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CN115354133B - Method for preventing local recrystallization of monocrystalline superalloy blade - Google Patents

Method for preventing local recrystallization of monocrystalline superalloy blade Download PDF

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CN115354133B
CN115354133B CN202210978837.8A CN202210978837A CN115354133B CN 115354133 B CN115354133 B CN 115354133B CN 202210978837 A CN202210978837 A CN 202210978837A CN 115354133 B CN115354133 B CN 115354133B
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recrystallization
heating rate
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CN115354133A (en
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赵金乾
李嘉荣
史报学
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AECC Beijing Institute of Aeronautical Materials
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    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/0068Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for particular articles not mentioned below
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B1/00Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/02Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F3/00Brightening metals by chemical means
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25FPROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00Electrolytic etching or polishing
    • C25F3/02Etching
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25FPROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00Electrolytic etching or polishing
    • C25F3/16Polishing

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses a method for preventing local recrystallization of a monocrystalline superalloy blade, which comprises the following steps in sequence: placing the monocrystal superalloy blade into a vacuum heat treatment furnace for recovery treatment; taking out the single-crystal superalloy blade from the vacuum heat treatment furnace, and directly mechanically polishing and grinding part of the blade; cleaning the mechanically polished single-crystal superalloy blade, and removing mechanically polished traces by adopting a local electrolytic machining or chemical corrosion mode; and carrying out solid solution aging treatment on the single-crystal superalloy blade. According to the technical scheme, the problem that the single-crystal superalloy blade is recrystallized in the subsequent solution heat treatment process due to the fact that large casting residual stress locally exists in the casting process due to the fact that the blade structure is complex can be effectively prevented.

Description

一种预防单晶高温合金叶片局部再结晶的方法A method to prevent local recrystallization of single crystal high temperature alloy blades

技术领域Technical field

本发明属于航空发动机涡轮叶片制造技术领域,具体涉及一种预防单晶高温合金叶片局部再结晶的方法。The invention belongs to the technical field of manufacturing aeroengine turbine blades, and specifically relates to a method for preventing local recrystallization of single crystal high-temperature alloy blades.

背景技术Background technique

涡轮叶片是涡轮发动机中最关键的零件之一,它的工作环境恶劣,同时承受高温、高应力。单晶高温合金几乎消除了所有晶界,具有良好的高温综合性能,被认为是制造先进航空发动机和地面燃机涡轮叶片的关键材料。Turbine blades are one of the most critical parts in turbine engines. They work in harsh environments and are subject to high temperatures and high stress. Single-crystal superalloys eliminate almost all grain boundaries and have good high-temperature comprehensive properties. They are considered key materials for manufacturing advanced aerospace engines and ground gas turbine turbine blades.

对于单晶高温合金而言,为了获得良好的力学性能,通常采用完全热处理的方法,但固溶处理温度高,再结晶倾向大。一方面,相对于铸造凝固过程中产生的晶界,再结晶的晶界强度明显较低;另一方面,再结晶产生横向晶界,形成了叶片的薄弱环节,严重影响了叶片的性能。因此,单晶高温合金和定向柱晶叶片必须尽量避免再结晶的产生。For single crystal superalloys, in order to obtain good mechanical properties, complete heat treatment is usually used, but the solution treatment temperature is high and the recrystallization tendency is large. On the one hand, compared with the grain boundaries produced during the casting solidification process, the strength of recrystallized grain boundaries is significantly lower; on the other hand, recrystallization produces transverse grain boundaries, forming a weak link in the blade and seriously affecting the performance of the blade. Therefore, single crystal superalloys and oriented columnar crystal blades must avoid recrystallization as much as possible.

叶片在定向凝固过程中,由于叶片的形状复杂,所以凝固冷却过程中的收缩局部存在过大的铸造残余应力集中,待定向凝固完成后,较大的铸造残余应力会导致后续在固溶热处理过程中容易出现再结晶缺陷。During the directional solidification process of the blade, due to the complex shape of the blade, there is excessive casting residual stress concentration in the shrinkage area during the solidification and cooling process. After the directional solidification is completed, the large casting residual stress will cause subsequent solution heat treatment. Recrystallization defects are prone to occur.

再结晶的形成是因为叶片在制备过程中铸造应力或外来应力在叶片内产生了一定的塑性变形,贮存了一定的应变能,在后续高温热处理过程中,应变能以再结晶的形式释放出来。铸造过程中因凝固收缩等产生铸造应力导致的塑性变形,如果密度较大就会造成热处理过程中形成再结晶,这种再结晶通常位置较为固定,并具有重复性强、尺寸大、数量少等特征。一般情况下,若叶片表面出现这种再结晶,则会造成整个叶片报废,这也是制约叶片合格率的一大重要因素。因此,急需开发一种预防单晶高温合金叶片局部再结晶的方法,以降低叶片产生再结晶的风险,进而提高叶片制造合格率。The formation of recrystallization is because the casting stress or external stress during the blade preparation process produces a certain plastic deformation in the blade and stores a certain amount of strain energy. During the subsequent high-temperature heat treatment process, the strain energy is released in the form of recrystallization. Plastic deformation caused by casting stress due to solidification shrinkage during the casting process. If the density is high, it will cause recrystallization during the heat treatment process. This kind of recrystallization is usually relatively fixed in position and has strong repeatability, large size, and small quantity. feature. Under normal circumstances, if this kind of recrystallization occurs on the blade surface, the entire blade will be scrapped, which is also an important factor restricting the blade qualification rate. Therefore, there is an urgent need to develop a method to prevent local recrystallization of single crystal superalloy blades to reduce the risk of recrystallization in the blades and thereby improve the blade manufacturing qualification rate.

申请公布号为CN107557869A的发明专利公开了一种避免单晶高温合金涡轮叶片铂丝芯撑位置再结晶的方法,对叶片芯撑位置采用手持打磨机打磨+毡轮低应力抛光+化学腐蚀表面处理+阶梯式回复热处理的顺序方式,减小叶片芯撑位置的塑性应变层及残余应力;化学腐蚀的腐蚀液为过氧化氢和盐酸,腐蚀液体积配比为H2O2:HCl=1:8-10;阶梯式回复热处理为:(700-850℃)/(2-4h)+(1200-1230℃)/(0.5-1h)+(1250-1270℃)/(0.5-1h)+(1200-1230℃)/(0.5-1h)+(1280-1300℃)/(0.5-1h)+(1250-1270℃)/(0.5-1h)+(1280-1300℃)/(0.5-1h),所有升温阶段的升温速率≤10℃/min,保温到时后,采用炉冷至200℃以下出炉。该技术方案是针对单晶高温合金涡轮叶片铂丝芯撑位置设计的避免再结晶的方法,其操作顺序、工艺参数等仅适用于避免叶片铂丝芯撑位置的再结晶,不适用于叶片本体;此外,先进行机械打磨和化学腐蚀,后进行回复热处理,这样的操作顺序不利于促进再结晶形核,所以在后续固溶时效处理时,依然会发生再结晶。The invention patent application publication number CN107557869A discloses a method to avoid recrystallization of the platinum wire core support position of single crystal high-temperature alloy turbine blades. The blade core support position is polished with a hand-held grinder + felt wheel low-stress polishing + chemical corrosion surface treatment + The sequential method of step recovery heat treatment reduces the plastic strain layer and residual stress at the blade core support position; the corrosive liquid for chemical corrosion is hydrogen peroxide and hydrochloric acid, and the volume ratio of the corrosive liquid is H 2 O 2 :HCl=1: 8-10; the step recovery heat treatment is: (700-850℃)/(2-4h)+(1200-1230℃)/(0.5-1h)+(1250-1270℃)/(0.5-1h)+( 1200-1230℃)/(0.5-1h)+(1280-1300℃)/(0.5-1h)+(1250-1270℃)/(0.5-1h)+(1280-1300℃)/(0.5-1h) , the heating rate in all heating stages is ≤10℃/min. After the heat preservation time is reached, use furnace cooling to below 200℃ and release. This technical solution is a method to avoid recrystallization designed for the position of the platinum wire core support of single crystal high-temperature alloy turbine blades. Its operation sequence, process parameters, etc. are only suitable for avoiding recrystallization at the position of the platinum wire core support of the blade and are not applicable to the blade body. ; In addition, mechanical polishing and chemical corrosion are performed first, followed by recovery heat treatment. This sequence of operations is not conducive to promoting recrystallization nucleation, so recrystallization will still occur during subsequent solid solution aging treatment.

发明内容Contents of the invention

单晶高温合金叶片在定向凝固过程中,由于叶片的形状复杂,所以在凝固冷却过程中的收缩局部存在过大的铸造残余应力集中,在定向凝固完成后,较大的铸造残余应力极易导致在后续固溶热处理过程中出现再结晶缺陷。本发明的目的在于预防由于叶片结构复杂原因在铸造过程中局部存在较大的铸造残余应力而导致单晶高温合金叶片在后续固溶热处理过程中产生再结晶。During the directional solidification process of single crystal superalloy blades, due to the complex shape of the blades, there is excessive casting residual stress concentration in the shrinkage area during the solidification and cooling process. After the directional solidification is completed, large casting residual stresses can easily lead to Recrystallization defects occur during subsequent solution heat treatment. The purpose of the present invention is to prevent single-crystal high-temperature alloy blades from recrystallizing during the subsequent solution heat treatment process due to the large local casting residual stress during the casting process due to the complex structure of the blade.

为实现上述目的,本发明提供一种预防单晶高温合金叶片局部再结晶的方法,按照先后顺序包括以下步骤:In order to achieve the above objectives, the present invention provides a method for preventing partial recrystallization of single crystal high-temperature alloy blades, which includes the following steps in sequence:

步骤一:将单晶高温合金叶片放置于真空热处理炉内,进行回复处理;Step 1: Place the single crystal high-temperature alloy blade in a vacuum heat treatment furnace for recovery treatment;

步骤二:从真空热处理炉内取出单晶高温合金叶片,对叶片局部直接进行机械抛磨;Step 2: Take out the single crystal high-temperature alloy blade from the vacuum heat treatment furnace, and directly mechanically polish part of the blade;

步骤三:将机械抛磨后的单晶高温合金叶片进行清洗,然后采用局部电解加工或者化学腐蚀的方式去除机械抛磨的痕迹;Step 3: Clean the mechanically polished single crystal high-temperature alloy blades, and then use local electrolytic processing or chemical corrosion to remove traces of mechanical polishing;

步骤四:将单晶高温合金叶片进行固溶时效处理。Step 4: Perform solid solution aging treatment on the single crystal high-temperature alloy blades.

本发明的预防单晶高温合金叶片局部再结晶的方法,处理顺序依次为:回复处理、机械抛磨、局部电解加工或者化学腐蚀、固溶时效处理。在本领域中,技术人员普遍认为在单晶高温合金叶片固溶时效处理前应禁止使用机械方式直接处理叶片本体,若直接对叶片本体进行机械处理,则会促进固溶时效过程中再结晶的发生。而本发明却克服了技术偏见,在叶片固溶时效处理前使用了机械方式直接处理叶片本体,并结合机械处理前对叶片进行回复处理的步骤,最终有效地避免了单晶高温合金叶片在固溶时效过程中发生再结晶。For the method of preventing partial recrystallization of single crystal high-temperature alloy blades of the present invention, the processing sequence is: recovery treatment, mechanical polishing, local electrolytic processing or chemical corrosion, and solid solution aging treatment. In this field, technicians generally believe that it is forbidden to use mechanical means to directly treat the blade body before solid solution aging treatment of single crystal superalloy blades. If the blade body is directly mechanically treated, it will promote recrystallization during the solid solution aging process. occur. However, the present invention overcomes the technical prejudice. It uses mechanical means to directly treat the blade body before the solid solution aging treatment of the blade, and combines the steps of restoring the blade before the mechanical treatment. Ultimately, it effectively avoids the solidification of single crystal high-temperature alloy blades. Recrystallization occurs during solution aging.

由低温向高温逐步递进的梯度回复处理,能够使铸造残余应力得到有效回复,残余应力较大时,单晶叶片局部表面已经形成了再结晶晶粒的核心。然而高温合金材料的组织结构特征决定了固溶前再结晶晶界迁移阻力大,难以生长。单晶高温合金再结晶过程的控制性环节为形核。The gradual gradient recovery treatment from low temperature to high temperature can effectively recover the casting residual stress. When the residual stress is large, the core of recrystallized grains has been formed on the local surface of the single crystal blade. However, the structural characteristics of high-temperature alloy materials determine that the recrystallization grain boundary migration resistance before solid solution is large and difficult to grow. The controlling link in the recrystallization process of single crystal superalloy is nucleation.

采用手持式电动、气动或者其他抛磨设备抛修叶片,去除叶片表面应力较大的区域,经过后续处理有效防止固溶处理过程中形核,或者去除回复过程中已经形成的再结晶晶粒核心。Use hand-held electric, pneumatic or other polishing equipment to polish and repair the blades to remove areas with greater stress on the blade surface. After subsequent treatment, it can effectively prevent nucleation during the solid solution treatment process, or remove the core of recrystallized grains that have formed during the recovery process. .

采用局部电解加工等非机械抛磨的方式去除所有的机械抛磨痕迹,防止抛磨的塑性变形在固溶处理过程中形核。由于机械抛磨在表面会形成严重的塑性变形层,尽管厚度较薄,但在固溶处理过程中依然会促使再结晶晶粒的形成。对于上述小心操作下的机械抛磨,变形层很薄,非机械方式可以有效去除。Use non-mechanical polishing methods such as local electrolytic machining to remove all mechanical polishing traces to prevent the plastic deformation caused by polishing from nucleating during the solution treatment process. Since mechanical polishing will form a severe plastic deformation layer on the surface, although the thickness is thin, it will still promote the formation of recrystallized grains during the solution treatment process. For the above-mentioned mechanical polishing with careful operation, the deformed layer is very thin and can be effectively removed by non-mechanical methods.

优选的是,步骤一中,采用由低温向高温逐步递进的梯度回复处理工艺,具体工艺为:以2-5℃/min的升温速率,从室温加热到400-600℃,保温5-6h;以2-5℃/min的升温速率,继续加热到650-700℃,保温4-5h;以2-5℃/min的升温速率,继续加热到870-900℃,保温1-2h;以2-5℃/min的升温速率,继续加热到1100-1150℃,保温1-2h;以2-5℃/min的升温速率,继续加热到1200-1250℃,保温0.5-1h;以2-5℃/min的升温速率,继续加热到1250-1280℃,保温0.5-1h;随炉冷却到280-300℃,出炉。Preferably, in step one, a gradient recovery treatment process is adopted that gradually progresses from low temperature to high temperature. The specific process is: heating from room temperature to 400-600°C at a heating rate of 2-5°C/min, and holding the temperature for 5-6 hours. ; Continue heating to 650-700°C at a heating rate of 2-5°C/min and keep warm for 4-5 hours; Continue heating to 870-900°C at a heating rate of 2-5°C/min and keep warm for 1-2 hours; At a heating rate of 2-5℃/min, continue to heat to 1100-1150℃ and keep warm for 1-2h; at a heating rate of 2-5℃/min, continue to heat to 1200-1250℃ and keep warm for 0.5-1h; at a heating rate of 2-5℃/min, keep warm for 0.5-1h; At a heating rate of 5°C/min, continue to heat to 1250-1280°C and keep warm for 0.5-1h; then cool to 280-300°C and come out of the oven.

在上述任一方案中优选的是,步骤二中,采用的机械抛磨工具为手持式电动磨削工具或者手持式气动磨削工具,磨头粒度为80-120目,打磨厚度为0.02-0.05mm。In any of the above solutions, it is preferred that in step two, the mechanical polishing tool used is a handheld electric grinding tool or a handheld pneumatic grinding tool, the grinding head size is 80-120 mesh, and the grinding thickness is 0.02-0.05 mm.

在上述任一方案中优选的是,步骤三中,采用局部电解加工的方式去除机械抛磨的痕迹,对经过机械抛磨的叶片局部进行电解腐蚀或者电解抛光。In any of the above solutions, it is preferred that in step three, local electrolytic machining is used to remove traces of mechanical polishing, and the mechanically polished blades are partially electrolytically etched or polished.

在上述任一方案中优选的是,在局部电解加工过程中,将叶片作为阳极,采用高温合金材料作为阴极;电解液的配比为NaCl:HCl:H2O=1-3g:1-5ml:100ml,电压为5-30V,电流为7-15A,电解加工的时间为5-10s。电解加工过程中可以采用低电压(如5-6V的电压)进行电解腐蚀,也可以采用高电压进行电解抛光,由于采用人工操作,所以电压需控制在36V以下的安全电压范围内。本发明经过大量试验证明,电解液的配比控制在NaCl:HCl:H2O=1-3g:1-5ml:100ml范围内,电解加工的时间控制在5-10s范围内,能够确保充分去除加工痕迹,而且不会破坏没有加工痕迹的区域。In any of the above solutions, it is preferred that during the local electrolytic processing, the blade is used as the anode and the high-temperature alloy material is used as the cathode; the electrolyte ratio is NaCl:HCl:H 2 O=1-3g:1-5ml :100ml, voltage is 5-30V, current is 7-15A, electrolytic processing time is 5-10s. During the electrolytic machining process, low voltage (such as 5-6V voltage) can be used for electrolytic corrosion, or high voltage can be used for electrolytic polishing. Due to manual operation, the voltage needs to be controlled within a safe voltage range below 36V. The present invention has proved through a large number of experiments that the proportion of electrolyte is controlled within the range of NaCl:HCl: H2O =1-3g:1-5ml:100ml, and the electrolytic processing time is controlled within the range of 5-10s, which can ensure sufficient removal Processing marks, and will not damage areas without processing marks.

在上述任一方案中优选的是,步骤三中,采用化学腐蚀的方式去除机械抛磨的痕迹,将叶片全部浸泡于腐蚀液中进行腐蚀。由于采用手动进行机械抛磨,加工过程中塑性变形的深度较浅,所以也可以采用化学腐蚀的方式去除全部机械抛磨的痕迹。In any of the above solutions, preferably, in step three, chemical etching is used to remove traces of mechanical polishing, and all the blades are immersed in the corrosive liquid for corrosion. Since manual mechanical polishing is used, the depth of plastic deformation during processing is shallow, so chemical etching can also be used to remove all traces of mechanical polishing.

在上述任一方案中优选的是,在化学腐蚀过程中,腐蚀液的配比为HCl:H2O2=100ml:10-15ml。In any of the above solutions, it is preferred that during the chemical etching process, the ratio of the corrosive liquid is HCl:H 2 O 2 =100ml:10-15ml.

在上述任一方案中优选的是,步骤四中,固溶处理工艺为:将单晶高温合金叶片放置于真空热处理炉内,以10℃/min的升温速率,从室温加热到1290℃,保温1h;以10℃/min的升温速率,继续加热到1300℃,保温2h;以10℃/min的升温速率,继续加热到1315℃,保温4h。In any of the above solutions, it is preferred that in step four, the solid solution treatment process is: place the single crystal high-temperature alloy blade in a vacuum heat treatment furnace, heat from room temperature to 1290°C at a temperature rise rate of 10°C/min, and maintain the temperature. 1h; continue heating to 1300℃ at a heating rate of 10℃/min and keep warm for 2h; continue heating to 1315℃ at a heating rate of 10℃/min and keep warm for 4h.

在上述任一方案中优选的是,步骤四中,时效处理工艺为:待固溶处理工艺结束后,强制冷却到550℃;以10℃/min的升温速率加热到1120℃,保温4h,然后强制冷却到550℃;以10℃/min的升温速率加热到870℃,保温32h,然后强制冷却到300℃,出炉。In any of the above solutions, it is preferred that in step four, the aging treatment process is: after the solution treatment process is completed, forced cooling to 550°C; heating to 1120°C at a heating rate of 10°C/min, holding for 4 hours, and then Forced cooling to 550°C; heating to 870°C at a heating rate of 10°C/min, holding for 32 hours, then forced cooling to 300°C, and released from the oven.

本发明的预防单晶高温合金叶片局部再结晶的方法,具有如下有益效果:The method of preventing partial recrystallization of single crystal high-temperature alloy blades of the present invention has the following beneficial effects:

1、首先进行回复处理,能够有效去除叶片局部应力集中处的铸造残余应力或者说应力集中累积到叶片表面,然后采用机械抛磨的方式高效去除局部应力集中结构,最后采用局部电解加工或者其他非机械抛磨的方式消除机械抛磨引起的塑性变形,从而有效的避免了由于叶片铸件局部存在较大的铸造残余应力集中而导致在后续固溶处理过程中产生再结晶。1. First, a recovery treatment is performed, which can effectively remove the casting residual stress at the local stress concentration of the blade, or the stress concentration accumulates on the blade surface. Then, mechanical polishing is used to efficiently remove the local stress concentration structure, and finally local electrolytic machining or other non-concentrated parts are used. Mechanical polishing eliminates plastic deformation caused by mechanical polishing, thereby effectively avoiding recrystallization during the subsequent solution treatment process due to the large local casting residual stress concentration in the blade casting.

2、采用机械抛磨可以实现大余量的加工处理,能够高效去除单晶叶片局部存在的较大残余应力区域,采用电解加工等非机械抛磨的方式可以进一步去除机械抛磨带来的塑性变形,从而有效的预防了单晶叶片局部出现较大的再结晶晶粒。2. The use of mechanical polishing can achieve large margin processing and can effectively remove the large residual stress areas that exist locally in single crystal blades. The use of non-mechanical polishing methods such as electrolytic processing can further remove the plasticity caused by mechanical polishing. deformation, thereby effectively preventing the local occurrence of larger recrystallized grains in the single crystal blade.

附图说明Description of the drawings

图1为按照本发明预防单晶高温合金叶片局部再结晶的方法的一优选实施例中消除了再结晶的叶片照片,处理顺序依次为:回复处理、机械抛磨、电解加工、固溶时效处理;Figure 1 is a photo of a blade in which recrystallization has been eliminated in a preferred embodiment of the method for preventing local recrystallization of single crystal high-temperature alloy blades according to the present invention. The processing sequence is: recovery treatment, mechanical polishing, electrolytic processing, and solid solution aging treatment. ;

图2为未按照本发明预防单晶高温合金叶片局部再结晶的方法的一对比例中发生了再结晶的叶片照片,处理顺序依次为:机械抛磨、电解加工、回复处理、固溶时效处理。Figure 2 is a photo of a blade that has recrystallized in a pair of examples of a method for preventing local recrystallization of single crystal high-temperature alloy blades that does not follow the present invention. The processing sequence is: mechanical polishing, electrolytic processing, recovery treatment, and solid solution aging treatment. .

图中标注说明:1-再结晶晶粒。Annotations in the figure: 1-Recrystallized grains.

具体实施方式Detailed ways

为了更进一步了解本发明的发明内容,下面将结合具体实施例详细阐述本发明。In order to further understand the content of the present invention, the present invention will be described in detail below with reference to specific embodiments.

实施例一:Example 1:

按照本发明预防单晶高温合金叶片局部再结晶的方法的一优选实施例,按照先后顺序包括以下步骤:According to a preferred embodiment of the method for preventing partial recrystallization of single crystal high-temperature alloy blades of the present invention, the following steps are included in order:

步骤一:将单晶高温合金叶片放置于真空热处理炉内,进行回复处理;Step 1: Place the single crystal high-temperature alloy blade in a vacuum heat treatment furnace for recovery treatment;

步骤二:从真空热处理炉内取出单晶高温合金叶片,对叶片局部直接进行机械抛磨;Step 2: Take out the single crystal high-temperature alloy blade from the vacuum heat treatment furnace, and directly mechanically polish part of the blade;

步骤三:将机械抛磨后的单晶高温合金叶片进行清洗,然后采用局部电解加工或者化学腐蚀的方式去除机械抛磨的痕迹;Step 3: Clean the mechanically polished single crystal high-temperature alloy blades, and then use local electrolytic processing or chemical corrosion to remove traces of mechanical polishing;

步骤四:将单晶高温合金叶片进行固溶时效处理。Step 4: Perform solid solution aging treatment on the single crystal high-temperature alloy blades.

步骤一中,采用由低温向高温逐步递进的梯度回复处理工艺,具体工艺为:以2℃/min的升温速率,从室温加热到400℃,保温6h;以2℃/min的升温速率,继续加热到650℃,保温5h;以2℃/min的升温速率,继续加热到870℃,保温2h;以2℃/min的升温速率,继续加热到1100℃,保温2h;以2℃/min的升温速率,继续加热到1200℃,保温1h;以2℃/min的升温速率,继续加热到1250℃,保温1h;随炉冷却到280℃,出炉。In step one, a gradient recovery process is adopted that gradually progresses from low temperature to high temperature. The specific process is: heating from room temperature to 400°C at a heating rate of 2°C/min, and holding for 6 hours; at a heating rate of 2°C/min, Continue to heat to 650°C and keep warm for 5 hours; continue to heat to 870°C at a heating rate of 2°C/min and keep warm for 2 hours; continue heating to 1100°C at a heating rate of 2°C/min and keep warm for 2 hours; keep warm for 2 hours at a heating rate of 2°C/min. At a heating rate of 1200°C, keep warm for 1 hour; at a heating rate of 2°C/min, continue heating to 1250°C and keep warm for 1 hour; cool to 280°C and come out of the oven.

步骤二中,采用手持式电动磨削工具对叶片局部直接进行机械抛磨,磨头粒度为80目,打磨厚度为0.05mm。In step two, a handheld electric grinding tool is used to directly mechanically polish part of the blade. The grinding head size is 80 mesh and the grinding thickness is 0.05mm.

步骤三中,采用局部电解加工的方式去除机械抛磨的痕迹,在电解加工过程中,将叶片作为阳极,采用高温合金材料作为阴极;电解液的配比为NaCl:HCl:H2O=3g:5ml:100ml,电压为5V,电流为7A,电解加工的时间为10s。In step three, local electrolytic machining is used to remove traces of mechanical polishing. During the electrolytic machining process, the blade is used as the anode and the high-temperature alloy material is used as the cathode; the electrolyte ratio is NaCl:HCl:H 2 O=3g :5ml:100ml, the voltage is 5V, the current is 7A, and the electrochemical processing time is 10s.

步骤四中,固溶处理工艺为:将单晶高温合金叶片放置于真空热处理炉内,以10℃/min的升温速率,从室温加热到1290℃,保温1h;以10℃/min的升温速率,继续加热到1300℃,保温2h;以10℃/min的升温速率,继续加热到1315℃,保温4h。时效处理工艺为:待固溶处理工艺结束后,强制冷却到550℃;以10℃/min的升温速率加热到1120℃,保温4h,然后强制冷却到550℃;以10℃/min的升温速率加热到870℃,保温32h,然后强制冷却到300℃,出炉。采用淬火后通入氩气的方式进行强制冷却。In step four, the solid solution treatment process is: place the single crystal high-temperature alloy blade in a vacuum heat treatment furnace, heat it from room temperature to 1290°C at a heating rate of 10°C/min, and hold it for 1 hour; use a heating rate of 10°C/min. , continue to heat to 1300°C and keep warm for 2 hours; continue to heat to 1315°C at a heating rate of 10°C/min and keep warm for 4 hours. The aging treatment process is: after the solution treatment process is completed, forced cooling to 550°C; heating to 1120°C at a heating rate of 10°C/min, holding for 4 hours, and then forced cooling to 550°C; heating at a heating rate of 10°C/min. Heat to 870°C, keep warm for 32 hours, then force cool to 300°C and take it out of the oven. Forced cooling is performed by passing in argon gas after quenching.

本实施例选择二代单晶DD6涡轮叶片,共选择100个叶片同时进行再结晶消除处理,重点关注叶身与缘板的过渡圆角区域,因为该区域存在较大的残余应力。如图1所示,经过本实施例的方法处理后,完全消除了叶片局部的再结晶,合格率达到98%以上,即100个叶片中有98个叶片完全消除了再结晶。In this embodiment, second-generation single crystal DD6 turbine blades are selected, and a total of 100 blades are selected for recrystallization elimination processing at the same time, focusing on the transition fillet area between the blade body and the edge plate, because there is a large residual stress in this area. As shown in Figure 1, after being processed by the method of this embodiment, local recrystallization of the blades is completely eliminated, and the pass rate reaches more than 98%, that is, 98 blades out of 100 blades have completely eliminated recrystallization.

本实施例的预防单晶高温合金叶片局部再结晶的方法,处理顺序依次为:回复处理、机械抛磨、电解加工、固溶时效处理。在本领域中,技术人员普遍认为在单晶高温合金叶片固溶时效处理前应禁止使用机械方式直接处理叶片本体,若直接对叶片本体进行机械处理,则会促进固溶时效过程中再结晶的发生。而本实施例却克服了技术偏见,在叶片固溶时效处理前使用了机械方式直接处理叶片本体,并结合机械处理前对叶片进行回复处理的步骤,最终有效地避免了单晶高温合金叶片在固溶时效过程中发生再结晶。For the method of preventing partial recrystallization of single crystal high-temperature alloy blades in this embodiment, the processing sequence is: recovery treatment, mechanical polishing, electrolytic processing, and solid solution aging treatment. In this field, technicians generally believe that it is forbidden to use mechanical means to directly treat the blade body before solid solution aging treatment of single crystal superalloy blades. If the blade body is directly mechanically treated, it will promote recrystallization during the solid solution aging process. occur. However, this embodiment overcomes the technical bias and uses mechanical means to directly treat the blade body before the solid solution aging treatment, combined with the steps of restoring the blade before mechanical treatment, which ultimately effectively avoids the problem of single crystal high-temperature alloy blades being damaged. Recrystallization occurs during solid solution aging.

由低温向高温逐步递进的梯度回复处理,能够使铸造残余应力得到有效回复,残余应力较大时,单晶叶片局部表面已经形成了再结晶晶粒的核心。采用手持式电动抛磨设备抛修叶片,去除叶片表面应力较大的区域,经过后续处理有效防止固溶处理过程中形核,或者去除回复过程中已经形成的再结晶晶粒核心。采用局部电解加工的方式完全去除机械抛磨的痕迹,防止抛磨的塑性变形在固溶处理过程中形核。The gradual gradient recovery treatment from low temperature to high temperature can effectively recover the casting residual stress. When the residual stress is large, the core of recrystallized grains has been formed on the local surface of the single crystal blade. Use hand-held electric polishing equipment to polish and repair the blades to remove areas with greater stress on the blade surface. After subsequent treatment, it can effectively prevent nucleation during the solid solution treatment process, or remove the core of recrystallized grains that have formed during the recovery process. Local electrolytic machining is used to completely remove traces of mechanical polishing and prevent the plastic deformation caused by polishing from nucleating during the solid solution treatment process.

实施例二:Example 2:

按照本发明预防单晶高温合金叶片局部再结晶的方法的另一优选实施例,其工艺顺序、使用的设备、原理、有益效果等与实施例一基本相同,不同的是:According to another preferred embodiment of the method for preventing partial recrystallization of single crystal high-temperature alloy blades according to the present invention, the process sequence, equipment used, principles, beneficial effects, etc. are basically the same as those of Embodiment 1, except that:

步骤一中,采用由低温向高温逐步递进的梯度回复处理工艺,具体工艺为:以3℃/min的升温速率,从室温加热到500℃,保温5.5h;以3℃/min的升温速率,继续加热到680℃,保温4.5h;以3℃/min的升温速率,继续加热到885℃,保温1.5h;以3℃/min的升温速率,继续加热到1125℃,保温1.5h;以3℃/min的升温速率,继续加热到1225℃,保温0.75h;以3℃/min的升温速率,继续加热到1265℃,保温0.75h;随炉冷却到290℃,出炉。In step one, a gradient recovery process is used that gradually progresses from low temperature to high temperature. The specific process is: heating from room temperature to 500°C at a heating rate of 3°C/min, and holding for 5.5 hours; heating at a heating rate of 3°C/min. , continue to heat to 680°C and keep warm for 4.5h; continue to heat to 885°C at a heating rate of 3°C/min and keep warm for 1.5h; continue heating to 1125°C at a heating rate of 3°C/min and keep warm for 1.5h; At a heating rate of 3℃/min, continue to heat to 1225℃ and hold for 0.75h; at a heating rate of 3℃/min, continue to heat to 1265℃ and hold for 0.75h; cool to 290℃ with the furnace and release.

步骤二中,采用手持式电动磨削工具对叶片局部直接进行机械抛磨,磨头粒度为120目,打磨厚度为0.02mm。In step two, a handheld electric grinding tool is used to directly mechanically polish part of the blade. The grinding head size is 120 mesh and the grinding thickness is 0.02mm.

步骤三中,采用电解加工的方式去除机械抛磨的痕迹,在电解加工过程中,将叶片作为阳极,采用高温合金材料作为阴极;电解液的配比为NaCl:HCl:H2O=1g:3ml:100ml,电压为15V,电流为15A,电解加工的时间为8s。In step three, electrolytic machining is used to remove traces of mechanical polishing. During the electrolytic machining process, the blade is used as the anode and the high-temperature alloy material is used as the cathode; the electrolyte ratio is NaCl:HCl:H 2 O=1g: 3ml: 100ml, the voltage is 15V, the current is 15A, and the electrolytic processing time is 8s.

实施例三:Embodiment three:

按照本发明预防单晶高温合金叶片局部再结晶的方法的另一优选实施例,其工艺顺序、使用的设备、原理、有益效果等与实施例一基本相同,不同的是:According to another preferred embodiment of the method for preventing partial recrystallization of single crystal high-temperature alloy blades according to the present invention, the process sequence, equipment used, principles, beneficial effects, etc. are basically the same as those of Embodiment 1, except that:

步骤一中,采用由低温向高温逐步递进的梯度回复处理工艺,具体工艺为:以5℃/min的升温速率,从室温加热到600℃,保温5h;以5℃/min的升温速率,继续加热到700℃,保温4h;以5℃/min的升温速率,继续加热到900℃,保温1h;以5℃/min的升温速率,继续加热到1150℃,保温1h;以5℃/min的升温速率,继续加热到1250℃,保温0.5h;以5℃/min的升温速率,继续加热到1280℃,保温0.5h;随炉冷却到300℃,出炉。In step one, a gradient recovery process is adopted that gradually progresses from low temperature to high temperature. The specific process is: heating from room temperature to 600°C at a heating rate of 5°C/min, and holding for 5 hours; at a heating rate of 5°C/min, Continue to heat to 700°C and keep warm for 4 hours; continue to heat to 900°C at a heating rate of 5°C/min and keep warm for 1 hour; continue heating to 1150°C at a heating rate of 5°C/min and keep warm for 1 hour; continue heating to 900°C at a heating rate of 5°C/min and keep warm for 1 hour. At a heating rate of 1250℃, keep warm for 0.5h; at a heating rate of 5℃/min, continue heating to 1280℃ and keep warm for 0.5h; cool to 300℃ with the furnace and take it out.

步骤二中,采用手持式电动磨削工具对叶片局部直接进行机械抛磨,磨头粒度为120目,打磨厚度为0.03mm。In step two, a handheld electric grinding tool is used to directly mechanically polish part of the blade. The grinding head size is 120 mesh and the grinding thickness is 0.03mm.

步骤三中,采用电解加工的方式去除机械抛磨的痕迹,在电解加工过程中,将叶片作为阳极,采用高温合金材料作为阴极;电解液的配比为NaCl:HCl:H2O=2g:1ml:100ml,电压为10V,电流为12A,电解加工的时间为5s。In step three, electrolytic machining is used to remove traces of mechanical polishing. During the electrolytic machining process, the blade is used as the anode and the high-temperature alloy material is used as the cathode; the electrolyte ratio is NaCl:HCl:H 2 O=2g: 1ml: 100ml, the voltage is 10V, the current is 12A, and the electrolytic processing time is 5s.

实施例四:Embodiment 4:

按照本发明预防单晶高温合金叶片局部再结晶的方法的另一优选实施例,其工艺顺序、使用的设备、原理、有益效果等与实施例一至实施例三基本相同,不同的是:According to another preferred embodiment of the method for preventing partial recrystallization of single crystal high-temperature alloy blades according to the present invention, the process sequence, equipment used, principles, beneficial effects, etc. are basically the same as those in Embodiments 1 to 3, except that:

步骤三中,采用化学腐蚀的方式去除机械抛磨的痕迹,将叶片全部浸泡于腐蚀液中进行腐蚀,腐蚀液的配比为HCl:H2O2=100ml:10ml。In the third step, chemical etching is used to remove traces of mechanical polishing, and all the blades are immersed in the corrosive liquid for corrosion. The ratio of the corrosive liquid is HCl:H 2 O 2 =100ml:10ml.

本实施例选择二代单晶DD6涡轮叶片,共选择100个叶片同时进行再结晶消除处理,重点关注叶身与缘板的过渡圆角区域,因为该区域存在较大的残余应力。经过本实施例的方法处理后,完全消除了叶片局部的再结晶,合格率达到95%以上,即100个叶片中有95个叶片完全消除了再结晶。In this embodiment, second-generation single crystal DD6 turbine blades are selected, and a total of 100 blades are selected for recrystallization elimination processing at the same time, focusing on the transition fillet area between the blade body and the edge plate, because there is a large residual stress in this area. After being processed by the method of this embodiment, local recrystallization of the blades is completely eliminated, and the pass rate reaches more than 95%, that is, 95 blades out of 100 blades have completely eliminated recrystallization.

实施例五:Embodiment five:

按照本发明预防单晶高温合金叶片局部再结晶的方法的另一优选实施例,其工艺顺序、使用的设备、原理、有益效果等与实施例四基本相同,不同的是:According to another preferred embodiment of the method for preventing partial recrystallization of single crystal high-temperature alloy blades according to the present invention, the process sequence, equipment used, principles, beneficial effects, etc. are basically the same as those of Embodiment 4, except that:

步骤三中,采用化学腐蚀的方式去除机械抛磨的痕迹,将叶片全部浸泡于腐蚀液中进行腐蚀,腐蚀液的配比为HCl:H2O2=100ml:15ml。In the third step, chemical corrosion is used to remove traces of mechanical polishing, and all the blades are immersed in a corrosive liquid for corrosion. The ratio of the corrosive liquid is HCl:H 2 O 2 =100ml:15ml.

对比例一:Comparative Example 1:

对比例一未按照本发明的预防单晶高温合金叶片局部再结晶的方法进行处理,对比例一的处理顺序依次为:机械抛磨、电解加工、回复处理、固溶时效处理。Comparative Example 1 was not processed according to the method of preventing local recrystallization of single crystal high-temperature alloy blades of the present invention. The processing sequence of Comparative Example 1 was: mechanical polishing, electrolytic processing, recovery treatment, and solid solution aging treatment.

本对比例中,机械抛磨、电解加工、回复处理、固溶时效处理四个阶段的工艺参数以及所使用的设备等分别与实施例一的四个阶段完全相同,只是处理顺序不同。In this comparative example, the process parameters and equipment used in the four stages of mechanical polishing, electrolytic machining, recovery treatment, and solution aging treatment are exactly the same as those in the first embodiment, except that the processing sequence is different.

本对比例选择二代单晶DD6涡轮叶片,共选择100个叶片同时进行再结晶消除处理,重点关注叶身与缘板的过渡圆角区域,因为该区域存在较大的残余应力。如图2所示,经过本对比例的方法处理后,叶片合格率仅为48%,即100个叶片中仅有48个叶片完全消除了再结晶,从图2中能够明显看到再结晶晶粒1。In this comparison example, second-generation single crystal DD6 turbine blades were selected, and a total of 100 blades were selected for recrystallization elimination processing at the same time, focusing on the transition fillet area between the blade body and the edge plate, because there is a large residual stress in this area. As shown in Figure 2, after being processed by the method of this comparative example, the blade qualification rate is only 48%, that is, only 48 blades out of 100 blades have completely eliminated recrystallization. The recrystallized crystals can be clearly seen from Figure 2. 1 grain.

对比例二:Comparative Example 2:

对比例二未按照本发明的预防单晶高温合金叶片局部再结晶的方法进行处理,对比例二的处理顺序依次为:机械抛磨、电解加工、固溶时效处理。Comparative Example 2 was not processed according to the method of preventing local recrystallization of single crystal high-temperature alloy blades of the present invention. The processing sequence of Comparative Example 2 was: mechanical polishing, electrolytic processing, and solid solution aging treatment.

本对比例中,机械抛磨、电解加工、固溶时效处理三个阶段的工艺参数以及所使用的设备等分别与实施例一完全相同,只是没有进行回复处理。In this comparative example, the process parameters and equipment used in the three stages of mechanical polishing, electrolytic processing, and solution aging treatment are exactly the same as those in Example 1, except that no recovery treatment is performed.

本对比例选择二代单晶DD6涡轮叶片,共选择100个叶片同时进行再结晶消除处理,重点关注叶身与缘板的过渡圆角区域,因为该区域存在较大的残余应力。经过本对比例的方法处理后,叶片合格率仅为13%,即100个叶片中仅有13个叶片完全消除了再结晶。In this comparison example, second-generation single crystal DD6 turbine blades were selected, and a total of 100 blades were selected for recrystallization elimination processing at the same time, focusing on the transition fillet area between the blade body and the edge plate, because there is a large residual stress in this area. After being processed by the method of this comparative example, the blade qualification rate is only 13%, that is, only 13 blades out of 100 blades have completely eliminated recrystallization.

特别说明:本发明的技术方案中涉及了诸多参数,需要综合考虑各个参数之间的协同作用,才能获得本发明的有益效果和显著进步。而且技术方案中各个参数的取值范围都是经过大量试验才获得的,针对每一个参数以及各个参数的相互组合,发明人都记录了大量试验数据,限于篇幅,在此不公开具体试验数据。Special note: The technical solution of the present invention involves many parameters, and the synergy between each parameter needs to be comprehensively considered in order to obtain the beneficial effects and significant progress of the present invention. Moreover, the value range of each parameter in the technical solution was obtained through a large number of tests. For each parameter and the combination of each parameter, the inventor has recorded a large amount of test data. Due to space limitations, the specific test data will not be disclosed here.

本领域技术人员不难理解,本发明的预防单晶高温合金叶片局部再结晶的方法包括上述本发明说明书的发明内容和具体实施方式部分以及附图所示出的各部分的任意组合,限于篇幅并为使说明书简明而没有将这些组合构成的各方案一一描述。凡在本发明的精神和原则之内,所做的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。It is easy for those skilled in the art to understand that the method for preventing local recrystallization of single crystal high-temperature alloy blades of the present invention includes any combination of the above-mentioned content of the invention and the specific embodiments of the description of the present invention and the various parts shown in the drawings. The length is limited. In order to make the description concise, each scheme composed of these combinations is not described one by one. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention shall be included in the protection scope of the present invention.

Claims (4)

1. A method for preventing local recrystallization of a single crystal superalloy blade comprises the following steps in sequence:
step one: placing the monocrystal superalloy blade into a vacuum heat treatment furnace for recovery treatment;
step two: taking out the single-crystal superalloy blade from the vacuum heat treatment furnace, and directly mechanically polishing and grinding part of the blade;
step three: cleaning the mechanically polished single-crystal superalloy blade, and removing mechanically polished traces by adopting a local electrolytic machining or chemical corrosion mode;
step four: carrying out solid solution aging treatment on the monocrystal superalloy blade;
in the first step, a gradient recovery treatment process gradually progressing from low temperature to high temperature is adopted, and the specific process is that the temperature is heated to 400-600 ℃ from room temperature at a heating rate of 2-5 ℃/min, and the temperature is kept for 5-6h; continuously heating to 650-700 ℃ at a heating rate of 2-5 ℃/min, and preserving heat for 4-5h; continuously heating to 870-900 ℃ at the heating rate of 2-5 ℃/min, and preserving heat for 1-2h; continuously heating to 1100-1150 ℃ at a heating rate of 2-5 ℃/min, and preserving heat for 1-2h; continuously heating to 1200-1250 ℃ at a heating rate of 2-5 ℃/min, and preserving heat for 0.5-1h; continuously heating to 1250-1280 ℃ at a heating rate of 2-5 ℃/min, and preserving heat for 0.5-1h; cooling to 280-300 ℃ along with the furnace, and discharging;
in the second step, the adopted mechanical polishing tool is a hand-held electric grinding tool or a hand-held pneumatic grinding tool, the granularity of the grinding head is 80-120 meshes, and the polishing thickness is 0.02-0.05mm;
in the third step, in the local electrolytic machining process, the blade is used as an anode, and a high-temperature alloy material is used as a cathode; the electrolyte is prepared from NaCl, HCl and H 2 O=1-3 g:1-5ml:100ml, voltage 5-30V, current 7-15A, electrolytic processing time 5-10s.
2. The method for preventing localized recrystallization of single crystal superalloy blades according to claim 1, wherein: and thirdly, removing the trace of mechanical polishing by adopting a local electrolytic machining mode, and carrying out electrolytic corrosion or electrolytic polishing on the local part of the blade subjected to mechanical polishing.
3. The method for preventing localized recrystallization of single crystal superalloy blades according to claim 1, wherein: and thirdly, removing the trace of mechanical polishing and grinding by adopting a chemical corrosion mode, and completely soaking the blade in a corrosion liquid for corrosion.
4. A method of preventing localized recrystallization of a single crystal superalloy blade according to claim 3, wherein: in the chemical etching process, the ratio of the etching liquid is HCl to H 2 O 2 =100ml:10-15ml。
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CN113969341A (en) * 2021-10-27 2022-01-25 北京航空航天大学 A kind of anti-recrystallization heat treatment method in the preparation process of cast turbine blade
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