CN102409276A - Method for eliminating original particle boundary in powder metallurgy high-temperature alloy - Google Patents
Method for eliminating original particle boundary in powder metallurgy high-temperature alloy Download PDFInfo
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- CN102409276A CN102409276A CN2011103637592A CN201110363759A CN102409276A CN 102409276 A CN102409276 A CN 102409276A CN 2011103637592 A CN2011103637592 A CN 2011103637592A CN 201110363759 A CN201110363759 A CN 201110363759A CN 102409276 A CN102409276 A CN 102409276A
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Abstract
The invention discloses a method for eliminating an original particle boundary in a powder metallurgy high-temperature alloy, belonging to the field of powder metallurgy high-temperature alloys. The method comprises the following steps of: performing high-temperature solution treatment on a powder metallurgy high-temperature alloy which is subjected to direct hot isostatic pressing at the high-temperature solution treatment temperature 1,180-1,220 DEG C; preserving heat for 1.5-4 hours; cooling in an air cooling way or at a cooling speed higher than the air cooling speed; and performing corresponding aging thermal treatment according to different powder metallurgy high-temperature alloys, wherein by performing the high-temperature solution treatment, the original particle boundary in the powder metallurgy high-temperature alloy can be eliminated or weakened effectively. The method has the advantages: original particle boundary in the powder metallurgy high-temperature alloy can be eliminated or weakened effectively by performing high-temperature solution treatment.
Description
Technical field
The invention belongs to and belong to the powder metallurgy high-temperature alloy technical field, a kind of method of eliminating original granule boundary in the powder metallurgy high-temperature alloy particularly is provided, be applicable to the superalloy powder product of direct heat hydrostatic pressing plasma rotating electrode method preparation.
Background technology
Excellent specific properties such as the superalloy that adopts PM technique to produce has that crystal grain is tiny, homogeneous microstructure, no macrosegregation, hot workability and good mechanical properties, extensive application in hot-end components such as the advanced engine turbine disk of aerospace field.The powder metallurgy superalloy of direct heat hydrostatic pressing since carbide or other precipitated phase in particle surface deposition according to qualifications; Form the primary particle border; The primary particle border has hindered diffusion and the metallurgical binding between the powder particle; Become potential break line source; The process plastic and the mechanical property of alloy have been reduced; Hindered growing up of crystal grain simultaneously; Make the microstructure of alloy be difficult to control (Prakash T L, Tewari S N and Ramakrishnan P.Prior particle boundary (PPB) precipitates and the fractographic features of hot isostatically pressed (HIP) Nimonic AP-1P/M superalloy [A] .Ramakrishnan P.Powder Metallurgy and Related High Temperature Materials [C] .New Delhi:Mohan Primlani for Oxford&IBH Publishing Co., 1985:402～420; Blackburn M J, Sprague R A.Production of components by hot isostatic pressing ofnickel-base superalloy powders [J] .Metals Technology, 1977,4 (8): 388-395.; AubinC; Davidson J H; Trottier J P.The influence of powder particle surface composition on the properties of a nickel-based superalloy produced by hot isostatic pressing [A] .Tien J K.Superalloys 1980 [C] .Metals Park; Ohio:American Soc.For Metals 1980:345-354.), is one of three big defectives in the powder metallurgy high-temperature alloy.
Chinese scholars is being done a large amount of work aspect the research elimination primary particle border.The composition of MC type carbide and oxide compound depends on the composition of alloy.Prevention primary particle border forms or removing measure may be summarized to be (1) adjustment alloy composition, reduces carbon content, adds strong carbide forming elements such as Hf, Nb, at the inner MC type carbide that forms of powder particle, separates out tendency to be reduced in the primary particle border; (2) adopt powder thermal pretreatment technology, bulky powder is first at lower M
23C
6Carry out thermal pretreatment in the type carbide equilibrium temperature scope, at the inner M that forms of powder particle
23C
6The type carbide rises to higher MC type carbide equilibrium temperature scope again and carries out the hot isostatic pressing compacting, separates out stable MC type carbide at powder particle surface during with minimizing HIP; (3) adopt the two-step approach heat and other static pressuring processes, in heat-processed, (generally be lower than 1050 ℃) at a lower temperature earlier and be incubated, and then be elevated to the hip temperature compacting; (4) under a little less than the high temperature of solidus curve, carry out hip treatment, and then carry out thermal distortion and obtain required grain structure; (5) adopt the thermoplasticity complete processing, can the crushed particles surface oxide film, carry out hot isostatic pressing being lower than under the MC type carbide formation temperature; (6) adopt the broken primary particle of hot extrusion technique border.
The direct heat hydrostatic pressing prepares the powder metallurgy high-temperature alloy product and has that technology is simple, cost is low, obtain characteristics such as uniform tissue easily, and Figure 21 (from the supplementary material in-migration) is seen in technical process
The powder metallurgy high-temperature alloy product solid solution temperature of domestic direct heat hydrostatic pressing generally is not higher than hip temperature, on the primary particle border, generates a large amount of precipitated phases after the solution treatment, forms tangible primary particle border; The primary particle border is more serious after the solution heat treatment.
Summary of the invention
The object of the present invention is to provide a kind of method of eliminating original granule boundary in the powder metallurgy high-temperature alloy, solved and on the primary particle border, generated a large amount of precipitated phases after the thermal treatment, form the problem on tangible primary particle border.
Technology of the present invention is:
Powder metallurgy high-temperature alloy behind the direct hot isostatic pressing is carried out high temperature solid solution to be handled; The high temperature solid solution treatment temp is 1180～1220 ℃; Soaking time is 1.5～4h; Select air cooling or cooling rate to cool off, carry out corresponding timeliness thermal treatment (the timeliness heat treating regime is constant, is conventional timeliness heat) again according to different powder metallurgy high-temperature alloys then greater than the type of cooling of air cooling cooling rate; The primary particle border in the powder metallurgy high-temperature alloy can eliminated or weaken to high temperature solid solution after handling effectively.
The reason that the fixed powder metallurgy high-temperature alloy product of direct hot isostatic pressing forms the primary particle border is in hot isostatic pressing and solution heat treatment process, on the primary particle border, to separate out; Different according to alloying constituent, the borderline precipitated phase of primary particle is mainly γ ' phase or carbide and a spot of oxycarbide and forms.For powder metallurgy high-temperature alloy, solution heat treatment has very big influence to the primary particle border.Solid solution temperature forms not dissolving fully of big γ ' if be lower than γ ' solid solution temperature on the primary particle border in the isostatic in the solution treatment process, in process of cooling, growing up forms tangible primary particle border; Solid solution temperature is higher than γ ' solid solution temperature, and the big γ ' that forms in the isostatic is dissolved fully, and the homogenizing degree improves, and does not form the primary particle border.And for the carbide phase of on the primary particle border, separating out in the isostatic, handle through high temperature solid solution, carbide dissolves gradually, only needs higher solid solution temperature and long solution treatment time.
High temperature solid solution provided by the invention is handled the method for eliminating original granule boundary in the powder metallurgy high-temperature alloy; Mainly be the powder metallurgy high-temperature alloy blank behind the hot isostatic pressing to be carried out the high temperature solid solution processing make the borderline precipitated phase of primary particle in the soak process, dissolve disappearance; To eliminate the primary particle border, promptly compare the solution heat treatment that higher solution heat treatment replaces standard with the standard solution heat treatment.Thereby the high temperature solid solution temperature is should be enough high, holding time long to be to guarantee that precipitated phase dissolves fully; Also should control simultaneously cooling rate after the solution treatment; If speed of cooling is slow; Then can cause the dissolved precipitated phase in process of cooling, on powder primary particle border, to separate out again, form the primary particle border.But solid solubility temperature can not be too high, soaking time can not be long, preventing grain growth, and influences the mechanical behavior under high temperature of alloy.For through heat treated powder metallurgy high-temperature alloy product, also can handle elimination or weaken the primary particle border in the powder metallurgy high-temperature alloy product, and then carry out the thermal treatment of standard timeliness through high temperature solid solution.
The present invention is simple to operate, does not influence production efficiency, can eliminate or weaken the primary particle border in the powder metallurgy high-temperature alloy effectively.
Description of drawings
Fig. 1 is the situation of instance interalloy 1 of the present invention through original granule boundary in the metallographic specimen after the standard thermal treatment, magnification 100.
Fig. 2 is the situation of instance interalloy 1 of the present invention through original granule boundary in the metallographic specimen after the standard thermal treatment, magnification 500.
Fig. 3 passes through after the corresponding timeliness thermal treatment situation of original granule boundary in the metallographic specimen, magnification 100 after handling through 1180 ℃/1.5h/AC high temperature solid solution again for instance interalloy 1 of the present invention.
Fig. 4 passes through after the corresponding timeliness thermal treatment situation of original granule boundary in the metallographic specimen, magnification 500 after handling through 1180 ℃/1.5h/AC high temperature solid solution again for instance interalloy 1 of the present invention.
Fig. 5 is the situation of instance interalloy 1 of the present invention through original granule boundary in the metallographic specimen of 1140/1.5h/AC high temperature solid solution processing back, magnification 100.
Fig. 6 is the situation of instance interalloy 1 of the present invention through original granule boundary in the metallographic specimen of 1140/1.5h/AC high temperature solid solution processing back, magnification 500.
Fig. 7 is instance interalloy 1 of the present invention situation of original granule boundary in the metallographic specimen after 1180 ℃/1.5h/AC high temperature solid solution processing, magnification 100.
Fig. 8 is for being instance interalloy 1 of the present invention situation of original granule boundary in the metallographic specimen after 1180 ℃/1.5h/AC high temperature solid solution processing, magnification 500.
Fig. 9 is the situation of instance interalloy 1 of the present invention through original granule boundary in the metallographic specimen of 1220 ℃/4h/AC high temperature solid solution processing back, magnification 100.
Figure 10 is the situation of instance interalloy 1 of the present invention through original granule boundary in the metallographic specimen of 1220 ℃/4h/AC high temperature solid solution processing back, magnification 500.
Figure 11 is the situation of instance interalloy 2 of the present invention through original granule boundary in the metallographic specimen after the standard thermal treatment, magnification 100.
Figure 12 instance interalloy 2 of the present invention is through the situation of original granule boundary in the metallographic after the standard thermal treatment, magnification 500.
Figure 13 passes through after the corresponding timeliness thermal treatment situation of original granule boundary in the metallographic specimen, magnification 100 after handling through 1180 ℃/2h/AC high temperature solid solution again for instance interalloy 2 of the present invention.
Figure 14 passes through after the corresponding timeliness thermal treatment situation of original granule boundary in the metallographic specimen, magnification 500 after handling through 1180 ℃/2h/AC high temperature solid solution again for instance interalloy 2 of the present invention.
Figure 15 for behind instance interalloy 2 hot isostatic pressings of the present invention without the situation of original granule boundary in the metallographic specimen of bakingout process, magnification 100.
Figure 16 for behind instance interalloy 2 hot isostatic pressings of the present invention without the situation of original granule boundary in the metallographic specimen of bakingout process, magnification 500.
Figure 17 is the situation of instance interalloy 2 of the present invention through original granule boundary in the metallographic specimen of 1180 ℃/2h/AC high temperature solid solution processing back, magnification 100.
Figure 18 is the situation of instance interalloy 2 of the present invention through original granule boundary in the metallographic specimen of 1180 ℃/2h/AC high temperature solid solution processing back, magnification 500.
Figure 19 is the situation of instance interalloy 2 of the present invention through original granule boundary in the metallographic specimen of 1220 ℃/4h/AC high temperature solid solution processing back, magnification 100.
Figure 20 is the situation of instance interalloy 2 of the present invention through original granule boundary in the metallographic specimen of 1220 ℃/4h/AC high temperature solid solution processing back, magnification 500.
Figure 21 prepares the technical process of powder metallurgy high-temperature alloy product for the direct heat hydrostatic pressing.
Embodiment
To existing powder metallurgy high-temperature alloy 1 and alloy 2, the present invention is detailed in conjunction with accompanying drawing and embodiment.
Powder metallurgy high-temperature alloy 1 and 2 composition provide in subordinate list 1.
Embodiment 1
Powder metallurgy high-temperature alloy 1 powder through 1180 ℃/130MPa/3h hot isostatic pressing after; Pass through again standard solid solution+timeliness (SHT:1140 ℃/1.5h/AC+870 ℃/1.5h/AC+650 ℃/24h/AC) after the thermal treatment; Metallographicobservation is found to have a large amount of primary particle borders in the alloy microscopic structure, and sample size is 10mm * 10mm * 10mm.1 sample of alloy behind the hot isostatic pressing is carried out a series of high temperature solid solutions at 1180～1220 ℃ handle, do not have the primary particle border in the metallographicobservation alloy microscopic structure, the result sees attached list 2.
Instance 2
Powder metallurgy high-temperature alloy 2 powder through 1180 ℃/130MPa/3h hot isostatic pressing after, metallographicobservation is found to have serious primary particle border in the alloy microscopic structure, sample size is 10mm * 10mm * 10mm.2 samples of alloy behind the hot isostatic pressing are carried out after a series of high temperature solid solutions handle at 1180～1220 ℃, and metallographicobservation finds that original granule boundary obviously reduces in the microstructure, and the result sees attached list 2.Alloy 2 standard thermal treatment systems are 1150 ℃/2h/AC+760 ℃/16h/AC/AC (SHT).
Embodiment 2
Among the present invention; The hot isostatic pressing system is 1180 ℃/130MPa/3h, and the solution treatment system of alloy 1 is 1140 ℃/1.5h/AC, has a large amount of primary particle borders in the alloy; See Fig. 5,6; Influence the plasticity and the mechanical property of alloy, this patent provides a kind of high temperature solid solution treatment process of eliminating original granule boundary in the powder metallurgy high-temperature alloy, and the plasticity and the enduring quality of the powder metallurgy high-temperature alloy product of direct heat hydrostatic pressing are made moderate progress.
Table 1 alloying constituent (massfraction, %) (should provide in the instance specific, rather than anti-scope)
| Alloy number | Cr | Co | Mo | Nb | W | Al | Ti | C | Ni |
| Alloy 1 | 13.0 | 8.0 | 3.5 | 3.5 | 3.5 | 3.5 | 2.5 | 0.06 | Surplus |
| Alloy 2 | 15.8 | 13.0 | 4.0 | 0.8 | 4.0 | 2.2 | 3.7 | 0.04 | Surplus |
Table 2 mechanical property (please with following figure number with amended corresponding)
Claims (1)
1. method of eliminating original granule boundary in the powder metallurgy high-temperature alloy; It is characterized in that; Powder metallurgy high-temperature alloy behind the direct hot isostatic pressing is carried out high temperature solid solution handle, the high temperature solid solution treatment temp is 1180～1220 ℃, and soaking time is 1.5～4h; Select air cooling or cooling rate to cool off, carry out corresponding timeliness thermal treatment again according to different powder metallurgy high-temperature alloys then greater than the type of cooling of air cooling cooling rate; The primary particle border in the powder metallurgy high-temperature alloy can eliminated or weaken to high temperature solid solution after handling effectively.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103551573A (en) * | 2013-10-22 | 2014-02-05 | 中国科学院金属研究所 | Previous particle boundary precipitation preventable high-temperature alloy powder hot isostatic pressing process |
| CN108425037A (en) * | 2018-04-12 | 2018-08-21 | 北京钢研高纳科技股份有限公司 | A kind of powder metallurgy superalloy and preparation method thereof |
| CN110116203A (en) * | 2019-06-06 | 2019-08-13 | 西北有色金属研究院 | A method of eliminating Ni-base P/M Superalloy primary granule border |
| CN113042755A (en) * | 2021-03-12 | 2021-06-29 | 飞而康快速制造科技有限责任公司 | Heat treatment method of GH3536 high-temperature alloy for additive manufacturing |
| CN113343516A (en) * | 2021-05-14 | 2021-09-03 | 华中科技大学 | Method for eliminating critical deformation of powder superalloy PPB and determining extrusion process parameters |
-
2011
- 2011-11-16 CN CN2011103637592A patent/CN102409276A/en active Pending
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| 刘建涛等: "FGH97合金的显微组织", 《材料热处理学报》 * |
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| 赵军普，陶宇，袁守谦，等: "粉末冶金高温合金中的原始颗粒边界（PPB）问题", 《粉末冶金工业》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103551573A (en) * | 2013-10-22 | 2014-02-05 | 中国科学院金属研究所 | Previous particle boundary precipitation preventable high-temperature alloy powder hot isostatic pressing process |
| WO2015058534A1 (en) * | 2013-10-22 | 2015-04-30 | 中国科学院金属研究所 | Hot isostatic pressing process for high-temperature alloy powder |
| CN108425037A (en) * | 2018-04-12 | 2018-08-21 | 北京钢研高纳科技股份有限公司 | A kind of powder metallurgy superalloy and preparation method thereof |
| CN108425037B (en) * | 2018-04-12 | 2019-07-23 | 北京钢研高纳科技股份有限公司 | A kind of powder metallurgy superalloy and preparation method thereof |
| CN110116203A (en) * | 2019-06-06 | 2019-08-13 | 西北有色金属研究院 | A method of eliminating Ni-base P/M Superalloy primary granule border |
| CN113042755A (en) * | 2021-03-12 | 2021-06-29 | 飞而康快速制造科技有限责任公司 | Heat treatment method of GH3536 high-temperature alloy for additive manufacturing |
| CN113343516A (en) * | 2021-05-14 | 2021-09-03 | 华中科技大学 | Method for eliminating critical deformation of powder superalloy PPB and determining extrusion process parameters |
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Application publication date: 20120411 |