X射线法测量ICF靶丸参数中表面轮廓法的应用

 在ICF靶参数测量中,用接触X射线显微辐射照相法记录微球X射线图像,采用精密表面轮廓仪处理微球X射线图像,直接测量了单层微球壁厚。与光干涉法比较,两种方法测量结果相差小于0.3μm。     

聚芳亚胺酮空心微球的制备

 利用微流体技术和双重乳液技术对大直径聚芳亚胺亚胺酮空心微球的制备条件进行了讨论。完成了微球壁厚和直径的控制研究,并讨论了密度不匹配对微球质量的影响。获得了直径0.6～2.0 mm,壁厚5.0～20.0 μm的聚合物微球材料,并对微球制备过程中相分离对聚合物微球形貌的影响进行了分析,结果表明：在聚合物微球外表面易于进行spinodal分相,而在内表面易于进行binodal分相,因此微球内外表面具有不同的形貌结构。同批次制备微球中,平均直径±5%范围内的微球数占88%,球形度大于99%。     

厚壁空心微球的球形度和壁厚均匀性的表征研究

为建立高效简洁的厚壁空心微球球形度和壁厚均匀性的表征和测量方法,以内径850μm、壁厚25μm的厚壁聚苯乙烯(PS)微球为测量对象,分析球形度和壁厚均匀性的表征方法,探讨测量过程中采样方式对表征微球球形度和壁厚均匀性的影响。研究表明:对于批量微球球形度和壁厚均匀性的表征,当抽样数目不小于30时,测量结果之间的差异很小;而对于单一微球的球形度和壁厚均匀性的表征,至少3个不同投影面的测量结果的平均值才趋于稳定。不同投影面导致球形度或壁厚均匀性较差的批次样品的测量结果有一定差异,多次投影测量可提高测量结果的可靠性。     

PS/Ag核壳结构复合微球的制备与性能

以乳液聚合法制备的平均粒径1.2~1.5μm单分散聚苯乙烯(PS)微球为核,经过超声敏化、化学镀、还原等过程制备了PS/Ag核壳结构复合微球。采用透射电镜、X射线衍射、红外光谱、紫外可见光谱对其形貌、物相、结构与光学性质进行了表征与分析。结果表明:PS/Ag复合微球粒径相对均一;通过多次敏化、控制二次银氨溶液浓度(0.002~0.006 mol/L),可实现对纳米银壳层厚度的调控;纳米银壳层沉积生长过程中,随着PS微球表面银粒子的增多、增大,复合微球的光学等离子体共振吸收峰产生显著的展宽与红移。     

微球辅助相移干涉三维形貌测量

相移干涉显微镜在微观物体三维形貌的重构横向分辨率上受衍射极限影响,一般在微米级,限制其应用。将高折射率微球嵌入Mirau型相移干涉显微系统中,利用微球超分辨机理提高了其三维重构横向分辨能力,通过和原子力显微镜的测量对比验证了方法的可行性。仿真分析了微球尺寸对光子纳米喷流效应和超分辨能力的影响;同时使用两种不同尺寸的微球对275nm线宽的标准光栅样品进行了三维形貌重构;结果表明,在两种微球的辅助下,相移干涉显微系统均能够精确还原样品的三维结构,光栅深度测量结果与原子力显微镜结果相当。在微球辅助下,系统的横向分辨能力达到了275nm,相较于不使用微球的情况下提高了2.1倍,微球的最高放大率达到了3.4倍。系统在微纳米测量等领域具有较高的应用价值。     

相移干涉法测量ICF微球内表面粗糙度

 通过分析光线通过微球壳层后各界面的相位分布,讨论了相移干涉法测量微球内表面粗糙度的基本原理,研究了微球上部壳层对内表面粗糙度测量的影响,得到了聚苯乙烯,聚a甲基苯乙烯微球的内表面形貌特征图像,测量数据与原子力显微镜测量数据在同一量级。以微球壳层对超光滑碳化硅及单晶硅片表面形貌的调制作用为研究对象,讨论了微球的外表面粗糙度以及微球壁厚对内表面粗糙度测量结果的影响,确定了相移干涉法测量微球内表面粗糙度的不确定度,实验结果表明：对于表面粗糙度小于30 nm、厚度小于9 mm的微球,测量不确定度小于0.4 nm。     

制备大直径无气泡聚苯乙烯空心微球

 高品质聚苯乙烯（PS）空心微球是惯性约束聚变（ICF）实验用多层塑料微球靶的重要芯轴,常由乳液技术制备。针对由乳液技术制备的PS微球壳壁内容易形成气泡而且大直径微球制备困难的问题,实验研究了对壳壁内存在的气泡以及消除方法和制备大直径PS微球的制备技术。     

ICF微球壳层掺溴含量的XRF表征

通过EC法与FP法的混合定量分析方法,建立了用于微球壳层掺杂元素含量测量的校准模型;基于对微球直径、PS、PVA层厚度对分析元素荧光强度影响的理论计算及XRF实验研究,将该模型用于ICF微球壳层掺溴含量的测量,得到微球壳层掺溴含量较为精确的分析结果,实验结果表明：XRF法测量ICF微球壳层掺溴含量具有较高的精度,在微球涂层厚度大于10 μm时,其测量相对误差在5％左右。     

基于聚合物共混的有机场效应晶体管光电性能研究

采用聚合物共混的方法制备了体异质结薄膜,将其作为光敏半导体层制备了有机场效应光晶体管.利用原子力显微镜表征了共混薄膜的分相情况,探究了器件提高激子解离效率的机理,并对比了聚合物共混前后有机场效应晶体管的光电性能变化和相分离情况.结果表明：制备的聚合物共混光晶体管在微弱光线条件下(0.038 mW/cm²,808 nm)具有较高的光敏性(为10⁶).通过共混聚合物半导体材料制备体异质结薄膜可以有效地提高激子解离的效率,通过双层绝缘层能进一步降低光晶体管的暗电流,从而提高器件的光敏性.     

金锥-聚合物球壳靶制备初步研究

 报道了研制快点火物理实验用带金锥固体球壳靶时，采用多次乳化技术制备聚合物空心微球，精密车床加工和电镀技术制备金锥，精密加工实现聚合物微球表面打孔的工艺。窄分布聚苯乙烯制备的空心微球直径与壁厚分布较窄。电镀液的配方、pH值、镀前处理、尖端效应等对镀层的表面质量和镀层与芯轴之间的结合力有重要的影响。采用精密车床加工可以在聚合物微球表面获得直径约120 μm的孔，初步实现金锥与聚合物微球的连接。     

搅拌法制备聚合物微球中油水相对壁厚的影响

为了研究乳液微封装技术中油水相对微球壁厚的影响,推导了在理想状态下微球壁厚、油相质量分数和油水相比这三者之间的函数关系。结果表明:当内相水滴半径和油相质量分数为常数时,微球壁厚是油水相比的单增函数;而当内相水滴半径和油水相比为常数时,微球壁厚是油相质量分数的单增函数。即提高油相质量分数或增大油水相比对增加壁厚而言具有等效性。根据此规律,在搅拌法制备小直径聚苯乙烯微球中,通过调整油水相的各参数,确定了制备小直径厚壁聚苯乙烯微球的关键工艺参数。实验表明:采用搅拌法制备10~25 m壁厚的小直径聚苯乙烯微球时,油相质量分数宜配制为5.3%~7.0%,油水相比宜控制在1.6~2.2之间,而外水相中聚乙烯醇质量分数宜控制在1%~3%之内。     

Fabrication of Nanostructured Composite Microspheres Based on the Self‐Assembly of Polymers and Functional Nanomaterials

This Review examines recent developments in the morphological control of polymer microspheres fabricated via the phase separation of polymers as well as the alignment of functional nanoparticles inside microspheres prepared by so‐called bottom‐up synthesis techniques. Several methods for adjusting the internal and surface morphologies of polymer microspheres based on the phase separation of polymer blends and block copolymers are discussed, and the effects of microsphere size on phase separated structures and theoretical simulations of morphologies are also reviewed. The alignment of functional nanoparticles in phase separated polymer microspheres and applications of nanostructured and hybrid polymer microspheres are summarized.     

显微红外反射光谱法快速鉴别珍珠粉真伪

珍珠是名贵的装饰品和中药材,在我国对其已有2000多年的应用历史。研究发现,贝壳内层的化学组成与珍珠相似,主要含有碳酸钙和各种氨基酸。贝壳粉也可在临床上做药用,但其药用价值远低于珍珠粉。然而,珍珠粉和贝壳粉外观特性极为相似,元素组成和形貌检测无法对其进行有效地鉴别。由于贝壳粉的成本低,常常冒充珍珠粉流入市场,侵害了消费者的利益。本研究通过珍珠粉和贝壳粉在不同温度下煅烧一定时间后显微红外反射光谱的差异实现珍珠粉真伪鉴别。实验结果表明,在一个大气压下经过400 ℃煅烧30 min后,珍珠粉中文石型碳酸钙部分转化为方解石型,而贝壳粉中文石型碳酸钙完全转化为方解石型。这种不同的相转变过程可以被显微红外反射光谱很好的区别。因此,可在此条件下利用红外反射光谱鉴别珍珠粉和贝壳粉相变差异。和传统的透射式红外光谱法相比,这种显微反射红外光谱法无需压片制样、快速灵敏。本研究也讨论了该方法针对其他常见伪品的适用性,如牡蛎粉和石决明粉,结果表明该方法能够简单、高效和准确地鉴别珍珠粉真伪。     

离子型表面活性剂对双重乳粒分散性能的影响

为了改善臭氧处理PS单层球与PVA溶液生成的双重乳粒在油相中的分散性,采用了低分子量阴离子型表面活性剂十二烷基硫酸钠(SDS)和十二烷基苯磺酸钠(SDBS)及高分子量混合型表面活性剂十八烷基胺聚氧乙烯醚双季铵盐(PAVDA)来改性该种PS单层球,测试并分析了不同表面活性剂对相应薄膜亲水接触角及其对PVA吸附速率的影响,同时也考察并对比了静电排斥作用和空间位阻作用对双重乳粒分散性的影响。实验结果表明这三种表面活性剂均能不同程度的改善双重乳粒在油相中的分散性。其中,经SDS和SDBS处理后,双重乳粒在油相中固化时会发生絮凝作用而无法以较高成活率制得大尺寸双层球;经PAVDA处理PS单层球后,实现了以较高的成活率制得700~900μm的PS-PVA双层空心微球。同时,也表明在改善PS单层球的分散性方面,空间位阻稳定作用较静电排斥作用更为有效。     

TOF-SIMS analysis of polystyrene/polybutadiene blend using chemical derivatization and multivariate analysis

Chemical imaging with high spatial resolution is one of the features of TOF-SIMS. However, degradation of the sample due to primary ion bombardment becomes problematic when the analysis area is small. Although polystyrene (PS) and polybutadiene (PB) separately show relatively distinct spectra, observation of their phase separation in PS/PB blends is difficult when the analysis area is small because degradation of both polymers and especially PS leads to disappearance of their characteristic peaks, resulting in low chemical image contrast. We therefore investigated the application of various forms of multivariate analysis (MVA) to the TOF-SIMS image data to improve the chemical image contrast. PCA, MCR, and the other forms of MVA provided improvement in contrast, but the images were still obscure and observation of phase separation remained difficult. Chemical derivatization using osmium tetroxide was also investigated, and found to give clear images of phase separation in the PS/PB blend. In quantitative determinations with MVA and chemical derivatization, PLS demonstrated the best predictive capability and chemical derivatization resulted in large deviations from both the bulk chemical composition and the determinations with MVA, particularly in regions of low PB content.     

A novel video-based microsphere localization algorithm for low contrast silica particles under white light illumination

On the basis of a brief review of four common image recognition algorithms for microspheres made of polystyrene or melamine resin, we present a new microsphere localization method for low-contrast silica beads under white light illumination. We compare both the polystyrene and silica procedures with respect to accuracy and precision by means of an optical tweezers setup providing CMOS video microscopy capability. By that we demonstrate that our new silica algorithm achieves a relative position uncertainty of less than ±1 nm for micron-sized microspheres, significantly exceeding the precision of the other silica approaches studied. Second, we present an advancement of our single microsphere tracking method to scenarios where two polystyrene, melamine resin or silica microspheres are in close-to-contact proximity. While the majority of the analysis algorithms studied generate artefacts due to interference effects under these conditions, we show that our new approach yields accurate and precise results.     

Young’s modulus of PS/CeO<Subscript>2</Subscript> composite with core/shell structure microspheres measured using atomic force microscopy

Organic–inorganic composite microspheres with PS as a core and CeO₂ as a shell were synthesized by in situ chemical precipitation method. The size of PS core was 117, 163, 206, and 241 nm, respectively, and the shell thickness was about 10 nm. The CeO₂ shell was composed of a large number of nanoparticles, of which the size was 4–6 nm. Atomic force microscopy was employed to probe the mechanical properties of core–shell structured ceria-coated polystyrene (PS/CeO₂) composite microspheres. On the basis of Hertz’s theory of contact mechanics, compressive moduli were measured by the analysis of force–displacement curves captured on the microsphere samples. For a fixed CeO₂ shell thickness, the Young’s modulus of composite microspheres increased with an increase of PS core size. The calculated Young’s moduli (E) values of composites for 136, 185, 242, and 261 nm in diameter were 5.78 ± 0.9, 7.23 ± 1.3, 11.46 ± 1.7, and 14.54 ± 1.4 GPa, respectively. The results revealed the effect of the CeO₂ shell on the elastic deformation of the PS core. This approach will provide fundamental insights into the actual role of organic/inorganic core/shell composite abrasives in chemical mechanical polishing.     

Polishing behavior of PS/CeO2 hybrid microspheres with controlled shell thickness on silicon dioxide CMP

Organic-inorganic composite microspheres with PS as a core and CeO₂ nanoparticles as a shell were synthesized by in situ decomposition reaction of Ce(NO₃)₃ on the surfaces of PS microspheres prepared through soap-free emulsion polymerization. The shell thickness of the composite microspheres could be turned by varying the concentration of Ce(NO₃)₃ in the reaction solution. The whole process required neither surface treatment for PS microspheres nor additional surfactant or stabilizer. The as-synthesized PS/CeO₂ composite microsphere samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). Oxide chemical mechanical polishing (CMP) performance of the PS/CeO₂ composite abrasives with different shell thickness was characterized by atomic force microscopy (AFM). The results indicated that the as-prepared core-shell structured composite microspheres (220-260 nm in diameter) possessed thin shell (10-30 nm) composed of CeO₂ nanoparticles (particle diameter of 5-10 nm), and the final CeO₂ contents of the composite microspheres ranged from 10 to 50 wt%. A possible mechanism for the formation of PS/CeO₂ composite microspheres was discussed also. The CMP test results confirmed that the novel core-shell structured composite abrasives are useful to improve oxide CMP performance. In addition, there is an obvious effect of shell thickness of the composite abrasives on oxide CMP performance.     

Microhardness Studies of the Interphase Boundary in Rubber‐Softened Glassy Polymer Blends Prepared with/without Compatibilizer

Abstract

The interphase boundary of incompatible polymer blends such as poly(methyl methacrylate) (PMMA)/natural rubber (NR) and polystyrene (PS)/NR, and of compatible blends such as PMMA/NR/epoxidized NR (ENR) and PS/NR/styrene–butadiene–styrene (SBS) block copolymer, where ENR and SBS were used as compatibilizers, was studied by means of microindentation hardness (H) and microscopy. Cast films of neat PMMA and PS, and blended films of PMMA/NR, PS/NR, PMMA/NR/ENR, and PS/NR/SBS were prepared by the solution method using a common solvent (toluene). Hardness values of 178 and 173 MPa were obtained on the surfaces of the neat PMMA and PS, respectively. After the inclusion of soft phases, the binary (incompatible) and the ternary (compatible) blend surfaces show markedly lower H‐values. Scanning electron and optical microscopy reveal a clear difference at the phase boundary of the surface of compatible (smooth boundary) and incompatible (sharp boundary) blends. The compatibilized blends were characterized by using microhardness measurements, as having the thinnest phase boundary (～30 µm), while incompatible blends were shown to present a boundary of about 60 µm. The hardness values indicate that the compatibilizer is smoothly distributed across the interface between the two blend components. Results highlight that the microindentation technique, in combination with microscopic observations, is a sensitive tool for studying the breadth and quality of the interphase boundary in non‐ or compatibilized polymer blends and other inhomogeneous materials.