CN103194692B - A kind of Martensitic steel for supercritical water reactor and preparation method thereof - Google Patents
A kind of Martensitic steel for supercritical water reactor and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to metal material field, relate to the effective martensitic steel of a kind of supercritical water reactor fuel sheath.The composition of steel is: C0.09 ~ 0.11, Cr11.7 ~ 12.2, Mn0.95 ~ 1.05, Mo0.95 ~ 1.05, W1.05 ~ 1.15, Ni0.95 ~ 1.1, N0.05 ~ 0.07, Ta0.13 ~ 0.18, Al0.04 ~ 0.06, Si0.12 ~ 0.18, V0.18 ~ 0.23, B<0.001, S<0.003, P<0.005, Fe surplus; Made by hot rolling, and heat-treat, heat treating regime is: 950 ~ 1050 DEG C/15 ~ 25min quenches; 750 ~ 800 DEG C/120min tempering.Material of the present invention has the excellent comprehensive performances such as hot strength is high, tough-brittle transition is low, high temperature creep-resisting, anti-supercritical water corrosion, irradiation induced radioactivity are low.By improving the content of Cr, to ensure its resistant to supercritical water corrosion performance; Increasing its hardening capacity and anti-radiation performance by adding W, V, Ta, Mn, Mo, full martensitic stucture can be obtained; By control Ni, Mo content, to reduce its induced radioactivity.
Description
Technical field
The invention belongs to metal material field, relate to the effective martensitic steel of a kind of supercritical water reactor fuel sheath, have that hot strength is high, resistant to supercritical water corrosion, and there is low radioactivity of inducting.
Background technology
Along with Economic development is to the continuous increase of energy demand, nuclear energy as a kind of safe, clean, efficiently energy form manifested its critical role in new energy field gradually.Entered the development of the 4th generation of technology such as nuclear energy system at present in the world, as water cooled reator unique in the 4th generation of technology such as nuclear energy system six kinds of candidate's heap-type, supercritical water reactor more meets the requirement of China's nuclear power relevant unit experience and technology hand down.Supercritical water reactor while all more existing light water reactor of performance improves a lot in every respect, also proposes new challenge in material, reactor design etc.
As the fuel tube that working condition in super heap is near water the harshest, inner wall surface thereof faces strong neutron irradiation, fission gas pressure and burn into fuel swelling, inhale hydrogen causes the crisp and harm such as involucrum and pellet interaction; Outer wall is subject to supercritical water high temperature, pressure, wash away, vibrate and corrode and the threat such as hydrogen embrittlement.This just requires can material to have, and hot strength is high, high temperature good toughness, high temperature creep-resisting, resistance to high temperature corrosion, Flouride-resistani acid phesphatase fragility and low activity.Existing water cooled reator, supercritical thermal power station cladding tubes or cooling tube material are not all suitable for the Service Environment of supercritical water reactor.
Ferrito-martensite steel, because having the advantages such as thermal conductivity is high, thermal expansivity is little, and void swelling is low, is the preferred material of nuclear reactor key part.The comparative maturity studied in the world ferrito-martensite steel mainly contain EUROFER97 steel, the F82H of Japan, HT9, HCM12A steel of the U.S. etc. (table 1 give their main component), these steel great majority are positioned at the chromium content of 7-9wt%, to obtain the high single-phase martensite steel of obdurability.But under the supercritical water environment of 550-650 DEG C, 25MPa, the martensitic steel of 7-9wt% chromium content exists serious surrosion, often raises 100 DEG C with temperature, surrosion improves 4-5 doubly, can not meet the demand of supercritical behavior to material far away.Therefore the working condition for supercritical water reactor is needed, the ferrito-martensite steel of exploitation hot strength high, good corrosion resistance, low radioactivity of inducting.
Table 1
Summary of the invention
For the working condition requirement of supercritical water reactor, the present invention proposes a kind ofly to be applicable to high-strength heat-resistant steel of supercritical water operating mode and preparation method thereof, chromium content is brought up to 12% to ensure the resistant to supercritical water corrosion performance of steel, add element Ni, Mn and N of expanding γ phase region and reduce ferrite content in steel, to ensure the magnitude mechanical performance of steel, machining property and High-Temperature Creep Performance.And by micro-alloying technology, add some trace elements (B, Mo) to guarantee to obtain single-phase martensite tissue.
The mass percentage of each composition of Martensitic steel for supercritical water reactor is as follows:
C:0.09 ~ 0.11%, Cr:11.7 ~ 12.2%, Mn:0.95 ~ 1.05%, Mo:0.95 ~ 1.05%, W:1.05 ~ 1.15%, Ni:0.95 ~ 1.1%, N:0.05 ~ 0.07%, Ta:0.13 ~ 0.18%, Al:0.04 ~ 0.06%, Si:0.12 ~ 0.18%, V:0.18 ~ 0.23%, B<0.001%, S<0.003%, P<0.005%, Fe surplus.
Chromium affects material one of corrosion proof important element in supercritical water.Increase with chromium content, the solidity to corrosion of steel increases, and its resistance to high temperature oxidation can there will be obvious raising.But because chromium in steel works to reduce γ phase region, when carbon content lower (content controls about 0.1%), after in steel, chromium content brings up to 12% from 9%, ferrite content in ferrito-martensite steel obviously raises, can not form full martensitic stucture under room temperature, the solidity to corrosion of steel and intensity reduce.Therefore for corrosion proof demand, chromium content is decided to be about 12%, ferrite content in steel is reduced by adding element Ni, Mn and N of expanding γ phase region, ensure the intensity of steel, in steel, the content of Ni can not be too high simultaneously, control 0.95 ~ 1.1%, to ensure that this alloy at room temperature can obtain martensitic stucture; And overcome Ni, in irradiation process, transmuting occurs, to ensure the radiation-resistant property of steel, being added with of a small amount of Ni is beneficial to improves its solidity to corrosion in supercritical water.
In steel of the present invention, W and Mo all plays and reduces γ phase region, expand the effect of alpha phase zone, and be carbide, requirement fusion reactor ferrito-martensite steel for low activation all adopts W to replace Mo to reduce the activity of material, because supercritical water reactor adopts thermal neutron spectrum, do not have fusion reactor strong to the radiation damage of material, therefore the content that present invention reduces W adopt part Mo to replace W.The interpolation of Mo can also play the effect of the temper brittleness of suppression or lightening material.
Mn is as expansion γ phase block elements, and the Mn content improved in the present invention can make ferrite content reduce equally.And Mn can effectively reduce the S content in steel as good deoxidation, sweetening agent, avoid the hot-short of the steel caused due to S too high levels.
N equally can expand γ phase region with C, and forms nitride with alloying element, and improve the intensity of steel, the interpolation of N can also improve the hardening capacity of steel.
When B is on the crystal boundary being distributed in steel, effectively can improve the creep rupture strength of steel, strengthening crystal boundary, reduces intergranular energy, and suppress ferrite forming core, in steel, the interpolation of a small amount of B just can improve the hardening capacity of steel greatly.
According to mentioned component, carry out vacuum metling, cast steel ingot, and carry out controlled rolling and cooling.Present invention also offers the heat treating method of above-mentioned Martensitic steel for supercritical water reactor, its concrete technology parameter is: quenching+high tempering, and wherein: quenching temperature is 950 ~ 1050 DEG C, tempering temperature is 850 ~ 860 DEG C, and tempering time is 90min-120min.
Concrete step of preparation process is as follows:
A () prepares steel ingot or continuous casting rod iron, the per-cent that its various composition accounts for total mass is: C0.09 ~ 0.11, Cr11.7 ~ 12.2, Mn0.95 ~ 1.05, Mo0.95 ~ 1.05, W1.05 ~ 1.15, Ni0.95 ~ 1.1, N0.05 ~ 0.07, Ta0.13 ~ 0.18, Al0.04 ~ 0.06, Si0.12 ~ 0.18, V0.18 ~ 0.23, B<0.001, S<0.003, P<0.005, Fe surplus;
B () carries out first time thermal distortion by the forging of steel ingot or continuous casting rod iron or rolling, obtain work in-process;
C described work in-process are heated to the scope of 1150 DEG C ~ 1200 DEG C by (), be again out of shape until obtain required shape and the goods of size by hot rolling;
D the goods being cooled to room temperature are heated to 950 ~ 1050 DEG C of temperature ranges and keep 15 ~ 25min by (), carry out austenitation heat treatment;
E goods by below the part cooling to 50 after austenitation heat treatment DEG C, and then are heated to 750 ~ 800 DEG C of temperature ranges and keep 100 ~ 130min by (), carry out tempering heat treatment and obtain martensitic steel goods.
Martensitic steel goods be can be made into seamless pipe by cold-stamped mode, need pony-roughing pass to anneal in cold-extrusion technology, annealing process is 800 ~ 820 DEG C/40min ~ 45min.
The forging of described step (b) or the temperature range of rolling are at 1100 DEG C ~ 900 DEG C.
Cooling operations after the thermal distortion of described step (b) before this dust and sand is carried out after being cooled to 600 DEG C in atmosphere, and is cooled to room temperature.
Described step (c) be cooling controlling and rolling controlling process, start rolling temperature at 1100 ~ 1050 DEG C, finishing temperature control, at about 850 ~ 950 DEG C, rolls the online spray cooling of rear employing.
The heat treating regime of described step (d) is: 950 ~ 1050 DEG C/15 ~ 25min quenches; 750 ~ 800 DEG C/120 ~ 150min tempering.Cooling operations after austenitation heat treatment is carried out in water.
Cooling operations after the tempering heat treatment of described step (e) is carried out in atmosphere.
According to steel prepared by mentioned component and thermal treatment process, be single-phase martensite steel (martensitic stucture content >95% is the macrograph of embodiment one as shown in Figure 1).The mechanical property of this martensitic steel is superior, uses for a long time under being applicable to the environment of less than 650 DEG C, and its room temperature tensile intensity is more than 917MPa, and unit elongation more than 20%, DBTT is-55 DEG C; At 600 DEG C, tensile strength is more than 482MPa, unit elongation more than 30%.At 550 DEG C, 25MPa, 200ppb O
2supercritical water in corrode 1000h after the surrosion of this martensitic steel be 459.42mg/dm
2, oxidated layer thickness is 38 μm, so have good resistant to supercritical water corrosion performance; These performances all meet the service requirements of supercritical water reactor.
This kind of super heap martensitic steel near water has B.C.T. structure, therefore swelling rate is lower than face-centred cubic austenitic stainless steel under neutron irradiation; W, V and Ta are carbides, the intermetallic compound having C to be formed is at high temperature very stable, the effect hindering strengthening is had after intercrystalline precipitation, so have very high hot strength, good high temperature creep property, good resistant to supercritical water corrosion characteristic and Flouride-resistani acid phesphatase embrittlement characteristic, can meet super service requirements of piling fuel canning material near water.This super heap martensitic steel near water has good hardening capacity equally, and can obtain whole martensitic stuctures, residual austenite content is very low.Same this kind of super heap martensitic steel near water is also applicable to fast reactor.
Accompanying drawing explanation
Fig. 1 is metallograph of the present invention (accompanying drawing of embodiment one)
Fig. 2 is the transmission electron microscope macrograph of way of example two of the present invention
Fig. 3 is the transmission electron microscope macrograph of example 950-1 of the present invention
Fig. 4 is the transmission electron microscope macrograph of example 950-2 of the present invention
Fig. 5 is the transmission electron microscope macrograph of example 950-5 of the present invention
Fig. 6 is the impact absorbing energy of example 950-5 of the present invention and the relation of probe temperature
Fig. 7 is the room temperature tensile intensity curve of example 950-1 and 950-5 of the present invention
Embodiment
Embodiment one:
A kind of Martensitic steel for supercritical water reactor, its various composition accounts for the per-cent of total mass: C0.09, Cr11.7, Mn1.05, Mo0.95, W1.05, Ni0.95, N0.06, Ta0.15, Al0.05, Si0.15, V0.2, B<0.001, S<0.003, P<0.005, Fe surplus, makes finished product by following steps:
A () prepares steel ingot or continuous casting rod iron, have the per-cent that following various composition accounts for total mass: C0.09, Cr11.7, Mn1.05, Mo0.95, W1.05, Ni0.95, N0.06, Ta0.15, Al0.05, Si0.15, V0.2, B<0.001, S<0.003, P<0.005, Fe surplus;
B () carries out first time thermal distortion to obtain work in-process by the forging of steel ingot or continuous casting rod iron or rolling;
C described work in-process are heated to 1150 DEG C of austenitizings by (), be again out of shape until obtain required shape and size by hot rolling;
D goods by below part cooling to 50 DEG C, and then are made sample by ().And be numbered 950-1 to 950-6;
E all samples is also heated to 950 DEG C of temperature ranges simultaneously and keeps the time cycle of 15min to carry out austenitation heat treatment by ();
F sample is cooled to less than 50 DEG C by () in water, and then the sample that difference is numbered is heated to 700 DEG C, 750 DEG C respectively, and also the time cycle of maintenance 20 and 120min carries out tempering heat treatment to 800 DEG C of temperature ranges accordingly.Concrete numbering and corresponding technique thereof are listed in the following table.
Heat treatment process of the present invention and feature thereof is embodied in example set in following table.The per-cent that its its composition accounts for total mass is C0.09, Cr11.7, Mn1.05, Mo0.95, W1.05, Ni0.95, N0.06, Ta0.15, Al0.05, Si0.15, V0.2, B<0.001, S<0.003, P<0.005, Fe surplus;
Embodiment two
A kind of Martensitic steel for supercritical water reactor, its composition accounts for the per-cent of total mass: C0.11, Cr12.2, Mn0.95, Mo1.05, W1.15, Ni1.1, N0.07, Ta0.18, Al0.06, Si0.18, V0.23, B<0.001, S<0.003, P<0.005, Fe surplus, and makes finished product by following steps:
A () prepares steel ingot or continuous casting rod iron, have the per-cent that following various composition accounts for total mass: C0.11, Cr12.2, Mn0.95, Mo1.05, W1.15, Ni1.1, N0.07, Ta0.18, Al0.06, Si0.18, V0.23, B<0.001, S<0.003, P<0.005, Fe surplus;
B () carries out first time thermal distortion to obtain work in-process by the forging of steel ingot or continuous casting rod iron or rolling;
C described work in-process are heated to 1200 DEG C of austenitizings by (), be again out of shape until obtain required shape and size by hot rolling;
D goods by below part cooling to 50 DEG C, and then are made sample by ().And be numbered 1000-7 to 1000-8 and 1050-9 to 1050-10 respectively;
E () sample is heated to respectively 1000 DEG C again and 1050 DEG C of temperature ranges keep the time cycle of 25min to carry out austenitation heat treatment;
F sample is cooled to less than 50 DEG C by () in water, and then the sample that difference is numbered is heated to 750 DEG C respectively, and also the time cycle of maintenance 20 and 120min carries out tempering heat treatment to 800 DEG C of temperature ranges accordingly.Concrete numbering and corresponding technique thereof are listed in upper table.
By the present invention through the sample of different heat treatment technique in known 800 DEG C of the result of the impact experiment of room temperature and-40 DEG C, the impact property that 120min tempering sample tool is best.Sample determination to this thermal treatment process ductile-brittle transition temperature of the present invention.Fig. 6 gives steel of the present invention through 800 DEG C, the impact absorbing energy of sample and the relation of probe temperature after 20min tempering.According to the definition of ductile-brittle transition temperature temperature, can learn that the present invention is through 800 DEG C from Fig. 7, ductile-brittle transition temperature degree ETT after 120min tempering
50value is for-55 DEG C, and its tensile strength is 917MPa, and unit elongation is 20%.
Claims (7)
1. a preparation method for Martensitic steel for supercritical water reactor, it is characterized in that being made by hot rolling, and heat-treat, concrete steps are as follows:
A () prepares steel ingot or continuous casting rod iron, have the per-cent that following various composition accounts for total mass: C0.09-0.11, Cr11.7-12.2, Mn0.95-1.05, Mo0.95-1.05, W1.05-1.15, Ni0.95-1.1, N0.05-0.07, Ta0.13-0.18, Al0.04-0.06, Si0.12-0.18, V0.18-0.23, B<0.001, S<0.003, P<0.005, Fe surplus;
B () carries out first time thermal distortion by the forging of steel ingot or continuous casting rod iron or rolling, obtain work in-process;
C described work in-process are heated to the scope of 1150 DEG C-1200 DEG C by (), be again out of shape until obtain required shape and the goods of size by hot rolling;
D the goods being cooled to room temperature are heated to 950-1050 DEG C of temperature range and keep 15-25min by (), carry out austenitation heat treatment;
E goods by below the part cooling to 50 after austenitation heat treatment DEG C, and then are heated to 750-800 DEG C of temperature range and keep 100-130min by (), carry out tempering heat treatment and obtain martensite goods; Described martensite goods wherein various composition account for the per-cent of total mass: C0.09-0.11, Cr11.7-12.2, Mn0.95-1.05, Mo0.95-1.05, W1.05-1.15, Ni0.95-1.1, N0.05-0.07, Ta0.13-0.18, Al0.04-0.06, Si0.12-0.18, V0.18-0.23, B<0.001, S<0.003, P<0.005, Fe surplus.
2. the method for the preparation of Martensitic steel for supercritical water reactor according to claim 1, is characterized in that martensite goods make seamless pipe by cold-stamped mode, needs pony-roughing pass to anneal in cold-extrusion technology, annealing process is 800 DEG C/40min.
3. the method for the preparation of Martensitic steel for supercritical water reactor according to claim 1, is characterized in that the forging of step (b) or the temperature range of rolling are at 1100 DEG C-900 DEG C.
4. the method for the preparation of Martensitic steel for supercritical water reactor according to claim 1, it is characterized in that cooling operations after the thermal distortion of step (b) before this dust and sand carry out in atmosphere after being cooled to 600 DEG C, and be cooled to room temperature.
5. the method for the preparation of Martensitic steel for supercritical water reactor according to claim 1, what it is characterized in that step (c) is cooling controlling and rolling controlling process, and start rolling temperature at 1100 DEG C, finishing temperature control, at 900 DEG C, rolls the online spray cooling of rear employing.
6. method according to claim 1, is characterized in that the heat treating regime of the austenitizing of step (d) is: 950-1050 DEG C/15-25min quenches, and the cooling operations after austenitation heat treatment is carried out in water.
7. method according to claim 1, is characterized in that the cooling operations after the tempering heat treatment of step (e) is carried out in atmosphere.
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| CN103805899A (en) * | 2014-02-10 | 2014-05-21 | 浙江大隆合金钢有限公司 | 12Cr10Co3W2MoNiVNbNB super martensite heat-resistant steel and production method thereof |
| CN106222371A (en) * | 2016-08-31 | 2016-12-14 | 无锡派克新材料科技股份有限公司 | A kind of heat resisting steel heat treatment method |
| CN106350647B (en) * | 2016-12-02 | 2018-08-24 | 机械科学研究总院青岛分院有限公司 | A kind of high nitrogen stainless bearing steel heat treatment process |
| CN107881368A (en) * | 2017-11-23 | 2018-04-06 | 宁波升鸿机械设备有限公司 | A kind of blower fan |
| CN108342661A (en) * | 2018-01-22 | 2018-07-31 | 江苏理工学院 | A kind of fired power generating unit heat-resisting steel alloy material and its manufacturing process |
| CN109504901A (en) * | 2018-12-11 | 2019-03-22 | 西安交通大学 | A kind of low activation martensitic steel and its heat treatment method of fast reactor fuel can |
| CN111733364B (en) * | 2020-07-08 | 2021-07-09 | 东莞理工学院 | Low-mismatching-degree high-strength steel and preparation method thereof |
| CN113355497B (en) * | 2021-06-04 | 2022-05-31 | 西安建筑科技大学 | Low-activation steel plate and preparation process thereof |
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