CN107130185A - A kind of resistance to irradiation martensite steel of low activation of new dispersion-strengtherning and its Technology for Heating Processing - Google Patents
A kind of resistance to irradiation martensite steel of low activation of new dispersion-strengtherning and its Technology for Heating Processing Download PDFInfo
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Abstract
The invention provides a kind of martensite steel, its essential element includes:8.0~8.8wt% Cr, 1.3~1.7wt% W, 0.15~0.25wt% V, 0.15~0.25wt% Ta, 0.30~0.70wt% Mn, 0.06~0.10wt% C, 0.02~0.06wt% N, 0.005~0.015wt% Zr;The application makes material M in process by reducing Cr contents, addition N element partly to replace C element23C6Amount of precipitation reduction;And by strictly controlling the composition proportion of each formation element of MX phases, separated out to greatest extent in MX phases form with ensureing Ta and V.The application, to obtain the tiny MX phases of Dispersed precipitate, effectively improves the high-temperature behavior during material military service by using special Technology for Heating Processing simultaneously.
Description
Technical field
The present invention relates to technical field of metal material, more particularly to martensite steel and preparation method thereof.
Background technology
Nuclear fusion energy is used as a kind of " cleaning " energy, it is desirable to which the structural material that fusion reactor is used is low-activation material, its mesh
Be to avoid material by Long-lived Radionuclides are produced after long-time neutron irradiation, reduce as far as possible due to structural material live
Potential radiological hazard, the post processing for reducing active nucleus waste matter and its expense caused by change.Both at home and abroad to fusion reactor
Low activation steel material has carried out substantial amounts of research, low activation ferrite/martensite (RAFM) steel is concentrated mainly on, such as Europe
CLAM steel of Eurofer steel, the F82H steel of Japan and China etc..But low activation martensitic steel is due to the limit of hot mastication
System, its upper limit temperature in use only has about 550 DEG C, constrains temperature in use of the material in fusion reactor.Improve low activation martensite
The use temperature upper limit of steel, and then the running temperature for improving fusion reactor blanket is designed, the thermal efficiency of fusion reactor can be effectively improved.
Oxide dispersion intensifying (Oxide dispersion strengthening, ODS) is to generally believe to have at present
Effect improves the technology of steel temperature in use.Due to dispersed oxide phase that is tiny in ODS steel and being evenly distributed, effectively hinder steel and exist
The migration of crystal boundary during the motion of deformation process Dislocations and high-temerature creep, makes material have higher high-temperature behavior.Mesh
Preceding low activation martensite/ferritic steel ODS (RAFM-ODS) overwhelming majority reported is prepared using powder metallurgical technique,
The mechanical alloying of the pre-alloyed powders such as iron, chromium and nano-oxide is realized by high-energy ball milling, and passes through hot pressed sintering or heat
Isostatic pressed processing obtains ODS steel.However, the ODS steel prepared using this method, due to the limitation of preparation technology and technology, single batch
Secondary yield is small, stability is poor between batch, size is small, it is impossible to faster to enter the industrial applications stage.Therefore, urgently provide at present
It is a kind of to have compared with high-mechanical property and the low activation martensitic steel of high-temperature behavior and preparation method thereof.
The content of the invention
Present invention solves the technical problem that being to provide a kind of low activation horse having compared with high-mechanical property and high-temperature behavior
Family name's body steel.
In view of this, this application provides a kind of martensite steel, by percentage to the quality, including:
Si<0.01%, P≤0.005%, S≤0.005%, O≤0.005%, Al≤0.01%, Ni≤0.005%, Nb
≤ 0.001%, Co≤0.005%, Cu≤0.005%, Mo≤0.005%;
Remaining is Fe;
And, C element, N element, Ta elements and V element meet formula (I) relation:
Wherein, w (C), w (N), w (Ta) and w (V) are C, N, Ta and V mass fraction respectively;
A is that 6~8, b is that 5~7, c is that 4~6, d is that 17~19, e is 0.07~0.1.
It is preferred that, the content of the Cr is 8.2~8.7wt%.
It is preferred that, the content of the N is 0.03~0.05wt%.
It is preferred that, the content of the C is 0.08~0.10wt%.
It is preferred that, the content of the Ta is 0.18~0.23wt%.
It is preferred that, the content of the Mn is 0.45~0.65wt%.
Present invention also provides a kind of preparation method of the martensite steel described in such scheme, comprise the following steps:
A), martensite steel ingot casting is forged, the elemental composition of the martensite steel ingot casting is as shown in claim 1;
B), the martensite steel ingot casting after forging is rolled, will be once returned after the martensite steel quenching after rolling
Fire, double tempering is carried out by the martensite steel ingot casting after being once tempered.
It is preferred that, the heating-up temperature of the quenching is 1050~1150 DEG C, and soaking time is 20~40min, the type of cooling
For water cooling.
It is preferred that, the temperature being once tempered is 840~860 DEG C, and soaking time is 20~40min, and the type of cooling is
Air cooling.
It is preferred that, the temperature of the double tempering is 720~760 DEG C, and soaking time is 50~80min, and the type of cooling is
Air cooling.
This application provides a kind of martensite steel, it includes:8.0~8.8wt% Cr;1.3~1.7wt% W;0.15
~0.25wt% V;0.15~0.25wt% Ta;0.30~0.70wt% Mn;0.06~0.10wt% C;0.02~
0.06wt% N;0.005%~0.015wt% Zr;The Cr contents of the present invention elect 8.0~8.8wt% as, suitably reduce Cr
Content can reduce low activation martensitic steel and form large-sized Cr in process23C6Phase, while ensureing that material has after irradiation
There are relatively low DBTT values;0.02~0.06wt% N element can partly substitute C element, further reduce large-sized Cr23C6Phase
Formed;0.15~0.25wt% V and 0.15~0.25wt% Ta can form the MX phases of dispersion-strengtherning, improve the synthesis of material
Mechanical property and high-temperature behavior;The application makes Ta and V most by rationally controlling the composition proportion of each component of MX phases simultaneously
Limits are separated out in tiny MX phases form;It is final make obtained martensite steel have preferable mechanical performance with it is high temperatures
Energy.
Further, during martensite steel is prepared, the application by using quenching technical and double tempering technique,
And by controlling the parameter in said process, separate out the MX small and disperseds in martensite steel, reduce M23C6Roughening, enter one
Step improves the mechanical performance and high-temperature behavior of martensite steel.
Brief description of the drawings
Fig. 1 is the TEM photos of martensite steel prepared by the embodiment of the present invention 1;
Fig. 2 is the TEM photos of martensite steel prepared by the embodiment of the present invention 2.
Embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, still
It should be appreciated that these descriptions are simply to further illustrate the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.
The embodiment of the invention discloses a kind of martensite steel, by percentage to the quality, including:
Si<0.01%, P≤0.005%, S≤0.005%, O≤0.005%, Al≤0.01%, Ni≤0.005%, Nb
≤ 0.001%, Co≤0.005%, Cu≤0.005%, Mo≤0.005%;
Remaining is Fe;
And, C element, N element, Ta elements and V element meet formula (I) relation:
Wherein w (C), w (N), w (Ta) and w (V) are C, N, Ta and V mass fraction respectively;
A is that 6~8, b is that 5~7, c is that 4~6, d is that 17~19, e is 0.07~0.1.
This application provides a kind of martensite steel, it replaces C element by adding appropriate N section, reduces Cr constituent contents,
And specific Technology for Heating Processing is combined, it is effectively reduced M23C6The precipitation of phase, separates out MX phases, the MX of small and dispersed to greatest extent
Relative to M23C6The growth rate compared under stabilization, high temperature is smaller, can effectively pin crystal boundary, the high temperature creep of raising material
Energy.
In the martensite steel of the application, Cr content is 8.0~8.8wt%, and in a particular embodiment, the Cr's contains
Measure as 8.2~8.7wt%, more specifically, the content of the Cr is 8.2wt%, 8.3wt%, 8.4wt%, 8.5wt%,
8.6wt% or 8.7wt%;Appropriate reduction Cr content can reduce low activation martensitic steel and form large-sized in process
Cr23C6Phase, while ensureing that material has relatively low DBTT values after irradiation.
W content is 1.3~1.7wt% in the application, in a particular embodiment, the content of the W can for 1.3wt%,
1.4wt%, 1.5wt%, 1.6wt% or 1.7wt%;The content of the Mn is 0.30~0.70wt%, in a particular embodiment,
The content of the Mn is 0.30wt%, 0.40wt%, 0.50wt%, 0.60wt% or 0.70wt%;The content of the Zr is
0.005~0.015wt%, it can crystal grain thinning.
The content of the C is 0.06~0.10wt%, in a particular embodiment, the content of the C is 0.06wt%,
0.07wt%, 0.08wt%, 0.09wt% or 0.10wt%;The content of the N is 0.02~0.06wt%, in specific embodiment
In, the content of the N is 0.03~0.05wt%, and addition N element part substitutes C element, can further reduce large-sized
Cr23C6Mutually formed.
V content is that 0.15~0.25wt%, Ta content are 0.15~0.25wt% in the application, in specific embodiment
In, the content of the Ta is 0.18~0.23wt%, and the content of the V is 0.16~0.23wt%.The Ta is to be formed
The MX phases of dispersion-strengtherning, improve the comprehensive mechanical property and high-temperature behavior of material.
In this application, described Si, P, S, O, Al, Ni, Nb, Co, Cu and Mo are impurity elements, should in actual production
When the element avoided, in this application, property is better more at least for above-mentioned element;Pass through neutron in being formulated by strict control composition
Long-lived Radionuclides Mo, Ni, Cu, Nb etc. can be produced after radiation, to ensure that it has certain low activation characteristic.
In the martensite steel of the application, the content of above-mentioned metallic element can not be enough to ensure that martensite steel has preferably
Mechanical performance and high-temperature behavior;Also need to make C, N, Ta and V content to meet formula (I) relation:
Wherein, w (C), w (N), w (Ta) and w (V) are C, N, Ta and V mass fraction respectively;
A is that 6~8, b is that 5~7, c is that 4~6, d is that 17~19, e is 0.07~0.1.
In formula (I), a, b, c, d and e are constant, are matched somebody with somebody according to the composition that above-mentioned relation formula can carry out each component of MX phases
Than calculating, it only just can guarantee that Ta, V when C, N, Ta, V meet this relational expression and separated out to greatest extent in MX phases form, so that
Effectively improve the high-temperature behavior of material.
Present invention also provides the preparation method of above-mentioned martensite steel, comprise the following steps:
A), martensite steel ingot casting is forged, the elemental composition of the martensite steel ingot casting is as shown in above-mentioned scheme;
B), the martensite steel ingot casting after forging is subjected to rolling process, one will be carried out after the martensite steel quenching after rolling
Secondary tempering, double tempering is carried out by the martensite steel ingot casting after being once tempered.
During martensite steel is prepared, the application is prepared for martensite steel ingot casting first;The martensite steel ingot casting
Preparation prepared according to technological means well known to those skilled in the art, this application is had no particular limits;Example
, the preparation of the martensite steel ingot casting can be according to first carrying out vacuum induction melting, then carries out vacuum consumable arc-melting;
During vacuum induction melting, easily oxidized alloy element deoxidation is fully added afterwards, and volatile alloy element is under atmosphere protection
Or melting tacit agreement stops vacuumizing addition;The vacuum consumable arc-melting is to further purification material.
According to the present invention, martensite steel ingot casting is forged and rolled successively, the forging is ability with the rolling
Technological means known to field technique personnel, has no particular limits to this application.During forging, the initial forging
Temperature be 1000~1300 DEG C, soaking time be 40~60min, the final forging temperature be 800~1000 DEG C;The rolling
Temperature is 1000~1200 DEG C, and soaking time is 50~70min, and the temperature of the finish to gauge is 800~900 DEG C, air cooling after rolling,
And the deflection of rolling is not less than 80%.
Then martensite steel ingot casting after rolling is heat-treated by the application, the heat treating regime be quenching technical-
Tempering process-double tempering technique.Specifically:
Quenching technical:Martensite steel after rolling is heated to 1050~1150 DEG C, 20~40min, water after coming out of the stove is incubated
It is cooled to room temperature.This operation stage controls the fluctuation range of quenching and preserving heat temperature within ± 20 DEG C, improves in-furnace temperature
Uniformity, the problems such as structural homogenity difference and uneven performance can be effectively improved.Low activation martensitic steel ingot casting 1050~
It is incubated at a temperature of 1150 DEG C, MX phases fail fully to be solid-solution in austenite, the MX phases of non-solid solution hinder austenite in holding stage
Grain coarsening, makes material avoid coarse grains while abundant austenitizing, makes to obtain comparatively fine former Ovshinsky after quenching
Body crystal grain.
Tempering process:Material after quenching is heated to coming out of the stove after 840~860 DEG C, 20~40min of insulation and is air-cooled to
Room temperature.Only MC precipitation in above-mentioned tempering range, without M23C6Separate out, can make C more sufficiently with tiny MC's
Form is separated out, and Dispersed precipitate improves the mechanical performance and high-temperature behavior of material among matrix;C is analysed in MC forms in material
Go out, reduce the content of C element in matrix, it is suppressed that M in subsequent processes23C6Separate out.This operation stage temperature is not
Preferably too high also unsuitable too low, such as temperature is relatively low, then can separate out M23C6 phases, temperature is higher, then tissue can be caused to occur austenite phase
Become.
Double tempering technique:Material after being once tempered is heated into air cooling after 720~760 DEG C, 50~80min of insulation to return
Fire.The tempering of this operation stage is further precipitation MX and M23C6, reduce material super saturated solid solution degree and lattice dot matrix it is abnormal
Become;Because a tempering stage consumes the C element of a part, this tempering stage M is reduced23C6Quantity and size, slow down
The M during high-temperature service23C6Roughening.The temper in this stage can continue to separate out the MX of small and dispersed, strengthen matrix,
Improve the high-temperature behavior of material.
The present invention proposes a kind of low activation martensite steel of resistance to irradiation of new dispersion-strengtherning, and the material is different from using powder smelting
Oxide dispersion intensifying steel prepared by gold process, with preferable comprehensive mechanical property, high-temperature behavior and low activation characteristic, can be fitted
When the temperature in use for improving low activation martensitic steel, the use requirement of fusion reactor and fission-type reactor structural material disclosure satisfy that.Tool
Body, the application replaces C element by adding appropriate N section, and appropriate reduction Cr contents effectively reduce M23C6Amount of precipitation;
By the composition proportion for rationally controlling each component of MX phases, it is ensured that Ta and V are separated out in MX phases form to greatest extent, disperse point
It is distributed in matrix and strengthens matrix;Further, the application is returned by adjusting Technology for Heating Processing, the superhigh temperature of 840~860 DEG C of increase
Fire, makes MC phases individually disperse educt, and reduction double tempering temperature promotes M23C6Precipitation, the low activation steel of resistance to irradiation can be effectively improved
Elevated temperature strength and high temperature endurance performance.The present invention is compared to RAFM-ODS steel, and method is simple, favorable repeatability, can be achieved big
Technical scale is produced;It is suitable for the preparation of various low activation martensitic steel section bars.The low activation martensitic steel room that the present invention is obtained
Warm tensile strength is more than 790MPa;550 DEG C of tensile strength are close to 610MPa;650 DEG C of tensile strength are more than 400MPa;Longitudinal direction and horizontal stroke
Work(is absorbed more than 200J to the room temperature impact of sample;The duration of creep exceedes under 600 DEG C, 190MPa stress conditions
10000h;
For a further understanding of the present invention, the preparation method of the martensite steel provided with reference to embodiment the present invention is entered
Row is described in detail, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
(1) by percentage to the quality, according to composition proportion:Cr 8.5%, W 1.5%, V 0.16%, Ta 0.20%, Mn
0.45%, C 0.08%, N 0.02%, Zr 0.005%~0.015%, Si<0.01%, P≤0.005%, S≤0.005%,
O≤0.005%, Al≤0.01%, Ni≤0.005%, Nb≤0.001%, Co≤0.005%, Cu≤0.005%, Mo≤
0.005% and the scaling loss amount proportioning raw material of alloy, wherein C, N, Ta and V meet formula (I) relational expression;
(2) raw material, oxidizable conjunction are sequentially added according to the scaling loss and boiling characteristics of alloying element in vaccum sensitive stove
Gold element deoxidation is fully added afterwards, and volatile alloy element is under atmosphere protection or melting latter stage stops vacuumizing addition, on
State raw material and the qualified ingot casting of composition is prepared after vacuum induction melting;
(3) ingot casting prepared is used into vacuum consumable arc-melting, further purifies material;
(4) ingot casting for obtaining step (3) is forged, and initial forging temperature is 1150 DEG C, is incubated 50min, finish-forging temperature
900 DEG C of degree;
(5) material of forging is subjected to rolling process, 1100 DEG C of rolling temperature is incubated 60min, and 850 DEG C of finishing temperature is rolled
Air cooling after system, total deflection is not less than 80%;
(6) it is heat-treated after material rolling, in water cooling is to room temperature after 1050~1150 DEG C of 20~40min of insulation, then
Room temperature is air-cooled to after 840~860 DEG C of 20~40min of insulation, then air cooling is tempered after 720~760 DEG C of 50~80min of insulation, is returned
The martensite steel of the tempered martensite of tiny MX phases Dispersed precipitate is obtained after fire, as shown in Figure 1.
The performance of martensite steel manufactured in the present embodiment is detected, testing result is:Martensite steel room manufactured in the present embodiment
The average 810MPa of warm tensile strength;550 DEG C of tensile strength average out to 595MPa;650 DEG C of tensile strength average out to 407MPa;It is all
The room temperature impact numerical value of vertical and horizontal sample is between 200-280J;Creep holds under 600 DEG C, 190MPa stress conditions
The long time is more than 10074h.
Embodiment 2
(1) by percentage to the quality, according to composition proportion:Cr 9.0%, W 1.5%, V 0.11%, Ta 0.25%, Mn
0.45%, C 0.08%, N 0.03%, Zr 0.005%~0.015%, Si<0.01%, P≤0.005%, S≤0.005%,
O≤0.005%, Al≤0.01%, Ni≤0.005%, Nb≤0.001%, Co≤0.005%, Cu≤0.005%, Mo≤
0.005% and the scaling loss amount proportioning raw material of alloy, wherein C, N, Ta and V meet formula (I) relational expression;
(2) above-mentioned raw material, easy oxygen are sequentially added according to the scaling loss and boiling characteristics of alloying element in vaccum sensitive stove
The deoxidation of chemical combination gold element is fully added afterwards, and volatile alloy element is under atmosphere protection or the stopping of melting latter stage is vacuumized and added
Enter, raw material prepare the qualified ingot casting of composition after vacuum induction melting;
(3) ingot casting prepared is used into vacuum consumable arc-melting, further purifies material;
(4) ingot casting for obtaining step (3) is forged, and initial forging temperature is 1150 DEG C, is incubated 50min, finish-forging temperature
900 DEG C of degree;
(5) material of forging is subjected to rolling process, 1100 DEG C of rolling temperature is incubated 60min, and 850 DEG C of finishing temperature is rolled
Air cooling after system, total deflection is not less than 80%;
(6) it is heat-treated after material rolling, in water cooling is to room temperature after 1050~1150 DEG C of 20~40min of insulation, then
Room temperature is air-cooled to after 840~860 DEG C of 20~40min of insulation, then air cooling is tempered after 720~760 DEG C of 50~80min of insulation, is returned
The martensite steel of the tempered martensite of tiny MX phases Dispersed precipitate is obtained after fire, as shown in Figure 2.Due to Ta in the present embodiment
Content is higher, promotes MX phases and separates out and grows up, therefore the MX in the present embodiment is relatively large sized.
The performance of martensite steel manufactured in the present embodiment is detected, testing result is:Martensite steel room manufactured in the present embodiment
The average 790MPa of warm tensile strength;550 DEG C of tensile strength average out to 585MPa;650 DEG C of tensile strength average out to 401MPa;It is all
The room temperature impact numerical value of vertical and horizontal sample is between 200-280J;Creep holds under 600 DEG C, 190MPa stress conditions
The long time is more than 9137h.
The explanation of above example is only intended to the method and its core concept for helping to understand the present invention.It should be pointed out that pair
, under the premise without departing from the principles of the invention, can also be to present invention progress for those skilled in the art
Some improvement and modification, these are improved and modification is also fallen into the protection domain of the claims in the present invention.
The foregoing description of the disclosed embodiments, enables professional and technical personnel in the field to realize or using the present invention.
A variety of modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The most wide scope caused.
Claims (10)
1. a kind of martensite steel, by percentage to the quality, including:
Si<0.01%, P≤0.005%, S≤0.005%, O≤0.005%, Al≤0.01%, Ni≤0.005%, Nb≤
0.001%, Co≤0.005%, Cu≤0.005%, Mo≤0.005%;
Remaining is Fe;
And, C element, N element, Ta elements and V element meet formula (I) relation:
<mrow>
<mfrac>
<mrow>
<mi>a</mi>
<mo>&CenterDot;</mo>
<mi>w</mi>
<mrow>
<mo>(</mo>
<mi>C</mi>
<mo>)</mo>
</mrow>
<mo>+</mo>
<mi>b</mi>
<mo>&CenterDot;</mo>
<mi>w</mi>
<mrow>
<mo>(</mo>
<mi>N</mi>
<mo>)</mo>
</mrow>
</mrow>
<mrow>
<mi>c</mi>
<mo>&CenterDot;</mo>
<mi>w</mi>
<mrow>
<mo>(</mo>
<mi>T</mi>
<mi>a</mi>
<mo>)</mo>
</mrow>
<mo>+</mo>
<mi>d</mi>
<mo>&CenterDot;</mo>
<mi>w</mi>
<mrow>
<mo>(</mo>
<mi>V</mi>
<mo>)</mo>
</mrow>
</mrow>
</mfrac>
<mo>></mo>
<mi>e</mi>
<mo>-</mo>
<mo>-</mo>
<mo>-</mo>
<mrow>
<mo>(</mo>
<mi>I</mi>
<mo>)</mo>
</mrow>
<mo>;</mo>
</mrow>
Wherein, w (C), w (N), w (Ta) and w (V) are C, N, Ta and V mass fraction respectively;
A is that 6~8, b is that 5~7, c is that 4~6, d is that 17~19, e is 0.07~0.1.
2. martensite steel according to claim 1, it is characterised in that the content of the Cr is 8.2~8.7wt%.
3. martensite steel according to claim 1, it is characterised in that the content of the N is 0.03~0.05wt%.
4. martensite steel according to claim 1, it is characterised in that the content of the C is 0.08~0.10wt%.
5. martensite steel according to claim 1, it is characterised in that the content of the Ta is 0.18~0.23wt%.
6. martensite steel according to claim 1, it is characterised in that the content of the Mn is 0.45~0.65wt%.
7. the preparation method of the martensite steel described in claim 1, comprises the following steps:
A), martensite steel ingot casting is forged, the elemental composition of the martensite steel ingot casting is as shown in claim 1;
B), the martensite steel ingot casting after forging is rolled, will be once tempered after the martensite steel quenching after rolling, will
Martensite steel ingot casting after being once tempered carries out double tempering.
8. preparation method according to claim 7, it is characterised in that the heating-up temperature of the quenching is 1050~1150
DEG C, soaking time is 20~40min, and the type of cooling is water cooling.
9. preparation method according to claim 7, it is characterised in that the temperature being once tempered is 840~860 DEG C,
Soaking time is 20~40min, and the type of cooling is air cooling.
10. preparation method according to claim 7, it is characterised in that the temperature of the double tempering is 720~760 DEG C,
Soaking time is 50~80min, and the type of cooling is air cooling.
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