CN105177262B - A kind of method for improving special grain boundary ratio in precipitation strength austenitic heat-resistance steel - Google Patents
A kind of method for improving special grain boundary ratio in precipitation strength austenitic heat-resistance steel Download PDFInfo
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- CN105177262B CN105177262B CN201510625858.1A CN201510625858A CN105177262B CN 105177262 B CN105177262 B CN 105177262B CN 201510625858 A CN201510625858 A CN 201510625858A CN 105177262 B CN105177262 B CN 105177262B
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Abstract
The invention belongs to precipitation strength austenitic heat-resistance steel fields, are related to a kind of method for improving special grain boundary ratio in precipitation strength austenitic heat-resistance steel.Optimization processing technique includes solid solution, cold rolling and annealing.It is characterized in that, the solution treatment first through 1150~1300 DEG C of 20~60min of holding；Deflection is carried out again as 20~60% room temperature rollings, and single pass rolling reduction is not less than 15%, then at a temperature of 1100~1250 DEG C, carries out periodical short-cycle annealing, water cooling.After optimization processing, special grain boundary is evenly distributed in precipitation strength austenite heat-resistance steel microscopic structure, and ratio is higher than 80%.The present invention improves strain storage energy by increasing deformation at room temperature amount, promote the generation recrystallized in precipitation strength austenitic steel, so as to improve special grain boundary ratio in the high Cr high Ni austenitic heat-resistance steels of precipitation strength type, optimize itself and the relevant performance of crystal boundary, especially corrosion resistance and Flouride-resistani acid phesphatase swelling ability.
Description
Technical field
The present invention is suitable for austenitic heat-resistance steel and face-centered cubic (the Face Centered that disperse educt is mutually strengthened
Cubic, fcc) structure Metal and Alloy.Low Σ CSL (Coincidence Site in particular in austenitic heat-resistance steel
Lattice, CSL) special construction crystal boundary content raising, provide a kind of technical method, the invention belongs to deform with heat treatment skill
Art field.
Background technology
Development cleaning, overcritical water cooling concept heap of efficient IVth generation and ultra supercritical thermal power generation system, to reducing CO2
Discharge, alleviating energy crisis are of great significance.The Service Environment of high temperature and pressure moisture vapor to the high temperature corrosion resistance of material and
Heat resistance proposes requirements at the higher level.At present, austenitic heat-resistance steel usually mutually improves its mechanical behavior under high temperature with disperse educt.But
It is that austenitic heat-resistance steel is Radiation hardness, resistance under the synergistic effect of neutron irradiation, higher temperature and harsh corrosive medium
Corrosive nature, the corrosion resistance especially in supercritical water still need to be further improved.The Radiation hardness of austenitic heat-resistance steel and
Corrosion resistance and grain boundary structure type in its microscopic structure and distribution in high temperature and pressure is closely related.Therefore, raising can be passed through
The method of special grain boundary ratio optimizes and improves the austenitic heat-resistance steel performance related with crystal boundary, such as grain boundary decision, irradiation are swollen
Swollen, segregation, sensitization and corrosion etc..
In polycrystalline material, intercrystalline is using crystal boundary as interface, the structure and property of some crystal boundaries are different from freely
Big angle crystal boundary, atom coincidence probability is relatively large, and the regularity of arrangement is higher, and crystal boundary energy is relatively low, referred to as low Σ CSL (Σ<
29) crystal boundary.1984, Japanese scholars Watanabe was put forward for the first time the saying of " grain boundary design and control ".Nineteen ninety-five, Lin
Et al. by further studying, developed into " bounding engineering " concept.At present, bounding engineering has become a kind of feasible extensively
Improve material intergranular corrosion resistance, stress corrosion, the effective way for improving the performances such as creep strength, high-temperature oxydation.By reasonable
Thermo-mechanical processi can with design effectively and control material crystal boundary be distributed.Mainly there are Deformation recrystallization and thermomechanical annealing：(1) exist
After deformation less than 10%, anneal within (tens hours) for a long time less than recrystallization temperature；After (2) 10~40% deformation,
Anneal, and repeat 3~7 times higher than the short time (5~60min) of recrystallization temperature.Both techniques are chiefly used in
The metal materials such as 304,316 austenitic stainless steels, nickel-base alloy, metal on the basis of annealing twin is formed, improve low Σ
CSL crystal boundary contents.Engelberg has found when in influence of the deformation history to deformation after unloading amount for studying 304 type stainless steels,
3 crystal boundaries of Σ of higher percentages and two level, three-level twin boundary are obtained when single pass heavy deformation is 5%/1050 DEG C/1h.And two
It is respectively 30% and 82% to walk large strain, does not obtain desired low Σ CSL crystal boundary contents but.Fang etc. is to 304 austenites
Stainless steel research shows that, small deformation amount (6%~10%) sample 1173K carry out for a long time (2~96h) annealing, can increase
The ratio of special grain boundary, and the connectivity of general big angle crystal boundary network is effectively blocked, improve the intercrystalline corrosion drag of material.
Kumar etc. thought in annealing process, the 304L austenitic stainless steels of different distortion amount (50~80%), 3 special grain boundaries of Σ
Generation process is different.The CSL crystal boundary scores that Sekine is observed in the PNC316 of bounding engineering control reach 86%, crystal boundary net quilt
Partition, after 700 DEG C of timeliness 100h, crystal boundary net does not have significant change, has very low void swelling rate.
But for crystal boundary work in more excellent 310 grades of austenitic heat-resistance steels of mechanical behavior under high temperature and structure stability
The research of journey design, is rarely reported.Due to the addition of high Cr, high Ni and carbide so that it is follow-up annealed
Precipitated phase is generated in journey, consumption strain storage energy inhibits the generation of recrystallization, special grain boundary content is not easy to improve.Therefore, this hair
It is bright to propose a kind of method for the medium deformation at room temperature and subsequent high temperature recrystallization annealing for increasing strain storage energy, improve special construction
Crystal boundary content, so as to improve improve 310 austenitic heat-resistance steels with the relevant performance of crystal boundary.The process that the present invention uses,
There is simple and easy to do, energy-saving consumption-reducing.
Invention content
It is the technical issues of solution in the present invention：Overcome and do not consider the competition process with recrystallization is precipitated in the prior art,
Precipitation process consumes system capacity, and the energy for being used in recrystallization is reduced, recrystallization lag, existing bounding engineering design method
Implementation result it is not good enough.The present invention provides a kind of highly practical, institutional framework stabilization, raising precipitation strength austenitic heat-resistance steels
The effective ways of middle special grain boundary content, to advanced optimize the corrosion-resistant and Flouride-resistani acid phesphatase swelling performance of austenitic heat-resistance steel.
The technical solution adopted by the present invention is：To add the high Cr high Ni austenitic heat-resistance steels of carbide
Hot rolled steel plate is material, and material composition is (wt.%)：C is not more than 0.1；Si:0.2~0.8；Mn:0~1.6；Cr:15~26；
Ni:16~28；Mo:0~3；Ti:0~0.5；W:0~0.5；Zr:0~0.5；V:0~0.5；P is not more than 0.02；S is not more than
0.015；Surplus is F.Improve the deformation heat treatment method of its special grain boundary ratio：Including solid solution, cold rolling and annealing.It is main special
Sign is following steps：
(1) solution treatment：Since alloy content is higher, in order to smoothly realize deformation at room temperature, need to be consolidated under at higher temperature
Molten processing.Within the temperature range of 1150~1300 DEG C, 20~60min is kept the temperature, then hardening；
(2) cold rolling：At room temperature, the rolling of medium deformation amount is carried out to the steel plate after solution treatment, deflection is ranging from
20~60%, control single pass rolling reduction is not less than 15%；
(3) it anneals：Within the temperature range of 1100~1250 DEG C, same temperature divides different cycles to anneal, first week
Phase is heat preservation 20min and then hardening, and second round is after keeping the temperature 20min hardening at such a temperature, then keeps the temperature hardening after 40min.
Period 3 is then the hardening after insulation annealing 60min at such a temperature on the basis of second round, and so on.Periodically move back
Ignition technique process schematic refers to Fig. 1.
The step (1) keeps the temperature 25~40min, water cooling to room temperature preferably at 1180~1250 DEG C.
Cold roling reduction in the step (2) is preferably 30~40%, and two passages are completed.
The step (3) carries out the annealing in 1~2 period, water cooling to room temperature preferably at 1150~1230 DEG C.
It is divided to two sections of heating in the step (1) and (3), the heating rate of room temperature~800 DEG C is not more than 10 DEG C/min；800
DEG C~heating rate of target temperature is 15~25 DEG C/min.
It is an advantage of the invention that：
(1) present invention is generally directed to the austenite heat-resistance stainless steel containing stabilizing element or with broad prospect of application
Nuclear power and ultra supercritical power station high-performance austenitic heat-resistance steel.By suitably deforming heat treatment process, crystal boundary class is controlled
Type, low Σ CSL crystal boundary contents are more than 80%, so as to advanced optimize the high-temperature behavior of austenitic heat-resistance steel, especially oxytolerant
The property changed, corrosive nature and the ability of anti-neutron irradiation swelling；
(2) in precipitation strength austenitic heat-resistance steel, in order to realize the recrystallization of annealing process and improve special grain boundary ratio
Example, the room temperature rolling deformation of the invention using medium deformation amount increase accumulation dislocation and strain storage energy, and in higher temperature
Under anneal；
(3) present invention is avoided using circulative cyclic annealing process in annealing process during soak, brilliant
Particle size is grown up, so as to fulfill optimization microstructure and the purpose of raising special grain boundary content.The technique used in the present invention
Method does not need to long-time heat preservation, it is not required that carries out recycling multiple cold deformation, the method is more easy, has operable
Property is strong, has both the advantages of saving time and cost.
Description of the drawings
Fig. 1 is the process schematic representation of periodic cycle of the present invention annealing
Fig. 2 is the special grain boundary distribution map of present example 1
Fig. 3 is the special grain boundary distribution map of present example 2
Fig. 4 is the special grain boundary distribution map of present example 3
Specific embodiment
For the technical solution that the present invention is furture elucidated, illustrated below by specific example.
Embodiment 1 carries out 310 austenitic heat-resistance steel of modified of rolled crystal boundary optimization processing, nominal chemical composition
For：25Cr, 20Ni, 0.1C, 0Mn, 2.0Mo, 0.65Si, 0.2Ti, 0.2Zr, 0.15W, 0.15V, the average crystal grain ruler of rolled
Very little is 30 μm.
The first step at 1200 DEG C, keeps the temperature 40min, room temperature rolling deformation is then carried out on two-roller mill, and deflection is
30%, two passages are completed；Second step, at 1120 DEG C, hardening is cooled to room temperature after keeping the temperature 20min, then at 1120 DEG C again
40min is kept the temperature, hardening is cooled to room temperature；Third walks, and to treated, sample carries out a solution polishing and EBSD tests, uses HKL-
5 softwares of Channel are analyzed, and different crystal boundary contents are as shown in table 1, and the special grain boundary content of Σ≤29 is up to 86.24%；It is distributed such as
Shown in Fig. 2.
Embodiment 2 is using the method for above-mentioned (1)~(3), and sample is after 1230 DEG C of temperature 30min are dissolved, progress
40% cold rolling at room temperature.The recrystallization annealing in 2 periods is then carried out at 1150 DEG C.It is organized to carry out EBSD observations, by
5 softwares of HKL-Channel analyze EBSD pictures, and the results are shown in Figure 3.The distribution of different special grain boundaries is more uniform,
The crystal boundary content of its content Σ≤29 is 83.15% (being shown in Table 1, the different crystal boundary contents (quantitative proportion, %) of each example steel).
Embodiment 3 carries out crystal boundary optimization processing according to the above method to 310 stainless steel of modified.Implement the nameization of steel
It studies and is divided into：Fe-25Cr-20Ni-0.2T-0.2Zr-0.1W-0.15V-2.0Mn-0.65Si-0.1C (wt.%), sample exists
After 1250 DEG C of temperature 40min solid solutions, 50% cold rolling at room temperature is carried out.The recrystallization in 1 period is then carried out at 1200 DEG C
Annealing.It is organized to carry out EBSD observations, the results are shown in Figure 4.The uniformity of microscopic structure is preferable, the number of different crystal boundary types
It is higher to measure percentage summation, up to 86.33%.
Table 1
Claims (4)
- A kind of 1. method for improving special grain boundary ratio in precipitation strength austenitic heat-resistance steel：Including solid solution, cold rolling and annealing, It is characterized in that following steps：Step 1: solution treatment：Using add carbide high Cr high Ni austenitic heat-resistance steels hot rolled steel plate as Material, for the austenite heat-resistance stainless steel containing stabilizing element, ingredient is (wt.%)：C is not more than 0.1; Si:0.2~ 0.8; Mn:0~1.6; Cr:15~26; Ni:16~28; Mo:0~3; Ti:0~0.5; W:0~0.5; Zr: 0~0.5; V:0~0.5;P is not more than 0.02;S is not more than 0.015;Surplus is Fe；In 1150~1300 DEG C of temperature model In enclosing, 20~60min is kept the temperature, then hardening；Step 2: cold rolling：At room temperature, two passes of medium deformation amount are carried out to the steel plate after solution treatment, are increased tired Product dislocation and strain storage energy, deflection ranging from 20~60%, control single pass rolling reduction are not less than 15%；Step 3: annealing：Within the temperature range of 1100~1250 DEG C, same temperature divides different cycles to anneal, first week Phase is heat preservation 20 min and then hardening, and second round is after keeping the temperature 20 min hardening at such a temperature, then quenches after keeping the temperature 40 min Water, period 3 are then the hardening after 60 min of insulation annealing at such a temperature on the basis of second round, and so on；Control Crystal boundary type, low Σ CSL crystal boundary contents optimize and improve the austenitic heat-resistance steel performance related with crystal boundary more than 80%.
- 2. a kind of method for improving special grain boundary ratio in precipitation strength austenitic heat-resistance steel according to claim 1：Its It is characterized in that in the step 1：It is divided to two sections of heating, the heating rate of room temperature~800 DEG C is not more than 10 DEG C/min；800 DEG C~mesh The heating rate for marking temperature is 15~25 DEG C/min；25~40min is kept the temperature at 1180~1250 DEG C.
- 3. a kind of method for improving special grain boundary ratio in precipitation strength austenitic heat-resistance steel according to claim 1：Its The cold roling reduction being characterized in that in the step 2 is characterized in that：Carry out two passes in room temperature, drafts for 30~ 40%, increase accumulation dislocation and strain storage energy, control single pass rolling reduction are not less than 15%.
- 4. a kind of method for improving special grain boundary ratio in precipitation strength austenitic heat-resistance steel according to claim 1：Its It is characterized in that the step 3：At 1150~1230 DEG C, the annealing in 1~2 period is carried out.
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| CN103205655A (en) * | 2013-03-21 | 2013-07-17 | 宝钢不锈钢有限公司 | Sn-containing austenitic stainless steel and manufacturing method thereof |
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