CN102435484B - Method for corroding previous particle boundary (PPB) of powdery high-temperature alloy - Google Patents
Method for corroding previous particle boundary (PPB) of powdery high-temperature alloy Download PDFInfo
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- CN102435484B CN102435484B CN201010295304.7A CN201010295304A CN102435484B CN 102435484 B CN102435484 B CN 102435484B CN 201010295304 A CN201010295304 A CN 201010295304A CN 102435484 B CN102435484 B CN 102435484B
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Abstract
The invention discloses a method for corroding the previous particle boundary (PPB) of powdery high-temperature alloy, which is characterized by comprising the following steps: corroding the surface of the alloy subjected to polishing treatment by using a corrodent for 10-20s; and then, observing the PPB of the alloy under an optical microscope, wherein the volume ratio of all components of the corrodent is as follows: HCl:HNO3:H2O2=(93-95): (3-4): (2-3). The method has the advantages that the clear PPB can be corroded by using the method provided by the invention, and the traditional technical prejudice for the detection of the PPB in the industry is overcome.
Description
Technical field
The present invention relates to metallographic structure detection field in the high temperature alloy physico-chemical examination technique, the caustic solution on a kind of powder metallurgy superalloy primary granule border is provided especially.
Background technology
The powder metallurgy superalloy diskware is mainly used on the important rotatable parts in modern advanced aero engine hot junction, it is bearing the superposition effect of the thermal stress that mechanical stress and the temperature difference cause, thereby require material to there is enough mechanical properties and physicochemical property, serviceability temperature high (approximately 650 ℃～750 ℃) particularly, and require to have high as far as possible low all cyclic fatigues and thermal fatigue property in the serviceability temperature scope, these are all the key factors of determining the diskware mission life.Therefore, require powder metallurgy superalloy to meet crystal grain tiny, even tissue, without macrosegregation, alloy degree of changing into is high, and yield strength is high, and fatigue behaviour waits well technical requirement.
Yet, starting powder granule boundary (PPB) is the typical defect in the powder metallurgy superalloy foundry goods, it forms in powder process and forging forming process, diffusion and metallurgical binding between powder particle have been hindered, starting powder granule boundary (PPB), once formation is difficult to eliminate in heat treatment process subsequently, has formed fracture origin subsequently, if micro-crack forms, it will be opened along the primary granule border extension very soon, forms crackle.The mechanical properties such as low-alloyed impact, stretching, lasting, fatigue lifetime can fall in the existence of starting powder granule boundary (PPB).
The pattern characteristics that reflect objectively starting powder granule boundary (PPB) in conventional high power detects, be the important starting point of judgement powder metallurgy product metallurgical quality, is also further to carry out the basis that property indices is analyzed.
At present, there are Iron and Steel Research Geueral Inst and Beijing Research Inst. of Aeronautic Material in the main unit of domestic production aviation powder metallurgy superalloy, and main alloy species has FGH95, FGH96 and FGH97.Consult the pertinent literature of FGH95, FGH96, FGH97, consulting Beijing Research Inst. of Aeronautic Material and Beijing Iron and Steel Research Geueral Inst development experience to these three kinds of powder metallurgy superalloys, for a long time, China continues to use inertial thinking always, adopts the method for common high temperature alloy mirco structure corrosion to carry out the check of PPB.But seldom show PPB while adopting this kind of method to test.
Everybody generally believes that Kalling reagent is best for corroding the reagent of PPB.As clear in the technical standard Q/3B1780 " FGH96 alloy high temperature insostatic pressing (HIP) product " Iron and Steel Research Geueral Inst and aeromotor at dawn (group) Ltd draft jointly adopts Kalling reagent: 5gCuCl
2+ 100mlHCl+10mlCH
3cH
2oH carries out the check of PPB.Yet, adopt this mordant to be checked aborning and also seldom show PPB.
According to foreign literature " ASSESSMENT OF RUSSIAN P/M SUPERALLOYEP741NP ", Superalloys 2004 and " Techniques for microstructuralcharacterization of powder-processed nickel-based superalloys ", the record of MaterialsScience and Engineering A360 (2003) 390_395, powder metallurgy superalloy forging Kalling reagent (5gCuCl that adopt in microstructure examination for aviation more
2+ 100mlHCl+100mlC
2h
5o) corrosion sample surface, then under optical microscope to powder metallurgy superalloy in original granule boundary evaluate examination.In addition, external also PPB caustic solution commonly used is: at first sample is ground with fine sandpaper, then use 20%H
2sO
4+ 80%CH
3oH electropolishing 170mlH
3pO
4+ 10mlH
2sO
4+ 15gCrO
3electro-etching is checked PPB, and, for nickel base superalloy, mordant commonly used also has:
Kallings?no.2：40～80ml?C
2H
5O+40ml?HCl+2g?CuCl
2；
Marble：50ml?H
2O+50ml?HCl+10g?CuSO
4；
Glyceregia:15ml HCL+10ml glycerine+5ml HNO
3;
Modified Glyceregia:60ml glycerine+50ml HCl+10ml HNO
3.
Adopt above mordant to carry out the metallographic structure inspection, can demonstrate crystal boundary, for the evaluation of grain size, and can not clearly demonstrate accurately the starting powder granule boundary (PPB) of material.
And it is believed that by HCl, HNO in the past
3, H
2o
2the mordant that proportioning forms can only be used as conventional nickel-base alloy and high temperature alloy mordant, and for the grain size evaluation, as GH4169, and the composition proportion scope is larger.
Summary of the invention
The object of the present invention is to provide the caustic solution on a kind of powder metallurgy superalloy primary granule border, by this caustic solution, powder metallurgy superalloy is carried out to the high power etching detection, can better show the starting powder granule boundary (PPB) of failing to eliminate in powder forming and heat treatment process, form, distribution and the size that can reflect objectively original powder particle border (PPB) in powder metallurgy superalloy, thereby correct is judged the material situation, and then the combination property of reflection material.
The invention provides the caustic solution on a kind of powder metallurgy superalloy primary granule border, it is characterized in that: described method is that the alloy surface after using mordant to polishing is corroded, etching time is 10～20s, then on its primary granule border of optical microphotograph Microscopic observation; We carry out a large amount of tests by the proportioning that changes solvent, the time of placement, the time of etch etc., finally obtain conclusion: the volume ratio of each composition of mordant of employing:
HCl: HNO
3: H
2o
2be 93～95: 3～4: just can erode away original powder particle border (PPB) in powder metallurgy superalloy at 2～3 o'clock, yet the proportioning of volume ratio outside this scope all can not observe powder metallurgy superalloy in original powder particle border (PPB).
Wherein in preferred mordant, the volume relationship of each composition is: 95%HCl+3%HNO
3+ 2%H
2o
2.
HNO in this kind of mordant
3with H
2o
2all have strong oxidizing property, the γ ' that current potential is higher is preferentially corroded, and is conducive to sketch the contours of PPB.
And at present everybody always habitual Kalling mordant oxidisability a little less than, the crystal boundary that free energy is high is preferentially corroded, and is conducive to sketch the contours of crystal boundary, can not well sketch the contours of PPB.
Simultaneously, the specimen surface that uses conventional card woods reagent corrosion to manifest also demonstrates less PPB under optical microscope, only has the caustic solution provided by the invention of use just to can be observed obvious PPB.If what PPB was a large amount of is present in powder metallurgy superalloy, can significantly reduce plasticity and the high temperature endurance performance of material, in serious situation, even can cause product can not meet the request for utilization of work.Therefore, PPB belongs to the major defect that affects the powder metallurgy superalloy usability.Objectively demonstrate pattern, distribution, quantity and the size of the PPB existed in alloy structure, can be assessed the combination property of material.Because PPB forms in starting material powder process and high temperature insostatic pressing (HIP) forming process, there are direct impact in its temperature, vacuum tightness, powder size, forming pressure, compaction etc. on material structure again.By the analysis to the PPB form, can detect the process rationality of feedback product manufacture process, thereby become the foundation of adjusting process parameter, optimize the material Fabrication parameter, further improve the structure property level of product.
Scientific and reasonable PPB check is to guarantee that such product meets the necessary means of request for utilization steady operation.By conventional sample detection faces mechanical buffing, wiping, air-dry after, adopt selected solution in the present invention to carry out etch as mordant, then observed with optical microscope, can find out the tissue topography shown in Fig. 4.By observing, can conclude that there is the starting powder granule boundary (PPB) of a greater number in tested sample, this result is observed and can be verified by fracture apperance.
Therefore, H
2o
2solution has unique effect to manifesting of PPB in the powder metallurgy superalloy product.Carry out the PPB inspection by this mordant, can realize that the science of material is checked and accepted, the manufacturing process of such material is improved and proposed to instruct simultaneously.
The caustic solution on powder metallurgy superalloy primary granule provided by the invention border, its advantage is: by adopting the caustic solution in the present invention, can erode away starting powder granule boundary (PPB) clearly, overcome the technology prejudice that the industry was checked for starting powder granule boundary (PPB) in the past.
The accompanying drawing explanation
Fig. 1 is for being used mordant: 80ml HCl+13ml HF+7ml HNO
3the time corrosive effect figure;
Fig. 2 is for being used Kalling reagent: 60ml C
2h
5o+40ml HCl+2g CuCl
2the time corrosive effect figure;
Fig. 3 is for being used mordant: 93%HCl+4%HNO
3+ 3%H
2o
2the time corrosive effect figure;
Fig. 4 is for being used mordant: 95%HCl+3%HNO
3+ 2%H
2o
2the time corrosive effect figure;
The impact fracture SME figure that Fig. 5 is powder metallurgy superalloy;
The metallograph that Fig. 6 is the corrosion of Kalling reagent;
Fig. 7 is for being used mordant 95%HCl+3%HNO
3+ 2%H
2o
2the metallograph of corrosion;
Fig. 8 is powder metallurgy superalloy high impact toughness fracture surface of sample shape appearance figure;
Embodiment
In order to check out PPB, we have carried out the serial experiment of different reagent, heterogeneity, the final caustic solution of creatively exploring a kind of powder metallurgy superalloy primary granule border PPB, below for concrete implementation process: and corrosion is all same area (concrete title) of identical alloy (title of alloy)
Embodiment 1
Choose the mordant 80ml HCl+13ml HF+7ml HNO that nickel base superalloy is commonly used
3, at first alloy FGH97 carries out polishing, then uses mordant 80ml HCl+13ml HF+7mlHNO
3alloy FGH97 is corroded on surface, and etching time is 30s, on its primary granule border (seeing Fig. 1) of optical microphotograph Microscopic observation.The profile of PPB does not appear as shown in Figure 1.
Embodiment 2
Choose Kalling reagent: 60ml C
2h
5o+40ml HCl+2g CuCl
2, at first alloy FGH97 carries out polishing, then uses Kalling reagent alloy FGH97 surface to be corroded, and etching time is greater than 30s, on its primary granule border (seeing Fig. 2) of optical microphotograph Microscopic observation.As shown in Figure 2, use Kalling reagent to demonstrate corrosive effect preferably, but only erode away the profile of the 2 self-existent PPB in place.
Embodiment 3
Choose mordant: 93%HCl+4%HNO
3+ 3%H
2o
2, at first alloy FGH97 carries out polishing, then uses mordant 93%HCl+4%HNO
3+ 3%H
2o
2alloy FGH97 is corroded on surface, and etching time is 10～20s, on its primary granule border (seeing Fig. 3) of optical microphotograph Microscopic observation.As shown in Figure 3, although while using this mordant, corrosive effect does not reach best, can find the profile of more PPB.
Embodiment 4
Choose mordant: 95%HCl+3%HNO
3+ 2%H
2o
2, at first alloy FGH97 carries out polishing, then uses mordant 95%HCl+3%HNO
3+ 2%H
2o
2alloy FGH97 is corroded on surface, and etching time is 10～20s, on its primary granule border (seeing Fig. 4) of optical microphotograph Microscopic observation.As shown in Figure 4, while using this mordant, by observation by light microscope, can obtain clear reflection PPB (arrow points), and regional area there is the webbed trend of gathering.
Embodiment 5
The FGH97 alloy impact specimen fracture apperance cut is carried out to the SEM observation, see Fig. 5.As shown in Figure 5, by the observation of impact fracture, can find many places PPB (tip sensing) fracture pattern, illustrate and use H
2o
2solution corrosion by observation by light microscope to powder metallurgy superalloy in PPB be outwardness.
Embodiment 6
The impact performance obviously preferably the FGH97 alloy carry out Kalling reagent etching detection and mordant 95%HCl+3%HNO
3+ 2%H
2o
2etching detection and impact fracture are observed, and see Fig. 6, Fig. 7 and Fig. 8.
Can find out, for the obvious higher FGH97 alloy high power sample of impact flexibility, in the metallograph under two kinds of mordant, be showed no obvious PPB.Observe impact fracture, have no significantly along PPB fracture pattern, present obvious ductile rupture.
By above test and analysis, can find out H
2o
2solution objectively reflects that there is form in PPB in powder metallurgy superalloy under optical microscope.Can check and use mordant as powder metallurgy superalloy PPB.
Claims (2)
1. the caustic solution on a powder metallurgy superalloy primary granule border, it is characterized in that: described method is that the alloy surface after using mordant to polishing is corroded, etching time is 10～20s, then on its primary granule border of optical microphotograph Microscopic observation;
Wherein, the volume ratio of described each composition of mordant:
HCl: HNO
3: H
2o
2be 93～95: 3～4: 2～3.
2. according to the caustic solution on the described powder metallurgy superalloy primary granule of claim 1 border, it is characterized in that: the volume ratio of described each composition of mordant is: 95%HCl+3%HNO
3+ 2%H
2o
2.
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| CN104677714B (en) * | 2013-11-30 | 2017-12-05 | 中国科学院金属研究所 | The macrostructure of steel and defect etching reagent and detection method |
| CN105256315A (en) * | 2015-09-16 | 2016-01-20 | 昆山全亚冠环保科技有限公司 | Metallographic corrosive agent and method for nickel-vanadium alloy |
| CN106908301A (en) * | 2015-12-23 | 2017-06-30 | 上海电气电站设备有限公司 | A kind of etching pit method of clear display nickel-base alloy austenite grain boundary |
| CN110438553B (en) * | 2019-09-04 | 2020-09-08 | 内蒙古工业大学 | Metallographic corrosive agent and corrosion method for observing gamma' phase in high-quality GH4738 alloy subjected to secondary forging |
| CN112665952B (en) * | 2020-10-29 | 2023-03-24 | 北京星航机电装备有限公司 | GH3128 high-temperature alloy welding seam metallographic structure corrosive agent and corrosion method |
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| CN101777577A (en) * | 2010-03-10 | 2010-07-14 | 彩虹集团公司 | Color organic light emitting display panel and manufacturing method thereof |
Non-Patent Citations (4)
| Title |
|---|
| Effect of Cu addition on corrosion resistance and shape memory effect of Fe-14Mn-5Si-9Cr-5Ni alloy;Hu Bao-quan et al;《Transactions of Nonferrous Metals Society of China》;20091231;第19卷;149-153 * |
| Hu Bao-quan et al.Effect of Cu addition on corrosion resistance and shape memory effect of Fe-14Mn-5Si-9Cr-5Ni alloy.《Transactions of Nonferrous Metals Society of China》.2009,第19卷 |
| SiO2非金属夹杂物对镍基粉末高温合金微观力学行为的影响;周晓明等;《航空材料学报》;20060630;第26卷(第3期);1-6 * |
| 周晓明等.SiO2非金属夹杂物对镍基粉末高温合金微观力学行为的影响.《航空材料学报》.2006,第26卷(第3期), |
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