太阳能电池浆料用亚微米球形银粉的制备工艺研究

以抗坏血酸为还原剂,AgNO3为银盐,聚乙二醇4000(PEG-4000)为分散剂,采用液相还原法制备亚微米球形银粉。采用L9(33)正交试验设计,考察抗坏血酸浓度、分散剂加入方式以及溶液pH值对银粉粒度的影响。分析得出制备亚微米球形银粉的优化条件为:pH=5,AgNO3浓度为0.5 mol/L,AgNO3和抗坏血酸溶液中分别加入一半分散剂,抗坏血酸的浓度为0.9 mol/L,PEG-4000/AgNO3(质量比)为1.2,反应温度为室温。通过激光粒度仪、XRD及SEM表征,表明在较优实验条件下制备的亚微米级银粉纯净,粒度分布均匀,呈球状。并将优化条件下所得银粉调制成太阳能电池用浆料,通过丝网印刷在硅片上并烧结,烧结膜银栅线的表面方阻为0.721 m/□,可满足太阳能电池的电性能要求。     

明胶作分散剂制备球形超细银粉

采用化学还原法,以抗坏血酸为还原剂,明胶为分散剂制备了球形超细银粉。探讨了反应过程中AgNO3溶液浓度、反应液pH值、明胶用量、试剂滴加顺序等因素对银粉粒度大小及分布的影响。在pH为7时,将0.5 mol/L的AgNO3溶液加入到0.25 mol/L的抗坏血酸溶液中,明胶用量为AgNO3质量的1.5%,且在产生沉淀后逐滴加入能制备出大小1.5 μm左右,粒度分布均匀的球形超细银粉。     

微米球形银粉粒径的优化分析

采用化学还原法制备微米银粉且用正交试验对工艺进行了优化.以聚乙二醇(PEG- 10000)为分散剂和乙醇为消泡剂,以抗坏血酸在超声波下和碱性环境下直接还原硝酸银得到银溶胶,经过滤、洗涤、恒温干燥处理得到银粉.研究滴加顺序、消泡剂用量、pH值对银粉粒径的影响,利用SEM、XRD对银粉进行分析.结果表明,在0.3 mol/L硝酸银溶液和25 mL消泡剂乙醇、T=40℃和pH=7条件下,超声波振荡时间10 min,可制备粒径1.13 μm左右,粒径分布窄的球形银粉.     

纳米银溶胶的固液分离研究

以次磷酸钠液相还原法制备纳米银溶胶,通过添加试剂破坏银溶胶的稳定性,使银粒子产生聚沉或絮凝,分析了纳米银溶胶的稳定条件.考查了加入氨水的工艺条件对从银溶胶中过滤分离纳米银粉的影响,控制溶胶的pH范围可以得到不同粒度的纳米银.用有机碱性混合试剂可使溶胶中的银粒子絮凝,易于固液分离,干燥后的银粉经快速渗透剂T分散后,银粉的粒度小（10 nm～20 nm）、稳定性好.提供了从银溶胶中过滤纳米银粉的新方法,该方法工艺简单、对设备要求低、能耗小、银粉的收率高,易于实现工业化.试样经TEM分析发现,该法制备的纳米银粉粒度小（10nm～40 nm）,分散性好.XRD物相分析证实其为纯的金属银.     

以Ag-Cu合金触点废料制备超细铜粉和银粉

以Ag-Cu合金废触点制备CuCl2和AgCl,采用葡萄糖预还原-水合肼二次还原法制备超细铜粉、氨-肼还原法制备超细银粉。结果表明:在反应温度为70℃,加入适量PVP和苯并三氮唑作为分散剂和抗氧化剂的条件下,所得微米级铜粉的粒度在0.3～0.6μm,粒度分布范围小,纯度高于99.9%。经3个月的抗氧化试验表明,所得铜粉产品的抗氧化性能较高。一定时间的球磨是氨-肼还原法制备超细银粉的关键,经24h湿法球磨后干燥所得银粉的粒度为1.90μm,分布均匀。     

微米银粉的正交实验法制备与表征

研究了以抗坏血酸为还原剂的液相还原法制备球形微米银粉时的主要因素对振实密度和形貌的影响。实验表明,酸性条件下制备的微米银粉分散性较好。正交实验表明,对银粉振实密度的影响大小的因素依次为底液pH、硝酸银浓度、分散剂PVP用量和实验温度。经过对银粉进行粒度、SEM和XRD等测定表征发现,优化条件下可制备得到振实密度为4.2 g/cm~3,平均粒径2.5μm,分散性良好的类球形银粉。     

光伏电池正极银浆用球形银粉的制备

采用化学还原法制备光伏电池正极银浆用球形银粉,通过扫描电镜(SEM)和激光粒度仪表征了银粉的形貌和粒度,研究还原剂的种类、表面活性剂浓度以及反应时间等工艺条件对银粉粒度及形貌的影响。结果表明,采用抗坏血酸作还原剂、聚乙烯吡咯烷酮(PVP)作分散剂时,可以得到分散性好、粒度约为1.5μm的球状银粉。将该银粉制成浆料,印刷、烘干并烧结后,表征了电极形貌,用四探针电阻仪测得烧结银层的方阻5 m?/□,可满足太阳能电池的电性能要求。     

正交设计法优化高分散超细银粉的制备工艺

以AgNO3为银源,抗坏血酸为还原剂,通过液相还原法制备了超细银粉。运用L25(56)的正交试验设计,考察了AgNO3浓度、抗坏血酸浓度、分散剂种类、分散剂用量、溶液pH值及反应温度对超细银粉的分散性及粒度的影响。分析得出制备超细银粉的优化条件:AgNO3浓度为0.15mol.L-1,抗坏血酸浓度为0.40mol.L-1,油酸为分散剂,分散剂用量为8%(相对AgNO3质量),pH值为4,反应温度为50℃。在优化的实验条件下,制备出高分散近球形的超细银粉,其平均粒度为0.89μm。并运用SEM、XRD对其进行了表征。     

通孔柱银浆用超细银粉的制备研究

通孔银浆料是低温共烧陶瓷(LTCC)基板配套的系列电子浆料中必不可少的一种材料,对银粉有很高的要求。用抗坏血酸还原体系制备银粉,研究硝酸银溶液浓度、p H值、还原剂浓度对银粉形貌及粒度分布的影响,采用扫描电子显微镜对制备的银粉进行表征分析,选取3种不同类型的银粉调制成通孔银浆进行匹配性试验。结果表明,均一性、分散性良好且平均粒径为2.0μm的球形银粉具有较好的应用潜力。     

粒径可控高振实密度球银的制备工艺研究

以硝酸银为原料,对苯二酚(C6H4(OH)2)为还原剂,链烷醇胺A为分散剂,用液相化学还原法制备高振实密度超细银粉。用激光粒度分布仪测试银粉的粒度分布与平均粒径,用扫描电子显微镜(SEM)和透射电子显微镜(TEM)分析银粉的形貌、粒径和团聚状态,用多晶X射线衍射(XRD)仪检测粉体的晶相。结果表明：通过调节硝酸银的浓度、硝酸银与还原剂的配比以及分散剂的用量等,可以实现对所制备球银粒径的控制;制备的超细银粉为面心立方晶体结构,呈规则球形,振实密度可达4.0 g/cm3。     

Effects of Post-weld Heat Treatment on Microstructure,Mechanical Properties and the Role of Weld Reinforcement in 2219 Aluminum Alloy TIG-Welded Joints

In as-welded state, each region of 2219 aluminum alloy TIG-welded joint shows diff erent microstructure and microhardness due to the diff erent welding heat cycles and the resulting evolution of second phases. After the post-weld heat treatment, both the amount and the size of the eutectic structure or θ phases decreased. Correspondingly, both the Cu content in α-Al matrix and the microhardness increased to a similar level in each region of the joint, and the tensile strength of the entire joint was greatly improved. Post-weld heat treatment played the role of solid solution strengthening and aging strengthening. After the post-weld heat treatment, the weld performance became similar to other regions, but weld reinforcements lost their reinforcing eff ect on the weld and their existence was more of an adverse eff ect. The joint without weld reinforcements after the post-weld heat treatment had the optimal tensile properties, and the specimens randomly crack in the weld zone.     

The First Phase of the SRIF Industrialized Base in ＂West Area＂ Has Been Put into Operation

After nearly two years＇ tense construction, the first phase of industrialized base of Shenyang Research Institute of Foundry （SRIF）, located at the Tiexi Casting and Forging Industrial Park in the west of Tiexi District, has now been completed and formally put into operation.     

Thermodynamics Study on the Decomposition of Chromite with KOH

Institute of Process Engineering, Chinese Academy of Sciences, China, has proposed a method for oxidative leaching of chromite with potassium hydroxide. Understanding the mechanism of chromite decomposition, especially in the potassium hydroxide fusion, is important for the optimization of the operating parameters of the oxidative leaching process. A traditional thermodynamic method is proposed and the thermal decomposition and the reaction decomposition during the oxidative leaching of chromite with KOH and oxygen is discussed, which suggests that chromite is mainly destroyed by reactions with KOH and oxygen. Meanwhile, equilibrium of the main reactions of the above process was calculated at different temperatures and oxygen partial pressures. The stable zones of productions, namely, K2CrO4 and Fe2O3, increase with the decrease of temperature, which indicates that higher temperature is not beneficial to thermodynamic reactions. In addition, a comparison of the general alkali methods is carried out, and it is concluded that the KOH leaching process is thermodynamically superior to the conventional chromate production process.     

Influence of Heat Treatment on Damping Behaviour of the Magnesium Wrought Alloy AZ61

The effect of isochronal heat treatments for 1h on variation of damping, hardness and microstructural change of the magnesium wrought alloy AZ61 was investigated. Damping and hardness behaviour could be attributed to the evolution of precipitation process. The influence of precipitation on damping behaviour was explained in the framework of the dislocation string model of Granato and Lücke.     

Effect of Rare Earth Doping on Impedance,Modulus and Conductivity Properties of Multiferroic Composites:0.5(BiLa_xFe_(1-x)O_3)–0.5(PbTiO_3)

The Lanthanum-doped bismuth ferrite–lead titanate compositions of 0.5(Bi LaxFe1-xO3)–0.5(Pb Ti O3)(x = 0.05,0.10,0.15,0.20)(BLxF1-x-PT) were prepared by mixed oxide method.Structural characterization was performed by X-ray diffraction and shows a tetragonal structure at room temperature.The lattice parameter c/a ratio decreases with increasing of La(x = 0.05–0.20) concentration of the composites.The effect of charge carrier/ion hopping mechanism,conductivity,relaxation process and impedance parameters was studied using an impedance analyzer in a wide frequency range(102–106Hz) at different temperatures.The nature of Nyquist plot confirms the presence of bulk effects only,and non-Debye type of relaxation processes occurs in the composites.The electrical modulus exhibits an important role of the hopping mechanism in the electrical transport process of the materials.The ac conductivity and dc conductivity of the materials were studied,and the activation energy found to be 0.81,0.77,0.76 and 0.74 e V for all compositions of x = 0.05–0.20 at different temperatures(200–300 °C).     

Quantitative Analysis of the Crystallographic Orientation Relationship Between the Martensite and Austenite in Quenching–Partitioning–Tempering Steels

The orientation relationships(ORs)between the martensite and the retained austenite in low-and medium-carbon steels after quenching–partitioning–tempering process were studied in this work.The ORs in the studied steels are identified by selected-area electron diffraction(SAED)as either K–S or N–W ORs.Meanwhile,the ORs were also studied based on numerical fitting of electron backscatter diffraction data method suggested by Miyamoto.The simulated K–S and N–W ORs in the low-index directions generally do not well coincide with the experimental pole figure,which may be attributed to both the orientation spread from the ideal variant orientations and high symmetry of the low-index directions.However,the simulated results coincide well with experimental pole figures in the high-index directions{123}_(bcc).A modified method with simplicity based on Miyamoto’s work was proposed.The results indicate that the ORs determined by modified method are similar to those determined by Miyamoto’method,that is,the OR is near K–S OR for the low-carbon Q–P–T steel,and with the increase of carbon content,the OR is closer to N–W OR in medium-carbon Q–P–T steel.     

Using Finite Element and Contour Method to Evaluate Residual Stress in Thick Ti-6Al-4V Alloy Welded by Electron Beam Welding

This work was to reveal the residual stress profile in electron beam welded Ti-6Al-4V alloy plates(50 mm thick) by using finite element and contour measurement methods.A three-dimensional finite element model of 50-mmthick titanium component was proposed,in which a column–cone combined heat source model was used to simulate the temperature field and a thermo-elastic–plastic model to analyze residual stress in a weld joint based on ABAQUS software.Considering the uncertainty of welding simulation,the computation was calibrated by experimental data of contour measurement method.Both test and simulated results show that residual stresses on the surface and inside the weld zone are significantly different and present a narrow and large gradient feature in the weld joint.The peak tensile stress exceeds the yield strength of base materials inside weld,which are distinctly different from residual stress of the thin Ti-6Al-4V alloy plates presented in references before.     

Microstructures and Tensile Properties of Ultrafine-Grained Ni–(1–3.5) wt% SiC_(NP) Composites Prepared by a Powder Metallurgy Route

Silicon carbide nanoparticle-reinforced nickel-based composites(Ni–Si CNP),with a Si CNPcontent ranged from1 to 3.5 wt%,were prepared using mechanical alloying and spark plasma sintering.In addition,unreinforced pure nickel samples were also prepared for comparative purposes.To characterize the microstructural properties of both the unreinforced pure nickel and the Ni–Si CNPcomposites transmission electron microscopy(TEM) was used,while their mechanical behavior was investigated using the Vickers pyramid method for hardness measurements and a universal tensile testing machine for tensile tests.TEM results showed an array of dislocation lines decorated in the sintered pure nickel sample,whereas,for the Ni–Si CNPcomposites,the presence of nano-dispersed Si CNPand twinning crystals was observed.These homogeneously distributed Si CNPwere found located either within the matrix,between twins or on grain boundaries.For the Ni–Si CNPcomposites,coerced coarsening of the Si CNPassembly occurred with increasing Si CNPcontent.Furthermore,the grain sizes of the Ni–Si CNPcomposites were much finer than that of the unreinforced pure nickel,which was considered to be due to the composite ball milling process.In all cases,the Ni–Si CNPcomposites showed higher strengths and hardness values than the unreinforced pure nickel,likely due to a combination of dispersion strengthening(Orowan effects) and particle strengthening(Hall–Petch effects).For the Ni–Si CNPcomposites,the strength increased initially and then decreased as a function of Si CNPcontent,whereas their elongation percentages decreased linearly.Compared to all materials tested,the Ni–Si CNPcomposite containing 1.5% Si C was found more superior considering both their strength and plastic properties.     

Directional Growth of Tin Crystals Controlled by Combined Solute Concentration Gradient Field and Static Magnetic Field

A new method was introduced to achieve directional growth of Sn crystals. Microstructures in liquid(Pb)/liquid(Sn) diffusion couples were investigated under various static magnetic fields. Results show that the β-Sn crystals mainly reveal an irregular dendritic morphology without or with a relatively low static magnetic field(B0.3 T). When the magnetic field is increased to 0.5 T, the β-Sn dendrites close to the final stage of growth begin to show some directional character. With a further increase in the magnetic field to a higher level(0.8–5 T), the β-Sn dendrites have an enhanced directional growth character, but the dendrites show a certain deflection. As the magnetic field is increased to 12 T, the directional growth of the β-Sn dendrites in the center of the couple is severely destroyed. The mechanism of the directional growth of the β-Sn crystals and the deflection of the β-Sn crystals with the application of static magnetic field was tentatively discussed.     

Growth Kinetics of Single Inclusion Particle in Molten Melts

On the basis of the single-particle framework, a new theory on inclusion growth in metallurgical melts is developed to study the kinetics of inclusion growth on account of reaction and collision. The studies show that the early growth of inclusion depends on reaction growth and Brawnian motion collision, and where the former is decisive, the late growth depends on turbulence collision and Stokes＇ collision, and where the former is dominant; collision growth is very quick during the smelting process, lessened in the refining process, but nearly negligible in the continuous casting process.