传热过程对多晶硅真空定向凝固过程的凝固界面及热应力的影响

以实验室10 t/a VODS型多晶炉为原型,对其凝固过程的热场、固液界面和热应力进行了瞬态模拟与实验验证。结果表明:在坩埚底部有水冷热交换块的真空定向凝固系统中硅料凝固会产生较大的热应力,增加环形保温结构使热区封闭后可改变炉内换热过程,从而改变硅料凝固情况;硅料在坩埚底部为石墨热交换块的系统中凝固时产生的热应力相对较小,但固液界面的形状会发生较大的改变,影响晶粒的生长。炉膛内径适当变宽有利于炉内热区温度分布更合理,使得硅料凝固时的固液界面更加理想。通过实验验证了多晶硅在坩埚底部无需进行水冷换热情况下进行真空定向凝固能达到冶金法生产太阳能级多晶硅的要求,这为提高冶金法制备太阳能级多晶硅质量、降低系统能耗具有一定的指导意义。     

定向凝固DZ4125柱晶高温合金晶粒生长过程组织演化及其竞争生长研究

采用Bridgman定向凝固方法制备DZ4125柱晶高温合金定向试棒,研究在恒定抽拉速率下定向晶粒生长过程微观组织演化及晶粒间竞争生长行为。结果表明,随着生长高度的增加,固液界面处温度梯度逐渐降低,一次枝晶间距增加。同时,γ′相尺寸随着生长高度的增加逐渐减小,且γ′相形貌由不规则的蝴蝶状向立方体状、近圆状转变。γ+γ′共晶组织和碳化物大多分布在枝晶间区域,且含量随着生长高度的增加逐渐增加。此外,由于定向凝固过程中晶粒的竞争生长,随着生长高度的增加柱状晶数量明显减少;在具有凸固液界面生长条件下晶粒表现为向近炉壁侧倾斜发散生长。     

Tb0．27Dy0．73Fe1．95合金定向凝固时的固液界面形貌与择优取向

在自制的超高温度梯度定向凝固装置中,通过对Tb0.27Dy0.73Fe1.95合金定向凝固条件和固液界面形貌及晶体生长取向间的关系进行分析,发现Tb0.27Dy0.73Fe1.95合金定向凝固时发生胞枝转变的的凝固条件为GL/V值介于9.60×102K.s/mm2～10.45×102K·s/mm2之间.固液界面形貌与晶体取向间有明显的对应关系,固液界面形貌为胞状晶或无侧向分枝的树枝晶时其择优取向为〈110〉,结晶形貌为树枝晶时其择优生长方向为〈112〉,而在胞-枝转变区晶体为〈110〉,〈112〉,〈113〉等多种取向的混合.当Tb0.27Dy0.73Fe1.95合金以较低的晶体生长速率定向凝固时易产生〈110〉择优生长方向,并且产生〈110〉择优生长方向时的晶体生长速率范围随温度梯度的增加而扩大.     

生长速率对NiAl-7.8Mo亚共晶合金定向凝固组织及界面形态的影响

采用高温度梯度定向凝固装置制备了NiAl-7.8Mo亚共晶合金,系统研究了生长速率对合金凝固时界面形态、枝晶生长及初生相析出的影响。随生长速率的增大,固液界面依次呈现平、胞枝、枝的形貌转变,初生β相的一次枝晶间距λ1在胞晶生长阶段逐渐增大,而在枝晶生长阶段λ1又逐渐减小;二次枝晶间距λ2随生长速率的增加一直减小。初生β相的析出量随生长速率的增加而增加。分析结果表明:生长速率增加导致熔体过冷度增加,使得NiAl初生相形核率增加,最终导致初生β相的析出量随生长速率的增加而增加。     

生长速率对NiAl-7.8Mo亚共晶合金定向凝固组织及界面形态的影响

采用高温度梯度定向凝固装置制备了NiAl-7.8Mo亚共晶合金,系统研究了生长速率对合金凝固时界面形态、枝晶生长及初生相析出的影响.随生长速率的增大,固液界面依次呈现平、胞枝、枝的形貌转变,初生β相的一次枝晶间距λ1在胞晶生长阶段逐渐增大,而在枝晶生长阶段λ1又逐渐减小;二次枝晶间距λ2随生长速率的增加一直减小.初生β相的析出量随生长速率的增加而增加.分析结果表明:生长速率增加导致熔体过冷度增加,使得NiAl初生相形核率增加,最终导致初生β相的析出量随生长速率的增加而增加.     

定向凝固Al-Mn-Be合金初生金属间化合物相生长行为及力学性能

对Al-3Mn-7Be合金(原子分数,%)在1~1500 mm/s的抽拉速率下进行定向凝固实验,研究了抽拉速率对合金组织演化、金属间化合物形貌演变和合金力学性能等的影响规律。结果表明,Be元素的加入使二元相图向高Mn区移动,引入了金属间化合物l相、T相、Be4Al Mn和准晶I相,而且Be的加入明显细化了合金的组织。随着抽拉速率的增加,固/液界面过冷度和溶质过饱和度增加,引起初生金属间化合物相的竞争生长,初生相先由λ相转变为T相,后转变为准晶I相,伴随着形成初生Be_4AlMn相。同时,初生相的形貌、尺寸和生长方式也随抽拉速率的增加而发生改变。随着抽拉速率的增加,定向凝固合金的强度先下降后提高,在抽拉速率较低和较高时,定向凝固合金均呈现了较大延伸率,这主要由其定向凝固组织、强化相的种类、形貌以及与基体构成的界面结构决定。     

定向凝固高Nb含量TiAl合金微观组织演化与溶质偏析规律

在Bridγman定向凝固炉中对Ti-46Al-(8,9,10)Nb合金进行定向凝固实验,研究了生长速率和Nb含量对Ti Al-Nb合金的微观组织、相变路径以及溶质偏析的影响,获得了定向凝固Ti Al-Nb合金相变过程与微观组织选择图.结果表明,生长速率的增加使得固/液界面发生了平界面-胞状界面-枝晶界面转变,并促进完全b相凝固转变为具有L+β→α包晶反应凝固过程,最终组织由α2/γ层片组织转变为具有a2/γ层片和B2相的多相组织.溶质Nb的添加对b相具有稳定作用,促进了完全b相凝固过程的发生以及α2/γ层片和B2相多相组织的形成.生长速率和Nb含量对相变过程和微观组织的影响与溶质偏析(S型偏析,β型偏析)过程密切相关.其中S型偏析程度的提高有利于促进包晶反应的发生,从而导致最终组织发生严重的溶质偏析以及大量B2相在枝晶心部的集中分布.bβ型偏析中溶质Nb在残余β相中的富集是形成B2相的主要来源,Nb的富集程度直接决定了B2相的形态和尺寸.根据关于生长速率和Nb含量的Ti-46Al合金相变过程和微观组织选择图可知,选择较高的Nb含量和较低的冷却速率能获得完全β相凝固过程,可以得到组织分布均匀、溶质偏析程度较低的定向凝固组织.     

高温合金电磁成形定向凝固柱状晶组织及形成条件

研究高温合金电磁成形定向凝固柱状晶组织及其形成条件的结果表明,①电磁成形中熔体下固/液界面处温度场近一维分布,获得了柱状晶组织;②电磁成形高温合金样件具有间断迹象的定向胞晶组织;③给定其他条件后,电磁成形过程中不同形状、尺寸的样件熔体平直固液界面开始出现下凹的临界凝固速率具有不同的特定值。在相同凝固速率条件下,大尺寸样件的固液界面更容易出现下凹。     

抽拉速率对Ti-47Al-3Nb-0.3Si定向凝固组织的影响

采用电阻加热定向凝固炉对Ti-47Al-3Nb-0.3Si合金在抽拉速率为5、15、50、100 μm/s下进行定向凝固试验,并观察和分析不同抽拉速率下的固液界面形貌、过渡区和定向生长区凝固组织.结果表明,抽拉速率为5 μm/s时,固/液界面以胞状界面向前推进,抽拉速率在15～100 μm/s时,固/液界面以树枝状向前推进,且随着抽拉速率的增大,一次枝晶间距减小.当抽拉速率为5～50 μm/s时,片层组织与生长方向夹角为45°,当抽拉速率增加到100μm/s时,片层组织与生长方向基本垂直.利用扫描电镜背散射观察定向生长区形貌发现,抽拉速率等于或大于15 μm/s时,在柱状晶内部或晶界处形成胞状Al偏析,且出现共晶γ相及Ti5(Si,Al)3相.     

加热器位置对多晶硅定向凝固热场的影响

运用有限元软件COMSOL Multiphysics 4.3a对多晶硅定向凝固过程进行了全局瞬态模拟,在多晶硅铸锭炉顶部加热器与侧部加热器的垂直距离分别为60、150、300 mm时,分析了其对多晶硅熔化以及结晶初期的影响。结果表明:距离为60 mm时硅料熔化所需时间最长,而距离为150、300 mm时硅料熔化时间与其相比分别少34、60 min;对于结晶初期的固液界面,距离为60 mm时固液界面接近于平面,有利于多晶硅晶体生长,而距离为150、300 mm时固液界面均呈现明显的凸形,并且后者比前者凸起的程度更大,会降低多晶硅锭的质量。     

铸造多晶硅中氧的热处理行为研究

研究了铸造多晶硅中不同温度单步退火下氧沉淀的形成规律。实验发现，单步热处理工艺下铸造多晶硅中氧沉淀的形成规律和单晶硅的基本相似，但是在铸造多晶硅中形成氧沉淀的量明显高于直拉单晶硅中氧沉淀的量；在含高密度位错的单晶硅中形成氧沉淀的量远高于无位错单晶硅中氧沉淀的生成量，而有晶界的多晶硅中形成氧沉淀生成量仅稍微高于无晶界单晶硅中氧沉淀生成量。以上结果表明，铸造多晶硅中位错对氧沉淀的形成有明显的促进作用，而晶界则对氧沉淀的促进作用不是很显著。最后，基于实验结果讨论了铸造多晶硅中初始氧浓度，位错和晶界对氧沉淀影响的机理。     

Numerical simulation on directional solidification of Al-Ni-Co alloy based on FEM

The ratio,of the temperature gradient at the solidifiationfront to the solidification rate of solid-liquid interface,plays a large part in columnar grain growth.The transient temperature fields of directional solidification of Al-Ni-Co alloy were studied by employing a finite element method.The temperature gradient at the solidification front and the solidification rate were analyzed for molten steels pouring at different temperatures.The results show that with different initial pouring temperatures,the individual ratio of the temperature gradient at solidification front to the solidification rate soars up in the initial stage of solidification,then varies within 2,000-6,000℃.s.cm-2,and finally goes down rapidly and even tend to be closed to each other when the solidification thickness reaches 5-6 cm.The simulation result is consistent with the practical production which can provide an available reference for process optimization of directional solidified Al-Ni-Co alloy.     

Electron-beam-induced current study of small-angle grain boundaries in multicrystalline silicon

Recombination activity of small-angle grain boundaries (SA GBs) in multicrystalline silicon (mc-Si) was studied by means of electron-beam-induced current (EBIC) technique. In the as-grown mc-Si, the EBIC contrasts of special Σ and random GBs were weak at both 300 and 100 K, whereas those of SA GBs were weak (<3%) at 300 K and strong (30–40%) at 100 K. In the contaminated mc-Si, SA GBs showed stronger EBIC contrast than Σ and R GBs at 300 K. It is indicated that SA GBs possess high density of shallow levels and are easily contaminated with Fe compared to other GBs.     

Continuous melting and directional solidification of silicon ingot with an electromagnetic cold crucible

In order to avoid contamination from the crucible and to modify the structures,a new solidification method based on cold crucible technology was used to prepare silicon ingots.A silicon ingot with square cross section was directionally solidified with a cold crucible.The mechanism of the cold crucible directional solidification of silicon ingot was revealed.Due to the induction heat that was released in the surface layer and the incomplete contact between the crucible and the melt,the lateral heat loss was reduced and the silicon ingot was directionally solidified.The structures,dislocation defects and the grain growth orientation of the ingot were determined.The results show that neither intergranular nor intragranular precipitates are found in the ingot,except for the top part that was the last to solidify.The average dislocation density is about 1 to 2×106 cm-2.The grains are preferentially <220> orientated.     

高温度梯度下Al-In偏晶合金定向凝固组织的演化规律

应用高温度梯度的方法，研究了在定向凝固条件下温度梯度与凝固速率的比值G／R对Al-17．5％In(质量分数)合金凝固组织的影响．结果表明，偏晶合金的定向凝固与共晶合金定向凝固的生长规律类似．在高温度梯度下，仅在很低的生长速度时才能形成二相有序排列的共生．在偏晶合金定向凝固进入稳态生长以后，在各自的相凝固前沿富集了另一相的溶质，由于两相的层间距不大，长大过程中的横向扩散占主导地位．随着生长速度的增大或温度梯度的降低，Al-17．5％In合金定向凝固组织从纤维结构到周期性或规则排列的串状结构再到弥散分布结构转变．这种转变与固一’液界面形状的转变有密切关系．     

混合方式对受控扩散凝固过共晶Al-Si合金初生硅相的影响

采用受控扩散凝固技术(CDS)制备Al-15％Si(质量分数)合金,研究混合方式对受控扩散凝固Al- 15％Si合金初生硅相尺寸、形貌和分布的影响.结果表明:受控扩散凝固可以明显细化初生硅相,改善初生硅相形貌和在组织中的分布.其中,液-液混合细化效果比固-液混合细化效果好,特别是通过液态纯铝与液态Al-25％Si合金的液-液混合受控扩散凝固制备得到的凝固组织,其初生硅相平均尺寸仅为14μm,且在组织中分布均匀.     

Small-angle subgrain boundaries emanating from dislocation pile-ups in multicrystalline silicon studied with synchrotron white-beam X-ray topography

The formation of dislocation pile-ups and related small-angle subgrain boundaries in block-cast multicrystalline silicon for photovoltaic applications has been studied by means of white-beam X-ray topography (WB-XRT). For this purpose, samples sliced perpendicular and parallel to the growth direction have been investigated in reflection and transmission geometry, respectively. During the growth process of the silicon ingot, the dislocation density increases. WB-XRT measurements revealed the formation of small-angle subgrain boundaries. The subgrains have a slightly changed orientation related to a rotation of ～0.07–0.80° around an axis parallel to the growth direction. This tilt results from the high number of dislocations forming dislocation pile-ups and walls. The spacings between dislocations in such subgrain boundaries were found to be between 297 and 28 nm. A qualitative model for the formation of dislocation pile-ups is proposed.     

Simulation of the Influence of Pulsed Magnetic Field on the Superalloy Melt with the Solid-Liquid Interface in Directional Solidification

The effect of the pulsed magnetic field on the grain refinement of superalloy K4169 has been studied in directional solidification. In the presence of the solid-liquid interface condition, the distributions of the electromagnetic force, flow field, temperature field, and Joule heat in front of the solid-liquid interface in directional solidification with the pulsed magnetic field are simulated. The calculation results show that the largest electromagnetic force in the melt appears near the solid-liquid interface, and the electromagnetic force is distributed in a gradient. There are intensive electromagnetic vibrations in front of the solid-liquid interface. The forced melt convection is mainly concentrated in front of the solid-liquid interface, accompanied by a larger flow velocity. The simulation results indicate that the grain refinement is attributed to that the electromagnetic vibration and forced convection increase the nucleation rate and the probability of dendrite fragments survival, for making dendrite easily fragmented, homogenizing the melt temperature, and increasing the undercooling in front of the solid-liquid interface.     

Optimization of deformation parameters of dynamic recrystallization for 7055 aluminum alloy by cellular automaton

In order to simulate the microstructure evolution during hot compressive deformation, models of dynamic recrystallization (DRX) by cellular automaton (CA) method for 7055 aluminum alloy were established. The hot compression tests were conducted to obtain material constants, and models of dislocation density, nucleation rate and recrystallized grain growth were fitted by least square method. The effects of strain, strain rate, deformation temperature and initial grain size on microstructure variation were studied. The results show that the DRX plays a vital role in grain refinement in hot deformation. Large strain, high temperature and small strain rate are beneficial to grain refinement. The stable size of recrystallized grain is not concerned with initial grain size, but depends on strain rate and temperature. Kinetic characteristic of DRX process was analyzed. By comparison of simulated and experimental flow stress–strain curves and metallographs, it is found that the established CA models can accurately predict the microstructure evolution of 7055 aluminum alloy during hot compressive deformation.     

Effect of strontium and solidification rate on eutectic grain structure in an AI-13 wt% Si alloy

The influence of strontium addition and solidification rate on eutectic grain structure in a near-eutectic AI-Si alloy was investigated. The characteristic temperature of eutectic nucleation (TN),minimum temperature prior to recalescence (TM),and the growth temperature (TG) during cooling were determined by quantitative thermal analysis. All characteristic temperatures were found to decrease continuously with increasing Sr content and solidification rate. Microstructural analysis also revealed that the eutectic grain size decreases with increasing Sr content and solidification rate. Such eutectic grain refinement is attributed to the increased actual under-cooling ahead of the liquid/solid interface during solidification.