SiO2/聚酰亚胺/SiO2复合薄膜绝缘性能及基于聚酰亚胺复合薄膜的后栅型场致发射性能的研究

使用射频磁控溅射和化学溶液法制备了SiO2/聚酰亚胺(PI)/SiO2绝缘膜。分别使用X射线衍射、扫描电镜对薄膜结构和薄膜表面形貌进行了表征;利用超高阻微电流测试仪测试了SiO2/PI/SiO2复合绝缘膜漏电流和电压击穿特性;采用SiO2/PI/SiO2作为绝缘膜,制作了后栅型场致发射器件,使用场发射测试系统测试了器件的开启电压、发射电流以及发光亮度。结果表明:SiO2/PI/SiO2复合绝缘膜具有高的击穿电压和低的漏电流密度,后栅器件中栅极对阴极表面的电场强度调控作用明显,阳极电压为750V时,栅极开启电压为91 V,阳极电流可达384μA,栅极漏电流仅为59μA,器件最高亮度可达600 cd/m2。     

SiO2-Al2O3气凝胶及纤维增强复合材料制备技术研究进展

SiO₂-Al₂O₃复合气凝胶(SAA)耐高温性能明显优于纯SiO₂、Al₂O₃气凝胶,可用于1 000℃以上高温环境,对高温窑炉、设备隔热保温具有重要意义。本文综述了SAA及纤维增强复合材料的制备技术研究进展,在阐明硅铝复合溶胶水解、聚合机理的基础上,讨论了前驱体种类、干燥方式、水、添加剂等对溶胶胶凝过程及气凝胶微观结构与物化性能的影响,简要介绍了SAA微观结构、高温烧结行为特点及硅铝物质的量比对孔结构及耐高温性能的影响,介绍了基于粉煤灰、煤矸石、高岭土等廉价原料的SAA制备方法,以及基于纳米颗粒组装、冰模板、壳聚糖模板的制备新方法。在纤维增强复合材料方面,介绍了以纤维为分散相、纤维预制体为主体骨架两类复合材料的制备方法及纤维种类(石英、莫来石、碳纤维、纳米SiO₂、碳纳米管、氧化锆等)对复合材料力学及耐高温性能的影响。最后梳理了目前复合气凝胶研究中存在的问题,展望了其发展趋势。     

纳米SiO2/Al2O3复合改性对环氧树脂绝缘性能的影响

以双酚A型环氧树脂E51为基体,纳米SiO₂/Al₂O₃为辅助填料,采用低温等离子体协同偶联剂对纳米填料进行接枝处理,控制低温等离子体处理时间,制备出纳米SiO₂/Al₂O₃/E51三元复合绝缘材料,研究纳米填料对环氧树脂复合材料介电性能、闪络电压、热分解温度及击穿强度等的影响。结果表明,纳米SiO₂填充量为3%,纳米Al₂O₃填充量为1.5%,并且采用偶联剂协同低温等离子体的处理时间为30 s时,复合试样各项电气性能均得到显著提升。初始分解温度较未改性时提高22℃;闪络电压较未改性时提高20.9%;击穿强度较未改性时提高23.1%。这一结果为提高环氧树脂电气性能提供了新的研究思路。     

超临界流体干燥法制备TiO2/ Fe2O3 和TiO2/ Fe2O3/ SiO2 复合纳米粒子及光催化性能

以TiCl₄ 、Fe (NO₃ )₃·9H₂O 和Na₂SiO₃19H₂O 为原料, 采用溶胶凝胶法结合超临界流体干燥法(SCFD)制备了纳米级TiO₂/ Fe₂O₃ 和TiO₂/ Fe₂O₃/ SiO₂ 复合光催化剂。以光催化降解苯酚对所得催化剂的催化活性进行了评价。结果表明, 纳米TiO₂/ Fe₂O₃ 复合粒子与单组分TiO₂ 比较, 复合粒子光催化活性高于单组分的TiO₂, 6h 苯酚降解率高达95.9 %。SiO₂ 的加入可以抑制纳米粒子粒径的长大和晶相的转变, 增强TiO₂ 纳米粒子的热稳定性。复合光催化剂中Fe₂O₃ 最佳掺入量为0.06 %, SiO₂ 最佳掺入量为10 %(摩尔分数) 。并用XRD、TEM 和FTIR 等手段进行了表征。TiO₂ 以锐钛矿型形式存在, SiO₂ 以无定性形式存在。比较了不同制备方法制得的TiO₂/ Fe₂O₃ 复合光催化剂, 得出超临界干燥法制备的光催化剂具有粒径小、比表面积大、分散性好、光催化活性高等特点。采用超临界流体干燥可直接得锐钛型纳米复合光催化剂。     

疏水型纳米SiO2-MTES复合薄膜的制备及性能

采用溶胶-凝胶技术,通过酸/酸二步法控制实验条件,由于表面活性剂具有特殊的表面活性性能,实验中采用表面活性剂十六烷基三甲基溴化氨(CTAB)为模板剂,正硅酸乙酯为硅源,甲基三乙氧基硅烷为有机硅烷,以及二次去离子水,盐酸为催化剂等原料制备SiO2-MTES(摩尔比11.15)前驱体溶胶.通过简单提拉迅速蒸发溶剂等方法制备二氧化硅-甲基三乙氧基硅烷的有机-无机复合薄膜,测得的红外透射光谱表明所制备的薄膜由于掺入甲基基团而疏水,接触角测试值约125度,其结果进一步支持这一结论.未加MTES的薄膜折射率为1.18,膜厚305nm.加入MTES后薄膜折射率为1.22,膜厚为289.6nm.透射光谱和机械性能测试结果表明所制备的疏水型纳米SiO2-MTES复合薄膜同时还具有良好的光学性能和机械性能.     

SiO2/聚四氟乙烯复合薄膜的制备及力学性能

采用空气辅助干法共混、冷压烧结并车削成膜的方法制备了SiO₂填充量为35wt%、厚度为50 μm的聚四氟乙烯（PTFE）基复合薄膜。系统研究了SiO₂颗粒粒径对SiO₂/PTFE薄膜复合材料的孔洞缺陷和力学性能等的影响,并研究了SiO₂在PTFE中的分散情况及分子间相互作用对其性能变化的影响机制。结果表明,随SiO₂粒径的逐渐增大,其在PTFE中的分散趋于均匀,同时PTFE能更好地包覆粒子,因此SiO₂/PTFE薄膜孔洞缺陷逐渐减少,力学性能逐渐增强;当SiO₂的粒径D₅₀为12 μm时,其在PTFE中的分散均匀性最佳,SiO₂/PTFE复合薄膜孔洞缺陷最少,具有较好的力学性能,断裂伸长率达19.5%,拉伸强度达9.2 MPa。      

SiO2/CeF3复合薄膜的电致发光

采用真空电子束蒸发气相沉积技术在重掺杂n型硅衬底上制备了SiO₂/CeF₃复合薄膜电致发光器件。对器件中各膜层的微观结构和成分进行了表征,并研究了器件的电致发光特性。结果表明：器件在正反接时的电致发光光谱存在明显差异,相应的伏安特性曲线不对称。器件正接时,电致发光光谱在504 nm(绿光区)处和680 nm(红光区)处各出现一个发光峰;反接时,电致发光光谱除了在684 nm(红光区)处出现一个较弱的发光峰外,在434 nm处还出现了一个很强的蓝色发光峰。     

聚酰亚胺/纳米Al_2O_3三层复合薄膜的制备

将掺杂纳米Al2O3的聚酰胺酸与未掺杂聚酰胺酸在玻璃板上逐层涂膜,热亚胺化制备了3层聚酰亚胺/纳米Al2O3复合薄膜.采用扫描电镜(SEM)对该薄膜的微观形貌进行了表征,测试了薄膜的热稳定性、力学性能及电击穿场强.结果表明,复合薄膜的热性能及电击穿场强均高于掺杂薄膜及未掺杂膜,当热失重达到10%时,复合薄膜的热分解温度达到了629.1℃;与掺杂薄膜相比,复合薄膜的力学性能得到明显提高,拉伸强度和断裂伸长率分别为117.4 MPa和18.5%.     

片状磁性纳米TiO2/SiO2/NiFe2O4制备及光催化性能

以锐钛矿磁性纳米TiO2/SiO2/NiFe2O4(TSN)为原料,采用水热法制备了片状磁性纳米TSN.利用XRD、TEM等技术对样品进行了表征.水热法处理后核壳结构的TSN部分转变为片状,催化剂磁性增强.以亚甲基兰溶液为模拟水样测试了样品的光催化性能,考察了催化剂加入量、反应时间、pH值等因素的影响.实验表明:片状磁性纳米TSN光催化性能明显优于粒状TSN.片状TSN具有良好的吸附性能,提高了光催化反应的初始速率.用于处理亚甲基兰废水时受pH值的影响较小,1小时的脱色率在90%以上.     

Preparation and thermoelectric properties of nc-Si:(Al2O3 + SiO2) composite film

A composite film of nanocrystalline Si (nc-Si) embedded in (Al₂O₃ + SiO₂) has been prepared on a quartz substrate by thermally evaporating a 400 nm thick Al film on a quartz substrate and annealing in air at 580 °C for 1 h. During annealing, the Al reacts with the SiO₂ of the quartz substrate and produces nc-Si, which is embedded in the (Al₂O₃ + SiO₂) film. The average size of nc-Si is ~ 22 nm and the thickness of the nc-Si:(Al₂O₃ + SiO₂) composite film is ~ 810 nm. It is found that the prepared film is thermoelectric with a Seebeck coefficient of − 624 μV/K at 293 K and − 225 μV/K at 413 K.     

Preparation of polyimide/Al2O3 composite films as improved solid dielectrics

Considerable demand for solid thin-film dielectrics with high dielectric constants for use in the fabrication of capacitors has been observed. In this study, polyimide (PI)/Al₂O₃ composite films were prepared by incorporating different micron-sized α-Al₂O₃ contents into PI derived from pyromellitic dianyhydride and 4,4′-oxydianiline via ultrasonication. Chemical structure, morphology, dielectric and thermal properties were investigated by Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), LCR meter and Perkin Elmer Pyris 6. FTIR spectra showed complete imidization, and all characteristic peaks of the imide groups are observed in PI and PI/Al₂O₃ composite films. XRD patterns revealed that the PI/Al₂O₃ composite exhibits peaks similar to those of α-Al₂O₃, indicating that the crystal structure of α-Al₂O₃ remains unchanged and stable after being doped into the PI matrix. SEM micrographs showed uniform distribution of α-Al₂O₃ particles in the PI matrix. Meanwhile, the dielectric constant, dielectric loss and thermal stability of PI/Al₂O₃ increases with the addition of α-Al₂O₃ content.     

Preparation and characterization of Nb2O5-Al2O3 composite oxide formed by cathodic electroplating and anodizing

Al foil was coated with niobium oxide by cathodic electroplating and anodized in a neutral boric acid solution to achieve high capacitance in a thin film capacitor. X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) revealed the niobium oxide layer on Al to be a hydroxide-rich amorphous phase. The film was crystalline and had stoichiometric stability after annealing at temperatures up to 600 °C followed by anodizing at 500 V, and the specific capacitance of the Nb₂O₅-Al₂O₃ composite oxide was approximately 27% higher than that of Al₂O₃ without a Nb₂O₅ layer. The capacitance was quite stable to the resonance frequency. Overall, the Nb₂O₅-Al₂O₃ composite oxide film is a suitable material for thin film capacitors.     

改性纳米SiO2/硅橡胶复合材料的制备及性能

为提高纳米SiO₂在硅橡胶（SR）基体中的分散性及两相间的界面结合力,设计以羟基硅油（HSO）和γ-甲基丙烯酰氧基丙基三甲氧基硅烷（KH570）为纳米SiO₂的表面封端改性剂,并将改性SiO₂与双组份加成型液体SR复合得到改性纳米SiO₂/SR复合材料。通过一系列表征手段对改性纳米SiO₂的形貌结构及其在乙醇中的分散性等进行分析,研究了改性纳米SiO₂对纳米SiO₂/SR复合材料的断面形貌、力学性能及热稳定性的影响。结果表明:KH570成功接枝到纳米SiO₂表面并与SR基体间形成化学键。当HSO协同KH570改性纳米SiO₂时,可有效改善纳米SiO₂在SR基体中的分散性能及纳米SiO₂与SR两相间的界面结合性能,并显著提高纳米SiO₂/SR复合材料的力学性能和热稳定性。将SiO₂∶HSO∶KH570以质量比为2.0∶0.2∶0.6处理的改性纳米SiO₂粒子,得到的改性纳米SiO₂/SR复合材料起始热分解温度提高了230℃。当SiO₂∶HSO∶KH570质量比为2.0∶0.2∶0.45时,改性纳米SiO₂/SR复合材料的拉伸强度和断裂伸长率分别提高了约1倍。      

核-壳结构粒子SiO_2@Bi_2O_3的制备及红外发射率研究

为了研究制备复合隐身粒子的方法,采用溶胶-凝胶法制备了核-壳结构SiO2@Bi2O3粒子.通过XRD、TEM及发射率测试仪对制备的材料的结构、形貌和性能进行了表征.XRD表明在700℃可以得到Bi2O3纯相;红外发射率测试表明,Bi2O3具有较低的红外发射率,在SiO2表面包覆Bi2O3后,在3～5μm和8～14μm两个测试波段都能降低SiO2的红外发射率.通过核-壳结构的形式,在较高发射率的样品表面涂覆红外发射率较低的样品,可以提高红外隐身效果.     

Preparation and properties of nano-SiC strengthening Al2O3 composite ceramics

The processing and mechanical behaviors of Al₂O₃-xwt.%SiC (x = 1, 2, 5, ASx) nano-composites prepared by the in situ synthesis of SiC from polycarbosilane (PCS) were investigated. The composites were densified by hot pressing. The microstructure and mechanical properties of the sintered composites were analyzed. The results showed that a fully dense structure was obtained when a few nano-SiC were doped and that the fracture toughness and strength were highly improved compared with those of monolithic Al₂O₃. The fracture toughness reached 5.1 MPa m^1/2 in AS2 composite. The maximum flexural strength was 516 MPa obtained in AS1 composite.     

Optical properties of Er-doped SiO2-GeO2-Al2O3 planar waveguide fabricated by sol–gel processes

In this paper, we report silica based planar waveguides doped with Er³⁺, and co-doped with GeO₂ and Al₂O₃. These sol–gel derived planar waveguides were fabricated on SOS (silica on silicon) using multiple spin-coating and rapid thermal processing (RTP). Investigation has been made on their characteristics in terms of their application in optical amplification and lasing, including photoluminescence (PL), fluorescence lifetime, refractive index, propagation loss, surface roughness, Fourier transform infrared (FTIR) spectrum and X-ray diffraction (XRD) analysis. The propagation loss of a 20-layer planar waveguide was measured to be about 1.6 dB/cm for TE₀ and 2.2 dB/cm for TM₀ mode. A strong emission transition (⁴I_13/2→⁴I_15/2) at 1.536 μm with a lifetime of 3.6 ms has been obtained for an optimized molar composition of 90SiO₂: 10GeO₂: 20AlO_1.5: 1ErO_1.5.     

SiO2或TiO2纳米粒子/含氟聚丙烯酸酯复合涂层的制备及其防腐蚀性能

通过在含氟聚丙烯酸酯(PFHI)溶液中添加固体纳米粒子,经涂覆热固化后得到了厚度约为1 μm的SiO₂或TiO₂纳米粒子/PFHI复合涂层,考察了SiO₂或TiO₂两种纳米粒子质量分数对复合涂层表面性质和防腐蚀性能的影响。利用Tafel极化曲线和电化学交流阻抗(EIS)测试研究了复合涂层在3.5wt% NaCl溶液中的电化学防腐蚀性能,并运用XPS、衰减全反射傅里叶变换红外光谱(ATR-FTIR)、TG-DTA、SEM、光学接触角(OCA)手段对复合涂层进行表征。结果表明,添加SiO₂或TiO₂纳米粒子均可大幅提高PFHI涂层的电化学防腐蚀性能,SiO₂与PFHI质量比为0.3的SiO₂/PFHI复合涂层电荷转移阻抗值R_ct与PFHI涂层相比上升了2个数量级。SiO₂或TiO₂纳米粒子增大了涂层表面粗糙度,与PFHI紧密结合形成致密的复合涂层,提高了涂层的疏水性和致密性,从而改善了涂层的抗腐蚀性能。