PA-PVA-CH塑料微球充D2和Ar

ICF塑料靶丸典型结构由3层组成：内层起支撑作用的聚苯乙烯（PS），中间起阻气作用的聚乙烯醇（PVA）和外部的烧蚀层碳氢（CH）。作为靶丸，空心塑料微球内的气体由燃料气体和诊断气体组成。燃料气体目前使用的主要是D2。塑料微球采用热扩散法充气，D2在塑料球壳中扩散很快，而Ar却渗透很慢，因此，塑料靶丸充气的核心工艺是如何充Ar和如何保D2。利用充Ar条件充D2或利用保D2技术保Ar都是很容易实现的。塑料微球充气在自行研制的充气系统中完成，球内气体采用四极质谱或X射线荧光谱仪进行测量。     

多层塑料微球的研制

2004年研究了PVA溶液的浓度对PS微球成活率的影响；并且通过O3处理，提高了PS微球球壳强度；并且还进行了内表面掺硫的多层塑料微球的研制；同时完成了二氧化硅气凝胶的增强和疏水改性研究。     

炉内成球法制备PVA涂层理论模拟研究

 根据炉内成球法制备PVA涂层原理，建立了炉内成球法在PS微球表面制备PVA涂层的数学模型，并利用数值方法进行了求解，研究了初始PS壁厚和直径、载气种类、炉内温度、PVA含量等实验条件的影响。计算结果表明，包裹PS微球的PVA水溶液复合微球在下落过程中速度迅速增加，短时间内达到最大值后又逐渐降低；复合微球的PVA水溶液涂层厚度逐渐减少，微球表观密度降低；炉内温度较低时，PVA涂层不易烘干；空气和纯Ar做炉内气氛时，微球烘干时间延长，而在He和Ar混合气体中，随着He含量增加，微球烘干时间缩短；小直径PS微球及高含量PVA溶液有利于制备厚的PVA涂层。     

非离子型表面活性剂Tween 20对大尺寸双层空心微球制备的影响

为了改善臭氧处理聚苯乙烯(PS)单层球与聚乙烯醇(PVA)溶液生成的双层乳粒在油相中的分散性,提高大尺寸双层球的成活率,在双层球制备过程中采用了非离子型表面活性剂Tween 20(T-20)来改性该种PS单层球。结果表明经表面活性剂T-20改性后显著降低了PS薄膜的亲水接触角,提高了PS与PVA间的相互作用,同时也大幅度提高了PS薄膜对PVA的吸附速率。红外光谱和紫外-可见分光光度计的测试结果证明:在PVA固化过程中,由于PVA与T-20的相比太大,PS表面吸附的表面活性剂T-20部分会被PVA置换、迁移至PVA溶液中。T-20的迁移提高了制备双层球过程中水相与外油相的粘度比且显著降低PVA溶液表面张力,从而有利于实现双重乳粒在油相中的单分散。因此,T-20是制备大尺寸PS-PVA双层空心微球有效的表面活性剂。     

臭氧改性及搅拌桨结构对大直径双层球制备的影响

随着高功率激光器的飞速发展,ICF物理实验对聚苯乙烯（PS）-聚乙烯醇（PVA）双层空心微球的规格要求逐渐提高,直径要求将达到700～900 m。针对该直径范围的PS-PVA双层空心微球,通过采用PS球臭氧化表面改性技术和搅拌桨叶轮结构优化技术,对传统乳液微封装法制备双层空心微球工艺进行了改进,臭氧化表面改性后PS固体核心发生憎水-亲水转变,提高了PS与PVA之间的作用强度;搅拌桨叶轮结构优化,改善了体系容器内溶液流场均匀性,使得微球在整个体系中的运动相对平稳,从而初步制得了直径范围在700～900 m的双层空心微球。     

臭氧化法表面改性聚苯乙烯薄膜

 为增强聚苯乙烯(PS)与聚乙烯醇(PVA)之间的结合力,进而提高PS-VA双层空心微球存活率。利用臭氧化改性法在酸性介质中对聚苯乙烯薄膜进行表面改性,用红外光谱对处理后的表面进行了半定量的分析。结果表明：改性过后聚苯乙烯表面产生羟基、羰基等极性基团;接触角测试证明,处理后的表面由憎水变为亲水,并通过纳米压痕划痕法得到了处理前后PS与PVA薄膜之间的相互作用强度,臭氧化改性后PS与PVA膜间作用强度增大了40%。     

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。     

充气过程对微球表面形貌的影响

对空心玻璃微球(HGM)在高温充气过程中的表面形貌进行了研究。分析局部晶化出现的时间和条件，并通过其表面形貌、成分分析探究了其随时间的变化规律。研究结果表明:影响HGM高温充气后表面形貌的因素主要有充气温度和充气压力；充气温度越高、压力越大表面形貌发生变化所需时间越短。导致表面形貌变化的本质原因是结晶分相，结晶成分主要由Na, B等元素组成。HGM的表面结晶分相使其表面粗糙度大幅度升高，但随着脱离充气环境后放置时间的延长而又逐渐降低。其表面粗糙度降低的主要原因是Na, B等元素的逆向迁移。     

ICF靶材料和靶制备技术研究进展

 主要介绍了中国工程物理研究院ICF靶材料科学与靶制备技术在材料研究、靶丸制备技术、薄膜制备技术、精密微工艺及靶参数测量等方面的主要研究进展。在靶材料研究方面,近年相继研制成功全氘代聚苯乙烯（D-PS）有机材料、微靶掺杂和激光吸收与X射线转换金属纳米或团簇材料;探索了新型有机气凝胶储氢材料,开展了金属小团簇理论研究和纳米金属复合材料的研究工作。在靶制备技术与工艺方面,完成了PS单层、双层和三层塑料空心微球的研制工作;利用低温等离子体聚合涂层技术,建立了微球表面沉积纯CH薄膜以及金属掺杂CH薄膜的工艺和技术;在玻璃微球充氩技术研究中,开展了原子力扫描显微镜对玻璃球壳钻孔工艺研究以及粒子辐照改性充气技术研究,等等。     

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。     

碳氢烧蚀层的厚度对聚乙烯醇薄膜阻气性能的影响

 以ICF实验塑料靶丸保气的需求为背景，研究了水蒸气在低压等离子体聚合碳氢（CH）膜、聚乙烯醇（PVA）膜、聚苯乙烯（PS）膜中的扩散渗透行为。根据实验数据，算出在40℃ 90%相对湿度下,水蒸气在三种样品膜中的渗透系数分别为1.906×10^-13，5.950×10^-15，.432×10 ^-14mol·m/(m²·s·Pa)，并借助多层复合膜模型的近似算法，算出在40 ℃ 90%相对湿度的外界环境下，类似多层塑料微球结构的三层复合膜中，PVA阻气层所处环境的相对湿度为53.06%，推导出PVA所处环境的相对湿度与外层CH层厚度的关系式。研究表明：CH烧蚀层越厚，PVA所处环境的相对湿度越小，保气性能越好。     

空心微球气体总量抽样测量误差分析

 间接驱动内爆靶丸由外层CH涂层，内层玻璃球壳和内部充入的气体组成。当玻璃球外涂CH后，球内的气体只能抽检而没有无损测量方法。在大量实验和数据基础上，研究了液滴法制备空心玻璃微球气体渗透系数的差异和分布，利用数理统计方法对实验数据进行了分析和处理，计算了空心玻璃微球对氘气渗透系数的误差，微球预充气挑选方案产生的误差及分布。最后根据现在的抽样测量方案计算了误判的概率。     

Synthesis of Fe3O4 hollow microsphere chains and their magnetic properties

Fe₃O₄ hollow microsphere chains with lengths of 8–11 μm have been solvothermally synthesized in the mixed solution of glycerol and water with 1 M NaOH. The hollow microspheres have diameters in the range 0.7–1 μm, and the thickness of the shells is 150–300 nm. The shell of the hollow microspheres is constructed by octahedrons of 100–170 nm. However, when the concentration of NaOH is adjusted to 3 M, the octahedron chains with lengths of 30–50 μm can be obtained. The magnetic saturation values of hollow microsphere chains and octahedron chains are 88.1 and 102.4 emu/g at room temperature, respectively.     

Uniform Fe3O4–PANi/PS composite spheres with conductive and magnetic properties and their hollow spheres

Core–shell multifunctional composite spheres consisting of Fe₃O₄–polyaniline (PANi) shell and polystyrene (PS) core were fabricated using core–shell-structured sulfonated PS spheres (with uniform diameter of 250 nm) as templates. PANi was doped in situ by sulfonic acid resulting the composite spheres are well conductive. Dissolved with solvent, PS cores were removed from the core–shell composite spheres and hollow Fe₃O₄–PANi spheres were obtained. Removing the PANi and PS components by calcinations produced hollow Fe₃O₄ spheres. The cavity size of the hollow spheres was uniformly approximate to 190 nm and the shell thickness was 30 nm. The cavity size and the shell thickness can be synchronously controlled by varying the sulfonation time of the PS templates. The shell thickness in size range was of 20–86 nm when the sulfonation time was changed from 1 to 4 h. These resulting spheres could be arranged in order by self-assembly of the templates. Both the Fe₃O₄–PANi/PS composite spheres and the hollow Fe₃O₄ spheres exhibit a super-paramagnetic behavior. Scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, and X-ray powder scattering were used to characterize these as-prepared spheres. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

掺钛空心玻璃微球制备技术

为实现惯性约束聚变靶用空心玻璃微球的均匀掺杂,采用溶胶-凝胶技术结合炉内成球法,以钛酸四丁酯为掺杂剂,对钛掺杂玻璃溶胶-钛掺杂玻璃凝胶-钛掺杂干凝胶粒子-钛掺杂空心玻璃微球（Ti-HGM）这一掺钛空心玻璃微球的制备方法进行了探索。实验结果表明:掺钛效应使空心玻璃微球壁厚均匀性、同心度有所降低,但对壁厚、直径控制基本无影响;Ti与Si原子分数比为2.23%的Ti-HGM掺杂基本均匀,近70%微球的保气半寿命在一个月以上。     

Synthesis and characterization of hard magnetic composites—Hollow microsphere/titania/barium ferrite

Hard magnetic composites—hollow microsphere (core)/titania (intermediate layer)/barium ferrite (magnetic shell) (M/T/B) were prepared by wet-chemical method. Barium ferrite nanoparticles were directly coated on the rutile titania-coated hollow microsphere forming light hard magnetic composites using sol-gel technique. The prepared composites were characterized with FESEM, EDS, XRD and vibrating sample magnetometry. The composites are composed of barium ferrite, hematite, titania and mullite. For the samples with 40 wt.% barium ferrite, its specific saturation magnetization with titania is increased to 17.88 emu/g in comparison with 9.6 emu/g without titania. The function of titania in the composites is also discussed.     

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.