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镍基高温合金差示扫描量热分析的影响因素研究:升降温速率和取样部位
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北京航空材料研究院,北京航空材料研究院,北京航空材料研究院,北京航空材料研究院,北京航空材料研究院,北京航空材料研究院,北京航空材料研究院

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TG132.3+2, TG115.25

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国家自然科学基金资助(项目号51304177),国家重点研发计划资助(项目号2016YFB0701404),国家科技支撑计划资助(项目号2015BAE03B01),重点实验室基金资助(项目号9140C430202150C43200)


The investigation of influence factors on differential scanning calorimetry (DSC) analysis of a Ni-base superalloy: heating/cooling rate and sampling position
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Science and Technology on Advanced High Temperature Structural Materials Laboratory,Beijing Institute of Aeronautical Materials,Science and Technology on Advanced High Temperature Structural Materials Laboratory,Beijing Institute of Aeronautical Materials,Science and Technology on Advanced High Temperature Structural Materials Laboratory,Beijing Institute of Aeronautical Materials,Science and Technology on Advanced High Temperature Structural Materials Laboratory,Beijing Institute of Aeronautical Materials,Science and Technology on Advanced High Temperature Structural Materials Laboratory,Beijing Institute of Aeronautical Materials,Science and Technology on Advanced High Temperature Structural Materials Laboratory,Beijing Institute of Aeronautical Materials,Science and Technology on Advanced High Temperature Structural Materials Laboratory,Beijing Institute of Aeronautical Materials

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    摘要:

    本研究对定向凝固DZ22镍基高温合金在5~40℃/min不同速率下进行升、降温差示扫描量热分析(DSC)试验,通过线性外推和取平均值的方法确定合金平衡态的相变温度。对不同取样部位的DZ22合金进行10℃/min下的升、降温DSC曲线的测定。结果表明,升、降温速率和取样部位均对DSC试验结果产生明显影响。(1)其中,DSC试验中的升温、降温速率对DZ22合金的相变温度测试结果包括液相线、MC碳化物、固相线、共晶γ′和次生γ′均产生明显影响,其中加热曲线随着升降温速率的升高向高温方向偏移,冷却曲线则向低温方向偏移,峰的高度随着升降温速率的升高而增大,但升温、降温曲线对应相变温度点平均值趋于一致,接近合金的平衡相变温度。采用升温、降温曲线外推法获得平衡态相变温度的方法存在一定的差异,而取升、降温曲线对应的相变温度平均值较为固定,是确定合金平衡相变温度是有效方法。DSC试验中不同升温和降温速率对相变温度结果的影响分别对高温合金热处理升温和凝固冷却过程中的实际工艺参数控制具有参考意义。(2)取样部位对DSC加热曲线低温段中的(γ+γ′)共晶和固相线温度产生明显影响,因显微偏析导致的组织差异导致同炉定向凝固试棒的底端和顶端的共晶(γ+γ′)和固相线温度分别相差17℃和20℃,而对曲线高温段的液相线和MC碳化物溶解温度影响不大;不同取样部位的合金加热完全熔化后组织趋于一致,再次凝固冷却过程中相变温度也趋于一致,因此DSC冷却曲线基本重合,取样部位对DSC冷却曲线无明显影响。对同一成分的高温合金而言,只有在取样部位的显微组织状态相近的情况下其DSC试验结果才具有比较意义。升降温速率和取样部位均会影响镍基高温合金DSC曲线中的相变温度结果,而以上因素在镍基高温合金热工艺参数的选择上应有所考虑。

    Abstract:

    The differential scanning calorimetry (DSC) experiments with different heating/cooling rates in the range of 5~40℃/min were performed on a directionally solidified (DS) Ni-base superalloy DZ22. The equilibrium transformation temperatures (zero-heating/cooling rate) of the alloy were obtained by linear extrapolating the different heating/cooling rates or averaging specific peak temperatures of both heating and cooling DSC curves. The DSC experiments with 10℃/min heating/cooling rate were carried out on samples cut from different position of DS testing bar. The results indicated that the heating/cooling rate and sampling position both had obvious effect on the values of phase transformation temperatures of DSC curves. (1) The heating and cooling rate had effect on the DSC results, including the phase transformation temperatures of liquidus, MC carbides, solidus, eutectic (γ+γ′) and secondary γ′. As the heating and cooling rate increased, the peak of transformation temperature on the heating DSC curve shifted to high temperature direction, whereas the cooling curve tended to deviate to lower temperature. The peak height increase accompanied by the heating/cooling rate increase. However, the average values of heating and cooling curves corresponding to the phase transformation temperature points are consistent. The equilibrium transformation temperatures of alloy acquired by linear extrapolating the different heating/cooling rates will result in some differences for the result, whereas to average specific peak temperature of both heating and cooling DSC curves is an effective method to determine the equilibrium phase transformation temperatures of superalloys. The influence of different heating and cooling rate on the phase transformation temperature results in DSC test has reference significance for the control of the actual process parameters in the process of heat treatment and solidification cooling of superalloy. (2) The sampling position had obvious effect on the eutectic (γ+γ′) dissolve and solidus temperatures of heating DSC curve in relative low temperature range, there is a 17℃ and 20℃ gap respectively for eutectic and solidus temperatures between samples cut from the top and bottom part of the same directionally solidified test bar due to the micro-segregation and microstructure difference. However, this difference is absent in liquidus and MC carbides dissolve temperatures in high temperature range. Upon cooling, the sampling position has minor effect on phase transformation temperature of DSC curve because the similar microstructure of the different sampling parts of the alloy formed in the following solidification cooling process after heating to a full liquid state and phase transformation temperature tends to be consistent. For a superalloy with the same composition, the DSC test results are only meaningful as the microstructure of the sample is similar. In General, the heating/cooling rate and sampling position had obvious effect on the phase transformation temperatures of DSC curves and these influence factors should be considered for selecting the process parameters of Ni-base superalloys.

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郑亮,许文勇,刘娜,刘杨,李周,肖程波,张国庆.镍基高温合金差示扫描量热分析的影响因素研究:升降温速率和取样部位[J].稀有金属材料与工程,2018,47(2):530~537.[Zheng Liang, Xu Wenyong, Liu Na, Liu Yang, Li Zhou, Xiao Chengbo, Zhang Guoqing. The investigation of influence factors on differential scanning calorimetry (DSC) analysis of a Ni-base superalloy: heating/cooling rate and sampling position[J]. Rare Metal Materials and Engineering,2018,47(2):530~537.]
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  • 收稿日期:2017-02-08
  • 最后修改日期:2017-04-29
  • 录用日期:2017-05-15
  • 在线发布日期: 2018-03-15
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