含羧基聚酰亚胺共聚物的挠性覆铜板的制备与性能

以4,4’-对苯二氧双邻苯二甲酸酐（HQDPA）和不同比例的4,4’-二氨基二苯醚（ODA）及3,5-二氨基苯甲酸（DABA）为反应单体,通过共聚的方法,制备了一系列聚酰胺酸（PPA）,将其涂覆于铜箔表面,通过热酰亚胺化后得到无胶型挠性覆铜板（FCCL）。研究表明,当二胺为DABA时,聚酰亚胺的力学性能和热学性能最好,表面接触角为61.3°,热膨胀系数为24×10^-6K^-1,介电常数为3.58,制备得到的FCCL的剥离强度达到1.18 N/mm。这种含羧基结构的聚酰亚胺的性能可以满足无胶型挠性印制电路对基底膜材料的尺寸稳定性和粘接性能的要求。     

2001年中国聚酰亚胺的研究与应用题录

3 ,3’ -二氨基二苯醚的全成及其聚酰亚胺 /虞鑫海、胡志强 (上海市合成树脂研究所 ) /绝缘材料 ,2 0 0 1 ,(4) :1 3～ 1 5。3 ,5 -二氨基苯甲酸 - 4’ -联苯酯及含液晶侧链的聚酰亚胺的合成与表征 /范浩军、顾宜、谢美丽 (四川大学高分子材料科学与工程系 ) /高分子学报 ,2 0 0 1 ,(4) :494～ 495。4-苯乙炔苯酐及其封端的聚酰亚胺 /陈鑫、(上海鑫扬化工实业有限公司 )、陈武荣 (桂林电器科学研究所) /绝缘材料 ,2 0 0 1 ,(4) :1 0～ 1 2。Ｎ -异丙基马来酰亚胺在渐变型耐温塑料光纤中的应用 /王东军、陈鹏磊、顾陈斌等 (中国科学院理化研…     

基于葡萄糖的星型胆甾相液晶化合物的合成及相行为

以葡萄糖为手性中心,6-（4-（苯甲酸基）苯）己二酸单酯（M1）、6-（4-（4-烷氧基苯甲酸基）苯）己二酸单酯（M2～M3）为侧臂,采用N,N′-二环己基碳化二亚胺（DCC）/4-二甲氨基吡啶（DMAP）成酯法,合成了星型化合物（GM1～GM3）。通过红外光谱（FT-IR）、核磁共振（1H-NMR）、偏光显微镜（PO...     

含有氢键的聚酰亚胺薄膜的制备和性能表征

以对硝基苯甲酸为原料,通过酰氯化、酰化、还原反应成功合成了4,4’-二氨基苯酰替苯胺(DBN),DBN分别和3,3’,4,4’-联苯四酸二酐(BPDA)、均苯四甲酸二酐(PMDA)通过两步法缩聚制备出聚酰亚胺薄膜,用红外(FT-IR),差示扫描量热仪(DSC)和热重分析(TGA),拉伸测试表征其结构和性能,结果表明,成功合成了含有酰胺键的聚酰亚胺薄膜,并且酰胺键的N-H分别和酰亚胺环中的C-N和C=O形成了氢键。将其与4,4’-二氨基二苯醚(ODA)聚酰亚胺薄膜相比,对应二酐(BPDA和PMDA)分别和DBN制备的聚酰亚胺薄膜表现出了优异的热性能和耐溶剂性,尤其是拉伸强度有了显著的提高。     

可溶性联苯型聚酰亚胺的合成及表征

选用3,3’,4,4’-联苯四甲酸二酐（BPDA）作为二酐单体，同时选用一种带有侧链的3,3’-二甲基-4,4’-二氨基二苯甲烷（DMMDA）作为二胺单体，采用两步法合成了可溶性的联苯型聚酰亚胺。探讨了单体配比、固含量、反应温度和反应时间等因素对聚酰胺酸黏度的影响，以及化学亚胺化时间对PI亚胺化程度的影响，并确定了聚酰亚胺最佳的合成条件。聚酰胺酸合成过程的最佳单体配比确定为1∶1，固含量为12%，反应温度为20℃，反应时间为8 h，最优条件下的聚酰胺酸特性黏度为1.88 d L/g；聚酰亚胺合成过程的最佳化学亚胺化时间为24 h,在该条件下亚胺化程度为98%。之后，对最优条件下合成的聚酰亚胺进行了一系列的结构和性能表征。结果表明，合成的聚酰亚胺相对分子质量较高（数均分子量（■）和重均分子量（■）分别为14万和21万）且分布较窄，在保持耐热性能和耐溶剂性能的同时，显著提高了成膜性、溶解性等加工性能，是制备耐溶剂纳滤膜的理想材料。     

邻苯二酚衍生的二（醚胺）化学改性3，3’，4，4-联苯基四羧酸二酐聚酰亚胺

以前曾指出由3，3’，4，4’-联苯基四羧酸二酐(BPDA)和1，2-双(4-氨基苯氧基)苯(亦称三苯基醚邻苯二酚二胺(TPEC))衍生的聚酰亚胺具有优异的拉伸性能和良好的热性能。本文对由BPDA、TPEC及其它芳香族二胺制备的共聚酰亚胺的性能做了初步评价。由BPDA和各种芳香族二胺制备的均聚酰亚胺通常具有良好的机械性能和热性能。然而，它们不溶于现有的各种有机溶剂中。在某些条件下，用BPDA与等摩尔TPEC和其它芳香族二胺混合物可以制备可有机溶解的BPDA型共聚酰亚胺。这些共聚酰亚胺可以形成坚韧的薄膜，它们具有较高的模量和强度。多数情况下，也具有较高的断裂伸长率。     

高性能、高韧性附加型树脂基复合材料基体及制备方法

本发明涉及一种高性能、高韧性附加型树脂基复合材料基体聚酰亚胺预聚物（SIOPI）及该预聚物的制备方法。首先将二胺溶于有机溶剂，再将3，3’，4，4’-联苯四酸二酐和2，2’，3，3’-联苯四酸二酐混合加入到有机溶剂中。     

一种可溶性双酮酐型共聚酰亚胺的合成及性能

以均苯四甲酸二酐(PMDA)和4,4’-对苯二甲酰二邻苯二甲酸酐(TDPA)为二酐单体,4,4’-(3-氨基苯氧基)二苯甲酮(BABP)为二胺单体,采用两步法低温溶液缩聚合成了系列双酮酐型共聚酰亚胺。采用红外光谱、X射线衍射、差示扫描量热分析、热重分析、拉伸测试和溶解性能测试对聚合物的结构与性能进行了表征,考察了TDPA/PMDA不同摩尔比对共聚酰亚胺溶解性、耐热性和力学性能的影响。结果表明,双酮酐型聚酰亚胺的玻璃化转变温度随TDPA摩尔含量的增加逐渐下降,溶解性能则逐渐提高,当TDPA/PMDA摩尔比为7/3时,共聚酰亚胺具有优良的耐热性能及力学性能,可溶于N,N-二甲基甲酰胺(DMF)等极性溶剂。     

含咪唑基磺化聚酰亚胺质子交换膜的结构与性能关系研究

将1,4,5,8-萘四羧酸二酐(NTDA)与4,4’-二(4-氨基苯氧基)联苯-3,3’二磺酸(BAPBDS)及3种共聚用二胺单体:2-(4-氨基苯基)-5-氨基-苯并咪唑(APABI)、1,3-二(4-氨基苯氧基)-5-(2-苯并咪唑基)苯(BAPBIB)及4,4’-二(4-氨基苯氧基)联苯(BAPB)在间甲酚中180℃进行无规共聚,分别制得了3种共聚物:主链含咪唑基磺化聚酰亚胺、含侧咪唑基磺化聚酰亚胺及不含咪唑基磺化聚酰亚胺。用溶液浇注法制得了具有良好机械性能的质子交换膜,测定了这些质子交换膜的离子交换容量、吸水率、质子导电率、水解稳定性和抗自由基氧化等性能,重点研究了含咪唑基二胺单体的化学结构对质子交换膜的抗自由基氧化性和水解稳定性的影响规律。     

液相色谱法测定食品包装用油墨中11种光引发剂的含量

目的 建立油墨中光引发剂的检测方法，从源头控制食品包装的安全。方法 油墨样品经乙酸乙酯和乙腈超声提取，体积分数为20%的乙腈溶液定容，固相萃取柱萃取后用乙腈定容，使用液相色谱进行测定。结果 11种成分在各自范围内线性关系良好（R≥0.999 5），平均加样回收率为90.0%～95.0%，相对标准偏差（n=6）小于3.5%。结论 建立了液相色谱同时测定油墨中2-甲基-1-(4-甲基硫代苯基)-2-(4-吗啉基)-1-丙酮、1-羟基环己基苯基酮、2-苯甲酰基苯甲酸甲酯、4-二甲氨基苯甲酸乙酯、4,4’-二（N,N-二甲氨基）二苯甲酮、安息香双甲醚、4-甲基二苯甲酮、4,4’-二（N,N-二乙氨基）二苯甲酮、对二甲氨基苯甲酸异辛酯、2-异丙基硫杂蒽酮、2,4-二乙基噻唑酮的方法。     

添加剂对聚酰亚胺液晶垂直取向剂性能的影响

研究了添加剂对PI取向性能、耐摩擦性、热稳定性以及透光率的影响。用均苯四甲酸二酐(PM-DA),对苯二胺(PDA),4-已氧基联苯酚-3’,5’-二胺基苯甲酸酯(C6-BBDA),制备了三元共聚型PI取向膜,并采用添加剂(封端剂和交联剂)对PI改性。通过调节添加剂的组成制备了4种PI。利用红外光谱仪(FT-IR)、热失重分析仪(TGA)、紫外分光光度计(UV-Vis)、偏光显微镜(POM)和预倾角测试仪对合成的PI进行了结构表征和性能测试。研究发现LC分子在4种PI膜上都获得了均匀的垂直取向;添加交联剂的PI膜具有良好的耐摩擦性,经摩擦强度为600mm摩擦后,仍对LC分子具有垂直取向的能力;加入添加剂的PI膜具有良好的热稳定性,此外,加入添加剂的PI膜仍具有较高的透光率。     

Transparent conductive film having sandwich structure of gallium-indium-oxide/silver/gallium-indium-oxide

New transparent conductive films having the sandwich structure of gallium-indium-oxide/silver/gallium-indium-oxide (GIO/Ag/GIO) were prepared by conventional magnetron sputtering method at ambient substrate temperature. The electrical and optical properties of the films were compared with those of conventional indium-tin-oxide (ITO) films and ITO/Ag/ITO sandwich films. The GIO/Ag/GIO (40 nm/8 nm/40 nm) sandwich films, in which the GIO film was deposited using a GIO ceramic target with In content [In/(Ga + In)] of 10 at.%, exhibited a low sheet resistance of 11.3 Ω/sq and a large average transmittance of over 92.9% in the visible region (400-800 nm). This GIO/Ag/GIO films also exhibited a novel characteristic of transparency in the ultraviolet region; they showed high transmittance of 82.2% at the wavelength of 330 nm and 40.8% at the wavelength of 280 nm, which was not shown in the ITO films and the ITO/Ag/ITO sandwich films. The GIO/Ag/GIO sandwich films are useful as transparent electrode for emitting devices of ultraviolet radiation because of both their high conductivity and high transparency in the ultraviolet region.     

含氟半脂环透明聚酰亚胺薄膜的制备和性能

分别将脂环族二酐单体1,2,3,4-环丁烷四酸二酐(CBDA,Ⅰ)、1,2,4,5-环戊烷四酸二酐(CPDA,Ⅱ)和1,2,4,5-环己烷四酸二酐(CHDA,Ⅲ)与芳香族含氟二胺1,4-双(4-胺基-2-三氟甲基苯氯基)苯(6FAPB,a)和4,4′-双(4-胺基-2-三氟甲基苯氧基)联苯(6FBAB,b)反应制备两个系列的含氟半脂环族聚酰亚胺(PI),研究了PI薄膜的热性能和光学性能.结果表明,制备出的PI薄膜具有良好的热稳定性,在氮气中起始热分解温度超过450℃、玻璃化转变温度超过250℃,在可见光范围内(400-700 nm)具有优良的透明性,450 nm处的透过率超过88%.两类PI薄膜在光通讯波段(1.30μm与1.55μm)均没有显著的吸收.     

Preparation and properties of fluorine-containing colorless polyimide nanocomposite films with organo-modified montmorillonites for potential flexible substrate

We prepared transparent polyimide (PI) and organo-modified montmorillonite (OMMT) nanocomposite films from the solution of poly(amic acid) and various amounts (0.5-2 wt%) of OMMT in N,N-dimethylacetamide (DMAc). The Poly(amic acid) was prepared from the reaction of 4,4'-(hexafluoroisopropylidene)diphthalic anhydride (6FDA) and 2,2'-bis (trifluoromethyl)-4,4'-diamino phenyl (TFDB). Dodecylamine (C12-) and dodecyltriphenylphosphonium chloride (C12PPh-Cl-) were used as organic modifiers in OMMT. The PI/OMMT nanocomposite films were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), transmission electron microscope (TEM), UV-Vis transmission spectra, thermomechanical analysis (TMA), and rheometric dynamic analysis (RDA). As the OMMT contents is increased, PI/OMMT nanocomposites generally show better properties compared to pristine PI films, although the transparency of the PI/OMMT nanocomposite films is sacrificed slightly. However, it is concluded that these nanocomposite films are good candidates for potential flexible substrates.     

Colorless and transparent polyimide nanocomposite films containing organoclay

A series of colorless and transparent polyimide (PI) nanocomposite films was synthesized from 4,4'-(hexafluoroisopropylidene) diphthalic anhydride (6FDA) and bis(3-aminophenyl) sulfone (APS) with various organoclay contents via solution intercalation polymerization to poly(amic acid)s, followed by thermal imidization. Varying the organoclay loading in the range of 0 to 1.00 wt% produced variations in the thermal properties, morphologies, and optical transparencies of the hybrids. The hybrid films exhibited high optical transparencies and almost no color, with cut-off wavelengths between 330 and 346 nm and very low yellow index (YI) values of 1.78-3.80. The hybrid PI films showed good thermal properties with glass transition temperatures of 236-245 degrees C. Most films did not show significant thermal decomposition below 450 degrees C. It was found that the addition of only a small amount of organoclay was sufficient to improve the thermal properties of the PI films, with maximum enhancements being observed at 0.50 wt% organoclay. Moreover, these PI hybrids also showed low coefficients of thermal expansion (CTE).     

Highly transparent polymer substrates for flexible displays using semi-interconnected interpenetrating polymer networks

Semi-interconnected interpenetrating polymer networks (SIPNs) based on unsaturated polyurethane (UP) and different monomers, including styrene and acrylate with an UP ratio of 50 wt%, were synthesized. The resulting SIPN films exhibited excellent optical transparency in the visible range with > 90% transmittance at 400 nm. The glass transition temperature (Tg) varied in the range of 100 approximately 135 degrees C depending on the unsaturated monomers introduced. They also had good flexibility compared to the conventional rigid polystyrene or polyacrylate due to the homogeneously dispersed elastic urethane moiety in the SIPNs. Below the glass transition temperature (Tg) of the SIPN substrates, the ITO-grown SIPN films exhibited good electrical and optical properties, showing potential as a promising substrate in flexible display applications.     

High performance polyimide composite films prepared by homogeneity reinforcement of electrospun nanofibers

Highly aligned polyimide (PI) and PI nanocomposite fibers containing carbon nanotubes (CNTs) were produced by electrospinning. Scanning electron microscopy showed the electrospun nanofibers were uniform and almost free of defects. Transmission electron microscopy indicated that the CNTs were finely dispersed and highly oriented along the CNT/PI nanofiber axis at a relatively low concentration. The as-prepared well-aligned electrospun nanofibers were then directly used as homogeneity reinforcement to enhance the tensile strength and toughness of PI films. The neat PI nanofiber reinforced PI films showed good transparency, decreased bulk density and significantly improved mechanical properties. Compared with neat PI film prepared by solution casting, the tensile strength and elongation at break for the PI film reinforced with 2 wt.% CNT/PI nanofibers were remarkably increased by 138% and 104%, respectively. The significant increases in the overall mechanical properties of the nanofibers reinforced polyimide films can be ascribed to good compatibility between the electrospun nanofibers and the matrix as well as high nanofiber orientation in the matrix. Our study demonstrates a good example for fabricating high performance and high toughness polyimide nanocomposites by using this facile homogeneity self-reinforcement method.     

High aspect ratio contact hole etching using relatively transparent amorphous carbon hard mask deposited from propylene

In this study, a high aspect ratio contact pattern, beyond 70 nm technology, in a very-large-scale integrated circuit, was achieved using hydrogenated amorphous carbon (a-C:H) film as the dry etching hard mask. The effect of temperature on the a-C:H deposits prepared by plasma enhanced chemical vapor deposition was studied. The a-C:H films resulting from propylene (C₃H₆) decomposition exhibited high transparency incorporated rich hydrogen concentration with a decreasing deposition temperature. A matrix of dispersed cross-linked sp³ clusters in a-C:H films, which has an increasing optical band gap and higher hydrogen content, is attributed to reduce the defect density of status and obtain high transmittance rate. Moreover, the higher transparency of a-C:H films could afford lithographic aligned capability as well as compressive stress and dry etching resistance. These explorations provided insights into the role of hydrogen in a-C film and also into the practicality of its future nano-scale device applications.     

Europium incorporated barium titanate thin films for optical applications

BaTiO₃:Eu (BT:Eu) thin films were deposited onto quartz substrates by RF magnetron sputtering. The effect on structural, morphological, optical and photoluminescence (PL) properties in the films with different Eu concentrations (0–5 wt%) were investigated. The X-ray diffraction (XRD) pattern of the undoped BT thin film revealed a tetragonal (T) phase with orientations along (101) plane. From XRD pattern, the crystallinity of the films increased with increase in Eu concentration. The SEM images revealed that the films exhibited tetragonal shape, crack free and good adherence to the substrate. Atomic force microscopy studies showed an increase of grain growth with doping concentration. The rms roughness value increased with increase in Eu concentration and the film surface revealed positive skewness and high value of kurtosis which make them suitable for tribological applications. X-ray photoelectron spectroscopy revealed the presence of barium, titanium, europium and oxygen in BT:Eu film. An average transmittance of >80 % (in visible region) was observed for all the films. Optical band gap of Eu doped BT films decreased from 3.86 to 3.53 eV. Such films with optical properties such as high transparency, decrease in band gap and high refractive index are suitable for optoelectronic applications. PL properties showed a sharp line at 625 nm and a broad line at 552 nm due to europium (Eu³⁺) transitions. PL phenomena were observed, owing to the electronic structure of Eu³⁺ ions as well as BT nanocrystallites in the films. The sharp and intense red luminescence is useful for photoelectric devices and optical communications.     

Dip coated 12CaO·7Al2O3 thin films through sol-gel process using metal alkoxide

Transparent nanostructured 12CaO·7Al₂O₃ thin films with cubic structure have been prepared on soda lime glass substrates via the sol-gel dip coating using the precursor sol solution at low temperature. The structural, compositional, morphological and optical properties of the 12CaO·7Al₂O₃ films and powder were studied using X-ray diffractometry (XRD), X-ray photoelectron spectroscopy, scanning electron microscopy (SEM) and atomic force microscopy. Optical properties of 12CaO·7Al₂O₃ films have been investigated using UV-visible spectroscopy. Two different precursor sols were prepared using calcium-2-ethyl hexonate and aluminium isopropoxide as precursor materials in isopropanol and ethylene glycol monomethyl ether solvents. Dip coated gel like films were dried at 120 °C for 15 min and subsequently heat-treated at 450 °C for 1 h in air atmosphere. The influence of films thickness and optical transparency with use of different solvent and sol concentration on microstructure of the films were established. In addition, XRD patterns revealed that 12CaO·7Al₂O₃ films have been composed of cubic phase. SEM observations exhibited that the films structure becomes more homogeneous using isopropanol as compared to ethylene glycol monomethyl ether solvent. The 12CaO·7Al₂O₃ films prepared using 2 (wt.%) sol in isopropanol had high transparency nearly 88% in wide visible range with maximum of 90% at 600 nm wavelength.