Synthesis and properties of novel soluble polyimides having a spirobisindane-linked dianhydride unit

A new synthetic procedure was elaborated allowing the preparation of semiaromatic dianhydride. N-Methyl protected 4-chlorophthalic anhydride was nitrated with HNO3 to produce N-methyl-4-chloro-5-nitrophthalimide (1). The aromatic nucleophilic substitution reaction between 5,5',6,6'-tetrahydroxy-3,3,3',3'-tetramethyl-1,1-spirobisindane and 1 afforded spirobisindane-linked bis(N-methylphthalimide) (2), which was hydrolyzed and subsequently dehydrated to give the corresponding dianhydride (3). The latter was polymerized with five different aromatic diamines to afford a series of aromatic polyimides. The properties of polyimides such as inherent viscosity, solubility, UV transparency and thermal stability were investigated to illustrate the contribution of the introduction of spirobisindane groups into the polyimide backbone. The resulting polyimides were readily soluble in polar solvents such as chloroform, THF and N-methyl-2-pyrrolidone. The glass-transition temperatures of these polyimides were in the range of 254-292 degrees C. The tensile strength, elongation at break, and Young's modulus of the polyimide film were 68.8-106.6 MPa, 5.9-9.8%, 1.7-2.0 GPa, respectively. The polymer films were colorless and transparent with the absorption cutoff wavelength at 286-308 nm.

反相高效液相色谱表征无定型聚芳醚酮（砜）成环解聚产物

建立了一种反相高效液相色谱表征无定型聚芳醚酮（砜）成环解聚产物的新方法.采用岛津VP-ODS C18反相色谱柱（150 mm×4.6 mm; 5 μm, i.d.）,以四氢呋喃/水为流动相,流速1.0 mL/min, 梯度淋洗方式;254 nm紫外检测,由此方法可将全部同系物组分有效地分离并可准确给出产物中各环状低聚体组分的百分含量.分析结果表明,酚酞聚醚酮、酚酞聚醚砜、双酚A聚砜经成环解聚反应高产率得到环状聚合体,最高成环率达97.57%.通过与激光质谱的比较证实了HPLC方法更适合于对成环解聚产物体系的表征.

Pink light emitting long-lasting phosphorescence in Sm3+-doped CdSiO3

Novel pink light emitting long-lasting afterglow CdSiO3:SM3+ phosphors are prepared by the conventional high-temperature solid-state method and their luminescent properties are investigated. XRD and photolurflinescence (PL) spectra are used to characterize the synthesized phosphors. The phosphors are well crystallized by calcinations at 1050degreesC for 5 h. These phosphors emit pink light and show long-lasting phosphorescence after they are excited with 254 nm ultraviolet light. The phosphorescence lasts for nearly 5 h in the light perception of the dark-adapted human eye (0.32mcd/m(2)). The phosphorescence mechanism is also investigated. All the results indicate that these phosphors have promising potential practical applications.

Luminescence properties of CdSiO3 : Mn2+ phosphor

A novel long-lasting phosphor CdSiO3:Mn2+ is reported in this paper. The Mn2+-doped CdSiO3 phosphor emits orange light with CIE chromaticity coordinates x = 0.5814 and y = 0.4139 under 254 nm UV light excitation. In the emission spectrum of 1% Mn2+-doped CdSiO3 phosphor, there is a broad emission band centered at 575 nm which can be attributed to the,pin-forbidden transition of the d-orbital electron associated with the Mn2+ ion. The phosphorescence can be seen by the naked eyes in the dark clearly even after the 254 nm UV irradiation have been removed for about 1 h. The mechanism of the origin of the long-lasting phosphorescence was discussed using the thermoluminescence curves.

A novel white light emitting long-lasting phosphor

A novel white light emitting long-lasting phosphor Cd1-xDyxSiO3 is reported in this letter. The Dy3+ doped CdSiO3 phosphor emits white light. The phosphorescence can be seen with the naked eye in the dark clearly even after the 254 nm UV irradiation have been removed for about 30 min. In the emission spectrum of 5% Dy3+ doped CdSiO3 phosphor, there are two emission peaks of Dy3+, 580 mn (F-4(9/2)-->H-6(13/2)) and 486 nm (F-4(9/2)-->H-6(15/2)), as well as a broad band emission located at about 410 nm. All the three emissions form a white light with CIE chromaticity coordinates x=0.3874, y=0.3760 and the color temperature is 4000 K under 254 mn excitation. It indicated that this phosphor is a promising new luminescent material for practice application.

VIV-UV excited luminescent properties of LnCa4O(BO3)3 : RE3+(Ln = Y, La, Gd; Re=Eu, Tb, Dy, Ce)

Calcium lanthanide oxyborate doped with rare-earth ions LnCa(4)O(BO3)(3):RE3+ (LnCOB:RE, Ln = Y, La, Gd, RE = Eu, Tb, Dy, Cc) was synthesized by the method of solid-state reaction at high temperature. Their fluorescent spectra were measured from vacuum ultraviolet (VUV) to visible region at room temperature. Their excitation spectra all have a broadband center at about 188 nm, which is ascribed to host absorption. Using Dorenbos' and J phi rgensen's work [P. Dorenbos, J. Lumin. 91 (2000) 91, R. Resfeld, C.K. J phi rgensen. Lasers and Excite States of Rare Earth [M], Springer, Berlin, 1977, p. 45], the position of the lowest 5d levels E(Ln,A) and charge transfer band E-ct were calculated and compared with their excitation spectra.Eu3+ and Tb3+ ions doped into LnCOB show efficient luminescence under VUV and UV irradiation. In this system, Ce3+ ions do not show efficient luminescence and quench the luminescence of Tb3+ ions when Tb3+ and Ce3+ ions are co-doped into LnCOB. GdCOB doped with Dy3+ shows yellowish white light under irradiation of 254 nm light for the reason that Gd ions transfer the energy from itself to Dy.

Microstructures and properties of melt-spun and as-cast Mg-20Gd binary alloy

Mg-20Gd(%, mass fraction) samples were prepared using melt-spinning and copper mold casting techniques. Microstructures and properties of the Mg-20Gd were investigated. Results show that the melt-spun ribbon is mainly composed of supersaturated alpha-Mg solid solution phase and the as-east ingot mainly contains alpha-Mg solid solution and Mg5Gd phase. The differential scanning calorimeter (DSC) curve of the ribbon exhibits a small exothermic peak in the temperature range from 630 to 680 K, which indicates that the ribbon contains a metastable phase (amorphous). Tensile strength at room temperature of the melt-spun ribbon and as-cast specimen are 308 and 254 MPa, respectively. The elongations of the two samples are less than 2%. The fracture surfaces demonstrate that the fracture mode of the as-cast Mg-20Gd is a typical cleavage fracture and that of the melt-spun sample is a combination of brittle fracture and ductile fracture.

Novel indigo light emitting long-lasting phosphors CdSiO3: RE3+ (RE = Y, La, Gd, Lu)

A series of novel indigo light emitting long-lasting phosphors CdSiO3: RE3+ (RE = Y, La, Gd, Lu) was prepared by the conventional high-temperature solid-state method. The XRD, photoluminescence (PL) spectra and afterglow intensity decay were used to characterize the synthesized phosphors. These phosphors emitted indigo light and showed long-lasting phosphorescence. The phosphorescence can be seen with the naked eye in the dark clearly even after the 254-nm UV irradiation have been removed for more than 30 min.

Fe在丝光沸石骨架中取代位置的DFT研究

中国科学院山西煤炭化学研究所