CN106756685A - A kind of method for refining nickel-based high-temperature alloy forge piece grain structure - Google Patents
A kind of method for refining nickel-based high-temperature alloy forge piece grain structure Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000000956 alloy Substances 0.000 title claims abstract description 24
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 23
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 20
- 238000007670 refining Methods 0.000 title abstract description 10
- 238000005242 forging Methods 0.000 claims abstract description 68
- 238000001953 recrystallisation Methods 0.000 claims abstract description 16
- 239000006104 solid solution Substances 0.000 claims abstract description 10
- 238000005516 engineering process Methods 0.000 claims abstract description 3
- 229910000601 superalloy Inorganic materials 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims 3
- 238000002791 soaking Methods 0.000 claims 1
- 238000004321 preservation Methods 0.000 abstract description 10
- 238000010791 quenching Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 150000002815 nickel Chemical class 0.000 abstract description 2
- 230000000171 quenching effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
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- Mechanical Engineering (AREA)
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Abstract
本发明公开了一种细化镍基高温合金锻件晶粒组织的方法,其特征在于采用中间保温的双道次变应变速率工艺促进材料发生完全再结晶,包括如下步骤:(1)将镍基高温合金锻坯进行固溶预处理,然后立即淬火;(2)将步骤1获得的锻坯加热至970℃~1010℃,保温至锻坯温度均匀后,采用中间保温的双道次变应变速率工艺对坯料施加变形:第一道次锻坯的应变速率为0.05s‑1~0.1s‑1,第一道次锻坯的变形量为20%~35%,第二道次锻坯的应变速率为0.01s‑1~0.001s‑1,两道次间的间隔时间为60s~240s,锻坯两道次的总变形量为50%~60%;(3)变形结束后,立即对锻件淬火。本发明能有效地以较小的总变形量达到细化镍基高温合金锻件晶粒组织的目的,为镍基高温合金锻件的品质跃升提供了新技术。The invention discloses a method for refining the grain structure of a nickel-based high-temperature alloy forging, which is characterized in that a double-pass variable strain rate process of intermediate heat preservation is adopted to promote complete recrystallization of the material, including the following steps: (1) the nickel-based The high-temperature alloy forging billet is subjected to solid solution pretreatment, and then quenched immediately; (2) The forging billet obtained in step 1 is heated to 970 ° C ~ 1010 ° C, and after the forging billet is kept at a uniform temperature, the double-pass variable strain rate of intermediate heat preservation is adopted. The process applies deformation to the billet: the strain rate of the first pass forging billet is 0.05s ‑1 ~ 0.1s ‑1 , the deformation amount of the first pass forging billet is 20% to 35%, and the strain rate of the second pass forging billet The speed is 0.01s ‑1 to 0.001s ‑1 , the interval between two passes is 60s to 240s, and the total deformation of the two passes of the forging billet is 50% to 60%; (3) After the deformation is completed, the forging is immediately Quenching. The invention can effectively achieve the purpose of refining the grain structure of nickel-based high-temperature alloy forgings with a small total deformation amount, and provides a new technology for the quality improvement of nickel-based high-temperature alloy forgings.
Description
技术领域:Technical field:
本发明属于锻造技术领域,涉及一种细化镍基高温合金锻件晶粒组织的方法。The invention belongs to the technical field of forging, and relates to a method for refining the grain structure of nickel-based superalloy forgings.
背景技术:Background technique:
镍基高温合金具有较高的强度和塑性、良好的耐腐蚀和抗氧化性能,以及良好的疲劳性能,是目前航空领域中应用最广泛的合金材料之一,被广泛的应用于制造航空发动机涡轮盘、机匣、压气机盘和叶片等关键零件。Nickel-based superalloys have high strength and plasticity, good corrosion resistance and oxidation resistance, and good fatigue properties. They are currently one of the most widely used alloy materials in the aviation field and are widely used in the manufacture of aero-engine turbines. Key parts such as discs, casings, compressor discs and blades.
细化晶粒组织是锻件生产制造过程中的一个重要目标。锻造等热成形工艺之所以能细化晶粒组织,是因为材料在热变形过程中会发生动态再结晶行为。然而,对于镍基高温合金在单道次以及恒定的工况(温度、应变速率)变形时,需要较大应变才能发生完全动态再结晶,如对于GH4169合金,在变形温度980℃和应变速率0.001s-1,使其发生95%的动态再结晶所需等效应变达到1.7(相当于变形程度82%)。显然,在实际模锻过程中,这样的大应变是难以达到的。虽然增大变形温度和降低应变速率,可以降低动态再结晶完全发生所需的应变,但是其会增大动态再结晶晶粒尺寸,明显地影响了晶粒细化效果。因此,急需发明一种新方法,利用该方法既能有效地降低镍基高温合金动态再结晶发生完全所需的应变,又能使得其再结晶晶粒组织细小。Refining the grain structure is an important goal in the manufacturing process of forgings. The reason why hot forming processes such as forging can refine the grain structure is because the material will undergo dynamic recrystallization behavior during hot deformation. However, when the nickel-based superalloy is deformed in a single pass and under constant working conditions (temperature, strain rate), a large strain is required for complete dynamic recrystallization to occur. For example, for the GH4169 alloy, at a deformation temperature of 980°C and a strain rate of s -1 , the equivalent strain required for 95% dynamic recrystallization to reach 1.7 (equivalent to 82% deformation). Obviously, in the actual die forging process, such a large strain is difficult to achieve. Although increasing the deformation temperature and decreasing the strain rate can reduce the strain required for dynamic recrystallization to occur completely, it will increase the grain size of dynamic recrystallization, which obviously affects the grain refinement effect. Therefore, there is an urgent need to invent a new method, which can not only effectively reduce the strain required for the dynamic recrystallization of nickel-based superalloys to occur completely, but also make the recrystallized grain structure fine.
发明内容:Invention content:
本发明的目的在于提供一种细化镍基高温合金锻件晶粒组织的方法,其特征是采用中间保温的双道次变应变速率工艺促进合金发生完全的再结晶,且无需增加变形温度或降低终锻阶段的应变速率,从而达到以较小的总变形量细化镍基高温合金锻件晶粒组织的目的,解决了现有方法难以在较小的应变条件下得到动态再结晶程度完全、晶粒细小的镍基高温合金锻件晶粒组织的难题。The purpose of the present invention is to provide a method for refining the grain structure of nickel-based superalloy forgings, which is characterized in that the double-pass variable strain rate process of intermediate heat preservation is used to promote the complete recrystallization of the alloy without increasing the deformation temperature or reducing the The strain rate in the final forging stage can be adjusted to achieve the purpose of refining the grain structure of nickel-based superalloy forgings with a small amount of total deformation. Difficulties in the grain structure of nickel-based superalloy forgings with fine grains.
本发明解决上述难题的方案是:The scheme that the present invention solves the above-mentioned difficult problem is:
步骤1:将镍基高温合金锻坯进行固溶预处理,然后立即淬火;固溶预处理的工艺为:将锻坯加热至1010~1040℃保温,保温时间为0.7小时~0.9小时;Step 1: Perform solid solution pretreatment on the nickel-based superalloy forging billet, and then quench immediately; the process of solid solution pretreatment is: heating the forging billet to 1010-1040°C for 0.7-0.9 hours;
步骤2:将步骤1获得的锻坯加热至970℃~1010℃,保温至锻坯温度均匀后,采用中间保温的双道次变应变速率工艺对坯料施加变形;其具体工艺为:第一道次锻坯的应变速率为0.05s-1~0.1s-1,第一道次锻坯的变形量为20%~35%,第二道次锻坯的应变速率为0.01s-1~0.001s-1,两道次间的间隔时间为60s~240s,锻坯两道次的总变形量为50%~60%;Step 2: Heat the forged billet obtained in step 1 to 970°C to 1010°C, keep it warm until the temperature of the forged billet is uniform, and apply deformation to the billet by using a double-pass variable strain rate process with intermediate heat preservation; the specific process is: the first pass The strain rate of the secondary forging blank is 0.05s -1 ~ 0.1s -1 , the deformation of the first pass forging blank is 20% ~ 35%, and the strain rate of the second pass forging blank is 0.01s -1 ~ 0.001s -1 , the interval between two passes is 60s~240s, and the total deformation of the two passes of the forging billet is 50%~60%;
步骤3:变形结束后,立即对锻件淬火。Step 3: Quench the forging immediately after deformation.
本发明的有益效果为:该方法充分利用了变形—位错—双道次保温—亚动态和动态再结晶的相互作用机制,最终实现了以相对较小的总变形量达到细化镍基高温合金锻件晶粒组织的目的,为镍基高温合金锻件的品质跃升提供了新技术。The beneficial effects of the present invention are: the method makes full use of the interaction mechanism of deformation-dislocation-double-pass heat preservation-metadynamic and dynamic recrystallization, and finally realizes the refinement of nickel-based high temperature with relatively small total deformation The purpose of the grain structure of alloy forgings provides a new technology for the quality improvement of nickel-based superalloy forgings.
附图说明:Description of drawings:
图1 GH4169合金锻坯经过固溶预处理之后的组织;Fig. 1 Microstructure of GH4169 alloy forging blank after solid solution pretreatment;
图2实施例1的应变速率—应变曲线;The strain rate-strain curve of Fig. 2 embodiment 1;
图3实施例1采用中间保温的双道次变应变速率工艺获得的GH4169合金锻件的晶粒组织;Fig. 3 Example 1 adopts the grain structure of the GH4169 alloy forging obtained by the double-pass variable strain rate process of intermediate heat preservation;
图4实施例1对比实验获得的GH4169合金锻件的晶粒组织:(a)恒应变速率为0.1s-1;(b)恒应变速率为0.01s-1;(c)变应变速率0.1s-1-0.01s-1;Figure 4 The grain structure of the GH4169 alloy forging obtained in the comparative experiment of Example 1: (a) constant strain rate is 0.1s -1 ; (b) constant strain rate is 0.01s -1 ; (c ) variable strain rate is 0.1s -1 1-0.01s -1 ;
图5实施例2的应变速率—应变曲线;The strain rate-strain curve of Fig. 5 embodiment 2;
图6实施例2采用中间保温的双道次变应变速率工艺获得的GH4169合金锻件的晶粒组织;Fig. 6 Example 2 adopts the grain structure of the GH4169 alloy forging obtained by the double-pass variable strain rate process of intermediate heat preservation;
图7实施例2对比实验获得的GH4169合金锻件的晶粒组织:(a)恒应变速率为0.1s-1;(b)恒应变速率为0.001s-1;(c)变应变速率0.1s-1-0.001s-1。Fig. 7 The grain structure of the GH4169 alloy forging obtained in the comparative experiment of Example 2: (a) constant strain rate is 0.1s -1 ; (b) constant strain rate is 0.001s -1 ; (c ) variable strain rate is 0.1s -1 1 -0.001s -1 .
具体实施方式:detailed description:
下面结合附图和具体实施方式对本发明进行详细说明。The present invention will be described in detail below in conjunction with the accompanying drawings and specific embodiments.
本发明是一种细化镍基高温合金锻件晶粒组织的方法,下面所有实施例中均选用典型的镍基高温合金—GH4169合金锻件为对象,其化学成分如表1所示。The present invention is a method for refining the grain structure of a nickel-based superalloy forging. In all the following examples, a typical nickel-based superalloy—GH4169 alloy forging is selected as the object, and its chemical composition is shown in Table 1.
表1本发明实例中所用材料的GH4169合金成分(wt.%)The GH4169 alloy composition (wt.%) of material used in the example of the present invention in table 1
实施例1Example 1
步骤1:将GH4169合金锻坯进行固溶预处理,然后立即淬火;固溶预处理的工艺为:将锻坯加热至1040℃保温,保温时间为0.75小时;GH4169合金锻坯经步骤1的预处理之后的组织如图1所示,通过固溶处理,得到了均匀的晶粒组织,通过截线法可以测得其平均晶粒尺寸约为75μm。Step 1: Perform solid solution pretreatment on the GH4169 alloy forging billet, and then quench immediately; the process of solid solution pretreatment is: heat the forging billet to 1040°C for 0.75 hours; The structure after treatment is shown in Figure 1. Through solution treatment, a uniform grain structure is obtained, and the average grain size can be measured by the intercept method to be about 75 μm.
步骤2:将步骤1获得的锻坯加热至1010℃,保温至锻坯温度均匀后,采用中间保温的双道次变应变速率工艺对坯料施加变形:第一道次锻坯的应变速率为0.1s-1,第一道次锻坯的变形量为30%(真应变0.35),第二道次锻坯的应变速率为0.01s-1,两道次间的间隔时间为60s,锻坯经历两阶段变形后的总变形量为60%(真应变0.92);实施例1的应变速率与应变的关系如图2所示。Step 2: Heat the forging billet obtained in step 1 to 1010°C, keep it warm until the temperature of the forging billet is uniform, and apply deformation to the billet by adopting the double-pass variable strain rate process of intermediate heat preservation: the strain rate of the first pass forging billet is 0.1 s -1 , the deformation of the first pass forging blank is 30% (true strain 0.35), the strain rate of the second pass forging blank is 0.01s -1 , the interval between two passes is 60s, the forging blank has experienced The total deformation after the two-stage deformation is 60% (true strain 0.92); the relationship between the strain rate and the strain in Example 1 is shown in Figure 2.
步骤3:变形结束后,立即对锻坯淬火。Step 3: Immediately after the deformation, the forging billet is quenched.
对GH4169合金锻件进行金相观察,结果如图3所示。对比图3和图1可知,本发明的方法可以达到促进GH4169合金动态再结晶发生完全、细化晶粒组织的目的。为了证明本发明方法的优越性,进行了对比实验,对比实验所选用的变形温度和锻坯的总变形量与本发明实施例1相同,区别在于对比实验采用恒应变速率以及无保温的变应变速率方式进行变形。图4(a)所示为以恒应变速率0.1s-1变形至总变形量60%(真应变0.92)时获得金相组织;图4(b)所示为以恒应变速率0.01s-1变形至总变形量60%(真应变0.92)时获得金相组织。图4(c)所示为先以恒应变速率0.1s-1变形至总变形量30%(真应变0.35),然后迅速降低应变速率至0.01s-1,再压缩至总变形量60%(真应变0.92)时获得的金相组织。由图4(a)可知,以恒应变速率0.1s-1变形至60%的变形量,在原始大晶界周围只发现少量的动态再结晶晶粒,金属组织以原始大晶粒为主。而在图4(b)和(c)中,也只发生了部分的动态再结晶,金相组织为混晶,未达到晶粒细化效果。因此,对比实验证明了本发明提出的方法具有优越性。The metallographic observation of the GH4169 alloy forging is shown in Figure 3. Comparing Fig. 3 and Fig. 1, it can be seen that the method of the present invention can achieve the purpose of promoting the dynamic recrystallization of GH4169 alloy completely and refining the grain structure. In order to prove the superiority of the method of the present invention, a comparative experiment has been carried out. The selected deformation temperature and the total deformation of the forging blank in the comparative experiment are the same as in Example 1 of the present invention. The difference is that the comparative experiment adopts constant strain rate and variable strain without heat preservation. Velocity mode for deformation. Figure 4(a) shows the metallographic structure obtained when the strain is deformed at a constant strain rate of 0.1s -1 to a total deformation of 60% (true strain 0.92 ) ; The metallographic structure is obtained when the deformation reaches 60% of the total deformation (true strain 0.92). Figure 4(c) shows that the deformation is first performed at a constant strain rate of 0.1s -1 to a total deformation of 30% (true strain 0.35), then the strain rate is rapidly reduced to 0.01s -1 , and then compressed to a total deformation of 60% ( The metallographic structure obtained when the true strain is 0.92). It can be seen from Fig. 4(a) that only a small amount of dynamic recrystallized grains are found around the original large grain boundaries at a constant strain rate of 0.1s -1 to 60% deformation, and the metal structure is dominated by the original large grains. In Figure 4(b) and (c), only part of the dynamic recrystallization occurred, and the metallographic structure was mixed crystal, which did not achieve the effect of grain refinement. Therefore, comparative experiments have proved that the method proposed by the present invention has superiority.
实施例2Example 2
步骤1:将GH4169合金锻坯进行固溶预处理,然后立即淬火;固溶预处理的工艺为:将锻坯加热至1040℃保温,保温时间为0.75小时;GH4169合金锻坯经步骤1的预处理之后的组织如图1所示,通过固溶处理,得到了均匀的晶粒组织,通过截线法可以测得其平均晶粒尺寸约为75μm。Step 1: Perform solid solution pretreatment on the GH4169 alloy forging billet, and then quench immediately; the process of solid solution pretreatment is: heat the forging billet to 1040°C for 0.75 hours; The structure after treatment is shown in Figure 1. Through solution treatment, a uniform grain structure is obtained, and the average grain size can be measured by the intercept method to be about 75 μm.
步骤2:将步骤1获得的锻坯加热至980℃,保温至锻坯温度均匀后,采用中间保温的双道次变应变速率工艺对坯料施加变形:第一道次锻坯的应变速率为0.1s-1,第一道次锻坯的变形量为30%(真应变0.35),第二道次锻坯的应变速率为0.001s-1,两道次间的间隔时间为120s,锻坯经历两阶段变形后的总变形量为60%(真应变0.92);实施例1的应变速率与应变的关系如图5所示。Step 2: Heat the forging billet obtained in step 1 to 980°C, keep it warm until the temperature of the forging billet is uniform, and apply deformation to the billet by using the double-pass variable strain rate process of intermediate heat preservation: the strain rate of the forging billet in the first pass is 0.1 s -1 , the deformation of the first pass forging blank is 30% (true strain 0.35), the strain rate of the second pass forging blank is 0.001s -1 , the interval between two passes is 120s, the forging blank has experienced The total deformation after the two-stage deformation is 60% (true strain 0.92); the relationship between the strain rate and the strain in Example 1 is shown in Figure 5.
步骤3:变形结束后,立即对锻坯淬火。Step 3: Immediately after the deformation, the forging billet is quenched.
对GH4169合金锻件进行金相观察,结果如图6所示。对比图6和图1可知,本发明的方法可以达到促进GH4169合金动态再结晶发生完全、细化GH4169合金晶粒组织的目的。为了证明本发明方法的优越性,进行了对比实验,对比实验所选用的变形温度和锻坯的总变形量与本发明实施例1相同,区别在于对比实验采用恒应变速率以及无保温的变应变速率方式进行变形。图7(a)所示为以恒应变速率0.1s-1变形至总变形量60%(真应变0.92)时获得金相组织;图7(b)所示为以恒应变速率0.001s-1变形至总变形量60%(真应变0.92)时获得金相组织。图7(c)所示为先以恒应变速率0.1s-1变形至总变形量30%(真应变0.35),然后迅速降低应变速率至0.001s-1,再压缩至总变形量60%(真应变0.92)时获得的金相组织。由图7(a)可知,以恒应变速率0.1s-1变形至60%的变形量,在原始大晶界周围只发现少量的动态再结晶晶粒,金属组织以原始大晶粒为主。在图7(b)中,由于以恒应变速率0.1s-1变形至60%的变形量,使得动态再结晶程度较高,但金相组织中仍存在少量的原始大晶粒,动态再结晶程度不够完全。图7(c)与图7(b)结果类似。因此,对比实验证明了本发明提出的方法具有优越性。The metallographic observation of the GH4169 alloy forging is shown in Figure 6. Comparing Figure 6 and Figure 1, it can be seen that the method of the present invention can achieve the purpose of promoting the dynamic recrystallization of GH4169 alloy completely and refining the grain structure of GH4169 alloy. In order to prove the superiority of the method of the present invention, a comparative experiment has been carried out. The selected deformation temperature and the total deformation of the forging blank in the comparative experiment are the same as in Example 1 of the present invention. The difference is that the comparative experiment adopts constant strain rate and variable strain without heat preservation. Velocity mode for deformation. Figure 7(a) shows the metallographic structure obtained when the strain is deformed at a constant strain rate of 0.1s -1 to a total deformation of 60% (true strain 0.92 ) ; The metallographic structure is obtained when the deformation reaches 60% of the total deformation (true strain 0.92). Figure 7(c) shows that the deformation is first performed at a constant strain rate of 0.1s -1 to a total deformation of 30% (true strain 0.35), then the strain rate is rapidly reduced to 0.001s -1 , and then compressed to a total deformation of 60% ( The metallographic structure obtained when the true strain is 0.92). It can be seen from Fig. 7(a) that only a small amount of dynamic recrystallization grains are found around the original large grain boundaries when the deformation is carried out at a constant strain rate of 0.1s -1 to 60%, and the metal structure is dominated by the original large grains. In Figure 7(b), due to the deformation at a constant strain rate of 0.1s -1 to 60% deformation, the degree of dynamic recrystallization is relatively high, but there are still a small amount of original large grains in the metallographic structure, and dynamic recrystallization Not quite enough. Figure 7(c) is similar to the results in Figure 7(b). Therefore, comparative experiments have proved that the method proposed by the present invention has superiority.
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