PMMA/SiO_2-TiO_2杂化纤维的制备与表征

以正硅酸乙酯和钛酸四丁酯为前驱体,乙烯基三乙氧基硅烷为偶联剂,采用溶胶凝胶原位聚合法制备了聚甲基丙烯酸甲酯/二氧化硅-二氧化钛(PMMA/SiO2-TiO2)杂化溶胶,陈化后用提拉法制得杂化纤维。研究了溶胶的杂化反应机理;使用红外光谱(IR)、扫描电子显微镜(SEM)、紫外-可见光谱(UV-Vis)、荧光光谱(FL)和热重分析(TGA)分析了杂化纤维的结构与性能。结果表明,PMMA与SiO2-TiO2之间通过化学键连接;纤维直径为150μm,在纤维内部有机无机相间形成均一的连续相;TiO2的引入增加了其抗紫外性;杂化纤维具有荧光性能;其耐热性能优于纯PMMA。     

PMMA／TiO2-SiO2高分子杂化材料的制备与表征

用溶胶凝胶法和共混法相结合的方法制备了PMMA/TiO2-SiO2高分子杂化材料。并用傅里叶红外光谱(FT-IR)、原子力显微镜(AFM)和透射电镜(TEM)等测试方法对所得复合微粒进行了表征。结果表明,TiO2-SiO2复合粒子呈核-壳结构,具有Ti-O-Si网络;该核壳结构可均匀地分散在聚甲基丙烯酸甲酯中,形成PMMA/TiO2-SiO2高分子杂化材料。与纯的聚合物材料相比,PMMA/TiO2-SiO2高分子杂化材料有较好的热稳定性、优良的紫外屏蔽和可见光透过特性。     

PMMA／SiO2杂化纤维的制备及表征

以正硅酸乙酯(TEOS)和PMMA低聚体为原料,乙烯基三乙氧基硅烷(VTEOS)为偶联剂,采用溶胶-凝胶法制备了PMMA/SiO2杂化溶胶,陈化后用提拉法制得PMMA/SiO2杂化纤维。研究了溶胶的杂化反应机理、成纤性能;使用IR、SEM、TGA及DSC分析了杂化纤维的结构与性能。结果表明,该杂化溶胶具有很好的拉丝性能,黏度为180 Pa.s~300 Pa.s时的成纤性能好,所制得的杂化纤维,其中PMMA与SiO2之间通过化学键连接,在纤维内部有机无机相间形成均一的连续相;其耐热性能优于纯PMMA。     

聚乳酸-聚乙二醇-聚乳酸/二氧化钛杂化材料的制备及表征

以辛酸亚锡为催化剂,合成了聚乳酸-聚乙二醇-聚乳酸(PLA-PEG-PLA)共聚物;基于溶胶凝胶(sol-gel)工艺,将PLA-PEG-PLA与TiO2溶胶杂化反应,制备了PLA-PEG-PLA/TiO2杂化材料。采用红外光谱(FT-IR)、光电子能谱(XPS)、差示扫描量热(DSC)和X射线衍射(XRD)方法对杂化材料进行表征和分析。FT-IR和XPS分析结果显示,TiO2溶胶与PLA-PEG-PLA间发生了杂化反应,形成了Ti-O-C键。DSC分析结果显示,随TiO2%(质量分数,下同)含量的增加,杂化材料的耐热性能提高。XRD证实了杂化材料为无定型结构,有利于降解。     

PEG/SiO2-TiO2杂化纤维的制备与表征

以正硅酸乙酯(TEOS)和钛酸四丁酯(TBT)为无机前驱体,采用溶胶-凝胶法制备了PEG/SiO2-TiO2杂化溶胶,通过提拉法制得杂化纤维,并对其进行了简单表征.结果表明,随钛硅物质的量比的增加或有机相质量的增加,溶胶的可纺性变好;有机相与无机相之间通过化学键连接;纤维直径为40μm左右;TiO2的引入增强了其抗紫外性,杂化纤维的耐热性优于纯PEG.     

PVA/SiO_2/TiO_2杂化纤维的制备与表征

采用溶胶-凝胶法以正硅酸乙酯(TEOS)和钛酸四丁酯(TBOT)为原料制备了SiO2/TiO2溶胶,并与PVA进行杂化,得到PVA/SiO2/TiO2杂化溶胶,陈化后用拉丝法制得PVA/SiO2/TiO2杂化纤维。研究了PVA和TBOT对杂化溶胶的黏度变化与成纤性能的影响,并对杂化纤维的性能进行了测试。用FT-IR、EDS、XRD和TG对制得的纤维进行了表征。结果表明,PVA有利于改善杂化溶胶的成纤性能,随钛含量增加杂化溶胶的黏度变化速度加快;杂化纤维中各组分分布较为均匀,通过杂化限制了PVA的结晶并改善了PVA的耐热性能。     

溶胶-凝胶法制备紫外光固化聚氨酯丙烯酸酯/环氧丙烯酸酯/纳米二氧化硅杂化材料

以正硅酸乙酯(TEOS)制备SiO2溶胶,γ-甲基丙烯酰氧丙基三甲氧基硅烷(KH-570)为硅烷偶联剂,通过溶胶-凝胶法制备聚氨酯丙烯酸酯/环氧丙烯酸酯/二氧化硅杂化材料。采用场发射扫描电镜(FESEM)以及热失重方法进行分析。结果表明,TEOS与(PUA+EA)质量比为0.4∶1时,树脂中二氧化硅颗粒粒径最小,大约在80 nm～100 nm,分散均匀,当配比达到0.6∶1时,二氧化硅出现团聚现象。杂化材料热失重温度达到350℃,热分解温度为143.8℃,比纯树脂体系提高了将近1倍。     

聚甲基丙烯酸丁酯-二氧化硅杂化材料的制备及性能

用硅酸钠制备了聚硅酸溶胶，作为制备有机／无机杂化材料的无机组分前驱物，以甲基丙烯酰氧丙基三甲氧基硅烷为偶联剂，通过溶胶-凝胶技术与甲基丙烯酸丁酯制得两相间有共价键结合的透明聚甲基丙烯酸丁酯／二氧化硅杂化材料。用红外光谱、透射电镜、TG和DSC等对杂化材料进行了表征，热失重分析表明，杂化材料的热稳定性随SiO2含量的增加而提高，且杂化材料的玻璃化温度Tg也有一定的提高，同时杂化材料的透光率可达80％，硬度比纯PBMA有很大的提高。     

低收缩块状PMMA/SiO_2杂化材料制备及性能表征

以甲基丙烯酸甲酯(MMA)、正硅酸乙酯(TEOS)和硅烷偶联剂(MPMS)为原料,采用溶胶-凝胶法制备出低收缩、具有良好光学性能的PMMA/SiO2杂化材料。通过透射电子显微镜、差热分析、红外吸收光谱和紫外光-可见分光光度计表征了杂化材料的微观形貌、热性能和透明性。结果表明材料的网络结构相对比较均匀,在可见光波长范围内材料均一性好;有机相和无机相之间是通过共价键相互连接的,没有出现有机相、无机相分离现象;杂化材料的透光率约90%。     

MSU-J及有机化修饰对PMMA杂化材料力学性能和热性能的影响

采用蠕虫状介孔SiO2(MSU-J)和γ-(甲基丙烯酰氧)丙基三甲氧基硅烷后嫁接法有机化修饰的MSU-J-G,与MMA原位聚合制备具有三维纳米网络结构的MSU-J/PMMA和MSU-J-G/PMMA杂化材料。研究了杂化材料的微观结构、力学性能和热性能。结果表明:杂化材料中MSU-J及MSU-J-G保持原有的蠕虫状介孔结构,且近90%孔道被PMMA填充。MSU-J或MSU-J-G质量分数为7%时,两类杂化材料的性能最优,相对于纯PMMA,其拉伸强度和模量分别提高了38.9%和40.2%(MSU-J)以及46.7%和39.5%(MSU-J-G),断裂伸长率及冲击强度略有下降。杂化材料的热分解温度(Td)及玻璃化转变温度(Tg)也得到了改善。相对于MSU-J,MSU-J-G在PMMA中分散更均匀,对于杂化材料的力学和热性能改善效果更佳。     

金沙土遗址加固材料的制备及性能研究

为了得到综合性能较好的成都金沙土遗址加固材料,采用自由基溶液共聚合和溶胶-凝胶法制备了丙烯酸-有机硅-环氧树脂三元体系的新型有机/无机杂化土遗址保护材料,并将其应用于成都金沙遗址土样的加固,实验结果表明,当TEOS含量为20%时,无机相尺寸为20~70 nm,平均粒度为45 nm,且分散均匀,无机和有机相之间以化学键相连接.增大TEOS的含量可以提高加固材料的耐光老化性和加固土的综合性能(如耐溶剂性、抗水解性等),同时降低加固土的渗透速率.SEM表明加固材料有效地填补了土中的孔洞,降低了孔隙率,并起到了支撑和加固的作用.     

杂化聚酰亚胺薄膜无机相形貌和介电性能研究

采用溶胶-凝胶法制备纳米二氧化硅及氧化铝溶胶,将其掺入聚酰胺酸溶液中,制得聚酰亚胺/二氧化硅-氧化铝杂化薄膜,利用原子力显微镜对杂化薄膜的无机相微观形貌进行表征,用精密阻抗分析仪测试杂化膜介电性能.研究表明:掺入无机组分含量均为4%时,随着掺入二氧化硅所占比例的增大,无机纳米粒子的平均粒径增加,当其与氧化铝质量比为8:1时无机相呈网络状,与聚酰亚胺基体界面模糊;掺入无机组分对杂化薄膜的介电性能产生影响,介电常数ε和介电损耗tgδ随频率增加而减小,在相同频率下随掺入二氧化硅所占比例增大,介电常数ε和介电损耗tgδ增大.     

核磁共振法研究核壳型二氧化硅/聚氨酯纳米复合材料中核与壳的键合方式

通过1H-NMR技术研究核壳型SiO2/聚氨酯纳米复合材料中有机相与无机相的反应情况。核磁共振谱图显示,壳材聚氨酯与核材二氧化硅的界面处形成了稳定的氢键,有机相与无机相复合成稳定的核壳结构的粒子。     

Organic/inorganic flame retardants containing phosphorus,nitrogen and silicon: Preparation and their performance on the flame retardancy of epoxy resins as a novel intumescent flame retardant system

This paper presents the preparation of novel organic/inorganic flame retardants containing phosphorus, nitrogen and silicon (organic/inorganic FRs). The organic/inorganic FRs were highly water resistant, as suggested by the water contact angle and water solubility tests. The organic/inorganic FRs were then incorporated into epoxy resins (EP) at different phosphorus/nitrogen ratios and the flame retardancy of EP/FRs composites was characterized. The results showed that synergistic effects on the flame retardancy of EP composites existed between the DOPO-VTS and TGIC-KH. The char residues for EP/FRs composites were increased, and the highest char residues were obtained in air atmosphere (3.8 wt.%) when the DOPO-VTS/TGIC-KH is 4/1. The MCC results also showed that the THR of epoxy resins were also decreased when the DOPO-VTS/TGIC-KH is 4/1, which was in accordance with the highest LOI and UL-94 results. The SEM, FTIR, XPS and TG-FTIR results of pyrolysis products in both condensed and gases phases indicated that the strategy of organic/inorganic FRs combined condensed phase and gases phase flame retardant strategies such as the phosphorus–nitrogen synergism systems, the silicon reinforced effects in the condensed phase and DOPO flame retardant systems in the gases phase, resulting in significant improvements in the flame retardancy of epoxy resins.     

Review on Recent Progress of All‐Inorganic Metal Halide Perovskites and Solar Cells

All‐inorganic perovskites are considered to be one of the most appealing research hotspots in the field of perovskite photovoltaics in the past 3 years due to their superior thermal stability compared to their organic–inorganic hybrid counterparts. The power‐conversion efficiency has reached 17.06% and the number of important publications is ever increasing. Here, the progress of inorganic perovskites is systematically highlighted, covering materials design, preparation of high‐quality perovskite films, and avoidance of phase instabilities. Inorganic perovskites, nanocrystals, quantum dots, and lead‐free compounds are discussed and the corresponding device performances are reviewed, which have been realized on both rigid and flexible substrates. Methods for stabilization of the cubic phase of low‐bandgap inorganic perovskites are emphasized, which is a prerequisite for highly efficient and stable solar cells. In addition, energy loss mechanisms both in the bulk of the perovskite and at the interfaces of perovskite and charge selective layers are unraveled. Reported approaches to reduce these charge‐carrier recombination losses are summarized and complemented by methods proposed from our side. Finally, the potential of inorganic perovskites as stable absorbers is assessed, which opens up new perspectives toward the commercialization of inorganic perovskite solar cells.     

HPLC-ICP-MS法测定水样中的甲基汞、乙基汞和无机汞

建立了高效液相色谱(HPLC)和电感耦合等离子体质谱(ICP-MS)联用测定环境水样中的甲基汞、乙基汞和无机汞的方法。实验使用的高效液相色谱流动相为含有0.06mol/L乙酸氨,20μg/LBi,0.1%(V/V)2-巯基乙醇的5%(V/V)甲醇-水溶液,色谱柱为C18反相柱(5μm,2.1mm×50mm),经前处理的水样在液相色谱中分离后,进入电感耦合等离子体质谱检测其甲基汞、乙基汞和无机汞的浓度。甲基汞、乙基汞和无机汞检出限分别为0.05μg/L、0.10μg/L和0.10μg/L。     

无机非金属纳米微粒的制备方法

本文简要介绍了固相法、液相法及气相法制备无机非金属纳米微粒的方法原理、研究现状及发展前景     

Effects of pH and initial Ca2+-H2PO4- concentration on fibroin mineralization

In the present study, the effects of pH and initial Ca²⁺-H₂PO₄^- (Ca-P) concentration on fibroin mineralization were studied. The crystal growth of calcium phosphates was regulated by regenerated silk fibroin for 8 h (at pH 4.0, 7.0 and 10.0, respectively). Meanwhile, different concentrations of Ca²⁺ were employed at a certain pH value, keeping the initial Ca-P molar ratio constant at 1.67, i.e., the stoichiometry of hydroxyapatite [Ca10(PO₄)₆(OH)₂, HAP]. The products were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM) and thermogravimetric analysis (TGA). The results demonstrated that, compared to pH 4.0 and 10.0, pH 7.0 promoted the transformation of brushite (CaHPO₄°2H₂O, DCPD) to HAP. In the composites of mineralized fibroin, DCPD is the main inorganic phase at both relatively low and high pH, while HAP is the main inorganic phase at pH 7.0. Additionally, the initial Ca-P concentration does not affect the kind of inorganic phase in the synthesized mineralized fibroin, but induce to different contents of inorganic mineral and different morphology of DCPD at pH 4.0 and pH 10.0.     

复合相变材料的制备

利用真空吸附法制备了有机无机复合相变材料,采用差示扫描量热仪(DSC)和扫描电镜进行测试,结果表明,此复合材料调温功能稳定,有机相变材料被无机多孔材料吸附到孔道中,并且相变材料在孔道中分布均匀.经热重法分析,此真空吸附方法制备的复合相变材料在100℃以下相变性能稳定,不会对环境造成污染.     

Chemically Stable Black Phase CsPbI3 Inorganic Perovskites for High-Efficiency Photovoltaics

Research on chemically stable inorganic perovskites has achieved rapid progress in terms of high efficiency exceeding 19% and high thermal stabilities, making it one of the most promising candidates for thermodynamically stable and high-efficiency perovskite solar cells. Among those inorganic perovskites, CsPbI₃ with good chemical components stability possesses the suitable bandgap (≈1.7 eV) for single-junction and tandem solar cells. Comparing to the anisotropic organic cations, the isotropic cesium cation without hydrogen bond and cation orientation renders CsPbI₃ exhibit unique optoelectronic properties. However, the unideal tolerance factor of CsPbI₃ induces the challenges of different crystal phase competition and room temperature phase stability. Herein, the latest important developments regarding understanding of the crystal structure and phase of CsPbI₃ perovskite are presented. The development of various solution chemistry approaches for depositing high-quality phase-pure CsPbI₃ perovskite is summarized. Furthermore, some important phase stabilization strategies for black phase CsPbI₃ are discussed. The latest experimental and theoretical studies on the fundamental physical properties of photoactive phase CsPbI₃ have deepened the understanding of inorganic perovskites. The future development and research directions toward achieving highly stable CsPbI₃ materials will further advance inorganic perovskite for highly stable and efficient photovoltaics.