Effect of particle size on the preparation and microwave absorption properties of FeSiAl magnetically soft alloy hollow microspheres

FeSiAl magnetically soft alloy hollow microspheres(MSAHMs) were prepared by self-reactive quenching technology based on Fe + Si + AI + KNO_3 reactive systems, in order to obtain absorbents with light weight, low frequency and high efficiency. Firstly, twice-balling adhesive precursor method was used to obtain FeSiAl magnetically soft alloy agglomerate powders. Then agglomerate powders with the mesh number of 150-240, 240-325 and 325-400 were sprayed through the flame field into the quenching water. At last, FeSiAl MSAHMs with coarse(average at 86.97 μm), medium(average at 52.16 μm) and fine particles(average at 31.80 μm) were got. Effect of particle size on the phases and microwave absorption properties in low frequency band was studied by XRD and vector network analyzer. The results show that,Fe_3 Si_(0.7)Al_(0.3) and Fe_3 Si_(0.5)Al_(0.5) appear in the phase components of FeSiAl MSAHMs,which is important to improve the microwave absorption properties in low frequency. In addition, the real part(ε′) and imaginary part(ε″) of complex permittivity, the real part(μ′) and imaginary part(μ″) of complex permeability of FeSiAl MSAHMs all present the trend of fine particles > medium particles > coarse particles. The microwave absorption properties in low frequency are improved with the increasing of particle size, and the absorption peak moves to lower frequency range. The properties of fine particles are the best. Their matching thickness of samples is at 5 mm, and the minimum reflectivity is-43 dB at this thickness. The absorption frequency band lower than-10 dB is 4.6-7.6 GHz with a bandwidth of 3 GHz.

STUDY ON PREPARATION OF UNIFORM POLYSTYRENE HOLLOW PARTICLES

Uniform polystyrene hollow particles were prepared successfully by employing SPG (Shirasu porous glass) emulsification technique. The oil phase composed of monomer [styrene (St) and N,N’-dimethylamino ethylmethacrylate (DMAEMA)], hexadecane (HD) and initiator was permeated through the uniform pores of SPG membrane into the aqueous phase (containing stabilizer, emulsifier and water-soluble inhibitor ) by a gas pressure to form uniform droplets. The droplets were then polymerized at 70℃. It was found that the hollow particles were obtained by adding a small amount of DMAEMA into the oil phase and by using NaNo2 as the water-soluble inhibitor, while only one-hole particles were obtained without adding DMAEMA, or when using diaminophenylene (DAP) or hydroquinone (HQ) as the inhibitor. The formation mechanism was discussed by the view of interfacial tensions between polymer and aqueous phase, HD and aqueous phase, and HD and polymer. Further more, it was found that hollow particles can be obtained even when DMAEMA content in the oil phase was very low, by increasing HD to high value.

Template Polymerization-solvent Extraction: A New Method for Fabrication of Hollow Polysiloxane Particles

Hollow polysiloxane particles with diameters between 1.40 and 1.60 micrometres were fabricated by consecutive cocondensation of methyltrimethoxysilane and diphenyldimethoxysilane monomers onto polydiphenylsiloxane, subsequently removing the templated polydiphenylsiloxane by exposure to solvents. TEM and AFM measurement reveal that there are obvious hollow sphere structures for the polysiloxane microsphere particles. The hollow spheres are envisioned to have applications in areas ranging from dye-industry, catalysis, pharmaceutics to materials science.

PREPARATION OF HOLLOW LATEX PARTICLES BY ALKALI-ACID TREATMENT

Hollow polymer latex particles were prepared by seeded emulsion polymerization. A seed latex consisting of styrene (St), butyl acrylate(BA) copolymer was first prepared, and seeded terpolymerization of St BA MA(methacrylic acid) were then carried out in the absence of surfactant. Final latex was treated by a two step treatment under alkaline and acidic conditions, thus, the particles with hollow structure were obtained. We discussed the effects of pH value, temperature and time in alkali and acid treatment processes on hollow structure within the polymer latex particles and amount of carboxylic group on particle surface. The results show that the hollow polymer latex particles with the largest hollow size can be obtained under a certain condition (pH12.5, 90°C, 3 h in alkali treatment stage and pH2.5, 85°C, 3 h in acid treatment stage).

Preparation of Porous Silicone Resin Sheet with Phase Inversion in Parallel with Non Solvent Induced Phase Separation and Application to Hollow Particle Formation

We have tried to prepare the porous silicone resin sheet with the phase inversion method in parallel with the non solvent induced phase separation method. In the experiment, ethyl acetate and water were adopted as a good solvent and a poor solvent for silicone resin, respectively and ethyl alcohol as an amphiphilic solvent was used to increase the solubility of ethyl acetate in water and decrease the interfacial tension by mass transfer from water to ethyl acetate. The concentration of silicone resin in ethyl acetate and the oil soluble surfactant species were changed. Increasing the concentration of silicone resin could depress coalescence between the water droplets in the (W/O) dispersion and increase the porosity and pore number density of silicone resin sheet. Span 80 among the oil soluble surfactant species made the porosity and pore number density larger. The effect of physical proparties of liquids concerned on the porosity and pore number density was discussed on the basis of dispersing behavior of liquid droplets in the liquid-liquid dispersion. The hollow silicone resin particles could be prepared by applying the preparation method presented here.

Effect of stirring on preparation of hollow copolymer particles by alkali/cooling method

Hollow particles were prepared by the treatment of styrene-methacrylic acid copolymer particles with alkali/cooling method. The influences of stirring position (in aqueous phase or at the interface of O/W) and stirring speed (90, 110 and 240 r/min) on the formation of hollow particles were investigated. It is found that the soft stirring in aqueous phase at 90 r/min leads to the formation of monohollow particles, while the violent stirring at the interface of O/W and 240 r/min gives non-hollow products. In contrast, the weak stirring in aqueous phase at 110 r/min results in sterically heterogeneous dispersion of methacrylic acid-rich regions within the original particles, and hence the formation of multihollow particles. Further investigation indicates that the change of stirring efficiency provides a way to tune the diffusion behavior of monomer styrene, and therefore influences the distribution of methacrylic acid units in the original particles as well as the morphology of the treated particles.

SYNTHESIS OF BOWL-LIKE PARTICLES BY EMULSION POLYMERIZATION AND RELEASE BEHAVIOR OF SOLVENT FROM THE PARTICLES

Poly(styrene-glycidyl methacrylate) particles having bowl-shaped hollow structures were synthesized by swollen seed emulsion polymerization. The PS emulsion synthesized through soap-free emulsion polymerization was swollen by toluene, and then the mixture of second monomers was added under polymerization condition. So a thin shell of poly(styrene-glycidyl methacrylate) cross-linked by triethylene glycol diacrylate was formed around the swollen PS particle. The bowl-shaped particles were obtained after the collapsing of the thin shell when the toluene emanated from the particles, but the shapes were effected by the degrees of cross-linking. The shape of the particles was observed by SEM. The release behavior of solvent from the particles was examined by TG.

气体雾化过程中涉及颗粒形貌和空心颗粒形成的金属液滴变形和破碎数值模拟

采用考虑液滴冷却和凝固的流体体积(VOF)方法模拟金属液滴在气体雾化过程中的变形和破碎。建立典型粉末形貌和液滴破碎行为之间的相关性,以指导球形粉末颗粒的制备。结果显示,当增加液滴的气动力与黏性力的比值时,球形颗粒的形成得到加强;然而,当减小这个比值时,预期的液滴破碎模型将被改变或仅仅只发生液滴的变形。从空心颗粒的形成和演变过程的数值模拟中观察到几种典型的情况,例如,开放的空心液膜的形成、液膜封闭、气泡的离心和气泡的脱离。通过提高气体速度或液滴温度,实现较高的非平衡拉普拉斯压力或较低的粘性力,促使气泡从液滴内部分离。

Dissolved metal ion removal by online hollow fiber ultrafiltration for enhanced size characterization of metal-containing nanoparticles with single-particle ICP-MS

Single particle-inductively coupled plasma mass spectrometry (SP-ICP-MS) is a powerful tool for size-characterization of metal-containing nanoparticles (MCNs) at environmentally relevant concentrations,however,coexisting dissolved metal ions greatly interfere with the accuracy of particle size analysis.The purpose of this study is to develop an online technique that couples hollow fiber ultrafiltration (HFUF) with SP-ICP-MS to improve the accuracy and size detection limit of MCNs by removing metal ions from suspensions of MCNs.Through systematic optimization of conditions including the type and concentration of surfactant and complexing agent,carrier pH,and ion cleaning time,HFUF completely removes metal ions but retains the MCNs in suspension.The optimal conditions include using a mixture of 0.05 vol.%FL-70 and 0.5 mmol/L Na2S2O_(3)(pH=8.0) as the carrier and 4 min as the ion cleaning time.At these conditions,HFUF-SP-ICP-MS accurately determines the sizes of MCNs,and the results agree with the size distribution determined by transmission electron microscopy,even when metal ions also are present in the sample.In addition,reducing the ionic background through HFUF also lowers the particle size detection limit with SP-ICP-MS (e.g.,from 28.3 to 14.2 nm for gold nanoparticles).This size-based ion-removal principle provided by HFUF is suitable for both cations (e.g.,Ag+) and anions (e.g.,AuCl_(4)^(-)) and thus has good versatility compared to ion exchange purification and promising prospects for the removal of salts and macromolecules before single particle analysis.

中空三维结构的硅碳负极的构筑及性能研究

硅碳材料作为高能量密度的锂电负极材料备受瞩目,但由于硅在充放电过程中巨大的体积膨胀效应,导致了其循环性能差,限制了其商业化应用。本工作利用薄层石墨柔性结构的特点,与纳米硅进行复合制备了中空结构的硅碳复合物,并通过对薄层石墨和纳米硅分别用含有羧基的羧甲基纤维素(CMC)和含有氨基的正硅酸乙酯(TEOS)进行表面修饰。相比于传统的机械混合工艺制备的硅碳负极材料存在纳米硅与碳材料复合不均一的问题,本工作修饰后的纳米硅与薄层石墨之间通过静电自组装作用,可形成更为均一的纳米硅与薄层石墨的复合物(S/MG)。通过造粒技术,构筑了由纳米硅/薄层石墨片层组成的中空结构的硅碳复合物颗粒,而颗粒外部由碳层进行包覆。通过SEM切片、EDS以及高分辨TEM等表征手段,可以看到颗粒内部由纳米硅与薄层石墨层结构构筑了微米尺寸的中空结构,该结构内部不但形成了导电的三维网络结构,而且为纳米硅的体积膨胀提供了充足的缓冲空间,从而大幅提升了硅碳负极材料循环稳定性。相比于传统石墨取代薄层石墨与纳米硅制备的硅碳复合物,薄层石墨制备的硅碳负极的比容量达到958 mAh/g,扣电在0.5 C下循环500次后容量保持率可维持在88%左右。本文作者也从实用角度评价了S/MG全电循环性能,与三元NCM811正极材料组装成的软包全电池,在1 C倍率充放电下,循环1000周后电池容量保持率可达86%,可为高能量密度锂电技术的研究提供实验依据。

Silver Hollow Microspheres: Large-scale Synthesis, Characterization and Electromagnetic Shielding Property

A facile and large-scale synthesis method to fabricate silver hollow microspheres with controllable morphologies and shell thickness is described using low-cost glass microspheres as templates. The method mainly involves two steps of the preparation of silver-coated glass microsphere core–shell particles by a controllable liquid reduced reaction of Ag[（NH3）2]＋ solution, which only produces silver nanoparticles anchored on the surface of the thiolated glass microsphere templates, and the removal of glass microspheres by wet chemical etching with HF solution. The products are well characterized by field emitted scanning electron microscopy （SEM）, transmitted electron microscopy （TEM）, X-ray photoelectron spectra （XPS）, X-ray diffraction （XRD） and energy dispersive X-ray （EDX） etc. The as-prepared core-shell particles and hollow particles have even and compact silver shells. The electromagnetic shielding coatings based on the silver hollow microspheres are demonstrated to have high conductivity, excellent shielding effectiveness and long durability, suggesting that the silver hollow microspheres obtained here are a novel light-weight electromagnetic shielding filler and will have extensive applications in the electromagnetic compatibility fields.

Preparation and Performance of Hollow Spherical Li4Ti5O12 Doped by Mg^2+

The microstructure and performance of Li4Ti5O12 doped by Mg prepared by hydrothermal method and solid phase method were investigated. Lithium dihydrate, magnesium acetate and tetrabutyl titanate were used as the main raw materials. This study reveals that Mg^2+ has influences on the spherical structure, crystal development of Li4Ti5O12 and the electrochemical performances. The hollow spherical structure is composed of nano-sheet structure and the nano-sheet structure can be affected by the Mg^2+ content. For Li4-xMgxTi5 O12, the sheet structure can be refined with the increment of Mg^2+ content when x value is 0-0.1 and coarsen with the increment of Mg^2+ content when x value is 0.1-0.2. The hollow spherical Li4Ti5O12 powders prepared by hydrothermal method have better performance. The optimal Mgdoped amount of hydrothermal method is 0.1. At 0.1 C, the first discharge capacity of Li3.9Mg0.1Ti5O12 prepared through hydrothermal method at 0.1 C and 10 cycles is 182 and 178 mA hg^-1, respectively.

Size Effect on the Radiation Stability Silicon Dioxide Sphere Particles

The effect of protons(E = 100 keV,F = 5×10^(15) cm^(-2)) exposure on the diffuse reflectance spectra of the SiO_(2 )with different size particles in wavelength range from 250 to 2500 nm have been investigated.Particles were nanosphere,submicrosphere,microsphere and submacrosphere,as well as solid micro-and nanocrystals.The synthesis of the particles was carried out by the formation of silica shells and dissolution of the polystyrene core particles.The surface morphology,surface area and crystal structure of the particles have been investigated.When evaluating the changes of the solar absorptance,it was found that the radiation stability of the micro-and submacro-hollow particles is higher than that of the other nanostructured particles,except for solid microcrystals.The low radiation stability of the hollow microparticles is due to the large void inside the hollow particles where radiation defects are not formed.

Quantitative analysis of deformation in hollow cylinder tests on anisotropic clay formations

A series of triaxial laboratory experiments are performed on thick-walled hollow cylindrical samples of boom clay.The aim of this testing program is to better understand the anisotropic deformation during the excavation.The testing conditions are similar to those to be experienced by host rocks around disposal galleries for radioactive waste.X-ray computed tomography is performed at different steps for each test with the samples remaining inside the loading cell.Initial analysis of the tomography images allows of the observation of the deformation of the central hole.In addition,particles manual tracking and 3D volumetric digital image correlation processing methods are considered being used to analyze the particles displacements and the boundary deformation of the sample quantitatively.An unsymmetrical damaged zone is induced around the hole,with a reverse deformation trend being found at the boundary after unloading,which indicates that the significant anisotropic deformation of boom clay can be induced by mechanical unloading.

Cylindrical Micro-hollow Cathode Discharge at Atmospheric Pressure

The mechanism of micro-hollow cathode discharge at atmospheric pressure is investigated through simulations using two-dimensional fluid model combined with a transport model for metastable atoms.In the simulations,electric potential,electric field,particle density,and mean electron energy of the discharge are calculated.The results show that the two characteristic regions of the discharge,i.e.cathode drop and negative glow can be distinguished in the simulation.The cathode drop is characterized by strong electric field and high mean electron energy,while quasi-neutral plasma of high density and exists in the negative glow.The peak value of electron density can reach the order of 1017cm-3.The electron temperature varies from several eV to tens of eV.The influence of cathode dimension on the discharge characteristics is also investigated.

聚合物中空微球的合成策略

在过去的20年中,聚合物中空微球由于其独特的结构和优异的性质受到了广泛的关注.它们表现出低密度、高比表面积和高负载力的特性,在催化、药物递送及能量存储等领域中展现出巨大的应用前景.本文综合评述了聚合物中空微球的合成策略,主要包括模板法、乳液聚合法、自组装与及微流控等,并详细阐述和讨论了这些合成策略的原理、典型过程以及优缺点.同时,还指出了现有合成策略面临的挑战以及聚合物中空微球存在的不足,并对聚合物中空微球的制备和应用前景进行了展望.

钴蓝基纳米球形粒子(SiO_(2)-CoAl_(2)O_(4))的制备条件及电泳性能研究

通过牺牲模板法,以Ps@SiO_(2)核壳结构粒子作为模板,成功制备了具有中空结构的SiO_(2)-CoAl_(2)O_(4)蓝色电泳粒子;研究了改性剂3-氨丙基三乙氧基硅烷、醇水比对Ps@SiO_(2)粒子形貌的影响;对升温速度、Co/Al比对蓝色中空电泳粒子的影响进行研究,当升温速度为1℃/min、Co/Al=0.8∶2时所制备粒子呈亮蓝色、结构完整,将所制备的蓝色粒子与带正电白色粒子进行复配后进行电泳显示测试,在20 V/mm的电场强度下,显示器件的响应速度在280 ms以内。

Characterization and photocatalytic properties of silver and silver chloride doped TiO_2 hollow nanoparticles

Using polystyrene （PSt） particles as template, PSt/TiO2 composite particles with AgCl incorporation were prepared through hydrolysis of tetrabutyl titanate in the presence of AgNO3 and NaCl. AgCl doped TiO2 hollow particles were successfully prepared with the PSt/TiO2 composite microspheres pretreated at 180 ℃ followed by calcination. The morphology of PSt/TiO2 particles and the crystal structures of the AgCl doped TiO2 hollow particles were characterized. The photocatalytic activity of the doped TiO2 hollow particles in degradation of Rhodamine B was tested under UV and visible lights and compared to that with Ag doped TiO2 particles. The results showed that TiO2 hollow particles, either doped with Ag or AgCl, demonstrated higher photocatalytic activity than the pure TiO2 particles. This enhancement in photocatalytic activity was more significant with AgCl doped TiO2 than that with Ag doped, and more distinct when the degradation was done under visible light than that under UV light.

某火电厂粉煤灰空心微珠的精细化分级及物化性质规律探究

为了获得高含量的空心微珠产品,针对采用传统选矿方法选别粉煤灰空心微珠效果较差的问题,采用自制重力沉降分级装置,通过湿式筛分—重力沉降分级工艺对某火电厂粉煤灰进行了分级试验。试验结果表明:原灰空心微珠含量37.68%,湿式筛分可对空心微珠起到一定的富集作用,-13μm、+13-23μm、+23μm产物的空心微珠含量分别为42.99%,12.51%,3.28%,重力沉降使空心微珠得到了进一步富集,最终产物的空心微珠含量为20.57%~78.43%,实现了空心微珠的有效分离。物化性质测试结果表明:随着筛分粒级的减小,CaO、TiO_(2)、Fe_(2)O_(3)含量升高,SiO_(2)含量降低;S3-H1至S3-H5的CaO、TiO_(2)、Fe_(2)O_(3)含量升高,Na_(2)O、SiO_(2)含量和硅铝比下降;空心微珠的粒度与硅铝比、SiO_(2)和Na_(2)O含量负相关,与CaO、TiO_(2)和Fe_(2)O_(3)含量正相关。