CN104878248B - High temperature alloy 625H and its manufacturing process - Google Patents
High temperature alloy 625H and its manufacturing process Download PDFInfo
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Abstract
The invention discloses high temperature alloy 625H, and it is formulated count by weight percentage, and concrete content composition includes：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%.Influence of the proportionate relationship to alloy UNS N06625 between Nb, Ti, Al element is found by special chemical composition design and collocation, to reach overcritical（750℃）Environment, not less than high-temperature duration life under 178MPa more than 1000 hours.
Description
Technical field
The present invention relates to high-temperature alloy material preparing technical field, is made more particularly to high temperature alloy 625H and its technique
Method.
Background technology
UNS N06625 alloys are ni-base wrought superalloy, are the solution strengthening types that element is need to strengthen based on molybdenum, niobium
Wrought superalloy, there is excellent corrosion resistance and inoxidizability.It is widely used in manufacture aerial motor spare part, aerospace
Structure member, chemical industry equipment and nuclear power generating equipment parts etc..In order to promote nuclear industry to develop, national grinding to a variety of heap-type
Hair, the material that China's forth generation nuclear power HTGR material has been selected based on UNS N06625 substantially, but in this material
On the basis of propose and higher want summing target.In order to meet it at 750 DEG C, high-temperature duration life is small more than 1000 under 178MPa
When technical indicator, and be able to can be reached at 750 DEG C by this research and development, high-temperature duration life is more than 100000 under 75.3MPa
The technical indicator of hour.
The content of the invention
In order to overcome the above-mentioned deficiencies of the prior art, above-mentioned technical indicator is reached, the present invention is by special chemical into setting up separately
Influence of the proportionate relationship to alloy UNS N06625 between Nb, Ti, Al element is found in meter and collocation, to reach overcritical（750
℃）Environment, not less than high-temperature duration life under 178MPa more than 1000 hours.
The technical solution adopted in the present invention is：High temperature alloy 625H, it is formulated count by weight percentage, concrete content
Composition includes：
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 of including above-mentioned content, high temperature alloy 625H also needed to add zirconium in the later stage of melting
Zr and rare earth alloy are to lift the performance of material.
A kind of technique for manufacturing above-mentioned high temperature alloy 625H, using the smelting process of vacuum metling+electroslag duplex（VIM+
ESR）, i.e. the technique of vacuum induction melting (VIM)+inert atmosphere protection electroslag remelting (ESR) duplex, and by forging and heat
Processing heat processing technique requirement is controlled and improved；Comprise the following steps：
A. vacuum induction furnace smelting：By above-mentioned ingredient composition, vacuum induction furnace smelting is put into；
B. electroslag refining；
C. forge：1130 DEG C of starting forging temperature, final forging temperature >=900 DEG C；
D. ultrasound detection；
E. it is heat-treated：>=1093 DEG C of solid solution+>=+700 DEG C of age-hardenings of 982 DEG C of stabilizing annealings；
F. ultrasound detection；
G. line sampling；
H. performance test：Including its composition, room temperature tensile properties, 750 DEG C of tensile properties, metallographic, 750 DEG C of high-temperature and durables
Can detection；
I. car light grinding finished product.
Further, the refining temperature in the step B：1520--1560 DEG C, refining time is more than 45min, tapping temperature
Spend for 1540-1580 DEG C.
Compared with prior art, the beneficial effects of the invention are as follows：Arranged in pairs or groups and controlled using suitable chemical element C, Nb, Ti, Al
The value volume and range of product of its hardening constituent is made, increases solid solution element Mo, Cr, Ni constituent content, limits Fe, Cu, Co element, strictly
Control S, Pb, Se, Bi, Hg constituent content, increase Zr, rare earth trace element effect；Using the smelting of vacuum metling+electroslag duplex
Sweetening process（VIM+ESR）To improve steel degree of purity and degasifying effect；Control hot-working（Forging and heat treatment）Temperature come
To suitable metallurgical structure.
Using new recipe configuration high temperature alloy 625H, i.e.,：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 zirconium Zr and rare earth alloy are added to lift the performance of material in the melting later stage.So that it is compared
Different UNS N06625 possess higher yield strength and high temperature endurance performance under 750 DEG C of high temperature.
Material of the present invention is the various parts raw material of the HTGR of forth generation nuclear power field.At present in system
The evaporator and in-pile component of the high temperature gas-cooled reactor project of forth generation nuclear power are largely using the steam manufactured by UNS N06625 materials
Pipe, support mandrel, container plate etc..Nuclear power as clean energy resource is that China gives priority to and promotion project, forth generation high temperature
HTGR is due to its small volume, power is big, safety coefficient is high as the national emphasis studied.And in petrochemical industry, military project etc.
Field can all use the material of this trade mark, be obviously improved mechanical property and high temperature endurance performance research and development 625H necessarily more added with
Its popularity of the promotion of power uses.
Embodiment
In order to deepen the understanding of the present invention, with reference to embodiment, the present invention is further described, and the embodiment is only used
In explaining the present invention, protection scope of the present invention is not formed and limited.
High temperature alloy 625H, it is formulated count by weight percentage, and concrete content composition includes：
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%.
The formula also also needs to add in the later stage of melting on the basis of including above-mentioned content in its high temperature alloy 625H
Zirconium Zr and rare earth alloy are to lift the performance of material.
A kind of technique for manufacturing above-mentioned high temperature alloy 625H, using the smelting process of vacuum metling+electroslag duplex（VIM+
ESR）, i.e. the technique of vacuum induction melting (VIM)+inert atmosphere protection electroslag remelting (ESR) duplex, and by forging and heat
Processing heat processing technique requirement is controlled and improved；Comprise the following steps：
A. vacuum induction furnace smelting：By above-mentioned ingredient composition, vacuum induction furnace smelting is put into；
B. electroslag refining；
C. forge：1130 DEG C of starting forging temperature, final forging temperature >=900 DEG C；
D. ultrasound detection；
E. it is heat-treated：>=1093 DEG C of solid solution+>=+700 DEG C of age-hardenings of 982 DEG C of stabilizing annealings；
F. ultrasound detection；
G. line sampling；
H. performance test：Including its composition, room temperature tensile properties, 750 DEG C of tensile properties, metallographic, 750 DEG C of high-temperature and durables
Can detection；
I. car light grinding finished product.
In step B, its refining temperature：1520--1560 DEG C, refining time is more than 45min, tapping temperature 1540-
1580 DEG C, there is preferable performance.
Now the principle of composition designed by 625H of the present invention is described further with effect：First, chemical composition is carried out
Analysis, alloy composition contrast are shown in Table 1；
The alloy composition of table 1 contrasts
Secondly, its mechanical property is analyzed, is shown in Table 2；
Table 2 is heat-treated reference value
Combined, the performance of chemical element, analyzed by above table：
（1）The effect of carbon：Carbon forms carbide dispersion with Nb, Ti element in 625H alloys and is distributed in transgranular reinforcing work
With.
（2）The effect of chromium：The key element of high temperature alloy high-temperature oxidation resistance and anti-corrosion capability, in the guarantor that high temperature is formed
Oxide-film is protected mainly by Cr2O3Composition.With Cr2O3Based on oxide-film it is finer and close, tack is also stronger, it is ensured that alloy exists
It is long-term use of under high temperature.
（3）The effect of silicon：Silicon produces SiO2 after high-temperature oxydation, is distributed in the interface of oxide-film and parent metal, can
To prevent oxygen from penetrating into, low-alloyed oxidation rate drops.Silicon and rare earth element simultaneously in the presence of, silicon improves the effect of antioxygenic property
It is more notable.Improve the compactness of oxidation-resistant film.
（4）The effect of manganese and iron：Low-alloyed antioxygenic property can drop in manganese and iron, increase oxidation rate, a small amount of manganese and sulphur
Hot-short and influence of the high-temperature and durable sulphur to its retention time can be reduced by forming MnS.
（5）The effect of nickel：Nickel forms face-centered cubic lattice with other alloys, i.e. austenite lattice, high temperature is not undergone phase transition,
Therefore its stability is good at high temperature.Nickel is parent in nickel base superalloy, and the characteristic of itself plays a leading role.Nickel is Ovshinsky
Body element, good combination property can be provided, solid solution can be formed with chromium under the good high temperature of stability, most have comparison high
Elevated temperature strength, there is high plasticity, good process industrial art performance in normal temperature.
（6）The effect of rare earth element：A small amount of rare earth is added in high temperature alloy can significantly improve the combination property of alloy, because
It is separated out in grain boundaries to purify crystal boundary with oxidizing substance formation compound, and can improve intensity in crystal grain thinning.
（7）The effect of aluminium：The essential element of γ ' phases is formed, aluminium can form Ni3Al with nickel in nickel chromium triangle system high temperature alloy
An important factor for phase is raising inoxidizability, and alloy high-temp intensity can be improved and improve creep rupture strength.
（8）The effect of titanium：The essential element of γ ' phases is formed, Ni3Al can be promoted to form and formed Ni3（Al, Ti）, carry
High γ ' phases reinforcing degree.
（9）The effect of niobium:Carbide forms NbC, crystal grain thinning.A large amount of Nb form γ ' '（Ni3Nb）It is
Main hardening constituent, γ ' is dissolved on a small quantity and mutually promotes γ ' precipitations, delay growing up for γ ', improve intensity.
（10）The effect of molybdenum:Its solution strengthening effect improves heat resistance in high temperature alloy.
（11）S、 P：It is the intensity and creep rupture life of inevitable objectionable impurities elements, particularly S to material in material
Influence and its seriously require its control 0.005%, a small amount of P can improve creep rupture strength.
Embodiment
Test objective：By for being not added with common the 625 of C, AL, Ti, to the 625-1 of increase AL, Ti composition, to increase C
Content, and the 625-2 of Cr, Mo, Nb content is adjusted, 4 groups are devised altogether to the 625H for adjusting AL, Ti, Nb content and ratio again
Implement experiment to implement；
Object：Referring to table 3, it is more than 99% simple metal material as raw material from Ni, Cr, Mo, Nb, Mn, AL, Ti, Zr content
Manufactured, remaining element controls in proportion；
Making step：Completed by above-mentioned A to I steps, i.e., according to 4 groups of embodiment design ingredient compositions of the present invention, vacuum sense
Stove is answered to smelt（Refining temperature：1520--1560℃；Refining time：More than 45 minutes, 1540--1580 DEG C of tapping temperature）→ electricity
Slag refining → forging（1130 DEG C of starting forging temperature, final forging temperature >=900 DEG C）→ ultrasound detection → heat treatment（1140 DEG C of solid solutions+990
DEG C+700 DEG C of age-hardenings of stabilizing annealing）→ ultrasound detection → line sampling → performance test（Composition, room temperature tensile, 750 DEG C
Stretching, metallographic, 750 DEG C of high-temperature and durables）→ car light grinds finished product；
Table 3 is embodied composition and carries out its preparing materials
Mechanics Performance Testing：Require that ASME SB-446 requirements have carried out mechanical property to this four groups of samples respectively according to American Standard
It can test, test result is as shown in table 4：
4 four groups of mechanical property contrasts of table
Raising alloy strength that can be different degrees of by increasing alloying element, but improve intensity unobvious.It is but logical
Cross increase AL, Ti content and control Al：Ti content=1:1, increase Nb content form NbC and promote γ ' mutually to separate out and can significantly change
Kind 750 DEG C yield strength, and its elongation will remote super other alloying component collocation.Certainly, this and final heat treatment
It is related.+ 700 DEG C of age-hardenings of+990 DEG C of stabilizing annealings are dissolved by rational 1140 DEG C of heat treatment temperature, be dissolved+
Stabilizing annealing can allow the composition of alloy and precipitated phase to be uniformly distributed elimination harmful phase, and 700 DEG C of timeliness promotes a small amount of γ ' phases
Separate out and improve alloy yield strength at 750 DEG C.
Grain size detects：As shown in table 5；
5 four groups of grain size contrasts of table
As can be seen from Table 5, be dissolved in same heat treatment temperature+Stabilizing Heat Treatment when, the high crystal grain of carbon content
Grow up slower, grain size≤5.0 grade should be controlled as requested.
Duration running detects：It is shown in Table 6；
The duration running of table 6 contrasts
It is raw from table 3 to table 6 as can be seen that by composition collocation reasonable in design by a series of excellent processing technologys
The 625H alloys that output is come can reach overcritical under suitable heat treatment process system（750℃）, high temperature is held under 178MPa
The long life-span was more than 1000 hours.The alloy of this composition mainly obtains suitable metallographic structure by composition collocation and production technology
（4.0-5.0 level grain sizes, increase hardening constituent and precipitated phase）, yield strength and elongation under 750 DEG C of environment are improved, so as to
Reach requirement of the high-temperature duration life more than 1000 hours under 178MPa.It is thus the HTGR of forth generation nuclear power field
Various parts high-quality raw material are provided, and more high-quality guarantee will be provided in civilian goods high temperature alloy field.
Using a kind of novel high-temperature alloy 625H designed by the present invention, the High Temperature Gas of forth generation nuclear power field disclosure satisfy that
The high temperature endurance performance requirement of the exotic material of cold dome is overcritical（750℃）, high-temperature duration life exceedes under 178MPa
1000 hours.
What embodiments of the invention were announced is preferred embodiment, but is not limited thereto, the ordinary skill people of this area
Member, easily according to above-described embodiment, understand the spirit of the present invention, and make different amplification and change, but as long as not departing from this
The spirit of invention, all within the scope of the present invention.
Claims (1)
1. high temperature alloy 625H, it is formulated count by weight percentage, and concrete content composition includes：
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%；On the basis of including above-mentioned content, high temperature alloy 625H is molten
In the later stage of refining, also need to add zirconium Zr and rare earth alloy to lift the performance of material；
High temperature alloy 625H technique, using the smelting process ESR of vacuum metling VIM+electroslag duplex, wherein VIM is vacuum sense
Answer melting, ESR is inert atmosphere protection electroslag remelting, and by forge and be heat-treated heat processing technique requirement be controlled and
Improve；Comprise the following steps：
A. vacuum induction furnace smelting：By above-mentioned ingredient composition, vacuum induction furnace smelting is put into；
B. electroslag refining, refining temperature：1520--1560 DEG C, refining time is more than 45min, and tapping temperature is 1540-1580 DEG C；
C. forge：1130 DEG C of starting forging temperature, final forging temperature >=900 DEG C；
D. ultrasound detection；
E. it is heat-treated：>=1093 DEG C of solid solution+>=+700 DEG C of age-hardenings of 982 DEG C of stabilizing annealings；
F. ultrasound detection；
G. line sampling；
H. performance test：Including its composition, room temperature tensile properties, 750 DEG C of tensile properties, metallographic, 750 DEG C of high temperature endurance performance inspections
Survey；
I. car light grinding finished product.
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| CN107841657B (en) * | 2017-09-30 | 2020-03-31 | 中国科学院金属研究所 | High-strength and high-toughness Ni-Cr-Mo-based casting alloy |
| CN110453164B (en) * | 2019-08-14 | 2020-12-22 | 河北工业大学 | Processing method for enhancing oxidation resistance of forged Ni-Cr-Co-based 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 |
| CN112176223B (en) * | 2020-09-03 | 2022-01-28 | 太原钢铁(集团)有限公司 | Method for controlling performance of nickel-based alloy wire |
| CN113584331A (en) * | 2021-06-30 | 2021-11-02 | 江西恒大高新技术股份有限公司 | Preparation method of aluminum-doped Inconel625 alloy applied to oxygen-containing high-temperature chlorine corrosion environment |
| CN113584381B (en) * | 2021-07-05 | 2023-03-07 | 重庆材料研究院有限公司 | High-strength copper-containing Ni-Fe-Cr-based age-hardening corrosion-resistant alloy and electroslag remelting method thereof |
| CN115233012B (en) * | 2022-07-19 | 2023-08-11 | 山西太钢不锈钢股份有限公司 | Manufacturing method of nickel-based superalloy hot rolled plate |
| CN115369289B (en) * | 2022-08-29 | 2024-02-09 | 江西宝顺昌特种合金制造有限公司 | Inconel625 forging for underwater flowmeter and preparation method thereof |
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| CN104233001B (en) * | 2013-06-08 | 2016-08-24 | 上海丰渠特种合金有限公司 | A kind of UNS N06625 high temperature alloy and preparation method thereof |
| CN103316949A (en) * | 2013-06-25 | 2013-09-25 | 浙江国邦钢业有限公司 | Corrosion-resistant alloy tube manufacturing process and corrosion-resistant alloy seamless steel tube |
| CN103484803A (en) * | 2013-10-12 | 2014-01-01 | 钢铁研究总院 | Processing technique of nickel-based heat-resisting alloy boiler pipe |
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