新型真空定向凝固装置的研制

采用双区加热技术，成功地研制了一台新型真空定向凝固装置，其主要性能指标为：温度梯度ＤＬ＝２５０℃／ｃｍ，最高温度１７００℃抽拉速度Ｒ＝０．１￣６０ｍｍ／ｍｉｎ，炉内真空度为０．１ｐａ（热态），定向材料最大尺寸为φ４０×３５０ｍｍ，可满足研制稀土超磁致伸缩Ｔｂ－Ｄｙ－Ｆｅ合金的要求。     

冶金法提纯工业硅的研究

以冶金级硅为原料进行了制备高纯多晶硅锭的研究,自行设计了真空感应熔炼与定向凝固设备、电子束熔炼设备.通过酸洗、真空感应熔炼与第一次定向凝固、电子束熔炼、真空感应熔炼与第二次定向凝固等组合步骤对工业硅进行提纯.利用电感耦合等离子体发射光谱仪(ICP-AES)进行成分分析,实验结果表明,定向凝固有效去除了金属杂质,电子束对蒸汽压高的元素,尤其是磷元素的去除作用明显.Al的浓度降低到了0.4×10~(-6),Fe、Ca、Ti、Mn、Cu、Zn等金属杂质的浓度降到了0.1×10~(-6)以下,P含量降低到1.5×10~(-6).     

Nb基超高温合金制备及定向凝固用坩埚的选择

目前Nb基超高温合金的制备主要是通过多次电孤熔炼得到成分均匀的铸锭.其定向凝固或者是在水冷铜坩埚内采用Czochralski技术进行,或者是采用不需要坩埚的悬浮区熔法实现,但这两种方法都不能得到较高的温度梯度.为了获得更好的定向凝固组织,需要在超高温超高真空定向凝固设备上进行有坩埚的整体定向凝固.结合国内外共晶自生复合材料常用的制备技术,提出了适用于铌基超高温合金整体定向凝固技术的坩埚材料及其涂层技术.     

定向凝固结合电子束制备高纯铜的研究

对定向凝固结合电子束制备5N高纯铜进行了研究。首先采用真空感应熔炼4N(99.99%)阴极铜并进行定向凝固实验,然后利用电子束对定向凝固后的铸锭进行重熔精炼,利用辉光放电质谱仪进行成分分析。实验结果表明:真空熔炼可以有效去除铜中饱和蒸气压高的杂质;通过定向凝固,杂质元素含量沿铸锭轴向逐渐升高;经过组合工艺提纯后,总杂质含量由13.6×10-6降低至4.0×10-6,铜的纯度提高至99.9996%。     

凝固速度对DZ22合金组织与性能的影响

近十多年来,用定向凝固工艺来制造涡轮叶片,已得到发动机设计者和冶金材料工作者的充分肯定,越来越多的发动机应用了定向凝固涡轮叶片和导向叶片,可以说定向凝固是继真空熔炼——精密铸造后的又一个成功。     

多晶硅真空定向凝固系统的仿真优化与实验研究

采用模拟和实验相结合的方法,研究了真空定向凝固系统中炉内底部保温层结构对多晶硅温度场及凝固过程中固-液界面的影响,对比了底部保温层为开口、半封闭与全封闭3种情况下的温度分布及凝固情况。模拟的结果表明,在底部保温层全封闭时,热区的辐射加热效果加强,同时也增加了冷区的散热效果,使坩埚中的硅料温度梯度增大。在此基础上,建立了不需要进行坩埚底部水冷换热的凝固系统,并进行了实验。实验结果与理论分析基本一致,说明可以通过调节炉内装置来优化多晶硅的真空定向凝固系统,对该系统的设计和优化起到指导与参考作用。     

电子束真空精炼直接定向凝固制备高纯铜的研究

以电子束真空熔炼直接定向凝固技术制备5N高纯铜大铸锭为研究目标,利用电子束熔炼原材料,熔体直接定向凝固后得到高纯铜铸锭.采用GDMS-VG9000辉光放电质谱仪和TCH600氧氢分析仪研究了金属杂质及氧氢元素的去除效果,通过EPMA-1600电子探针研究了提纯后元素的分布情况.结果表明:真空电子束熔炼直接定向凝固技术可将原料为4N(99.9988711％)的电解阴极铜板,制备出纯度5N(99.9997235％)、Φ59 mm大尺寸高纯铜铸锭,杂质元素总量降低了75.506％,中间凝固组织为单晶;五种含量较高的元素Ag、Cu、O、P和S均匀分布,没有出现杂质的偏聚现象;与原材料相比,0、H元素分别降低了86.47％,85.00％.研究表明真空电子束精炼直接定向凝固技术能够制备氧氢含量较低的5N大尺寸高纯铜铸锭.     

用冷坩埚真空感应熔炼设备制备稀土合金的技术

用冷坩埚真空感应熔炼技术制备稀土合金，消除了坩埚材料对炉料的污染，为产品获得理想的成分均匀性和准确性，提高获得率提供了条件。本文介绍了冷坩埚真空感应熔炼技术，以及在此基础上发展的搅拌合金液、翻转合金锭及组合模具铸造、压力铸造和离心铸造的方法，以及在铸造过程中直接进行定向凝固的方法。     

真空感应熔炼和定向凝固制备多晶硅中铝的除杂

用真空感应熔炼和定向凝固法制备多晶硅,通过成分测定和理论计算研究了铝杂质的除杂机理。结果表明,在真空熔炼保温阶段(T≥1723 K),硅中的铝杂质明显蒸发;在随后的定向凝固过程中,铝杂质的分凝偏析是主要的,但仍有部分铝蒸发。建立了一个包括铝分凝和蒸发机制的新模型,模拟铝在硅中的分布曲线。模拟结果与铝在硅中的实际分布符合得很好。     

Nb基超高温合金的制备技术及定向凝固组织

Nb基超高温合金的制备技术主要包括粉末冶金、真空电弧熔炼和定向凝固等，其中定向凝固可以显著提高该合金的高低温力学性能。Nb基超高温合金的定向凝固组织主要由沿着定向凝固方向生长的初生Nbss枝晶、铌硅化物块或板条以及（Nbss＋铌硅化物）共晶等组成，定向凝固速率和固液界面前沿液相中的温度梯度会显著影响其组织形貌及尺寸。在其定向生长过程中，Nbss、铌硅化物及（Nbss＋铌硅化物）共晶各相之间竞争生长，形成不同的组织形貌及尺寸，但在合适的条件下，共晶两相可以实现平行耦合生长。     

深过冷熔体激发快速定向凝固

阐述了深过冷的方法，深过冷的遗传性，深过冷度的理论极限以及深过冷熔体激发发快速定向凝固的试验方法及其凝固过程，给出了深过冷熔体（Ｃｕ－５ｗｔ％）激发快速定向凝固与铸态试验激发快速定向凝固的初步试验结果。     

A model for distribution of aluminum in silicon refined by vacuum directional solidification

We propose a simple numerical model for distribution of Aluminum (Al) in silicon ingot during vacuum directional solidification, including segregation from silicon crystal to silicon melt as well as evaporation from silicon melt to vacuum atmosphere. According to the model, the effective segregation K_eff and the total evaporation coefficient k_T(Al)of Al under the experimental conditions are 0.0137 and 2.6755 × 10⁻⁶ m·s⁻¹, respectively. In comparison with experimental results, the segregation of Al is dominated at the beginning of solidification, whereas at the last stage of solidification the removal of Al is mainly depended on the evaporation. It is also found that the critical influences on aluminum removal during vacuum directional solidification are temperature and solidification rate.     

Effect of boron and zirconium on directional solidification behaviour and segregation of DS IN738 superalloy

The effect of boron and zirconium on the directional solidification behaviour and segregation of IN738 superalloy has been studied. It was found that additions of boron and zirconium enlarge the solidus-liquidus temperature interval and increase the amount of residual melt during solidification. Boron gives the alloy a tendency to form developed dendrites, while zirconium enhances a cellular solidified structure. Both boron and zirconium are shown to be rejected to the residual melt during solidification, and shown to change the segregation of alloying elements by interaction.     

Microstructure Formation in Al-Bi-Co Immiscible Alloys Directionally Solidified with Different Melt Superheat Temperatures

The directional solidification has been carried out for the Al-4Bi-2.5Co (wt pct) alloys with different melt superheat temperatures. The microstructure characterization and the quantitative metallographic analysis have been performed. The results indicated that the Bi-rich sphere size and cellular spacing decrease with increasing melt superheat temperature. The interaction between the advancing solidification interface and the Bi-rich spheres with different sizes was analyzed. The effect of the melt superheat treatment on microstructure evolution was discussed for the immiscible alloys. The microstructure development in ternary Al-Bi-Co alloys directionally solidified with different melt superheat temperatures was clarified.     

多晶硅真空电磁感应熔炼除磷及其过程研制

磷是多晶硅中的主要杂质元素之一,目前采用的酸洗以及定向凝固工艺无法将其含量降低到太阳能级多晶硅所要求的范围之内。采用自行设计的真空电磁感应熔炼炉及定向凝固炉研究了真空度、精炼时间和精炼温度对除磷效果的影响。研究结果表明当炉内压强为5.0×10-1 Pa时,精炼温度和时间分别为1723K和60min时,精炼后硅中磷含量由原来的2.0×10-5（质量分数）降低到1.8×10-6（质量分数）;研究推导出了在压强为5×10-1Pa下磷的含量随精炼时间和精炼温度的关系式如下：XP=X0Pexp[（-1.43×10-4-3.1×10-7T）t]同时还对真空感应熔炼除磷过程进行了热力学与动力学分析。     

高温合金定向凝固技术研究进展

首先回顾了定向凝固的发展历史,重点分析了液态金属冷却定向凝固的技术特点。总结了高温度梯度下制备的定向凝固法单晶高温合金在组织和性能方面的研究现状,结合作者在本领域的研究,着重分析了定向凝固温度梯度、凝固速率、晶体取向、熔体超温处理、熔体对流控制对组织和性能的作用规律和机制,认为高温度梯度定向凝固是细化组织、减少缺陷、提高合金性能的重要途径。最后展望了高温合金定向凝固的发展趋势。     

The size effect on solidification in eutectic bismuth-tin (Bi-Sn) nanowires by in-situ annealing processes

The size effects on solidification and the formation mechanism of the segmented eutectic Bi-43Sn nanowires during in situ annealing have been investigated. A directional solidification along the wire axis limits the segmented eutectic nanowire to arrange axially during the in situ annealing processes due to directional solidification. In 70 nm nanowires, the small size confines the convection in liquid, which results in differences in the microstructure and composition profiles between 70 and 200 nm nanowires. In the vacuum hydraulic pressure injection process, the directional cooling helps the formation of single crystal, and the isotropic solidification leads to polycrystalline microstructure.     

The solidification characteristics of near rapid and supercooling directional solidification

In the comparison of the solidification characteristics of supercooling directional solidification (SDS) with constrained directional solidification (DS) and with the consideration of the inheritance of supercooled melt, the SDS technique established with the combination of melt supercooling and traditional DS was proposed. An exploring study on SDS techniques was also conducted using appropriate facilities, designed and manufactured by the authors’ laboratory and the deep supercooling of Cu–5.0%Ni alloy, and its DSs were implemented.     

The solidification characteristics of near rapid and supercooling directional solidification

In the comparison of the solidification characteristics of supercooling directional solidification (SDS) with constrained directional solidification (DS) and with the consideration of the inheritance of supercooled melt, the SDS technique established with the combination of melt supercooling and traditional DS was proposed. An exploring study on SDS techniques was also conducted using appropriate facilities, designed and manufactured by the authors’ laboratory and the deep supercooling of Cu–5.0%Ni alloy, and its DSs were implemented.