新型二苯甲酮光引发剂的合成及其光聚合性能

本文合成了一种新型二苯甲酮基复合光引发剂4-(2-羟基-3-叔丁基)二苯甲酮(OEBP),采用红外光谱、核磁共振氢谱对其结构进行表征。并采用实时红外光谱研究了OEBP光引发剂引发丙烯酸酯类单体的光聚合行为。结果表明,该引发剂的最大吸收光谱在280 nm,随着紫外光照的进行,OEBP的最大吸收峰280 nm逐渐减少,其变化呈线性关系。随着引发剂浓度的增加,单体的最大速率和转化率先增大后减小;随着光强的增大,单体转化率和最大聚合速率都增大。OEBP与传统的光引发剂二苯甲酮/4-二甲基氨基苯甲酸乙酯(BP/EDAB)引发效率相当。     

环氧有机硅阳离子光聚合引发体系的增感研究

研究了裂解型和夺氢型自由基光引发剂种类及用量对脂环族环氧官能化聚有机硅氧烷预聚物(CEPS)阳离子光聚合中二芳基碘鎓盐SR—1012引发体系增感作用的影响。结果表明，自由基型光引发剂对SR—1012有很好的增感作用，增感后的体系感应可达112．2mJ／cm^2。自由基光引发剂与SR—1012的最佳配比为不超过1：2(重量比)。     

光敏有机硅聚氨酯丙烯酸酯预聚体光聚合性能的研究

采用实时红外法（Real time infrared spectrum,RTIR）详细研究了光引发剂及活性单体对光敏有机硅聚氨酯丙烯酸酯（Polysiloxane urethane acrylate,PSUA）体系的光聚合性能的影响。研究发现,断裂型光引发剂的引发效率要高于夺氢型的光引发剂的引发效率,其中Irgaeure 1700引发体系的聚合速率最快。光引发剂最佳用量为0．5％～1％。体系的双键转化率随单体官能度的增加而降低。含单体HEA和IBOA的感光体系的双键转化率最大,基本完全聚合;而含TPGDA和HDDA的体系的双键转化率大约在90％～95％之间;含TMPTA的体系的双键转化率只有80％左右。含不同活性单体体系的双键转化速率的大小顺序为：TPGDA≈HDDA〉HEA〉TMPTA〉IBOA,体系的双键转化率和双键转化速率都随着单体含量的增加而减小。     

温度对1,6-己二醇二丙烯酸酯紫外光聚合的影响

对在低温下呈固态的1,6-己二醇二丙烯酸酯体系进行紫外光辐照，并用近红外光谱技术研究聚合体系的光聚合及后固化行为，用顺磁共振光谱技术证明后固化过程自由基的衰竭现象，从而探讨1,6-己二醇二丙烯酸酯在固态下进行紫外光聚合的聚合动力学。实验发现固态1,6-己二醇二丙烯酸酯体系可以进行光聚合，并伴有后固化现象；升高反应温度可提高双键转化率；引发剂1173的含量对体系聚合程度有较大影响。     

Study on cationic photopolymerization reaction of epoxy polysiloxane

The effects of epoxy monomers, concentration of photoinitiator and radical photoinitiators on the photosensitive properties of cationic phopolymerization system with a novel epoxy polysiloxane oligomer (CEPS) were investigated via a gel yield method. The results showed that among the tested epoxy monomers, the reactivity of ERL-4221 with cycloaliphatic epoxy groups was the highest. The optimum concentration of diaryldiodonium salt (SR-1012) was determined as 4-5 wt.%. Increasing the amounts of ERL-4221 in the CEPS cationic photopolymerization system, UV-curing rate increased. Radical photoinitiators with ArCO structure possessed sensitization capacity to the cationic photoinitiator SR-1012. The photosensitivity of the CEPS system could be up to 165 mJ/cm². Adding a small amount of IPA and BP could greatly improve the photosensitivity of CEPS cationic photosensitive system. The optimal quantity of isopropanol added to the system was not more than 2 wt.%.     

The effect of temperature on the induction period in the photoinitiated polymerization of tripropylene glycol diacrylate

The effect of temperature on the kinetics of the photopolymerization of tripropylene glycol diacrylate was studied by real-time FTIR–attenuated total reflection (ATR) spectroscopy. The temperature behaviour of the polymerization rate was found to be dependent on the photoinitiator used. The induction period strongly decreases with increasing temperature. It was shown by quantitative determination of the oxygen concentration that the decay of the induction period is solely due to the decreasing solubility of oxygen in the acrylate.     

增塑对UV固化型高分子固体电解质性能的影响

将合成的大分子量的聚乙二醇丙烯酸酯(PEGDA)齐聚物与光引发刑、LiClO4组成光敏体系，与一定比例的碳酸乙烯酯(EC)、碳酸丙烯酯(PC)或其混合物进行混合，经紫外光辐照制得了一种新型的高分子固体电解质膜，考察了增塑刑种类和用量对光固化速率、电导率和机械性能的影响。结果表明，增塑是提高UV固化型高分子固体电解质导电性能的有效方法，在机械性能满足使用要求的条件下，增塑的UV固化型固体电解质的电导率可以高达10^-4S／cm左右。     

Synthesis of amidoxime polymer gel to extract uranium compound from seawater by UV radiation curing

A new amidoxime polymer gel for uranium extraction from seawater was successfully prepared by photoinitiated crosslinking polymerization. It involves UV-induced radical polymerization of acrylonitrile (AN) and methacrylic acid (MAA) monomers with crosslinking agent and photoinitiator: an alternative synthesis pathway to gamma radiation. Characteristic peaks of Fourier transform infrared spectroscopy (FTIR) indicated that nitrile group was completely converted into amidoxime group. Eight hours of 60 W UV curing was enough for polymer gel formation. For the 4 to 1 ratio of AN to MAA, crosslinking agent concentration of 1 g/100 mL-monomers and photoinitiator content of 60 mL/100 mL-monomer, maximum uranium adsorption capacity of 17.02 mg/g adsorbent in seawater was achieved for sample spiked with 10 ppm uranium. For seawater sample spiked with 2,245 ppm uranium, the adsorption capacity reached 432.41 mg/g adsorbent. The amidoxime polymer gel could be regenerated for at least eight cycles while retaining about 50% of the uranium uptake capacity. Thus, the present amidoxime polymer adsorbent is a high-efficiency seawater uranium recovery agent for both high and low uranium concentrations.     

单晶硅表面钝化层在低能电子辐照前后的SIMS和XPS分析

为了研究低能电子辐照对单晶硅器件表面钝化材料中产生的化学微结构的变化,在轻掺杂P型单晶硅基底上制作了三种表面钝化膜,分别是单一SiO2钝化膜、SiO2/Si3N4复合钝化膜、硼硅玻璃/Si3N4复合钝化膜,开展了表面钝化单晶硅在最大能量70 keV的加速器电子束下的辐照实验.样品在空气气氛下辐照6 h,用二次离子质谱(...     

Probing Co/Si interface behaviour by X-ray photoelectron spectroscopy （XPS） and atomic force microscopy （AFM）

In this work, we investigate the Co-Si reaction, the Co growth mode at room temperature, diffusion behaviour as well as morphology evolution during annealing on both H-terminated and clean Si（001） and Si（lll） surfaces. From in-situ X-ray photoelectron spectroscopy （XPS） investigation, ＂Co-Si＂ reaction appears to occur on both H-terminated and clean surfaces at room temperature （RT） and the silicide crystallinity is improved upon annealing. Co growth mode on H-terminated Si surfaces occurs in a pseudo layer-by-layer manner while small close-packed island growth mode is observed on the clean Si surface. Upon annealing at different temperatures, Co atom concentration decreases versus annealing time, which in part is attributed to Co atoms inward diffusion. The diffusion behaviour on both types of surfaces demonstrates a similar trend. Morphology study using ex-situ atomic force microscopy （AFM） shows that the islands formed on Si（001） surface after annealing at 700℃ are elongated with growth directions alternate between the two perpendicular [110 ] and [ 110] directions. Triangular islands are observed on Si （111） surface.     

Comparison of glow argon plasma-induced surface changes of thermoplastic polymers

Modification of high-density polyethylene (PE), polytetrafluoroethylene (PTFE), polystyrene (PS), polyethyleneterephthalate (PET) and polypropylene (PP) by Ar plasma was studied. The amount of the ablated material was determined by gravimetry. Wettability of polymers after the plasma treatment was determined from the contact angle measurement. The changes in the surface morphology of polymers were observed using atomic force microscopy (AFM). Chemical structure of modified polymers was characterized by X-ray photoelectron spectroscopy (XPS) and electron paramagnetic resonance (EPR). Surface changes were also studied by the determination of electrokinetic potential (ζ-potential). It was found that under the plasma treatment the polymers are ablated and their surface morphology and roughness are changed dramatically. XPS measurements indicate an oxidation of the polymer surface. The plasma treatment results in a dramatic increase of the ζ-potential. EPR data show different radical amount present on the treated surface of all polymers. Most significant changes due to the degradation of polymer chains are observed on PTFE.     

Effect of Si implantation on the microstructure of silicon nanocrystals and surrounding SiO2 layer

Si nanocrystals (Si-nc) embedded in a SiO₂ layer have been characterized by means of transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). For local Si concentration in excess  8 × 10²¹ Si⁺/cm³, the size of the Si-nc was found to be 3 nm and comparatively homogeneous throughout the whole implanted layer. For local Si concentration in excess of 2.4 × 10²² Si⁺/cm³, the Si-nc diameter ranges from 2 to 12 nm in the sample, the Si-nc in the middle region of the implanted layer being bigger than those near the surface and the bottom of the layer. Also, Si-nc are visible deeper than the implanted depth. Characterization by XPS shows that a large quantity of oxygen was depleted from the first 25 nm in this sample (also visible on TEM image) and most of the SiO₂ bonds have been replaced by Si–O bonds. Experimental and simulation results suggest that a local Si concentration in excess of 3 × 10²¹ Si/cm³ is required for the production of Si-nc.     

两种裂解型有机硅大分子光引发剂的合成与性能

以2-羟基-2-甲基-对羟乙基醚基苯基丙酮-1(2959)和氨基硅油为原料合成了双官能度和四官能度两种裂解型有机硅大分子光引发剂NH2-2959-2和NH2-2959-4。研究了两种光引发剂的紫外吸收和降解,引发光聚合及自上浮性能。结果表明,两种光引发剂均在275 nm有最大吸收峰,紫外吸收峰强度随着紫外光辐照时间的延长逐渐减弱。NH2-2959-4光引发剂体系的光聚合速率明显高于NH2-2959-2体系。与小分子光引发剂2959相比,NH2-2959-2和NH2-2959-4均具有较好的自上浮能力,可以在体系中自发地向表面迁移,形成浓度的梯度分布。     

氢气流量对类金刚石薄膜结构与性能的影响

采用直流/射频耦合反应磁控溅射法在Si（100）衬底上成功制备出类金刚石（DLC）薄膜。利用表面轮廓仪、Raman光谱仪、X射线光电子能谱仪表征所制备薄膜在不同氢气流量下的沉积速率和化学结构,讨论了氢气流量对薄膜沉积速率和化学结构的影响;利用纳米压痕技术及曲率弯曲法表征薄膜的力学性能;利用扫描电镜和原子力显微镜表征薄膜的表面形貌与粗糙度。研究表明：随着氢气流量的增加,所制备薄膜的沉积速率逐渐减小,而薄膜中sp³键的含量逐渐增大。当氢气流量为25 mL/min时,薄膜中sp³键的含量为36.3%,薄膜的硬度和体弹性模量分别达到最大值17.5 GPa和137 GPa。同时,所制备薄膜的内应力均低于0.5 GPa,有望成功制备出低内应力的高质量DLC厚膜。随着氢气流量的增加,DLC薄膜的表面变得更致密光滑,且表面均方根粗糙度由5.40 nm降为1.46 nm。     

硅胶表面季铵功能化接枝过程的29SiCP/MSNMR和XPS法研究

本工作采用29SiCP/MSNMR和XPS测试方法对硅胶表面接枝季铵功能基团的过程和机理进行了分析。XPS光谱分析结果表明，硅基季铵化产品的XPS谱中含有Si、O、C、N元素，并出现了以R4N+形式存在的401.26eV结合能峰，表明硅胶表面已被季铵化。TGA-DTA分析其接枝率为 0.46mmol/g，同时，本工作采用29SiCP/MSNMR法对接枝机理进行探索研究，得出了接枝的可能反应途径和产品分子结构。     

Wear mechanism and microstructures of Mo-implanted 4Cr5MoV1Si steel

tance and microstructure of implanted specimen were1 Introduction discussed according to the results of RBS, GXRD and The influence of pulsed beam in ion implantation XPS.is a topic of interest in both ion beam modification 2 Experimentaland radiation effect research.[1-3] Currently, a majorapplication of ion implantation is to improve the cor- Square steel samples (0.36wt.%…     

Experimental Observations of the Chemistry of the SiO2/Si Interface

Changes in silicon surface preparation prior to thermal oxidation are shown to leave a signature by altering the final SiO2/Si interface structure. Surface analytical techniques, including XPS, static SIMS, ion milling, and newly developed wet-chemical profiling procedures are used to obtain detailed information on the chemical structure of the interface. The oxides are shown to be essentially SiO2 down to a narrow transitional interface layer (3-7 ?). A number of discrete chemical species are observed in this interface layer, including different silicon bonds (e.g., C-, OH-, H-) and a range of oxidation states of silicon (0 ? +4). The effect of surface preparation and the observed chemical species are correlated with oxide growth rate, surface-state density, and flatband shifts after irradiation.     

电离辐射下双界面Si3N4/SiO2/Si的等离激元

用X光激发电子能谱(XPS)分析技术对Si3N4/SiO2/Si双界面系统经60Co电离辐照前后处于纯Si态的一级等离激元(定位于B.E. 116.95 eV)、处于SiO2态的一级等离激元(定位于B.E. 122.0 eV)和处于Si3N4态的一级等离激元(定位于B.E. 127.0 eV)进行了研究.实验结果显示:存在一个由Si3N4态等离激元和SiO2态等离激元构成的界面及由SiO2态等离激元和Si态等离激元构成的界面,在电离辐射的作用下,SiO2态-Si3N4态等离激元界面区中心向Si3N4态表面方向推移,同时SiO2态/Si3N4态等离激元界面区亦被展宽;电离辐照相当程度地减少位于SiO2态-Si态界面至Si衬底之间SiO2态的一级等离激元的浓度:同时偏置电场对SiO2/Si界面等离激元有显著作用.文中就实验现象以光电子能损进行了机制分析.