多晶硅表面金属催化化学腐蚀法制绒研究现状

在多晶硅太阳能电池的生产过程中, 金刚线切割技术(Diamond wire sawn, DWS)具有切割速度快、精度高、原材料损耗少等优点, 受到了广泛关注。金刚线切割多晶硅表面形成的损伤层较浅, 与传统的酸腐蚀制绒技术无法匹配, 金属催化化学腐蚀法应运而生。金属催化化学腐蚀法制绒具有操作简单、结构可控且易形成高深宽比的绒面等优点, 具有广阔的应用前景。本文总结了不同类型的金属催化剂在制绒过程中的腐蚀机理及其形成的绒面结构, 深入分析和讨论了具有代表性的银、铜的单一及复合催化腐蚀过程及绒面结构和电池片性能。最后对金刚线切割多晶硅片表面的金属催化化学腐蚀法存在的问题进行了分析, 并展望了未来的研究方向。     

Investigation on thermal conductivity and mechanical properties of Si3N4 ceramics via one-step sintering

High thermal conductivity Si₃N₄ ceramics were fabricated using a one-step method consisting of reaction-bonded Si₃N₄ (RBSN) and post-sintering. The influence of Si content on nitridation rate, β/(α+β) phase rate, thermal conductivity and mechanical properties was investigated in this work. It is of special interest to note that the thermal conductivity showed a tendency to increase first and then decrease with increasing Si content. This experimental result shows that the optimal thermal conductivity and fracture toughness were obtained to be 66 W (m K)^-1 and 12.0 MPa m^1/2, respectively. As a comparison, the nitridation rate and β/(α+β) phase rate in a static pressure nitriding system, i.e., 97% (MS10), 97% (MS15), 97% (MS20) and 8.3% (MS10), 8.3% (MS15), 8.9% (MS20), respectively, have obvious advantages over those in a flowing nitriding system, i.e., 91% (MS10), 91% (MS15), 93% (MS20) and 3.1% (MS10), 3.3% (MS15), 3.3% (MS20), respectively. Moreover, high lattice integrity of the β-Si₃N₄ phase was observed, which can effectively confine O atoms into the β-Si₃N₄ lattice using MgO as a sintering additive. This result indicates that one-step sintering can provide a new route to prepare Si₃N₄ ceramics with a good combination of thermal conductivity and mechanical properties.     

Novel silicon-contained lignin-based carbon fibers derived from bamboo pulping black liquor with improved electrochemical performance for supercapacitors

Carbon fibers (CFs) are a promising candidate as electrode materials for flexible supercapacitors given its light weight and moderate cost. In this study, the lignin used was partially separated from kraft bamboo pulping black liquor and the higher molecular weight fraction, unavoidably contains a small amount of silicon compounds, so named silicon-contained lignin. Novel CFs were prepared using commercial polyacrylonitrile (PAN) and the lignin by electrospinning and further carbonization. Even in the presence of silicon compounds, the fibrous morphology of precursor fibers was significantly good, and the CFs with uniform fiber diameter and high specific surface area up to 182 m²/g were obtained with an increase in silicon-contained lignin. The CFs fabricated from silicon-contained lignin and commercial PAN had higher specific capacitance (22.20 mF/cm² at 10 mA/cm²) and superb cycling stability (94.21%) than that from silicon-free lignin or pure PAN separately.     

Fabrication,microstructural characterization and gas permeability behavior of porous silicon nitride ceramics with controllable pore structures

Porous Si₃N₄ ceramics with monomodal and bimodal pore structure were prepared by cold isostatic pressing and freeze-casting, respectively. Both the pore structure and permeability behavior of the porous Si₃N₄ ceramics were tailored by altering the pressure of cold isostatic pressing and the composition and content of solvent during freeze-casting. The specimens obtained by cold isostatic pressing exhibited smaller Darcian and non-Darcian permeability than those of freeze-casted samples due to their lower open porosity, smaller pore size and higher tortuosity. On the other hand, compared with the ice-templated specimens having the same solvent volume in the ceramic slurries as them during freeze-casting, the emulsion-ice templated samples showed smaller open porosity, macropore size and Dacian permeability, but the similar non-Darcian permeability because of their larger micropores and better pore interconnectivity.     

Synthetic fayalite Fe2SiO4 by kinetically controlled reaction between hematite and silicon carbide

The present work explores the preparation of fayalite α-Fe₂SiO₄, the iron-rich end-member of the olivine solid-solution series, as a tar removal catalyst for biomass gasification. The synthetic procedure was developed starting from the stoichiometric mixture of hematite and micrometer size silicon carbide and employing thermal treatments in controlled atmospheres at 1000-1100°C supported by thermodynamic modeling to assess the required redox conditions. The treatments in dry and humidified inert gas yielded phase mixtures containing metallic Fe as one of the main phases, thus emphasizing a shortage of oxygen supply. XRD and TGA studies of precursor mixtures on heating in dry CO₂ demonstrated a multistep mechanism of the overall reaction including (a) fast reactivity between silicon carbide and hematite at ~920°C with formation of metallic Fe and amorphous silica followed by (b) formation of fayalite involving oxygen supplied in the form of CO₂ and competing with (c) over-oxidation to thermodynamically favorable Fe₃O₄+SiO₂ mixture. Comparative studies of reactivity in powdered and pelletized samples emphasized the importance of the kinetic factor in the formation of Fe₂SiO₄ while preventing further oxidation. The preferential formation of fayalite in the CO₂ atmosphere is shown to be favored by shorter treatments of compacted samples at higher temperatures. The procedure was designed (2-step heating to 1100°C in CO₂ followed by fast cooling) for the preparation of pelletized fayalite α-Fe₂SiO₄ catalyst with only minor traces of surface over-oxidation which can be suppressed by adding 10 vol.% of forming gas to CO₂ flow.     

单晶硅表层机械力学特性的各向异性分析

为探究挠性筋结构单晶硅材料的各向异性特性以及KOH腐蚀工艺对其力学性能的影响规律,进行纳米压痕实验,并结合原子力显微镜观察单晶硅表层3个主晶面上压痕裂纹形貌随晶向的变化规律,分析单晶硅材料表层弹性模量、硬度、断裂韧性等机械力学特性参数在(001)、(110)及(111)3个主要晶面上沿各个晶向的变化规律;分析挠性筋结构单晶硅材料(001)晶面的KOH腐蚀工艺对其材料表面机械特性的影响规律.结果表明:挠性筋单晶硅在(001)晶面上弹性模量的各向异性变化幅度明显,硬度及断裂韧性各向异性的变化幅度不大;挠性筋单晶硅在(110)晶面弹性模量和断裂韧性的各向异性变化幅度明显,硬度各向异性变化幅度不大;挠性筋单晶硅在(111)晶面硬度值、弹性模量及断裂韧性参数的变化幅度幅值均较小;确定了单晶硅表层3个晶面裂纹最易扩展的晶向方向,KOH腐蚀工艺使得单晶硅表面质量降低,腐蚀后暴露的表面微裂纹、缺陷等会使得单晶硅(001)晶面表层硬度、断裂韧性降低,从而降低了挠性筋结构的实际断裂强度.     

Ultrathin Dual‐Scale Nano‐ and Microporous Membranes for Vascular Transmigration Models

Selective cellular transmigration across the microvascular endothelium regulates innate and adaptive immune responses, stem cell localization, and cancer cell metastasis. Integration of traditional microporous membranes into microfluidic vascular models permits the rapid assay of transmigration events but suffers from poor reproduction of the cell permeable basement membrane. Current microporous membranes in these systems have large nonporous regions between micropores that inhibit cell communication and nutrient exchange on the basolateral surface reducing their physiological relevance. Here, the use of 100 nm thick continuously nanoporous silicon nitride membranes as a base substrate for lithographic fabrication of 3 µm pores is presented, resulting in a highly porous (≈30%), dual‐scale nano‐ and microporous membrane for use in an improved vascular transmigration model. Ultrathin membranes are patterned using a precision laser writer for cost‐effective, rapid micropore design iterations. The optically transparent dual‐scale membranes enable complete observation of leukocyte egress across a variety of pore densities. A maximal density of ≈14 micropores per cell is discovered beyond which cell–substrate interactions are compromised giving rise to endothelial cell losses under flow. Addition of a subluminal extracellular matrix rescues cell adhesion, allowing for the creation of shear‐primed endothelial barrier models on nearly 30% continuously porous substrates.     

电感耦合等离子质谱法检测保健食品中的硅

目的建立电感耦合等离子体质谱法检测保健食品中硅含量的分析方法。方法将保健食品类试样进行灰化,加入氢氧化钠形成共熔体,将共熔体与水混合,得到溶解液,采用电感耦合等离子体质谱法对溶解液进行硅含量检测。通过加标回收率和国家标准物质的分析实验验证该方法的准确性和可靠性。结果实验标准曲线的线性范围在0.0～10.0μg/mL,回归方程的相关系数达到1.0000。方法的检出限为0.050 mg/L,标准物质加标回收率在96.4%～103.3%,精密度小于2.5%;国家标准物质柑橘叶和紫菜测定值均在标准值允许的范围内。结论该方法具有快速、批量、灵敏度高的特点,适用于保健食品中硅含量的测定。     

304不锈钢不同精炼渣碱度下夹杂物的演变

 为了提高304不锈钢的产品质量，结合生产实际，利用热力学计算和扫描电镜能谱分析方法, 研究了硅脱氧条件下，LF精炼渣碱度对304不锈钢在LF精炼、连铸过程夹杂物变化规律的影响。试验结果表明,随着冶炼过程进行，全氧质量分数和夹杂物数量依次减小。304不锈钢采用1.75高碱度炉渣，可以得到较低的全氧质量分数和夹杂物数量，但是夹杂物中Al2O3质量分数高，夹杂物熔点高。采用1.53低碱度炉渣，钢液中全氧质量分数较采用高碱度炉渣高，但是夹杂物中CaO、Al2O3质量分数相对较低，SiO2和MnO质量分数较高，夹杂物熔点低。针对304不锈钢产品可以采用不同的生产工艺路线来满足产品的不同需求。     

粉煤灰提铝残渣低温碱溶过程工艺研究

循环流化床粉煤灰“一步酸溶法”提取氧化铝工艺过程中产生的尾渣主要成分为无定形二氧化硅,且具有较高的活性,是制备白炭黑、分子筛、硅酸钠水玻璃的理想原料。对该提铝残渣在氢氧化钠溶液中的溶出过程做了研究,探讨了液固比、碱浓度、溶出时间、溶出温度工艺条件对二氧化硅和氧化铝溶出效果的影响。研究结果表明：在氢氧化钠碱液的浓度为4 mol/L、反应温度为70 ℃、液固比为6、反应时间为4 h的条件下,二氧化硅的溶出率最高,达到93%。提铝残渣碱溶后固体渣经XRD分析,其无定形二氧化硅基本已溶出,剩余物主要为锐钛矿与莫来石等。