Mg-Gd-Y-Zr合金净化熔剂研究
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摘要
稀土元素具有改善合金的铸造性能,细化合金组织,提高合金的力学性能及耐腐蚀性能等作用。上海交通大学轻合金国家工程中心现已开发出了一系列具有高强、耐热、耐蚀等性能的含稀土镁合金,如GW系列、NZK系列镁合金,大大拓展了镁合金的应用领域。当前,含稀土镁合金的净化问题已成为制约其推广应用的关键瓶颈之一,原因在于现有熔剂的主体成分MgCl2会与稀土元素发生反应,不仅导致昂贵稀土的大量损耗,而且影响合金成分与性能的稳定。而不含MgCl2的熔剂去除夹杂物的能力较差,净化效果不够理想。因此,开发稀土镁合金专用高效净化熔剂是一个亟待解决的关键问题。
本文针对新型高强耐热Mg-Gd-Y稀土镁合金的净化难题,开展了该合金专用净化熔剂的研究,并开发出了JDY和JDGd系列专用熔剂。借助力学性能试验机、光学显微镜(OM)、金相图像分析仪、带能谱分析(EDAX)的扫描电子显微镜(SEM)、X射线衍射仪(XRD)、电感耦合等离子直读光谱仪(ICP)、电化学测试系统等分析手段,研究了JDY和JDGd系列熔剂对GW103K稀土镁合金组织形貌、杂质含量、相组成、稀土元素损耗量、力学性能、耐腐蚀性能以及铸造流动性等的影响规律;采用差热分析仪(DTA)等分析手段研究了稀土氯化物添加剂对熔剂工艺性能与工作性能的影响规律。此外还分析了稀土元素损耗的机制。主要研究成果如下:
1)含有一定量的氯化稀土的新型熔剂,能够显著去除镁熔体中的非金属夹杂物,使总夹杂含量的体积分数从0.81%下降到0.33%;在总夹杂体积分数相同的情况下,使粒径尺寸大于10μm的夹杂物含量从26.49%下降到14.42%;但熔剂中氯化稀土量超过一定程度后(如含量超过8%),使用过程中熔剂易于结团难以分散,不仅降低了净化效果,而且会增加熔剂夹杂。
2)采用质量占合金质量2~3%的JDY系列熔剂净化处理后,合金中Y元素的损耗率随着熔剂中YCl3含量的增加而减小,且在熔剂中YCl3含量超过7.5%后,Y损耗率降低不再明显,基本维持在11.2%左右。相同条件下,采用JDGd系列熔剂净化处理后,合金中Gd的损耗率随着熔剂中GdCl3含量的增加而降低,且在熔剂中GdCl3含量超过7.5%后,损耗率降低不再明显,基本维持在4.4%左右。
3)经JDY和JDGd系列熔剂精炼后,由于合金中稀土元素损耗的降低以及合金中夹杂的减少,合金的力学性能、耐腐蚀性能和铸造流动性得到较大提高,当YCl3添加量达到2.5%时,合金试样的力学性能σb和δ分别达到最大值228.25MPa和5.26%,其试样腐蚀速率降低到最低的0.452mg·cm-2·d-1,而流动性(在金属模具温度是150℃的情况下浇注)试样的长度达到121cm;当GdCl3添加量达到2.5%时,合金试样的力学性能σb和δ分别达到最大值225.63MPa和5.12%,其试样腐蚀速率降低到最低的0.513mg·cm-2·d-1,而流动性试样的长度达到122cm;但是添加过多的YCl3/GdCl3 (如添加量超过熔剂质量的8%),易使熔剂聚结成团,不仅降低熔剂的铺展性,而且导致合金中出现熔剂夹杂,反而降低了力学性能、耐腐蚀性能及铸造流动性。
4)通过熔剂成分优化、物化性能测试以及熔剂制备及精炼工艺优化等试验,验证了新型熔剂JDRJ+ YCl3既能有效降低稀土损耗,又可以起到良好的净化效果,是一种优于现有的JDMJ和RJ-6的稀土镁合金专用净化熔剂。
Rare earth compounds are able to purify alloy melt, refine alloy structure, improve casting ability, mechanical properties, corrosion resistance and so on. A series of RE magnesium alloys with the high performance have been developed, such as GW series and NZK series, which is greatly helpful to expand magnesium application field.
However, RE magnesium alloy can not be purified by present fluxes, because rare earth can react with MgCl2 in the fluxes which lead to mass loss of rare earth compound, and the effect of the flux without MgCl2 can not reach the expected level. Therefore, new kinds of fluxes suitable for RE magnesium alloy refining need to be developed as soon as possible.
According to the purifying problems of the Mg-Gd-Y alloy, the present study researched on developing new fluxes JDY and JDGd. Also, the study has investigated the effects of the new fluxes JDY and JDGd on the impurity content, microstructure, phase, loss of RE compound, mechanical properties, corrosion resistance and casting fluidity of RE magnesium alloy GW103K by experimental methods such as inductively coupled plasma analyzer(ICP), optical microscopy(OM), image analysis apparatus with a Leco image analysis software, scanning electron microscopy(SEM) with energy dispersive X-ray analyses (EDAX), X-ray diffractometer (XRD), electrochemical measuring system.The main research results are as followed:
1) The new fluxes containing some chloridize rare earth can greatly remove the impurities, and reduce the content of impurities larger than 10μm from 26.49% to 14.42%. However, when the chloridize rare earth is excessive, the flux will be inclined to become conglomeration, which will lead to flux impurities in the alloy melt.
2) The Y losses of alloys which are purified by the new fluxes JDY decrease as the YCl3 content increases, when the addition of YCl3 is 7.5wt%, the loss of Y will keep steady in some 11.2wt%; The Gd losses of alloys which are purified by the new fluxes JDGd decreas as the GdCl3 content increases, when the addition of GdCl3 is 7.5wt%, the loss of Y will keep steady in some 4.4wt%.
3) After refined by the fluxes JDY和JDGd,mechanical properties, corrosion resistance and casting fluidity of RE magnesium alloy are improved greatly. When the addition of YCl3 is 2.5%, the alloy examples’mechanical propertiesσb andδreach to the highest 228.25MPa and 5.26%, and the corrosion rate decreases to the lowest 0.452mg·cm-2·d-1 , and the casting fluidity longth is the longest 121cm; When the addition of GdCl3 is 2.5%, the alloy examples’mechanical propertiesσb andδreach to the highest 225.63MPa and 5.12%, and the corrosion rate decreases to the lowest 0.513mg·cm-2·d-1 , and the casting fluidity longth is the longest 122cm.
4) According to the experiments of flux composition optimization, physical and chemical properties testing and refining draft optimization, the research results show that the new complex fluxes JDRJ+2.5%YCl3/GdCl3 can not only greatly reduce the loss of Y and Gd, but also purify the alloy melt effectively, which is better than the present fluxes RJ-6 and JDMJ.
本文针对新型高强耐热Mg-Gd-Y稀土镁合金的净化难题,开展了该合金专用净化熔剂的研究,并开发出了JDY和JDGd系列专用熔剂。借助力学性能试验机、光学显微镜(OM)、金相图像分析仪、带能谱分析(EDAX)的扫描电子显微镜(SEM)、X射线衍射仪(XRD)、电感耦合等离子直读光谱仪(ICP)、电化学测试系统等分析手段,研究了JDY和JDGd系列熔剂对GW103K稀土镁合金组织形貌、杂质含量、相组成、稀土元素损耗量、力学性能、耐腐蚀性能以及铸造流动性等的影响规律;采用差热分析仪(DTA)等分析手段研究了稀土氯化物添加剂对熔剂工艺性能与工作性能的影响规律。此外还分析了稀土元素损耗的机制。主要研究成果如下:
1)含有一定量的氯化稀土的新型熔剂,能够显著去除镁熔体中的非金属夹杂物,使总夹杂含量的体积分数从0.81%下降到0.33%;在总夹杂体积分数相同的情况下,使粒径尺寸大于10μm的夹杂物含量从26.49%下降到14.42%;但熔剂中氯化稀土量超过一定程度后(如含量超过8%),使用过程中熔剂易于结团难以分散,不仅降低了净化效果,而且会增加熔剂夹杂。
2)采用质量占合金质量2~3%的JDY系列熔剂净化处理后,合金中Y元素的损耗率随着熔剂中YCl3含量的增加而减小,且在熔剂中YCl3含量超过7.5%后,Y损耗率降低不再明显,基本维持在11.2%左右。相同条件下,采用JDGd系列熔剂净化处理后,合金中Gd的损耗率随着熔剂中GdCl3含量的增加而降低,且在熔剂中GdCl3含量超过7.5%后,损耗率降低不再明显,基本维持在4.4%左右。
3)经JDY和JDGd系列熔剂精炼后,由于合金中稀土元素损耗的降低以及合金中夹杂的减少,合金的力学性能、耐腐蚀性能和铸造流动性得到较大提高,当YCl3添加量达到2.5%时,合金试样的力学性能σb和δ分别达到最大值228.25MPa和5.26%,其试样腐蚀速率降低到最低的0.452mg·cm-2·d-1,而流动性(在金属模具温度是150℃的情况下浇注)试样的长度达到121cm;当GdCl3添加量达到2.5%时,合金试样的力学性能σb和δ分别达到最大值225.63MPa和5.12%,其试样腐蚀速率降低到最低的0.513mg·cm-2·d-1,而流动性试样的长度达到122cm;但是添加过多的YCl3/GdCl3 (如添加量超过熔剂质量的8%),易使熔剂聚结成团,不仅降低熔剂的铺展性,而且导致合金中出现熔剂夹杂,反而降低了力学性能、耐腐蚀性能及铸造流动性。
4)通过熔剂成分优化、物化性能测试以及熔剂制备及精炼工艺优化等试验,验证了新型熔剂JDRJ+ YCl3既能有效降低稀土损耗,又可以起到良好的净化效果,是一种优于现有的JDMJ和RJ-6的稀土镁合金专用净化熔剂。
Rare earth compounds are able to purify alloy melt, refine alloy structure, improve casting ability, mechanical properties, corrosion resistance and so on. A series of RE magnesium alloys with the high performance have been developed, such as GW series and NZK series, which is greatly helpful to expand magnesium application field.
However, RE magnesium alloy can not be purified by present fluxes, because rare earth can react with MgCl2 in the fluxes which lead to mass loss of rare earth compound, and the effect of the flux without MgCl2 can not reach the expected level. Therefore, new kinds of fluxes suitable for RE magnesium alloy refining need to be developed as soon as possible.
According to the purifying problems of the Mg-Gd-Y alloy, the present study researched on developing new fluxes JDY and JDGd. Also, the study has investigated the effects of the new fluxes JDY and JDGd on the impurity content, microstructure, phase, loss of RE compound, mechanical properties, corrosion resistance and casting fluidity of RE magnesium alloy GW103K by experimental methods such as inductively coupled plasma analyzer(ICP), optical microscopy(OM), image analysis apparatus with a Leco image analysis software, scanning electron microscopy(SEM) with energy dispersive X-ray analyses (EDAX), X-ray diffractometer (XRD), electrochemical measuring system.The main research results are as followed:
1) The new fluxes containing some chloridize rare earth can greatly remove the impurities, and reduce the content of impurities larger than 10μm from 26.49% to 14.42%. However, when the chloridize rare earth is excessive, the flux will be inclined to become conglomeration, which will lead to flux impurities in the alloy melt.
2) The Y losses of alloys which are purified by the new fluxes JDY decrease as the YCl3 content increases, when the addition of YCl3 is 7.5wt%, the loss of Y will keep steady in some 11.2wt%; The Gd losses of alloys which are purified by the new fluxes JDGd decreas as the GdCl3 content increases, when the addition of GdCl3 is 7.5wt%, the loss of Y will keep steady in some 4.4wt%.
3) After refined by the fluxes JDY和JDGd,mechanical properties, corrosion resistance and casting fluidity of RE magnesium alloy are improved greatly. When the addition of YCl3 is 2.5%, the alloy examples’mechanical propertiesσb andδreach to the highest 228.25MPa and 5.26%, and the corrosion rate decreases to the lowest 0.452mg·cm-2·d-1 , and the casting fluidity longth is the longest 121cm; When the addition of GdCl3 is 2.5%, the alloy examples’mechanical propertiesσb andδreach to the highest 225.63MPa and 5.12%, and the corrosion rate decreases to the lowest 0.513mg·cm-2·d-1 , and the casting fluidity longth is the longest 122cm.
4) According to the experiments of flux composition optimization, physical and chemical properties testing and refining draft optimization, the research results show that the new complex fluxes JDRJ+2.5%YCl3/GdCl3 can not only greatly reduce the loss of Y and Gd, but also purify the alloy melt effectively, which is better than the present fluxes RJ-6 and JDMJ.
引文
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