CN106077647A - A kind of laser gain material controls the method for fragility Laves phase during manufacturing nickel base superalloy - Google Patents
A kind of laser gain material controls the method for fragility Laves phase during manufacturing nickel base superalloy Download PDFInfo
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- 229910001068 laves phase Inorganic materials 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 40
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 18
- 229910000601 superalloy Inorganic materials 0.000 title claims abstract description 18
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Abstract
本发明公开了一种激光增材制造镍基高温合金过程中控制脆性Laves相的方法。先对激光增材制造工艺参数进行初步优化，采用冷却介质对基材底部冷却；再采用激光调制技术对光源进行调制，获得较优激光调制参数，方波：峰值功率：600～1000W，脉冲频率：10HZ～100HZ，占空比：0.3～0.6；锯齿波：波峰600～1200W，波谷0W，脉冲频率：10HZ～100HZ；正弦波的参数为：波峰600～1000W，波谷0W，脉冲频率：10HZ～100HZ；最后按上述参数进行镍基高温合金激光增材制造成形，获得具有全部细小等轴枝晶组织及细小离散Laves相的成形零件。本发明通过激光调制方法，能有效控制激光增材制造镍基高温合金过程中Laves相的析出行为，降低激光增材制造零件的开裂敏感性，改善显微组织。
The invention discloses a method for controlling the brittle Laves phase in the process of laser additive manufacturing of nickel-base superalloy. Preliminary optimization of laser additive manufacturing process parameters, using cooling medium to cool the bottom of the substrate; then using laser modulation technology to modulate the light source to obtain better laser modulation parameters, square wave: peak power: 600 ~ 1000W, pulse frequency : 10HZ～100HZ, duty cycle: 0.3～0.6; sawtooth wave: peak 600～1200W, valley 0W, pulse frequency: 10HZ～100HZ; parameters of sine wave: peak 600～1000W, valley 0W, pulse frequency: 10HZ～ 100HZ; Finally, laser additive manufacturing of nickel-based superalloys is carried out according to the above parameters to obtain formed parts with all fine equiaxed dendrite structures and fine discrete Laves phases. Through the laser modulation method, the invention can effectively control the precipitation behavior of Laves phase in the process of laser additive manufacturing of nickel-based superalloy, reduce the cracking sensitivity of laser additive manufacturing parts, and improve the microstructure.
Description
技术领域technical field
本发明涉及激光金属材料加工领域，尤其涉及一种激光增材制造镍基高温合金过程中控制脆性Laves相的方法。The invention relates to the field of laser metal material processing, in particular to a method for controlling the brittle Laves phase in the process of laser additive manufacturing of nickel-based superalloys.
背景技术Background technique
激光增材制造技术是一种将激光熔覆与快速原型相结合的技术，由于具有材料利用率高、生产周期短、成本低等特点而被广泛应用于零件的快速成形、修复及表面改性等。Inconel 718是一种析出强化型、含Nb镍基高温合金，因具有良好的组织稳定性、可焊性、高温强度、高温疲劳、蠕变性能以及高温抗氧化能力等优异机械性能而被广泛地应用于航空航天、核工业及能源动力等领域。激光增材制造镍基合金最显著的特征之一就是Nb元素的偏析及Laves相的枝晶间析出。然而，脆性金属间化合物Laves相的形成对成形件的最终性能非常不利。一方面，Laves相的析出会消耗基体中有用的合金元素。另一方面，脆性Laves相为裂纹提供了形核和长大的有利位置，在残余应力或其他外载应力作用下可为裂纹的形核和生长扩展提供条件。Laves相的析出将导致成形件的拉伸性能、断裂韧性及疲劳性能显著下降。而且，粗糙的长链状Laves相将增加激光增材制造Inconel 718合金的热裂敏感性。因此，必须控制Laves相的析出行为。Laser additive manufacturing technology is a technology that combines laser cladding and rapid prototyping. It is widely used in rapid prototyping, repair and surface modification of parts due to its high material utilization rate, short production cycle and low cost. Wait. Inconel 718 is a precipitation-strengthened, Nb-containing nickel-based superalloy, which is widely used for its excellent mechanical properties such as good structural stability, weldability, high-temperature strength, high-temperature fatigue, creep performance, and high-temperature oxidation resistance. Used in aerospace, nuclear industry and energy power and other fields. One of the most notable features of laser additive manufacturing of nickel-based alloys is the segregation of Nb elements and the interdendritic precipitation of Laves phase. However, the formation of brittle intermetallic Laves phase is very detrimental to the final properties of the formed parts. On the one hand, the precipitation of Laves phase will consume useful alloying elements in the matrix. On the other hand, the brittle Laves phase provides a favorable position for crack nucleation and growth, and can provide conditions for crack nucleation and growth under the action of residual stress or other external stresses. The precipitation of Laves phase will lead to a significant decrease in the tensile properties, fracture toughness and fatigue properties of the formed parts. Moreover, the rough long-chain Laves phase will increase the hot cracking sensitivity of Inconel 718 alloy manufactured by laser additive manufacturing. Therefore, the precipitation behavior of the Laves phase must be controlled.
近几十年来，国内外学者一直致力于寻找有效控制Laves相的方法。Qi等人通过均匀化热处理工艺完全消除了激光增材制造Inconel718合金中产生的Laves相。然而，尽管高温均匀化热处理可以作为一种有效的方法来消除或减少Laves相，但要把Laves相溶解到一定程度，就不可避免地会导致一些新问题的出现，如热处理后发生再结晶、晶粒粗化及成形件变形等。因此，不能完全依赖后续热处理来处理Laves相问题，而是通过优化或改进加工工艺本身来控制Nb元素偏析与Laves相的形成。目前，关于控制Laves相的研究主要集中在焊接方面。Radhakrishna等人比较了钨电极惰性气体保护焊(GTA)与电子束(EB)焊接熔池显微组织，发现电子束焊接工艺具有更大的冷却速率，从而减小了枝晶间Nb元素偏析及Laves相的数量。他们也发现，在GTA焊接中减少能量输入，Laves相的数量将受到抑制。Ram等人在GTA焊接工艺中采用脉冲电流技术，发现扩散区Nb元素偏析减轻，网状链接的Laves相减少，时效响应及应力断裂性能明显提高。Murthy等与GM Reddy等发现在718电子束焊接中采用电子束振荡技术可以有效减小Nb元素偏析，并获得离散、细小的Laves相。Manikandan等发现氦气与复合电流脉冲模式对控制焊接熔合区Nb元素偏析及Laves相的形成是有益的。基于上述研究，Nb元素偏析及Laves相形成通过改变凝固条件是可以被抑制的，如改变冷却速率等。In recent decades, scholars at home and abroad have been devoting themselves to finding ways to effectively control the Laves phase. Qi et al. completely eliminated the Laves phase produced in the laser additive manufacturing Inconel718 alloy through a homogenization heat treatment process. However, although high-temperature homogenization heat treatment can be used as an effective method to eliminate or reduce the Laves phase, to dissolve the Laves phase to a certain extent will inevitably lead to some new problems, such as recrystallization after heat treatment, Grain coarsening and deformation of formed parts, etc. Therefore, the follow-up heat treatment cannot be completely relied on to deal with the problem of Laves phase, but the segregation of Nb element and the formation of Laves phase can be controlled by optimizing or improving the processing technology itself. At present, the research on the control of Laves phase mainly focuses on welding. Radhakrishna et al. compared the microstructure of tungsten electrode inert gas shielded welding (GTA) and electron beam (EB) welding pool, and found that the electron beam welding process has a greater cooling rate, thereby reducing the segregation of Nb elements between dendrites and Number of Laves phases. They also found that by reducing the energy input in GTA welding, the number of Laves phases will be suppressed. Ram et al. used pulse current technology in the GTA welding process and found that the segregation of Nb elements in the diffusion zone was reduced, the Laves phase of the network link was reduced, and the aging response and stress fracture performance were significantly improved. Murthy et al. and GM Reddy et al. found that the use of electron beam oscillation technology in 718 electron beam welding can effectively reduce the segregation of Nb elements and obtain discrete and fine Laves phases. Manikandan found that helium and compound current pulse mode are beneficial to control the segregation of Nb element and the formation of Laves phase in the welding fusion zone. Based on the above studies, the segregation of Nb elements and the formation of Laves phase can be suppressed by changing the solidification conditions, such as changing the cooling rate.
然而，关于激光增材制造过程中Nb元素偏析及Laves相控制方面的研究比较少见。Dinda等人研究了沉积路径及扫描速度对元素偏析行为的影响，发现沉积路径及扫描速度对元素偏析行为基本不产生影响。Y.Chen等人与Y.C.Zhang等人分别研究了基材持续水冷及液氮冷却对激光沉积718合金显微组织的影响，发现提高基材冷却速率可以减少Nb元素偏析及Laves相形成，但并没有完全去除长链状Laves相。However, studies on the segregation of Nb elements and the control of Laves phase in the laser additive manufacturing process are relatively rare. Dinda et al. studied the influence of deposition path and scanning speed on element segregation behavior, and found that deposition path and scanning speed have basically no effect on element segregation behavior. Y.Chen et al. and Y.C.Zhang et al. studied the effects of substrate continuous water cooling and liquid nitrogen cooling on the microstructure of laser-deposited 718 alloy, and found that increasing the substrate cooling rate can reduce Nb element segregation and Laves phase formation, but not The long-chain Laves phase was not completely removed.
发明内容Contents of the invention
本发明的目的是提供一种操作简便、可快速响应的激光增材制造镍基高温合金Laves相的控制方法。具体过程如下：The object of the present invention is to provide a method for controlling the Laves phase of nickel-base superalloy manufactured by laser additive manufacturing with simple operation and quick response. The specific process is as follows:
S1、对激光增材制造工艺参数进行初步优化，获得初步激光增材制造工艺窗口，优化参数：平均激光功率为300～800W，扫描速度为6～10mm/s，送粉量为8-12g/min，光斑直径为1～2mm，载气流量10～12L/min；S1. Preliminarily optimize the process parameters of laser additive manufacturing, obtain the preliminary laser additive manufacturing process window, and optimize parameters: the average laser power is 300-800W, the scanning speed is 6-10mm/s, and the powder feeding amount is 8-12g/ min, spot diameter is 1-2mm, carrier gas flow rate is 10-12L/min;
S2、激光增材制造过程中采用冷却介质对基材底部进行冷却，降低成形过程中的热积累；S2. During the laser additive manufacturing process, the cooling medium is used to cool the bottom of the substrate to reduce the heat accumulation during the forming process;
S3、进行镍基高温合金的激光增材制造成形，激光光源波形调制为方波、锯齿波或正弦波；其中，方波的参数为：峰值功率：600～1000W，脉冲频率：10HZ～100HZ，占空比：0.3～0.6；锯齿波参数为：波峰600～1200W，波谷0W，脉冲频率：10HZ～100HZ；正弦波的参数为：波峰600～1000W，波谷0W，脉冲频率：10HZ～100HZ；获得具有全部细小等轴枝晶组织及细小离散的Laves相，从而降低激光增材制造零件的开裂敏感性，改善显微组织。S3. Perform laser additive manufacturing of nickel-based superalloys. The waveform of the laser light source is modulated into a square wave, a sawtooth wave or a sine wave; wherein, the parameters of the square wave are: peak power: 600-1000W, pulse frequency: 10HZ-100HZ, Duty cycle: 0.3～0.6; sawtooth wave parameters: peak 600～1200W, valley 0W, pulse frequency: 10HZ～100HZ; sine wave parameters: peak 600～1000W, valley 0W, pulse frequency: 10HZ～100HZ; It has all the fine equiaxed dendrite structure and fine discrete Laves phase, thereby reducing the cracking sensitivity of laser additive manufacturing parts and improving the microstructure.
所述步骤S1中，所采用的激光增材制造方法是：同轴送粉式激光增材制造方法，或侧向送粉式激光增材制造方法。In the step S1, the laser additive manufacturing method adopted is: a coaxial powder feeding laser additive manufacturing method, or a lateral powder feeding laser additive manufacturing method.
所述步骤S2中，所述冷却介质为自来水、去离子水或液氮。In the step S2, the cooling medium is tap water, deionized water or liquid nitrogen.
所述步骤S2中，所述基材为碳钢、不锈钢或镍基合金。In the step S2, the base material is carbon steel, stainless steel or nickel-based alloy.
所述的步骤S3中，采用比色高温计对熔池温度进行测量，并对采集的温度数据进行计算分析，熔池温度的测量及数据计算分析的具体步骤包括：In the step S3, the temperature of the melting pool is measured by a colorimetric pyrometer, and the collected temperature data is calculated and analyzed. The specific steps of measuring the temperature of the molten pool and calculating and analyzing the data include:
S3.1、对两个比色高温计进行固定，其中一个高温计从试样侧面定点测量熔池温度，另一个温度计跟随激光熔覆头一起运动，同步测量熔池瞬时温度变化；S3.1. Fix two colorimetric pyrometers, one of which measures the temperature of the molten pool at a fixed point from the side of the sample, and the other thermometer moves with the laser cladding head to simultaneously measure the instantaneous temperature change of the molten pool;
S3.2、比色高温计探头光斑与熔池中心的位置校准，比色高温计与激光熔覆头轴向呈15度角，且两个比色高温计光斑要小于单道沉积层的宽度；S3.2. Calibrate the position of the colorimetric pyrometer probe spot and the center of the molten pool. The colorimetric pyrometer is at an angle of 15 degrees to the axial direction of the laser cladding head, and the two colorimetric pyrometer spots are smaller than the width of a single deposition layer. ;
S3.3、采集并分析温度数据，高温计采集频率设计为1ms，温度采集完成后，对温度数据进行光滑处理，并对处理的曲线进行求导，获得熔池表面的冷却速率。S3.3. Collect and analyze temperature data. The pyrometer collection frequency is designed to be 1ms. After the temperature collection is completed, the temperature data is smoothed, and the processed curve is derived to obtain the cooling rate on the surface of the molten pool.
本发明一方面可极大提高熔池的冷却速率(最高可达到106～107℃/s)，显著提高熔池过冷；另一方面，周期性的能量输入将造成熔池周期性地快速加热及快速冷却。这两方面的因素将，促进晶粒的形核；细化凝固组织；抑制Nb元素偏析，减少Laves相形成，进而获得低体积分数且细小、离散分布的Laves相颗粒。本发明不仅解决了激光增材制造镍基高温合金过程中由于脆性长链状Laves相形成而导致的热裂问题，而且能够有效减少有用合金元素偏析，从而降低激光增材制造零件的开裂敏感性，改善显微组织。On the one hand, the present invention can greatly increase the cooling rate of the molten pool (up to 10 6 ~ 10 7 ℃/s), and significantly improve the supercooling of the molten pool; on the other hand, periodic energy input will cause the molten pool to periodically Rapid heating and rapid cooling. These two factors will promote the nucleation of grains; refine the solidification structure; inhibit the segregation of Nb elements, reduce the formation of Laves phase, and then obtain low volume fraction, fine and discretely distributed Laves phase particles. The invention not only solves the problem of thermal cracking caused by the formation of brittle long-chain Laves phase in the process of laser additive manufacturing of nickel-based superalloys, but also can effectively reduce the segregation of useful alloy elements, thereby reducing the cracking sensitivity of laser additive manufacturing parts , to improve the microstructure.
附图说明Description of drawings
图1采用传统激光增材制造获得的金相组织图；Figure 1 is a metallographic structure diagram obtained by traditional laser additive manufacturing;
图2采用本发明激光调制方法获得的金相组织图；Fig. 2 adopts the metallographic structure diagram that the laser modulation method of the present invention obtains;
图3采用传统激光增材制造获得的SEM图；Figure 3 is the SEM image obtained by traditional laser additive manufacturing;
图4采用本发明激光调制方法获得的SEM图。Fig. 4 is an SEM image obtained by using the laser modulation method of the present invention.
以下结合说明书附图和具体实施例对本发明作进一步详细说明。The present invention will be described in further detail below in conjunction with the accompanying drawings and specific embodiments.
具体实施方式detailed description
实施例1Example 1
S1、对激光增材制造工艺参数进行初步优化，获得初步激光增材制造工艺窗口，优化参数：平均激光功率为400W，扫描速度为6mm/s，送粉量为8g/min，光斑直径为1～2mm，载气流量10L/min；S1. Preliminarily optimize the process parameters of laser additive manufacturing, obtain the preliminary laser additive manufacturing process window, and optimize the parameters: the average laser power is 400W, the scanning speed is 6mm/s, the powder feeding amount is 8g/min, and the spot diameter is 1 ～2mm, carrier gas flow rate 10L/min;
S2、采用自来水对镍基基材底部进行冷却，降低成形过程中的热积累；S2. Use tap water to cool the bottom of the nickel-based substrate to reduce heat accumulation during the forming process;
S3、进行镍基高温合金的激光增材制造成形，激光光源控制选用方波，方波的参数为：峰值功率：600W，脉冲频率：10HZ～100HZ，占空比：0.6。S3. Carry out laser additive manufacturing of nickel-based superalloys. The laser light source is controlled by a square wave. The parameters of the square wave are: peak power: 600W, pulse frequency: 10HZ-100HZ, duty cycle: 0.6.
图2是采用本发明激光调制方法获得的金相组织图；从图2中可以看出金相组织由细小的等轴状枝晶组成；图1中采用传统激光增材制造获得的金相组织由粗大的柱状枝晶组成。图4是采用本发明激光调制方法获得的SEM图，Laves相细小离散形貌，而图3中采用传统激光增材制造获得的Laves相呈粗大的长链状，说明了本发明控制方法的有效性。Fig. 2 is the metallographic structure diagram that adopts the laser modulation method of the present invention to obtain; From Fig. 2, it can be seen that the metallographic structure is composed of fine equiaxed dendrites; the metallographic structure obtained by traditional laser additive manufacturing in Fig. 1 Composed of thick columnar dendrites. Figure 4 is an SEM image obtained by using the laser modulation method of the present invention, the Laves phase is fine and discrete, while the Laves phase obtained by traditional laser additive manufacturing in Figure 3 is in the shape of a thick long chain, which illustrates the effectiveness of the control method of the present invention. sex.
采用比色高温计对熔池温度进行测量，并对采集的温度数据进行分析与冷却速率计算。熔池温度的测量及处理的具体步骤包括：The temperature of the molten pool is measured by a colorimetric pyrometer, and the collected temperature data is analyzed and the cooling rate is calculated. The specific steps of measuring and processing the molten pool temperature include:
S3.1、对两个比色高温计进行固定，其中一个高温计从试样侧面定点测量熔池温度，另一个温度计跟随激光熔覆头一起运动，同步测量熔池瞬时温度变化；S3.1. Fix two colorimetric pyrometers, one of which measures the temperature of the molten pool at a fixed point from the side of the sample, and the other thermometer moves with the laser cladding head to simultaneously measure the instantaneous temperature change of the molten pool;
S3.2、比色高温计探头光斑与熔池中心的位置校准，比色高温计与激光熔覆头轴向呈15度角，且两个比色高温计光斑要小于单道沉积层的宽度；S3.2. Calibrate the position of the colorimetric pyrometer probe spot and the center of the molten pool. The colorimetric pyrometer is at an angle of 15 degrees to the axial direction of the laser cladding head, and the two colorimetric pyrometer spots are smaller than the width of a single deposition layer. ;
S3.3、采集并分析温度数据，高温计采集频率设计为1ms，温度采集完成后，对温度数据进行光滑处理，并对处理的曲线进行求导，获得熔池表面的冷却速率。S3.3. Collect and analyze temperature data. The pyrometer collection frequency is designed to be 1ms. After the temperature collection is completed, the temperature data is smoothed, and the processed curve is derived to obtain the cooling rate on the surface of the molten pool.
实施例2Example 2
S1、对激光增材制造工艺参数进行初步优化，获得初步激光增材制造工艺窗口，优化参数：平均激光功率为400W，扫描速度为10mm/s，送粉量为12g/min，光斑直径为1～2mm，载气流量12L/min；S1. Preliminarily optimize the process parameters of laser additive manufacturing, obtain the preliminary laser additive manufacturing process window, and optimize the parameters: the average laser power is 400W, the scanning speed is 10mm/s, the powder feeding amount is 12g/min, and the spot diameter is 1 ～2mm, carrier gas flow rate 12L/min;
S2、采用去自来水对镍基基材底部进行冷却，降低成形过程中的热积累；S2. Use tap water to cool the bottom of the nickel-based substrate to reduce heat accumulation during the forming process;
S3、进行镍基高温合金的激光增材制造成形，激光光源控制选用锯齿波，锯齿波参数为：波峰900W，波谷0W，脉冲频率：90HZ。S3. Carry out laser additive manufacturing of nickel-based superalloys. The laser light source is controlled by a sawtooth wave. The parameters of the sawtooth wave are: peak 900W, valley 0W, pulse frequency: 90HZ.
实施例3：Example 3:
S1、对激光增材制造工艺参数进行初步优化，获得初步激光增材制造工艺窗口，优化参数：平均激光功率为600W，扫描速度为8mm/s，送粉量为10g/min，光斑直径为1mm，载气流量10L/min；S1. Preliminarily optimize the process parameters of laser additive manufacturing, obtain the preliminary laser additive manufacturing process window, and optimize the parameters: the average laser power is 600W, the scanning speed is 8mm/s, the powder feeding amount is 10g/min, and the spot diameter is 1mm , carrier gas flow rate 10L/min;
S2、采用液氮对镍基基材底部进行冷却，降低成形过程中的热积累；S2. Use liquid nitrogen to cool the bottom of the nickel-based substrate to reduce heat accumulation during the forming process;
S3、进行镍基高温合金的激光增材制造成形，激光光源控制选用正弦波，正弦波的参数为：波峰700W，波谷0W，脉冲频率：30HZ。S3. Carry out laser additive manufacturing of nickel-based superalloys. The laser light source is controlled by a sine wave. The parameters of the sine wave are: peak 700W, valley 0W, pulse frequency: 30HZ.
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