下,才能生成偏钛酸锌(ZnTiO₃)。     

光谱法研究Zn2+对枸杞超氧化物歧化酶JZ活力和结构的影响

针对提取的天然抗氧性物质超氧化物歧化酶量少,稳定性差等问题,实验以枸杞为原料,采用硫酸铵盐析分级分离方法提取了枸杞超氧化物歧化酶(superoxide disutase of lycium,SOD-LY),紫外光谱法确定了其类型;考察了不同种类的锌盐ZnSO4,ZnCl2,Zn(CH3COO)2和Zn(NO3)2对SOD-LY活力的影响,选择出能显著提高其活力的锌盐.采用傅里叶变换红外光谱、紫外光谱、荧光光谱法研究了最佳锌盐同SOD-LY分子的作用方式.结果表明,提取的SOD-LY 属于Cu/Zn-SOD类型.不同浓度锌盐的存在均可影响SOD-LY的活性.其中,Zn(NO3)2对SOD-LY活力影响最大;红外光谱表明,Zn(NO3)2使SOD-LY二级结构中β-片层、β-转角和β-反平行结构减少,α-螺旋和无规则卷曲结构增多.荧光光谱分析得出,Zn2+与SOD-LY之间的相互作用力主要为静电引力,有利于稳定SOD-LY的活性中心,使得SOD-LY活力增强.Zn2+与SOD-LY结合常数(KΛ)为1.666×103 L·mol-1,结合位点数(n)为1.238,结合距离(r0)为3.62 nm,该研究为提高SOD的活力、稳定性及扩展其应用提供理论帮助.     

A study on the blending effect of polyvinyledene fluoride in the ionic transport mechanism of plasticized polyvinyl chloride + lithium perchlorate gel polymer electrolytes

The gel polymer electrolytes composed of the blend of polyvinylchloride (PVC) and polyvinylidene fluoride (PVdF) as host polymers, the mixture of ethylene carbonate (EC) and propylene carbonate (PC) as a plasticizer, and LiClO₄ as a salt was studied. An attempt was made to investigate the effect of PVdF in the plasticized PVC + LiClO₄ system in three blend ratios. The differential scanning calorimetry study confirms the formation of polymer–salt complex and miscibility of the PVC and PVdF. The X-ray diffraction results of plasticized PVC (S1, S2, S3) and PVdF-blended films (S4, S5, S6) were compared, in that an increase in PVC concentration decreases the degree of crystallinity for S1 and S3, respectively, but drastically increases for PVC (S2). The increase in PVC content has not accounted in the conductivity studies also noted. However, the blending effect of PVdF showed decreases in crystallinity homogeneously for (S6 > S5 > S4), which were reflected in ionic conductivity measurements. The surface morphology of the films were also studied by scanning electron microscope, and it corroborates the same. Paper presented at the Third International Conference on Ionic Devices (ICID 2006), Chennai, Tamilnadu, India, Dec. 7–9, 2006.     

一种用于电子纸的电泳液的显示性能研究

用有机颜料汉沙黄(P.Y.3)、苏丹黑和合适的稳定剂为原料配制了一种性能稳定的电泳显示液.分析了此电泳显示液中颜料微粒的带电机理及其影响因素,研究了在改变电压方向时反射光谱与吸收光谱的变化及其原因,光谱分析结果表明体系中存在的各种吸附使显示效果受到局限,反射谱与吸收谱的变化在表征器件的显示特性时呈现出一致性,器件的反射光强和反射率在不同波长上有区域选择性,同时对比度也有区域选择性,这决定了在监测器件的响应时应选择的波长范围以及可利用的光源.兼顾灵敏性和测试信号强度的需求,选用峰值波长为470 nm的蓝光二极管为光源,电泳槽的厚度为0.2 mm,用荧光光谱仪监测相同周期不同幅值脉冲电压作用下颜料微粒在493 nm波长处的反射光强的变化,并由示波器记录并输出反射光强随驱动电压的变化,还结合相关理论讨论了驱动电压对器件的反射光强和对比度的影响.     

水溶胶CdSe/CdS核/壳结构纳米晶制备及光学性质的研究

以巯基乙酸为稳定剂在水溶液中合成了水溶胶CdSe/CdS核/壳结构的量子点,利用X射线粉末衍射(XRD)和X射线光电子能谱(XPS)对量子点结构进行了表征;并对化学组成和尺寸分布进行了研究。通过紫外-可见吸收光谱、激发光谱与发射光谱研究了它们的发光特性。     

Ultrasound-assisted surface treatment of ZrO2 with BSA and incorporating in PVC to improve the properties of the obtained nanocomposites: Fabrication and characterization

This paper describes the preparation of poly(vinyl chloride) (PVC) nanocomposites (NCs) reinforced with modified zirconia (ZrO₂) nanoparticles (NPs). The ZrO₂ NPs were defined as efficient filler for PVC NCs. For achieving the best dispersion and improvement of properties, the surface of ZrO₂ NPs was modified by Bovine Serum Albumin (BSA). Carboxylic acids and amines are important functional groups of BSA which handle the grafting BSA on the surface of ZrO₂ NPs. The PVC/ZrO₂-BSA NCs were fabricated by incorporation of various amounts of the ZrO₂-BSA NPs (3, 6 and 9 wt%) into PVC matrix. All the above processes were accomplished by ultrasonication as a green and environmentally-friendly method. Also, the magnetic and mechanical stirrer was used for the preparation of samples but the results are not suitable and the aggregation was observed which indicated the use of ultrasonic irradiation is the best method for the preparation of NC. The products were characterized by Fourier transform infrared spectroscopy, Transmission electron microscopy, Field emission scanning electron microscopy, X-ray diffraction, Thermogravimetric analysis, Ultraviolet–visible spectroscopy, photoluminescence spectroscopy, energy dispersive X-ray spectroscopy, wettability, and mechanical tests. The achieved PVC/ZrO₂-BSA NCs showed high thermal stability, good mechanical, optical and wettability properties compared to the pure PVC. In addition, among the obtained NCs, the PVC/ZrO₂-BSA NC 6 wt% showed the best improvement.