CN104878248A - High temperature alloy 625H and technological making method thereof - Google Patents
High temperature alloy 625H and technological making method thereof Download PDFInfo
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Abstract
The invention discloses a high temperature alloy 625H, the formula of which comprises the following specific ingredients, by weight, C being less than or equal to 0.04-0.05%, Si being less than or equal to 0.20%, Mn being less than or equal to 0.10%, P being less than or equal to 0.015%, S being less than or equal to 0.005%, 22.50-23.00% of Cr, 0.20-0.30% of Ti, 0.30-0.40% of Al, 9.50-10.00% of Mo, 3.65-4.15% of Nb+Ta, Fe being less than or equal to 0.50%, Cu being less than or equal to 0.05%, Co being less than or equal to 0.05%, and Ni being greater than or equal to 60.00%. Through special chemical composition design and match, the influence of proportional relationship between Nb, Ti and Al elements on the alloy UNS N06625 is found out such that high temperature rupture life excesses 1000 hours in a supercritical environment (750 DEG C) and at the pressure of no less than 178 MPa.
Description
Technical field
The present invention relates to high temperature alloy preparing technical field, particularly relate to superalloy 625H and manufacturing process thereof.
Background technology
UNS N06625 alloy is ni-base wrought superalloy, is take molybdenum, niobium as the solution strengthening type wrought superalloy of main strengthening element, has excellent solidity to corrosion and oxidation-resistance.It is widely used in and manufactures aerial motor spare part, aerospace structure unit, chemical industry equipment and nuclear power generating equipment component etc.In order to advance nuclear industry to develop, country is to the research and development of multiple heap-type, and the material based on UNS N06625 selected substantially by China's forth generation nuclear power high temperature gas cooled reactor material, but has higher requirement and index on this material foundation.In order to meet it at 750 DEG C, the technical indicator of high-temperature duration life more than 1000 hours under 178MPa, and can be able to reach at 750 DEG C by these research and development, the technical indicator of high-temperature duration life more than 100000 hours under 75.3MPa.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, reach above-mentioned technical indicator, the present invention finds the impact of proportionlity alloy UNS N06625 between Nb, Ti, Al element by special chemical Composition Design and collocation, to reach at overcritical (750 DEG C) environment, under being not less than 178MPa, high-temperature duration life was more than 1000 hours.
The technical solution adopted in the present invention is: superalloy 625H, and its formula counts by weight percentage, and concrete content composition comprises:
C：≤0.04%~0.05% Si：≤0.20% Mn：≤0.10%
P：≤0.015% S：≤0.005% Cr：22.50~23.00%；
Ti :0.20%~0.30% AL :0.30%~0.40% Mo: 9.50%~10.00% Nb+Ta:3.65%~4.15% Fe：≤0.50% Cu：≤0.05%
Co：≤0.05% Ni：≥60.00%。
Further, on the basis comprising above-mentioned content, this superalloy 625H, in the later stage of melting, also needs to add zirconium Zr and rare earth alloy to promote the performance of material.
A kind of technique manufacturing above-mentioned superalloy 625H, adopt the smelting technology (VIM+ESR) of vacuum metling+electroslag duplex, the technique of i.e. vacuum induction melting (VIM)+inert atmosphere protection esr (ESR) duplex, and by requiring control and improve to forging and thermal treatment heat processing technique; Comprise the steps:
A. vacuum induction furnace smelting: by above-mentioned ingredient composition, dropped into vacuum induction furnace smelting;
B. electroslag refining;
C. forge: open forging temperature 1130 DEG C, final forging temperature >=900 DEG C;
D. ultrasonic test;
E. thermal treatment: >=1093 DEG C of solid solution+>=982 DEG C stabilizing annealings+700 DEG C of age hardenings;
F. ultrasonic test;
G. to rule sampling;
H. performance test: comprise its composition, room temperature tensile properties, 750 DEG C of tensile properties, metallographic, 750 DEG C of high temperature endurance performances detect;
I. car light grinding finished product.
Further, the refining temperature in described step B: 1520--1560 DEG C, refining time is greater than 45min, and tapping temperature is 1540-1580 DEG C.
Compared with prior art, the invention has the beneficial effects as follows: adopt suitable chemical element C, Nb, Ti, Al collocation to control the value volume and range of product of its strengthening phase, increase the constituent content of solid solution element Mo, Cr, Ni, the element of restriction Fe, Cu, Co, strict control S, Pb, Se, Bi, Hg constituent content, increases the trace element effect of Zr, rare earth; Adopt the smelting technology (VIM+ESR) of vacuum metling+electroslag duplex to improve steel purity and degasifying effect; The temperature controlling hot-work (forging and thermal treatment) obtains suitable metallurgical structure.
Adopt new recipe configuration superalloy 625H, that is: C :≤0.04% ~ 0.05%; Si :≤0.20%; Mn :≤0.10%; P :≤0.015%; S :≤0.005%; Cr:22.50 ~ 23.00%; Ti: 0.20% ~ 0.30%; AL: 0.30% ~ 0.40%; Mo:9.50% ~ 10.00% Nb+Ta:3.65% ~ 4.15% Fe :≤0.50%; Cu :≤0.05%; Co :≤0.05%; Ni: >=60.00%.And add zirconium Zr and rare earth alloy to promote the performance of material in the melting later stage.Make it compare different UNS N06625 and have higher yield strength and high temperature endurance performance under 750 DEG C of high temperature.
Material of the present invention is the various component starting material of the high temperature gas cooled reactor in forth generation nuclear power field.The vaporizer of the current high temperature gas-cooled reactor project of forth generation nuclear power in system and in-pile component use vapour pipe, support stick axle, container plate etc. manufactured by UNS N06625 material in a large number.Nuclear power as clean energy is that China gives priority to and promotion project, and forth generation high temperature gas cooled reactor is because its volume is little, power is large, the high emphasis as country's research of safety coefficient.And all can use the material of this trade mark in the field such as petrochemical complex, military project, promotion its popularity necessarily stronger at the 625H significantly promoting mechanical property and high temperature endurance performance research and development uses.
Embodiment
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the present invention is further described, and this embodiment, only for explaining the present invention, not forming protection scope of the present invention and limiting.
Superalloy 625H, its formula counts by weight percentage, and concrete content composition comprises:
C：≤0.04%~0.05% Si：≤0.20% Mn：≤0.10%
P：≤0.015% S：≤0.005% Cr：22.50~23.00%；
Ti :0.20%~0.30% AL :0.30%~0.40% Mo: 9.50%~10.00% Nb+Ta:3.65%~4.15% Fe：≤0.50% Cu：≤0.05%
Co：≤0.05% Ni：≥60.00%。
This formula on the basis comprising above-mentioned content, also at its superalloy 625H in the later stage of melting, also need to add zirconium Zr and rare earth alloy to promote the performance of material.
A kind of technique manufacturing above-mentioned superalloy 625H, adopt the smelting technology (VIM+ESR) of vacuum metling+electroslag duplex, the technique of i.e. vacuum induction melting (VIM)+inert atmosphere protection esr (ESR) duplex, and by requiring control and improve to forging and thermal treatment heat processing technique; Comprise the steps:
A. vacuum induction furnace smelting: by above-mentioned ingredient composition, dropped into vacuum induction furnace smelting;
B. electroslag refining;
C. forge: open forging temperature 1130 DEG C, final forging temperature >=900 DEG C;
D. ultrasonic test;
E. thermal treatment: >=1093 DEG C of solid solution+>=982 DEG C stabilizing annealings+700 DEG C of age hardenings;
F. ultrasonic test;
G. to rule sampling;
H. performance test: comprise its composition, room temperature tensile properties, 750 DEG C of tensile properties, metallographic, 750 DEG C of high temperature endurance performances detect;
I. car light grinding finished product.
In step B, its refining temperature: 1520--1560 DEG C, refining time is greater than 45min, and tapping temperature is 1540-1580 DEG C, has good performance.
Now just designed by 625H of the present invention, the principle of composition is described further with effect: first, analyze chemical composition, and alloy composition contrasts in table 1;
Table 1 alloy composition contrasts
Secondly, its mechanical property is analyzed, in table 2;
Table 2 thermal treatment reference value
[0017]combined by above table, the performance of chemical element, analyze:
(1) effect of carbon: carbon forms carbide dispersion and is distributed in intracrystalline and plays strengthening effect in 625H alloy with Nb, Ti element.
(2) effect of chromium: the key element of superalloy high-temperature oxidation resistance and anti-corrosion capability, high temperature formed protection oxide film primarily of Cr
2o
3composition.With Cr
2o
3the oxide film being master is finer and close, and tack is also comparatively strong, can ensure alloy at high temperature life-time service.
(3) effect of silicon: silicon produces SiO2 after high temperature oxidation, is distributed in the interface of oxide film and matrix metal, oxygen can be stoped to infiltrate, fall low-alloyed oxidation rate.When silicon and rare earth element exist simultaneously, the effect that silicon improves antioxidant property is more remarkable.Improve the compactness of oxidation-resistant film.
(4) effect of manganese and iron: low-alloyed antioxidant property can fall in manganese and iron, increases oxidation rate, a small amount of manganese and sulphur formed MnS can reduce hot-short with high-temperature and durable sulphur on the impact of its hold-time.
(5) effect of nickel: nickel and other alloy forming surface centered cubic lattice, i.e. austenite lattice, high temperature does not undergo phase transition, therefore its at high temperature good stability.Nickel is parent in nickel base superalloy, and the characteristic of itself plays a leading role.Nickel is austenizer, can provide good over-all properties, can form sosoloid, have higher hot strength most, have high plasticity when normal temperature, good process industrial art performance under good stability high temperature with chromium.
(6) effect of rare earth element: add the over-all properties that a small amount of rare earth significantly can improve alloy in superalloy, purifies crystal boundary because it can form compound with oxidizing substance in grain boundaries precipitation, and at crystal grain thinning, can improve intensity.
(7) effect of aluminium: the principal element forming γ ' phase, in nickel chromium triangle system superalloy, aluminium can form Ni3Al phase with nickel, is the important factor improving oxidation-resistance, and can improve alloy high-temp intensity raising creep rupture strength.
(8) effect of titanium: the principal element forming γ ' phase, can promote Ni3Al to be formed and form Ni3(Al, Ti), improve γ ' phase reinforcing degree.
(9) effect of niobium: carbide forms NbC, crystal grain thinning.It is main strengthening phase that a large amount of Nb forms γ ' ' (Ni3Nb), dissolves in γ ' on a small quantity and promotes γ ' precipitation mutually, delay growing up of γ ', improves intensity.
(10) effect of molybdenum: its solution strengthening effect improves heat resistance in superalloy.
(11) S, P: be that in material, inevitable detrimental impurity element, particularly S affect the intensity of material and creep rupture life and seriously require that it controls 0.005%, a small amount of P can improve creep rupture strength.
Embodiment
Test objective: by for not adding common 625 of C, AL, Ti, to the 625-1 increasing AL, Ti composition, to increasing C content, and adjusting the 625-2 of Cr, Mo, Nb content, devising 4 groups of enforcement tests altogether to the 625H again adjusting AL, Ti, Nb content and ratio and implementing;
Object: see table 3, select Ni, Cr, Mo, Nb, Mn, AL, Ti, Zr content to be greater than 99% pure metal material and manufacture as raw material, all the other elements control in proportion;
Making step: complete by above-mentioned A to I step, namely according to the present invention's 4 groups of embodiment design mix batchings, vacuum induction furnace smelting (refining temperature: 1520--1560 DEG C; Refining time: be greater than 45 minutes, tapping temperature 1540--1580 DEG C) → electroslag refining → forging (open forging temperature 1130 DEG C, final forging temperature >=900 DEG C) → ultrasonic test → thermal treatment (+700 DEG C of age hardenings of 1140 DEG C of solid solutions+990 DEG C of stabilizing annealings) → ultrasonic test → line sampling → performance test (composition, room temperature tensile, 750 DEG C of stretchings, metallographic, 750 DEG C of high-temperature and durables) → car light grinds finished product;
table 3 is specifically implemented as and point carries out its preparing materials
Mechanics Performance Testing: require that ASME SB-446 requires to have carried out Mechanics Performance Testing to these four groups of samples respectively according to American Standard, test result is as shown in table 4:
Table 4 four groups of mechanical property contrasts
Can raising alloy strength in various degree by increasing alloying element, but it is not obvious to improve intensity.But by increasing AL, Ti content and control Al:Ti content=1:1, increase Nb content and form NbC and promote that γ ' separates out the yield strength significantly can improving 750 DEG C mutually, and its elongation far to surpass the collocation of other alloying constituent.Certainly, this and final thermal treatment are also related.By+700 DEG C of age hardenings of rational thermal treatment temp 1140 DEG C of solid solutions+990 DEG C of stabilizing annealings, solid solution+stabilizing annealing can allow the composition of alloy and precipitated phase be uniformly distributed elimination harmful phase, and the timeliness of 700 DEG C promotes that a small amount of γ ' separates out mutually and improves alloy yield strength 750 DEG C time.
Grain fineness number detects: as shown in table 5;
Table 5 four groups of grain fineness number contrasts
As can be seen from Table 5, when same thermal treatment temp carries out solid solution+Stabilizing Heat Treatment, the grain growth that carbon content is high is slower, should control grain fineness number≤5.0 grade as requested.
Rupture test detects: in table 6;
Table 6 rupture test contrasts
As can be seen from table 3 to table 6, by the complete processing of composition reasonable in design collocation by a series of excellence, the 625H alloy produced is under suitable heat treatment process system, and can reach at overcritical (750 DEG C), under 178MPa, high-temperature duration life was more than 1000 hours.The alloy of this composition mainly obtains suitable metallographic structure (4.0-5.0 level grain fineness number by composition collocation and production technique, increase strengthening phase and precipitated phase), improve the yield strength under 750 DEG C of environment and elongation, thus reach the requirement of high-temperature duration life more than 1000 hours under 178MPa.Thus for the various component of the high temperature gas cooled reactor in forth generation nuclear power field provide the starting material of high-quality, and more high-quality guarantee will be provided in civilian goods superalloy field.
Adopt a kind of novel high-temperature alloy 625H designed by the present invention, the high temperature endurance performance that can meet the high temperature material of the high temperature gas cooled reactor in forth generation nuclear power field requires that under 178MPa, high-temperature duration life was more than 1000 hours at overcritical (750 DEG C).
What embodiments of the invention were announced is preferred embodiment, but is not limited thereto, those of ordinary skill in the art; very easily according to above-described embodiment, understand spirit of the present invention, and make different amplifications and change; but only otherwise depart from spirit of the present invention, all in protection scope of the present invention.
Claims (4)
1. superalloy 625H, its formula counts by weight percentage, and concrete content composition comprises:
C：≤0.04%~0.05% Si：≤0.20% Mn：≤0.10%
P：≤0.015% S：≤0.005% Cr：22.50~23.00%；
Ti :0.20%~0.30% AL :0.30%~0.40% Mo: 9.50%~10.00% Nb+Ta:3.65%~4.15% Fe：≤0.50% Cu：≤0.05%
Co：≤0.05% Ni：≥60.00%。
2. superalloy 625H according to claim 1, is characterized in that: on the basis comprising above-mentioned content, and this superalloy 625H, in the later stage of melting, also needs to add zirconium Zr and rare earth alloy to promote the performance of material.
3. the technique of a manufacturing license 1 and the superalloy 625H of power described in 2, it is characterized in that: the smelting technology (VIM+ESR) adopting vacuum metling+electroslag duplex, wherein VIM is vacuum induction melting, ESR is inert atmosphere protection esr, and by requiring control and improve to forging and thermal treatment heat processing technique; Comprise the steps:
Vacuum induction furnace smelting: by above-mentioned ingredient composition, dropped into vacuum induction furnace smelting;
Electroslag refining;
Forging: open forging temperature 1130 DEG C, final forging temperature >=900 DEG C;
Ultrasonic test;
Thermal treatment: >=1093 DEG C of solid solution+>=982 DEG C stabilizing annealings+700 DEG C of age hardenings;
Ultrasonic test;
Line sampling;
Performance test: comprise its composition, room temperature tensile properties, 750 DEG C of tensile properties, metallographic, 750 DEG C of high temperature endurance performances detect;
Car light grinding finished product.
4. the manufacturing process of superalloy 625H according to claim 3, it is characterized in that: the refining temperature in described step B: 1520--1560 DEG C, refining time is greater than 45min, and tapping temperature is 1540-1580 DEG C.
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| CN110453164A (en) * | 2019-08-14 | 2019-11-15 | 河北工业大学 | A kind of processing method of enhancing forging state Ni-Cr-Co based alloy antioxygenic property |
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| CN107841657A (en) * | 2017-09-30 | 2018-03-27 | 中国科学院金属研究所 | A kind of high tough Ni Cr Mo base casting alloys |
| CN110453164A (en) * | 2019-08-14 | 2019-11-15 | 河北工业大学 | A kind of processing method of enhancing forging state Ni-Cr-Co based alloy antioxygenic property |
| CN111139414A (en) * | 2019-11-27 | 2020-05-12 | 北京钢研高纳科技股份有限公司 | Stabilizing treatment process of precipitation hardening type nickel-based high-temperature alloy |
| CN111139414B (en) * | 2019-11-27 | 2021-09-07 | 北京钢研高纳科技股份有限公司 | Stabilizing treatment process of precipitation hardening type nickel-based high-temperature alloy |
| CN112941370B (en) * | 2019-12-10 | 2022-11-01 | 中国科学院金属研究所 | Method for controlling delta phase precipitation in Nb-containing nickel-based superalloy |
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Address after: 225700, No. 19, Zhang Guo Town, Xinghua, Jiangsu, Taizhou Patentee after: Jiangsu Xinhua Alloy Co., Ltd Address before: 225700, No. 19, Zhang Guo Town, Xinghua, Jiangsu, Taizhou Patentee before: Jiangsu Xinhua Alloy Electric Apparatus Co., Ltd. |
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