硅在H13型热作模具钢中作用的研究
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摘要
为了降低成本、节约资源，课题组开发了一种新型高热强性热作模具钢SDH3钢（H13型），其合金化特点是高硅低钼的新合金化思路。本文通过组织与性能测试进一步验证了高硅低钼的新合金化思路的合理性，并借助热膨胀相变仪、扫描电镜（SEM）、透射电镜（TEM）、X射线衍射（XRD）、三维原子探针(3DAP)、模量与内耗测试仪等先进测试分析设备系统的研究了硅含量对SDH3热作模具钢的组织与性能的影响、回火动力学的影响、残余奥氏体量和稳定性的影响、以及钢中碳化物演变规律的影响；并从模量的角度研究了硅对SDH3钢高温热稳定性的影响，建立SDH3钢的模量的数学模型；最后讨论了SDH3钢热疲劳的微观机理，获得以下主要研究结果。
采用热力学计算软件Jmatpro对四种硅含量的SDH3钢的相变特性进行模拟计算，结果表明，硅含量对平衡相组成（包括碳化物）影响不明显；硅含量的增加导致SDH3钢Ac1和Accm点温度升高，其珠光体转变C曲线左移，贝氏体转变C曲线右移。性能测试发现，经过1060℃淬火和580℃两次回火后硬度为50HRC，室温无缺口冲击功大于300J，韧性优于H13钢；SDH3钢的热稳定性和热疲劳性能均优于H13钢。
采用BAHR DIL805A热膨胀相变仪、TEM、3DAP以及XRD等分析了硅含量对SDH3钢回火过程的影响。结果表明，SDH3钢中硅含量增加促使回火转变温度向高温移动，当钢中硅含量由0.6%增加到1.2%时，回火转变温度区间相应的向高温移动约150℃，而继续增加钢中硅含量时，无明显变化。结合动力学分析认为随着硅含量增加导致钢回火转变激活能提高，从而阻碍钢的回火转变，回火稳定性得以提高。硅含量的增加提高了淬火SDH3钢中残余奥氏体量，且其中碳含量增加。硅含量对SDH3钢不同状态下的碳化物尺寸大小有显著影响，提高钢中硅含量，可以促进细小碳化物的析出，并有效抑制碳化物的长大粗化，增加钢的回火稳定性。
利用模量与内耗仪研究了不同硅含量的SDH3钢的模量及内耗随温度和时间的变化规律。研究结果表明，模量随温度的变化可分为三个阶段：温度低于550℃和高于670℃时，模量随温度呈线性变化，而当温度在550℃-670℃之间时，模量随温度升高下降逐渐加快。而不同温度下SDH3钢的模量随时间的变化趋势也可分为三个阶段：初始阶段模量随着时间逐渐升高，在这个阶段出现一个明显的内耗峰，硅含量越高，在这个阶段的时间越短，说明提高硅含量有利于加快SDH3钢的回火稳定；第二阶段当模量达到最大值并保持不变的稳定阶段，硅含量越高，在这个阶段的时间越长，说明提高硅含量有利于提高SDH3钢的热稳定性；第三阶段模量随着保温时间的延长而降低并逐渐趋于稳定值。通过公式推导SDH3钢模量随温度变化的数学模型，结合试验数值，拟合获得了硅含量分别为0.6％、1.2％、1.5％和1.8％的SDH3钢的模量的数学表达式分别为G_1=72.99-3.82*exp((T-684.53)/176.96)、 G_2=74.68-4.63*exp((T-707.43)/182.89)、G_3=73.64-3.81*exp((T-715.10)/167.36)、G_4=73.70-3.25*exp((T-682.05)/160.70)，从公式看出，硅含量对模量的变化有显著影响；考虑SDH3钢第二相的影响，对模量-时间模型进行了修正，使其更好的描述SDH3钢的模量随时间的变化。
采用加速试验法模拟压铸模表面的温度变化过程，研究了SDH3钢的抗热疲劳性能，并结合透射电镜等分析了微观组织演化对热疲劳性能的影响。结果表明，提高SDH3钢的硅含量，能显著提高SDH3钢的抗热疲劳性能。通过热疲劳试样的显微组织分析发现，热疲劳过程中，疲劳裂纹尖端应力集中区出现的碳化物偏聚和粗化，成为裂纹生长的快速通道；热疲劳微裂纹在晶界处优先萌生，并沿晶界扩展。SDH3钢中硅含量不高（0.6wt.%）时，热疲劳过程中的碳化物以相互平行的M3C型合金渗碳体为主，其中部分向M2C型转变，而硅含量较高（1.5wt.%）时，则主要是以球状或椭球状M23C6型Cr23C6碳化物沿马氏体板条界或晶界析出，可见提高SDH3钢中的硅含量，能有效抑制钢中合金渗碳体的析出，而主要以M23C6型碳化物沿马氏体板条界或晶界析出和长大。SDH3钢中热疲劳裂纹优先在晶界处萌生，并借助晶界处析出的碳化物为媒介沿晶界扩展。
SDH3steel, a new H13-type of hot work die steel, was developed to reduce the productcost and resource. The high silicon but low molybdenum system alloy design theory isapplied on SDH3steel. In this thesis, the microstructures and properties of SDH3steel weretested to check and verify its reasonableness and accuracy of alloy design. The effect ofsilicon on the microstructures and properties, temper kinetics, the content of retainedaustenite and its thermal stability, and carbides solution and dissolution of SDH3steel werestudied by means of DIL85A linear dilatometer, scanning electron microscopy (SEM),transmission electron microscopy (TEM), X-ray diffraction (XRD), three-dimension atomprobe (3DAP), and modulus and internal friction testing instrument (M&IF). What’s more,the effect of silicon on the thermal resistance of SDH3steel was studied by modulusinvestigation, and the mathematics model of modulus of SDH3steel has been established.Finally, the micro-mechanism of thermal fatigue of SDH3steel was analyzed. The mainconclusions are summarized as follows.
Firstly, from the JmatPro ware of the thermodynamics analysis, phase transformations ofSDH3steel with four levels of Si-content were analyzed by simulating calculation. Theresults of the analysis and computation show that there is no significant effect of Si-contenton equilibrium phase compositions including carbides of SDH3steel. The temperatures ofAc1and Accm will be rise as the content of silicon increases in SDH3steel. The curve ofperlitic transformation to time left moved but the curve of bainite transformation to time rightmoved, with the increase of silicon content in SDH3steel. The results of measurement andtest of properties of SDH3steel show that SDH3steel performs significant secondaryhardening during tempering. The temperature of secondary hardening is about500℃. Afterquenching at1060℃and double tempering at580℃,the hardness of SDH3steel was50HRCand the room temperature non-notch impact energy exceed300J which excels that of AISIH13steel. Similarly, both thermal stability and thermal fatigue resistance of SDH3steel wassuperior to that of AISI H13steel.
The effect of silicon content on the kinetics of SDH3steel during tempering was studiedby means of BAHR DIL85A linear dilatometer, combined with TEM,3DAP and XRD. The experiment results showed that temper transformation moved to higher temperature withincrease of silicon content in SDH3steel. For example, the temperature of tempertransformation would raise about150℃as the content of silicon increased from0.6%to1.2%in SDH3steel. But the temperature changed little when the content of silicon was more than1.2%. Analyzing and calculating the experiment data, it was found that the activation energyincreased markedly as the content of silicon increases in SDH3steel during tempering, whichindicated temper transformation was retarded and temper resistant stability was improvedattributing to effect of higher silicon content in SDH3steel. The content of retainedaustenite increased obviously with increase of silicon content in quenched SDH steel.Meanwhile, the content of solution carbon in retained austenite was higher with higher siliconcontent in SDH3steel. The content of carbon in retained austenite was highest in overtempered SDH3steel but lowest in quenched SDH3steel with the same silicon content. Itindicated that carbon atoms partitioning from decomposed retained austenite to remainaustenite happened during tempering. As a result, the content of carbon in retained austeniterose steadily with time holding during tempering, and its temper resistance was improved.During tempering, Si rejects the carbide and a Si-rich region is present, adjacent to the carbide.The diffusion of carbon atoms were block and as a result coarsening of the carbides wasretarded. Silicon promote precipitation of fine carbides at a lower temperature but retardcoarsening of the carbides at a higher temperature. So temper resistance of SDH3steel wasimproved.
The modulus with temperature and time of SDH3steel with different silicon contentwere tested by modulus and internal friction testing instrument, and its internal friction wastested also by the instrument. The test results indicated that the trend of modulus withtemperature were similar to varied silicon content in SDH3steel. There was an exponentialrelationship between modulus and temperature in SDH3steel. The whole process can bedivided into three stages: modulus varied directly with temperature when the temperature wasbelow550℃or higher than670℃, modulus varied nonlinear with temperature when thetemperature was range from550℃to670℃. The modulus of SDH3steel rose quickly atfirst with holding time during isothermal processes at different temperatures. When themodulus reached to the maximum value it remained unchanged for a period of time and then decreased gradually to be a constant finally. There was a significant peak of internal frictioncorresponding in the modulus rising at first stage. There was an interesting phenomenon thatthe higher the content of silicon in SDH3steel, the quicker the modulus reached to themaximum, and the longer time the modulus remained unchanged. It indicated that silicon hadeffect on improving temper transformation and increasing the thermal stability of SDH3steel.In conclusion, based on the physical mechanism of modulus, the functions of modulus forSDH3steel under variable temperatures were developed by using physics formulas, andnumerical simulation of experimental results were carried out. Finally, accurate equations ofmodulus for SDH3steel with6.0%,1.2%1.5%and1.8%silicon content wereG_1=72.99-3.82*exp((T-684.53)/176.96), G_2=74.68-4.63*exp((T-707.43)/182.89),G_3=73.64-3.81*exp((T-715.10)/167.36) and G_4=73.70-3.25*exp((T-682.05)/160.70),respectively. Considering the effect of the second phase on modulus due to the microstructureof SDH3steel, mathematical models of modulus was modified and a new and appropriatemodel of modulus for SDH3steel was developed.
A study on thermal fatigue of SDH3steel was carried out by simulation test of thechanges of the surface temperature of aluminum die-casting dies at temperature range fromroom temperature to700℃. The experiment results showed that the thermal fatigue resistanceof SDH3steel was improved markedly with higher silicon content in SDH3steel. Meanwhileproblem in the thermal fatigue process is the affect on the microstructure at heat affect zoneduring heat cycle. Alloy carbides were easy to aggregate in the heat affect zone, and carbidescoarsening were investigated on stress field on crackle tip, which was easy channel of thermalfatigue crack fast growth. It was observed that thermal fatigue crack favorably initiated andpropagated at grain boundary. A technique named carbon extraction replica was used to takeprecipitates from the heat affect zone. Particle shape, distribution, size, and density weresurveyed by employing TEM, and precipitate composition was examined by energydispersive X-ray (EDX) analysis units. The results showed that a great quantity of plate-likecementites (M3C) was observed and a small quantity of needle-like Mo2C was found inSDH3steel with0.6%silicon. Comparatively, only globular Cr23C6precipitation at the grainboundary was observed in SDH3steel with1.5%silicon. It indicates that silicon has effect oninhibiting the precipitation of cementite, however, promoting the precipitation of Cr23C6at the grain boundary, which is in accord with the early study. In SDH3steel, the thermal fatiguecrack favorably initiated at grain boundary and propagated across the grain boundary.
采用热力学计算软件Jmatpro对四种硅含量的SDH3钢的相变特性进行模拟计算，结果表明，硅含量对平衡相组成（包括碳化物）影响不明显；硅含量的增加导致SDH3钢Ac1和Accm点温度升高，其珠光体转变C曲线左移，贝氏体转变C曲线右移。性能测试发现，经过1060℃淬火和580℃两次回火后硬度为50HRC，室温无缺口冲击功大于300J，韧性优于H13钢；SDH3钢的热稳定性和热疲劳性能均优于H13钢。
采用BAHR DIL805A热膨胀相变仪、TEM、3DAP以及XRD等分析了硅含量对SDH3钢回火过程的影响。结果表明，SDH3钢中硅含量增加促使回火转变温度向高温移动，当钢中硅含量由0.6%增加到1.2%时，回火转变温度区间相应的向高温移动约150℃，而继续增加钢中硅含量时，无明显变化。结合动力学分析认为随着硅含量增加导致钢回火转变激活能提高，从而阻碍钢的回火转变，回火稳定性得以提高。硅含量的增加提高了淬火SDH3钢中残余奥氏体量，且其中碳含量增加。硅含量对SDH3钢不同状态下的碳化物尺寸大小有显著影响，提高钢中硅含量，可以促进细小碳化物的析出，并有效抑制碳化物的长大粗化，增加钢的回火稳定性。
利用模量与内耗仪研究了不同硅含量的SDH3钢的模量及内耗随温度和时间的变化规律。研究结果表明，模量随温度的变化可分为三个阶段：温度低于550℃和高于670℃时，模量随温度呈线性变化，而当温度在550℃-670℃之间时，模量随温度升高下降逐渐加快。而不同温度下SDH3钢的模量随时间的变化趋势也可分为三个阶段：初始阶段模量随着时间逐渐升高，在这个阶段出现一个明显的内耗峰，硅含量越高，在这个阶段的时间越短，说明提高硅含量有利于加快SDH3钢的回火稳定；第二阶段当模量达到最大值并保持不变的稳定阶段，硅含量越高，在这个阶段的时间越长，说明提高硅含量有利于提高SDH3钢的热稳定性；第三阶段模量随着保温时间的延长而降低并逐渐趋于稳定值。通过公式推导SDH3钢模量随温度变化的数学模型，结合试验数值，拟合获得了硅含量分别为0.6％、1.2％、1.5％和1.8％的SDH3钢的模量的数学表达式分别为G_1=72.99-3.82*exp((T-684.53)/176.96)、 G_2=74.68-4.63*exp((T-707.43)/182.89)、G_3=73.64-3.81*exp((T-715.10)/167.36)、G_4=73.70-3.25*exp((T-682.05)/160.70)，从公式看出，硅含量对模量的变化有显著影响；考虑SDH3钢第二相的影响，对模量-时间模型进行了修正，使其更好的描述SDH3钢的模量随时间的变化。
采用加速试验法模拟压铸模表面的温度变化过程，研究了SDH3钢的抗热疲劳性能，并结合透射电镜等分析了微观组织演化对热疲劳性能的影响。结果表明，提高SDH3钢的硅含量，能显著提高SDH3钢的抗热疲劳性能。通过热疲劳试样的显微组织分析发现，热疲劳过程中，疲劳裂纹尖端应力集中区出现的碳化物偏聚和粗化，成为裂纹生长的快速通道；热疲劳微裂纹在晶界处优先萌生，并沿晶界扩展。SDH3钢中硅含量不高（0.6wt.%）时，热疲劳过程中的碳化物以相互平行的M3C型合金渗碳体为主，其中部分向M2C型转变，而硅含量较高（1.5wt.%）时，则主要是以球状或椭球状M23C6型Cr23C6碳化物沿马氏体板条界或晶界析出，可见提高SDH3钢中的硅含量，能有效抑制钢中合金渗碳体的析出，而主要以M23C6型碳化物沿马氏体板条界或晶界析出和长大。SDH3钢中热疲劳裂纹优先在晶界处萌生，并借助晶界处析出的碳化物为媒介沿晶界扩展。
SDH3steel, a new H13-type of hot work die steel, was developed to reduce the productcost and resource. The high silicon but low molybdenum system alloy design theory isapplied on SDH3steel. In this thesis, the microstructures and properties of SDH3steel weretested to check and verify its reasonableness and accuracy of alloy design. The effect ofsilicon on the microstructures and properties, temper kinetics, the content of retainedaustenite and its thermal stability, and carbides solution and dissolution of SDH3steel werestudied by means of DIL85A linear dilatometer, scanning electron microscopy (SEM),transmission electron microscopy (TEM), X-ray diffraction (XRD), three-dimension atomprobe (3DAP), and modulus and internal friction testing instrument (M&IF). What’s more,the effect of silicon on the thermal resistance of SDH3steel was studied by modulusinvestigation, and the mathematics model of modulus of SDH3steel has been established.Finally, the micro-mechanism of thermal fatigue of SDH3steel was analyzed. The mainconclusions are summarized as follows.
Firstly, from the JmatPro ware of the thermodynamics analysis, phase transformations ofSDH3steel with four levels of Si-content were analyzed by simulating calculation. Theresults of the analysis and computation show that there is no significant effect of Si-contenton equilibrium phase compositions including carbides of SDH3steel. The temperatures ofAc1and Accm will be rise as the content of silicon increases in SDH3steel. The curve ofperlitic transformation to time left moved but the curve of bainite transformation to time rightmoved, with the increase of silicon content in SDH3steel. The results of measurement andtest of properties of SDH3steel show that SDH3steel performs significant secondaryhardening during tempering. The temperature of secondary hardening is about500℃. Afterquenching at1060℃and double tempering at580℃,the hardness of SDH3steel was50HRCand the room temperature non-notch impact energy exceed300J which excels that of AISIH13steel. Similarly, both thermal stability and thermal fatigue resistance of SDH3steel wassuperior to that of AISI H13steel.
The effect of silicon content on the kinetics of SDH3steel during tempering was studiedby means of BAHR DIL85A linear dilatometer, combined with TEM,3DAP and XRD. The experiment results showed that temper transformation moved to higher temperature withincrease of silicon content in SDH3steel. For example, the temperature of tempertransformation would raise about150℃as the content of silicon increased from0.6%to1.2%in SDH3steel. But the temperature changed little when the content of silicon was more than1.2%. Analyzing and calculating the experiment data, it was found that the activation energyincreased markedly as the content of silicon increases in SDH3steel during tempering, whichindicated temper transformation was retarded and temper resistant stability was improvedattributing to effect of higher silicon content in SDH3steel. The content of retainedaustenite increased obviously with increase of silicon content in quenched SDH steel.Meanwhile, the content of solution carbon in retained austenite was higher with higher siliconcontent in SDH3steel. The content of carbon in retained austenite was highest in overtempered SDH3steel but lowest in quenched SDH3steel with the same silicon content. Itindicated that carbon atoms partitioning from decomposed retained austenite to remainaustenite happened during tempering. As a result, the content of carbon in retained austeniterose steadily with time holding during tempering, and its temper resistance was improved.During tempering, Si rejects the carbide and a Si-rich region is present, adjacent to the carbide.The diffusion of carbon atoms were block and as a result coarsening of the carbides wasretarded. Silicon promote precipitation of fine carbides at a lower temperature but retardcoarsening of the carbides at a higher temperature. So temper resistance of SDH3steel wasimproved.
The modulus with temperature and time of SDH3steel with different silicon contentwere tested by modulus and internal friction testing instrument, and its internal friction wastested also by the instrument. The test results indicated that the trend of modulus withtemperature were similar to varied silicon content in SDH3steel. There was an exponentialrelationship between modulus and temperature in SDH3steel. The whole process can bedivided into three stages: modulus varied directly with temperature when the temperature wasbelow550℃or higher than670℃, modulus varied nonlinear with temperature when thetemperature was range from550℃to670℃. The modulus of SDH3steel rose quickly atfirst with holding time during isothermal processes at different temperatures. When themodulus reached to the maximum value it remained unchanged for a period of time and then decreased gradually to be a constant finally. There was a significant peak of internal frictioncorresponding in the modulus rising at first stage. There was an interesting phenomenon thatthe higher the content of silicon in SDH3steel, the quicker the modulus reached to themaximum, and the longer time the modulus remained unchanged. It indicated that silicon hadeffect on improving temper transformation and increasing the thermal stability of SDH3steel.In conclusion, based on the physical mechanism of modulus, the functions of modulus forSDH3steel under variable temperatures were developed by using physics formulas, andnumerical simulation of experimental results were carried out. Finally, accurate equations ofmodulus for SDH3steel with6.0%,1.2%1.5%and1.8%silicon content wereG_1=72.99-3.82*exp((T-684.53)/176.96), G_2=74.68-4.63*exp((T-707.43)/182.89),G_3=73.64-3.81*exp((T-715.10)/167.36) and G_4=73.70-3.25*exp((T-682.05)/160.70),respectively. Considering the effect of the second phase on modulus due to the microstructureof SDH3steel, mathematical models of modulus was modified and a new and appropriatemodel of modulus for SDH3steel was developed.
A study on thermal fatigue of SDH3steel was carried out by simulation test of thechanges of the surface temperature of aluminum die-casting dies at temperature range fromroom temperature to700℃. The experiment results showed that the thermal fatigue resistanceof SDH3steel was improved markedly with higher silicon content in SDH3steel. Meanwhileproblem in the thermal fatigue process is the affect on the microstructure at heat affect zoneduring heat cycle. Alloy carbides were easy to aggregate in the heat affect zone, and carbidescoarsening were investigated on stress field on crackle tip, which was easy channel of thermalfatigue crack fast growth. It was observed that thermal fatigue crack favorably initiated andpropagated at grain boundary. A technique named carbon extraction replica was used to takeprecipitates from the heat affect zone. Particle shape, distribution, size, and density weresurveyed by employing TEM, and precipitate composition was examined by energydispersive X-ray (EDX) analysis units. The results showed that a great quantity of plate-likecementites (M3C) was observed and a small quantity of needle-like Mo2C was found inSDH3steel with0.6%silicon. Comparatively, only globular Cr23C6precipitation at the grainboundary was observed in SDH3steel with1.5%silicon. It indicates that silicon has effect oninhibiting the precipitation of cementite, however, promoting the precipitation of Cr23C6at the grain boundary, which is in accord with the early study. In SDH3steel, the thermal fatiguecrack favorably initiated at grain boundary and propagated across the grain boundary.
引文
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