CN112525916B - Method for displaying harmful phase of isothermal forging die material for turbine disc - Google Patents
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- 239000000463 material Substances 0.000 title claims abstract description 62
- 238000010275 isothermal forging Methods 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000005498 polishing Methods 0.000 claims abstract description 51
- 239000011159 matrix material Substances 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 230000003287 optical effect Effects 0.000 claims abstract description 13
- 230000000694 effects Effects 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
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- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 2
- 238000004445 quantitative analysis Methods 0.000 claims description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 239000010937 tungsten Substances 0.000 claims description 2
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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Abstract
Description
技术领域technical field
本发明是一种涡轮盘用等温锻模材料有害相的显示方法，属于高温合金技术领域。The invention relates to a method for displaying harmful phases of an isothermal forging die material for a turbine disk, and belongs to the technical field of superalloys.
背景技术Background technique
高温合金主要是指能在600℃以上高温和复杂应力环境下长期服役的先进金属结构材料，具有优异的高温强度和环境抗力、良好的抗疲劳性能和断裂韧性等综合性能。高温合金大量用于制造航空发动机的热端部件，被誉为“燃气涡轮的心脏”。此外，高温合金还是舰船动力和发电用燃气轮机、运载火箭发动机、超超临界电站机组热端部件、化工领域、等温锻模以及海洋工程装备的关键材料。涡轮盘是航空发动机重要的核心热端部件，其工作条件极其恶劣，飞行时承受着复杂的热、机械载荷，各部位所承受的应力和温度均不相同，因此要求涡轮盘材料有足够的力学性能，特别是在其使用温度范围内要有尽可能高的疲劳、持久性能和良好的抗蠕变能力。当前先进燃气涡轮多采用粉末高温合金制备涡轮盘件，涡轮盘的成形离不开等温锻造，因此等温锻造模具材料的性能和寿命就成为涡轮盘制备的关键因素。现有涡轮盘等温锻造模具材料在制备过程中偶尔会产生有害相，如粗大硬脆的碳化物相，尺寸可达几十微米，形状还带有尖角，相当于高温合金中的夹杂物，直接影响模具的性能和寿命。已经发现出现有害碳化物相的等温锻模1100℃拉伸强度降低约50MPa，1100℃持久寿命降低50％。因此，涡轮盘用等温锻模材料有害相的识别显示和定量表征具有重要的意义。大尺寸等温锻模的制造过程中，由于截面厚大而冷却速度慢，有时会发生较为严重的宏观偏析，造成有害相及不均匀的分布特征。要准确测得有害相的平均含量，应选用合适的放大倍率，至少要测量上百个视场才具有较好的统计性，通常需采用图像自动分析仪。采用该方法的重要限制因素就是是否能够获得有害相和基体的高反衬的图像，以免自动检测时误检或漏检。因此，在基体中高质量的单相显示有害相，具有重要的意义。Superalloys mainly refer to advanced metal structural materials that can serve for a long time under high temperature and complex stress environment above 600 °C, and have excellent high temperature strength and environmental resistance, good fatigue resistance and fracture toughness and other comprehensive properties. Superalloys are widely used in the manufacture of hot-end parts of aero-engines and are known as "the heart of gas turbines". In addition, high-temperature alloys are also key materials for ship power and power generation gas turbines, launch vehicle engines, hot-end components of ultra-supercritical power plant units, chemical industry, isothermal forging dies, and marine engineering equipment. The turbine disk is an important core hot-end part of an aero-engine. Its working conditions are extremely harsh, and it is subjected to complex thermal and mechanical loads during flight. The stress and temperature of each part are different. Therefore, the material of the turbine disk is required to have sufficient mechanical properties. Performance, especially in its service temperature range to have as high as possible fatigue, durable performance and good creep resistance. At present, advanced gas turbines mostly use powdered superalloys to prepare turbine disks. The formation of turbine disks is inseparable from isothermal forging. Therefore, the performance and life of isothermal forging die materials become the key factors in the preparation of turbine disks. The existing turbine disk isothermal forging die materials occasionally produce harmful phases during the preparation process, such as coarse, hard and brittle carbide phases, which can reach tens of microns in size and have sharp corners, which are equivalent to inclusions in superalloys. Directly affect the performance and life of the mold. It has been found that the tensile strength of the isothermal forging die at 1100 ° C is reduced by about 50 MPa, and the durability life at 1100 ° C is reduced by 50% in the presence of harmful carbide phases. Therefore, the identification, display and quantitative characterization of harmful phases in isothermal forging die materials for turbine disks are of great significance. In the manufacturing process of large-size isothermal forging dies, due to the thick section and slow cooling rate, sometimes serious macro-segregation occurs, resulting in harmful phases and uneven distribution characteristics. To accurately measure the average content of harmful phases, an appropriate magnification should be selected, and at least hundreds of fields of view must be measured to have good statistics, and an automatic image analyzer is usually required. The important limiting factor of using this method is whether it is possible to obtain high-contrast images of the harmful phase and the matrix, so as to avoid false detection or missed detection during automatic detection. Therefore, it is of great significance that a high-quality single phase exhibits a detrimental phase in the matrix.
发明内容Contents of the invention
本发明针对上述现有技术中存在的不足设计提供了一种涡轮盘用等温锻模镍基高温合金材料有害相的显示方法，其目的是为了解决涡轮盘用等温锻模材料有害相仅能显示相边界而相内衬度和基体无法区分的问题，通过新的处理工艺的设计，使有害相与基体形成明显不同的相衬光学干涉效应，形成显著的干涉色差，从而实现有害相整体相对于基体清晰区分的单相显示。该发明方法可实现图像分析仪高灵敏度辨认、自动识别和定量统计高温合金中的有害相，目前已成功应用于涡轮盘用等温锻模材料有害相的显示与定量表征，同时还可用于其它金属材料析出相与基体的区分显示。The invention provides a method for displaying the harmful phase of the isothermal forging die material of the turbine disk, aimed at solving the problems existing in the above-mentioned prior art. The harmful phase of the isothermal forging die material for the turbine disk The phase boundary and the phase contrast and the matrix cannot be distinguished. Through the design of the new treatment process, the harmful phase and the matrix form a significantly different phase contrast optical interference effect, forming a significant interference chromatic aberration, so as to achieve the harmful phase as a whole relative to the matrix. A single-phase display with a clearly differentiated matrix. The inventive method can realize high-sensitivity identification, automatic identification and quantitative statistics of harmful phases in superalloys by image analyzers, and has been successfully applied to the display and quantitative characterization of harmful phases in isothermal forging die materials for turbine disks, and can also be used for other metals The distinction between the material precipitates and the matrix is shown.
本发明的目的是通过以下技术方案实现的：The purpose of the present invention is achieved through the following technical solutions:
该种涡轮盘用等温锻模镍基高温合金材料有害相的显示方法首先对涡轮盘用等温锻模材料试样进行去残余应力抛光，然后将涡轮盘用等温锻模材料试样放入预先升温至400-500℃的加热炉中，保温15-45min，取出后自然冷却到室温，使涡轮盘用等温锻模材料试样表面的有害相形成厚度为40-80nm的透光薄膜与涡轮盘用等温锻模材料试样基体形成明显区别的光学干涉效应。This method of displaying harmful phases of the isothermal forging die material for turbine disks using nickel-based superalloys firstly performs residual stress-removing polishing on the isothermal forging die material samples for turbine disks, and then puts the isothermal forging die material samples for turbine disks into pre-heated Put it in a heating furnace at 400-500°C, keep it warm for 15-45min, take it out and cool it down to room temperature naturally, so that the harmful phase on the surface of the isothermal forging material sample for the turbine disk forms a light-transmitting film with a thickness of 40-80nm and is used for the turbine disk The isothermal forging material sample matrix forms a distinct optical interference effect.
在实施中，所述涡轮盘用等温锻模材料试样的有害相包括粗大硬脆的富钨碳化物相。In practice, the harmful phase of the isothermal forging die material sample for a turbine disk includes a coarse, hard and brittle tungsten-rich carbide phase.
在实施中，对涡轮盘用等温锻模材料试样进行去残余应力抛光的步骤如下：In practice, the steps for removing residual stress and polishing the isothermal forging die material samples for turbine disks are as follows:
步骤一、采用100-200#砂纸磨平涡轮盘用等温锻模材料试样的金相磨面后用流水冲洗试样表面；Step 1. Use 100-200# sandpaper to smooth the metallographic grinding surface of the isothermal forging die material sample for the turbine disk, and then rinse the surface of the sample with running water;
步骤二、从小到大逐级经400-1200#的砂纸磨削涡轮盘用等温锻模材料试样的金相磨面，每磨完一道砂纸后都充分流水冲洗，试样平转90度再磨下一道砂纸，把前道划痕磨掉；Step 2: Grind the metallographic grinding surface of the isothermal forging die material sample for the turbine disk with 400-1200# sandpaper step by step from small to large. After each sandpaper is ground, fully rinse it with running water, turn the sample horizontally by 90 degrees and then Grind down a pass of sandpaper to remove the previous scratches;
步骤三、选用海军呢作为抛光织物对涡轮盘用等温锻模材料试样的金相磨面进行抛光，抛光织物经沉淀过滤后的纯净水浸湿后覆盖在抛光盘上，设置抛光盘转速为200-400转/分钟，然后选用抛光磨料粒度为1-3μm的研磨膏或喷雾悬浮液进行抛光，抛光时间为1-3min，然后用流水冲洗0.5-2min；该步骤为粗抛，以保证磨削量和光洁度；Step 3: Choose navy wool as the polishing fabric to polish the metallographic grinding surface of the isothermal forging die material sample for the turbine disk. The polishing fabric is soaked in the pure water after sedimentation and filtration and then covered on the polishing disk. Set the polishing disk speed to 200-400 rev/min, and then choose polishing paste or spray suspension with a polishing abrasive particle size of 1-3μm for polishing, the polishing time is 1-3min, and then rinse with running water for 0.5-2min; chipping and finish;
步骤四、再设置抛光盘转速为200-400转/分钟，选用医用超细MgO粉的高浓度水悬浊液作为磨料，对涡轮盘用等温锻模材料试样的金相磨面进行抛光，抛光时每间隔0.5-1min添加3-4次搅拌均匀的磨料，抛光1-3min后用流水冲洗0.5-1min，上述操作为精抛，保证获得最高的光洁度和无残余应变层；抛光后用浸酒精的棉球擦拭涡轮盘用等温锻模材料试样的金相磨面，同时用吹风机吹干，获得无残余应力的涡轮盘用等温锻模材料试样。Step 4. Set the speed of the polishing disc to 200-400 rpm, and select a high-concentration aqueous suspension of medical ultrafine MgO powder as the abrasive to polish the metallographic grinding surface of the isothermal forging die material sample for the turbine disc. When polishing, add 3-4 times of evenly stirred abrasives every 0.5-1min. After polishing for 1-3min, rinse with running water for 0.5-1min. The above operation is fine polishing, which ensures the highest smoothness and no residual strain layer; after polishing, dip Wipe the metallographic grinding surface of the isothermal forging die material sample for turbine disc with alcohol cotton ball, and dry it with a hair dryer at the same time to obtain the isothermal forging die material sample for turbine disc without residual stress.
进一步，步骤一中，应磨去剖切涡轮盘用等温锻模材料试样留下的变形层和烧伤层。Further, in step one, the deformed layer and burnt layer left by the isothermal forging die material sample used for cutting the turbine disk should be ground away.
进一步，步骤三中，所述粒度为1-3μm的抛光磨料为人造金刚石研磨膏或Al2O3喷雾悬浊液。Further, in step three, the polishing abrasive with a particle size of 1-3 μm is synthetic diamond abrasive paste or Al 2 O 3 spray suspension.
进一步，步骤四中，所述医用超细MgO粉的高浓度水悬浊液的配比为100ml H2O+2gMgO。Further, in step 4, the proportion of the high-concentration aqueous suspension of the medical ultrafine MgO powder is 100ml H 2 O+2gMgO.
进一步，步骤二中，由小到大逐级的砂纸砂的顺序为400#、800#、1000#。Further, in step 2, the order of the sandpaper sands step by step from small to large is 400#, 800#, 1000#.
在实施中，涡轮盘用等温锻模材料试样是采用机械砂轮片切割或电火花线切割切取。In practice, the isothermal forging die material samples for turbine discs are cut by mechanical grinding wheel cutting or wire electric discharge cutting.
在实施中，将轮盘用等温锻模材料试样的金相磨面朝上放入耐热陶瓷坩埚并加盖后，再放入加热炉中，冷却时取出坩埚并打开盖。In the implementation, put the metallographic surface of the isothermal forging die material sample for the roulette into the heat-resistant ceramic crucible and cover it, then put it into the heating furnace, take out the crucible and open the cover when cooling.
在光学显微镜下对最终获得无残余应力的涡轮盘用等温锻模材料试样做金相观察时，可以看到有害相整体呈蓝色特征色，与白亮色的合金基体明显不同，不但在灰度图像模式下获得了有害相和基体的整体衬度差别，在彩色模式下还可以获得明显颜色差异，有害相整体被清晰的单相显示出来。不单是衬度的差异(黑白灰度图像模式下)，还有颜色的差异(彩色模式下)。可实现图像分析仪高灵敏度辨认、自动识别和尺寸和含量的定量统计高温合金中的有害相，目前已成功应用于涡轮盘用等温锻模材料有害相的显示与定量表征。When the metallographic observation of the isothermal forging die material sample for the turbine disk without residual stress is carried out under the optical microscope, it can be seen that the harmful phase has a blue characteristic color as a whole, which is obviously different from the white and bright alloy matrix, not only in the gray In contrast image mode, the overall contrast difference between the harmful phase and the matrix can be obtained. In the color mode, an obvious color difference can also be obtained, and the overall harmful phase is clearly displayed by a single phase. Not only the difference in contrast (in black and white grayscale image mode), but also the difference in color (in color mode). It can realize high-sensitivity identification, automatic identification, and quantitative statistics of size and content of harmful phases in superalloys by image analyzers. It has been successfully applied to the display and quantitative characterization of harmful phases in isothermal forging die materials for turbine disks.
本发明技术方案的特点及技术上的效果是：The characteristics and technical effects of the technical solution of the present invention are:
传统高温合金中有害相的显示通常采用各种混合酸组成的金相试剂，通过化学作用腐蚀显示出相界，勾勒出有害相的轮廓，但有害相的内部和基体没有明显的反衬。因此传统化学试剂酸蚀仅能显示相边界而相内衬度和基体无法区分。而如果采用碱蚀试剂显示有害相则整体为暗黑色，与疏松缺陷的衬度又无法区分。本发明技术方案的方法是基于相衬干涉原理，利用有害相与基体相的化学成分差异，通过高精度抛光和较低温度加热、保温工艺使得有害相和合金基体形成不同厚度的特征纳米透光薄膜，使有害相与合金基体形成明显不同的光学干涉效应，形成明显不同的干涉色差，从而实现区别于基体的有害相整体清晰显示。该方法可实现图像分析仪高灵敏度辨认、自动识别和定量统计高温合金中的有害相，目前已成功应用于涡轮盘用等温锻模材料有害相的显示与定量表征，同时还可用于其它金属材料析出相与基体的区分显示。The display of harmful phases in traditional superalloys usually uses metallographic reagents composed of various mixed acids to display phase boundaries through chemical corrosion and outline the outline of harmful phases, but there is no obvious contrast between the interior of the harmful phases and the matrix. Therefore, acid etching with traditional chemical reagents can only show the phase boundary, and the phase contrast and matrix cannot be distinguished. However, if alkaline etching reagents are used to display harmful phases, the overall color will be dark black, which cannot be distinguished from the contrast of loose defects. The method of the technical solution of the present invention is based on the principle of phase contrast interference, utilizes the chemical composition difference between the harmful phase and the matrix phase, and makes the harmful phase and the alloy matrix form characteristic nano light transmission of different thicknesses through high-precision polishing and low-temperature heating and heat preservation processes The thin film makes the harmful phase and the alloy matrix form a significantly different optical interference effect, forming a significantly different interference chromatic aberration, so as to realize the overall clear display of the harmful phase that is different from the matrix. This method can realize high-sensitivity identification, automatic identification and quantitative statistics of harmful phases in superalloys by image analyzers. It has been successfully applied to the display and quantitative characterization of harmful phases in isothermal forging die materials for turbine disks. It can also be used for other metal materials The distinction between the precipitated phase and the matrix is shown.
本发明技术方案相对酸性腐蚀试剂，不仅仅可以显示轮廓和相边界，还可以单相整体突出显示有害相，形成区别于基体的均匀衬度，由于不采用化学试剂，安全环保；Compared with the acidic corrosion reagent, the technical solution of the present invention can not only display the outline and phase boundary, but also highlight the harmful phase of the single phase as a whole, forming a uniform contrast different from the matrix. Since no chemical reagent is used, it is safe and environmentally friendly;
本发明技术方案为了实现有害相的单相显示，涡轮盘用等温锻模材料试样的金相磨面的光洁度要求极高，所以采用了多级精细磨样和抛光，最后一级采用了很少采用的超细医用MgO悬浮液，有利于形成无残余应变层的高光洁度表面，防止因应变层存在使试样在最后加热保温时表面产生脏乱的伪色和应变痕；In order to realize the single-phase display of harmful phases in the technical solution of the present invention, the smoothness of the metallographic grinding surface of the isothermal forging die material sample for the turbine disc is extremely high, so multi-stage fine grinding and polishing are adopted, and the last stage adopts a very high The less used ultra-fine medical MgO suspension is conducive to the formation of a high-gloss surface with no residual strain layer, and prevents the surface of the sample from causing dirty false colors and strain marks during the final heating and heat preservation due to the existence of the strain layer;
本发明技术方案，在高光洁度表面的基础上通过适当的加热和保温形成合适厚度的纳米级干涉薄膜，由于有害相和基体呈现不同的膜厚，因而可以形成不同的光学干涉效应和颜色，从而实现有害相整体(非轮廓边界)和基体的区别显示。The technical scheme of the present invention forms a nano-scale interference film with a suitable thickness through proper heating and heat preservation on the basis of a high-gloss surface. Since the harmful phase and the matrix have different film thicknesses, different optical interference effects and colors can be formed, thereby Realize the differential display of harmful phases as a whole (non-contour boundary) and matrix.
加热温度过低或者保温时间过短，干涉膜厚度偏薄，有害相在光学金相下的色彩偏离特征色，不能和基体形成很好的反衬；而高温长时加热，形成的氧化膜过厚，透光率不足，会错过能形成光学干涉的厚度而使其特征色暗淡，也无法得到相对于基体的合适对比度。通过实验获得合适的加热温度和时间在400-500℃/15-45min范围内，可获得有害相与基体均匀、鲜明的颜色反衬。If the heating temperature is too low or the holding time is too short, the thickness of the interference film is too thin, and the color of the harmful phase under the optical metallography deviates from the characteristic color, which cannot form a good contrast with the substrate; while heating at high temperature for a long time, the formed oxide film is too thick , the light transmittance is insufficient, the thickness that can form optical interference will be missed, and the characteristic color will be dim, and the appropriate contrast with respect to the substrate cannot be obtained. Through experiments, the suitable heating temperature and time are in the range of 400-500°C/15-45min, and uniform and bright color contrast between the harmful phase and the matrix can be obtained.
本发明技术方案方法简单、成本低，仅需要普通加热炉和较低的加热温度和较短的保温时间，能够形成一定厚度的纳米干涉薄膜呈整体均匀蓝色特征，和基体合金的白亮衬底形成鲜明反差，高质量的单相显示和区分有害相，具备单一醒目特征颜色的有害相高质量显像节约了后续图像处理成本，可提高检测效率和准确度，为显微观察以及图像分析仪高精度识别和高效定量分析奠定了基础。The technical solution of the present invention is simple in method and low in cost. It only needs a common heating furnace, a lower heating temperature and a shorter holding time, and can form a nano-interference film with a certain thickness, which has the overall uniform blue feature, and the white and bright substrate of the matrix alloy. Form a sharp contrast, high-quality single-phase display and distinguish harmful phases, high-quality imaging of harmful phases with a single eye-catching characteristic color saves subsequent image processing costs, can improve detection efficiency and accuracy, and is ideal for microscopic observation and image analyzers High-precision identification and efficient quantitative analysis have laid the foundation.
具体实施方式detailed description
以下将结合实施例对本发明技术方案作进一步地详述：Below in conjunction with embodiment technical solution of the present invention will be described in further detail:
实施例1Example 1
采用本发明方法完成涡轮盘用等温锻模材料有害相的显示的方法如下：Adopt the method of the present invention to complete the method for the display of the harmful phase of the isothermal forging die material for the turbine disk as follows:
(1)采用机械砂轮片切割或电火花线切割切取涡轮盘用等温锻模材料镍基高温合金试样；(1) Use mechanical grinding wheel cutting or wire electric discharge cutting to cut out nickel-based superalloy samples for isothermal forging die materials for turbine disks;
(2)采用200#砂纸磨平金相磨面，并磨去剖切试样留下的变形层和烧伤层，后用流水冲洗试样表面；(2) Use 200# sandpaper to smooth the metallographic grinding surface, and grind away the deformed layer and burn layer left by the sectioned sample, and then rinse the surface of the sample with running water;
(3)从小到大逐级经400、800、1000#三个等级的砂纸磨削金相表面，每磨完一道砂纸后都充分流水冲洗，试样平转90度再磨下一道砂纸；(3) Grind the metallographic surface with 400, 800, and 1000# sandpaper step by step from small to large. After each sandpaper is ground, it is fully washed with running water, and the sample is turned 90 degrees before grinding the next sandpaper;
(4)选用海军呢作为抛光织物，抛光织物经沉淀过滤后的纯净水浸湿后覆盖在抛光盘上，转速300转/分钟，抛光磨料选用3μm的Al2O3喷雾悬浊液，抛光时间2min，然后用流水冲洗1min；( 4 ) Choose navy cloth as the polishing fabric, and the polishing fabric is covered on the polishing disc after being soaked in pure water after sedimentation and filtration. The rotating speed is 300 rpm. 2min, then rinse with running water for 1min;
(5)抛光盘转速为300转/分钟，磨料为医用超细MgO粉的高浓度水悬浊液，比例为100ml H2O+2g MgO粉搅拌均匀，抛光时每间隔1min添加4次搅拌均匀的MgO悬浊液，抛光3min后用流水冲洗0.5min，后用浸酒精的棉球擦拭抛光表面同时用吹风机吹干，获得无残余应变层精细抛光表面的涡轮盘用等温锻模材料试样；(5) The speed of the polishing disc is 300 rpm, and the abrasive is a high-concentration aqueous suspension of medical ultrafine MgO powder. The ratio is 100ml H 2 O + 2g MgO powder and stir evenly. Add 4 times at intervals of 1min during polishing and stir evenly After polishing for 3 minutes, rinse with running water for 0.5 minutes, wipe the polished surface with a cotton ball soaked in alcohol and dry it with a hair dryer at the same time to obtain an isothermal forging die material sample for a turbine disc with a finely polished surface without a residual strain layer;
(6)将抛光后的试样磨面朝上放入耐热陶瓷坩埚并加盖，放入预先升温至400℃的加热炉中保温40min，然后取出坩埚自然冷却到室温，打开坩埚盖取出试样。(6) Put the polished sample face up into a heat-resistant ceramic crucible and cover it, put it in a heating furnace heated to 400°C and keep it warm for 40 minutes, then take out the crucible to cool down to room temperature naturally, open the crucible cover and take out the test sample. Sample.
(7)在光学显微镜下对试样做金相观察，可以看到有害相M6C碳化物整体呈蓝色特征色，与白亮色的合金基体明显不同，有害相被清晰的单相显示出来。采用该方法处理后的试样可进一步应用于图像分析仪高灵敏度辨认、自动识别和定量统计高温合金中的有害相。(7) Metallographic observation of the sample under an optical microscope, it can be seen that the harmful phase M 6 C carbide has a blue characteristic color as a whole, which is obviously different from the white and bright alloy matrix, and the harmful phase is displayed by a clear single phase . The sample processed by the method can be further applied to the image analyzer for high-sensitivity identification, automatic identification and quantitative statistics of harmful phases in superalloys.
实施例2Example 2
采用本发明方法完成涡轮盘用等温锻模材料有害相的显示的方法如下：Adopt the method of the present invention to complete the method for the display of the harmful phase of the isothermal forging die material for the turbine disk as follows:
(1)采用机械砂轮片切割或电火花线切割切取涡轮盘用等温锻模材料镍基高温合金试样；(1) Use mechanical grinding wheel cutting or wire electric discharge cutting to cut out nickel-based superalloy samples for isothermal forging die materials for turbine disks;
(2)采用200#砂纸磨平金相磨面，并磨去剖切试样留下的变形层和烧伤层，后用流水冲洗试样表面；(2) Use 200# sandpaper to smooth the metallographic grinding surface, and grind away the deformed layer and burn layer left by the sectioned sample, and then rinse the surface of the sample with running water;
(3)从小到大逐级经400、800、1000#三个等级的砂纸磨削金相表面，每磨完一道砂纸后都充分流水冲洗，试样平转90度再磨下一道砂纸；(3) Grind the metallographic surface with 400, 800, and 1000# sandpaper step by step from small to large. After each sandpaper is ground, it is fully washed with running water, and the sample is turned 90 degrees before grinding the next sandpaper;
(4)选用海军呢作为抛光织物，抛光织物经沉淀过滤后的纯净水浸湿后覆盖在抛光盘上，转速300转/分钟，抛光磨料选用粒3μm的人造金刚石研磨膏，抛光时间2min，然后用流水冲洗1min；(4) Select navy wool as the polishing fabric, and the polishing fabric is covered on the polishing disk after being soaked in pure water after sedimentation and filtration, with a rotating speed of 300 rpm, and the polishing abrasive is selected from artificial diamond abrasive paste with a particle size of 3 μm, and the polishing time is 2 minutes, and then Rinse with running water for 1min;
(5)抛光盘转速为300转/分钟，磨料为医用超细MgO粉的高浓度水悬浊液，比例为100ml H2O+2g MgO粉搅拌均匀，抛光时每间隔1min添加4次搅拌均匀的MgO悬浊液，抛光3min后用流水冲洗0.5min，后用浸酒精的棉球擦拭抛光表面同时用吹风机吹干，获得无残余应变层精细抛光表面的涡轮盘用等温锻模材料试样；(5) The speed of the polishing disc is 300 rpm, and the abrasive is a high-concentration aqueous suspension of medical ultrafine MgO powder. The ratio is 100ml H 2 O + 2g MgO powder and stir evenly. Add 4 times at intervals of 1min during polishing and stir evenly After polishing for 3 minutes, rinse with running water for 0.5 minutes, wipe the polished surface with a cotton ball soaked in alcohol and dry it with a hair dryer at the same time to obtain an isothermal forging die material sample for a turbine disc with a finely polished surface without a residual strain layer;
(6)将抛光后的试样磨面朝上放入耐热陶瓷坩埚并加盖，放入预先升温至470℃的加热炉中保温20min，然后取出坩埚自然冷却到室温，打开坩埚盖取出试样。(6) Put the polished sample into a heat-resistant ceramic crucible with the grinding surface up and cover it, put it in a heating furnace heated to 470°C and keep it warm for 20 minutes, then take out the crucible and cool it to room temperature naturally, open the crucible cover and take out the test sample. Sample.
(7)在光学显微镜下对试样做金相观察，可以看到有害相M6C碳化物整体呈蓝色特征色，与白亮色的合金基体明显不同，有害相被清晰的单相显示出来。采用该方法处理后的试样可进一步应用于图像分析仪高灵敏度辨认、自动识别和定量统计高温合金中的有害相。(7) Metallographic observation of the sample under an optical microscope, it can be seen that the harmful phase M 6 C carbide has a blue characteristic color as a whole, which is obviously different from the white and bright alloy matrix, and the harmful phase is displayed by a clear single phase . The sample processed by the method can be further applied to the image analyzer for high-sensitivity identification, automatic identification and quantitative statistics of harmful phases in superalloys.
实施例3Example 3
采用本发明方法完成涡轮盘用等温锻模材料有害相的显示的方法如下：Adopt the method of the present invention to complete the method for the display of the harmful phase of the isothermal forging die material for the turbine disk as follows:
(1)采用机械砂轮片切割或电火花线切割切取涡轮盘用等温锻模材料镍基高温合金试样；(1) Use mechanical grinding wheel cutting or wire electric discharge cutting to cut out nickel-based superalloy samples for isothermal forging die materials for turbine disks;
(2)采用200#砂纸磨平金相磨面，并磨去剖切试样留下的变形层和烧伤层，后用流水冲洗试样表面；(2) Use 200# sandpaper to smooth the metallographic grinding surface, and grind away the deformed layer and burn layer left by the sectioned sample, and then rinse the surface of the sample with running water;
(3)从小到大逐级经400、800、1000#三个等级的砂纸磨削金相表面，每磨完一道砂纸后都充分流水冲洗，试样平转90度再磨下一道砂纸；(3) Grind the metallographic surface with 400, 800, and 1000# sandpaper step by step from small to large. After each sandpaper is ground, it is fully washed with running water, and the sample is turned 90 degrees before grinding the next sandpaper;
(4)选用海军呢作为抛光织物，抛光织物经沉淀过滤后的纯净水浸湿后覆盖在抛光盘上，转速300转/分钟，抛光磨料选用3μm的Al2O3喷雾悬浊液，抛光时间2min，然后用流水冲洗1min；( 4 ) Choose navy cloth as the polishing fabric, and the polishing fabric is covered on the polishing disc after being soaked in pure water after sedimentation and filtration. The rotating speed is 300 rpm. 2min, then rinse with running water for 1min;
(5)抛光盘转速为300转/分钟，磨料为医用超细MgO粉的高浓度水悬浊液，比例为100ml H2O+2g MgO粉搅拌均匀，抛光时每间隔1min添加4次搅拌均匀的MgO悬浊液，抛光3min后用流水冲洗0.5min，后用浸酒精的棉球擦拭抛光表面同时用吹风机吹干，获得无残余应变层精细抛光表面的涡轮盘用等温锻模材料试样；(5) The speed of the polishing disc is 300 rpm, and the abrasive is a high-concentration aqueous suspension of medical ultrafine MgO powder. The ratio is 100ml H 2 O + 2g MgO powder and stir evenly. Add 4 times at intervals of 1min during polishing and stir evenly After polishing for 3 minutes, rinse with running water for 0.5 minutes, wipe the polished surface with a cotton ball soaked in alcohol and dry it with a hair dryer at the same time to obtain an isothermal forging die material sample for a turbine disc with a finely polished surface without a residual strain layer;
(6)将抛光后的试样磨面朝上放入耐热陶瓷坩埚并加盖，放入预先升温至500℃的加热炉中保温15min，然后取出坩埚自然冷却到室温，打开坩埚盖取出试样。(6) Put the polished sample face up into a heat-resistant ceramic crucible and cover it, put it in a heating furnace heated to 500°C for 15 minutes, then take out the crucible to cool down to room temperature naturally, open the crucible cover and take out the test sample. Sample.
(7)在光学显微镜下对试样做金相观察，可以看到有害相M6C碳化物整体呈蓝色特征色，与白亮色的合金基体明显不同，有害相被清晰的单相显示出来。采用该方法处理后的试样可进一步应用于图像分析仪高灵敏度辨认、自动识别和定量统计高温合金中的有害相。(7) Metallographic observation of the sample under an optical microscope, it can be seen that the harmful phase M 6 C carbide has a blue characteristic color as a whole, which is obviously different from the white and bright alloy matrix, and the harmful phase is displayed by a clear single phase . The sample processed by the method can be further applied to the image analyzer for high-sensitivity identification, automatic identification and quantitative statistics of harmful phases in superalloys.
通过不同的温度配合不同的保温时间组合，温度较低时需要较长的保温时间，而温度相对较高，保温时间可以缩短。通过实施例验证，以上方案都可以获得满意的干涉色，从而有效显示有害相。By combining different temperatures with different holding time combinations, a longer holding time is required when the temperature is low, and the holding time can be shortened when the temperature is relatively high. As verified by the examples, the above schemes can obtain satisfactory interference colors, thereby effectively displaying harmful phases.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1068060A (en) * | 1996-08-27 | 1998-03-10 | Agency Of Ind Science & Technol | Method of coloring titanium alloy by thermal oxidation |
| CN102364323A (en) * | 2011-10-18 | 2012-02-29 | 广东电网公司电力科学研究院 | A display method of tempered martensitic steel carbide color metallography and its special electrothermal metallographic color development device |
| CN102486460A (en) * | 2010-12-01 | 2012-06-06 | 中国科学院金属研究所 | A Distinguishing Method of Laves Phase and Carbide Phase in High-Nb Fe-Ni-Based Superalloy |
| CN104111230A (en) * | 2014-06-19 | 2014-10-22 | 中国科学院金属研究所 | Classified display and quantitative detection method for martensite and residual austenite in M-A island |
| CN104236981A (en) * | 2014-09-15 | 2014-12-24 | 温州瑞明工业股份有限公司 | Polishing method for metallographic sample of aluminum alloy |
-
2020
- 2020-11-03 CN CN202011213700.0A patent/CN112525916B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1068060A (en) * | 1996-08-27 | 1998-03-10 | Agency Of Ind Science & Technol | Method of coloring titanium alloy by thermal oxidation |
| CN102486460A (en) * | 2010-12-01 | 2012-06-06 | 中国科学院金属研究所 | A Distinguishing Method of Laves Phase and Carbide Phase in High-Nb Fe-Ni-Based Superalloy |
| CN102364323A (en) * | 2011-10-18 | 2012-02-29 | 广东电网公司电力科学研究院 | A display method of tempered martensitic steel carbide color metallography and its special electrothermal metallographic color development device |
| CN104111230A (en) * | 2014-06-19 | 2014-10-22 | 中国科学院金属研究所 | Classified display and quantitative detection method for martensite and residual austenite in M-A island |
| CN104236981A (en) * | 2014-09-15 | 2014-12-24 | 温州瑞明工业股份有限公司 | Polishing method for metallographic sample of aluminum alloy |
Non-Patent Citations (2)
| Title |
|---|
| 彩色金相技术的浅析与应用;李永德等;《河北工程大学学报(自然科学版)》;20170925;第34卷(第03期);第93-96页 * |
| 碳纤维增强铜基复合材料的光学金相试样的制作方法;甘永学等;《理化检验.物理分册》;19880815(第04期);第51-52页 * |
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