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鎳基高溫合金差示掃描量熱分析的影響因素研究:升降溫速率和取樣部位
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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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國(guó)家自然科學(xué)基金資助(項(xiàng)目號(hào)51304177),國(guó)家重點(diǎn)研發(fā)計(jì)劃資助(項(xiàng)目號(hào)2016YFB0701404),國(guó)家科技支撐計(jì)劃資助(項(xiàng)目號(hào)2015BAE03B01),重點(diǎn)實(shí)驗(yàn)室基金資助(項(xiàng)目號(hào)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:

    本研究對(duì)定向凝固DZ22鎳基高溫合金在5~40℃/min不同速率下進(jìn)行升、降溫差示掃描量熱分析(DSC)試驗(yàn),通過(guò)線性外推和取平均值的方法確定合金平衡態(tài)的相變溫度。對(duì)不同取樣部位的DZ22合金進(jìn)行10℃/min下的升、降溫DSC曲線的測(cè)定。結(jié)果表明,升、降溫速率和取樣部位均對(duì)DSC試驗(yàn)結(jié)果產(chǎn)生明顯影響。(1)其中,DSC試驗(yàn)中的升溫、降溫速率對(duì)DZ22合金的相變溫度測(cè)試結(jié)果包括液相線、MC碳化物、固相線、共晶γ′和次生γ′均產(chǎn)生明顯影響,其中加熱曲線隨著升降溫速率的升高向高溫方向偏移,冷卻曲線則向低溫方向偏移,峰的高度隨著升降溫速率的升高而增大,但升溫、降溫曲線對(duì)應(yīng)相變溫度點(diǎn)平均值趨于一致,接近合金的平衡相變溫度。采用升溫、降溫曲線外推法獲得平衡態(tài)相變溫度的方法存在一定的差異,而取升、降溫曲線對(duì)應(yīng)的相變溫度平均值較為固定,是確定合金平衡相變溫度是有效方法。DSC試驗(yàn)中不同升溫和降溫速率對(duì)相變溫度結(jié)果的影響分別對(duì)高溫合金熱處理升溫和凝固冷卻過(guò)程中的實(shí)際工藝參數(shù)控制具有參考意義。(2)取樣部位對(duì)DSC加熱曲線低溫段中的(γ+γ′)共晶和固相線溫度產(chǎn)生明顯影響,因顯微偏析導(dǎo)致的組織差異導(dǎo)致同爐定向凝固試棒的底端和頂端的共晶(γ+γ′)和固相線溫度分別相差17℃和20℃,而對(duì)曲線高溫段的液相線和MC碳化物溶解溫度影響不大;不同取樣部位的合金加熱完全熔化后組織趨于一致,再次凝固冷卻過(guò)程中相變溫度也趨于一致,因此DSC冷卻曲線基本重合,取樣部位對(duì)DSC冷卻曲線無(wú)明顯影響。對(duì)同一成分的高溫合金而言,只有在取樣部位的顯微組織狀態(tài)相近的情況下其DSC試驗(yàn)結(jié)果才具有比較意義。升降溫速率和取樣部位均會(huì)影響鎳基高溫合金DSC曲線中的相變溫度結(jié)果,而以上因素在鎳基高溫合金熱工藝參數(shù)的選擇上應(yīng)有所考慮。

    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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鄭亮,許文勇,劉娜,劉楊,李周,肖程波,張國(guó)慶.鎳基高溫合金差示掃描量熱分析的影響因素研究:升降溫速率和取樣部位[J].稀有金屬材料與工程,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
  • 錄用日期:2017-05-15
  • 在線發(fā)布日期: 2018-03-15
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