CN1264999C - Method for producing low-carbon steel or low-alloy steel plate having submicron crystal grain - Google Patents
Method for producing low-carbon steel or low-alloy steel plate having submicron crystal grain Download PDFInfo
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Abstract
The present invention discloses a making method for a low carbon steel or low alloy steel plate having submicron crystal grains, which comprises the following steps: the original steel blank is austenitized above the temperature of Ac3; then, the original steel blank is rolled in a heating mode under the temperature higher than Ar3, and the accumulation pressing amount of the original steel blank is from 40 to 90%; after the original steel blank is milled, the original steel blank is rapidly cooled; then, the original steel blank is rolled in a warming and cooling mode under the room temperature of 600 DEG C to room temperature, and the accumulation pressing amount of the original steel blank is greater than 40%; the original steel blank is directly cooled or coiled into a plate after rolling, can be cooled or coiled into a plate after the temperature of the original steel blank is kept for certain time, and can also be further and subsequently treated by a heat treatment process. The steel plate made by the present invention is composed of base body phase crystal grains, and few cementite grains which are dispersed and distributed. The diameters of the base body phase crystal grains are all within the range of 1.0 mu m to 0.2 mu m on a full plate thick section from the surface to the center part of the steel plate. The diameters of the cementite grains which are dispersed and distributed are all smaller than 0.2 mu m. The steel plate has the advantages of good structure stability (crystal grains are difficult to grow up), simple, convenient and practical making method.
Description
Technical field
The present invention relates to a kind of soft steel or low alloy steel steel plate manufacture method, particularly the soft steel or the low alloy steel of sub-micron grain (being that crystal grain diameter is in 1.0 μ m～0.1 mu m range).
Background technology
Soft steel and low alloy steel are usage quantity steel grades the most widely in the ferrous materials Application Areas.In order to improve the intensity of steel, common way is to add alloying element such as Mn, Si or carry out controlled rolling, controlled chilling, thermal treatment etc., also or add microalloy elements such as Nb, V.But for steel, not only require to have high intensity, high other good comprehensive performances such as toughness, but also need consider the problem of economize on resources (alloying element is few) and sustainable use aspects such as (easily recyclings).Grain refining is one of effective means few in number.But the most obtainable crystal grain minimum size of manufacture method of existing suitability for industrialized production superfine crystal particle steel plate is greater than the steel plate of 4～5 μ m.And the up-to-date patent of relevant ultra-fine grain steel also mainly concentrates on the micron-class superfine crystal grain steel.As, becoming the strain inducing dynamic phase trasnsition technology that ultra-fine grain steel is studied focus, the minimum ferrite crystal grain that can obtain is usually more than 1 μ m.Also do not adopt rolling method, as the disclosed a kind of method of European Patent Application No. EP0903412, at first general＜0.3%C steel is heated to Ac
3Above temperature is carried out austenitizing, then at Ar
3Above temperature is depressed more than 50%, requires three directions of X, Y and Z simultaneously or exert pressure continuously when depressing, and to be higher than the speed cooling of 3 ℃/s, can obtain the super fine organization of grain-size less than 3 μ m at last.
The grain refining of heavy-gauge steel iron construction material to there be suitable difficulty below 1 μ m.Up to now, the method for acquisition macro nanometer and submicron iron structure material can be summed up as " intense plastic strain " and " gross distortion is in conjunction with phase transformation " two big classes.
Intense plastic strain is the main method of the fine and close sub-micron grain blocks of large ferrous materials of preparation, comprising: revolve the extruding of crowded, isogonism, accumulation ply rolling weldering (accumulative roll-bonding) and three axial deformation processing etc.Revolve and extrude normally dish shape of the material that is equipped with, diameter and thickness are respectively 10～20mm and 0.2～0.5mm.The normally pole or the square rod of isogonism extruding preparation, long 70～100mm, diameter of section or diagonal lines＜20mm.The accumulation ply rolling soldering method that is proposed by [Scripta Materialia, 39 (1998): 1221] such as Saito is with thin plate lamination, rolling and make its automatic seam repeatedly.The titaniferous IF steel plate of average grain diameter 27 μ m, 500 ℃ through after 5 ply rolling circulations, grain-size is reduced to below the 0.5 μ m.But this method not only operation is loaded down with trivial details, and exists the interface to cause plasticity to worsen (stretch percentage elongation is than the low order of magnitude of conventional IF steel) between each layer owing to ply rolling.Utilize three axial deformation processing (or press working is processed, repeatedly is interrupted to three-dimensional pressure) also grain refining can be arrived submicron order.Belyakov etc. [Materialia Transactions JIM, 41 (2000): 476] are at 600 ℃ of (0.5T
m) with 10
-3s
-1Strain rate AISI 304 austenitic stainless steels are repeatedly compressed, found that in low strain that to the middle range of strain the feature of microstructure depends on to have the evolutionary process that the high density dislocation wall elongates subgrain.Along with strained carries out, these subgrains more and more trend towards equiax crystal, and the position of subgrain boundary also increases gradually to difference simultaneously, finally cause the position to the generation that differs from more than 20 °, average grain size has only 0.3 μ m super fine organization.But, the three axial deformation working method specimen size that can adapt to is limited.
Gross distortion has then utilized distortion and phase transformation in the characteristics separately aspect the thinning microstructure in conjunction with phase-change method.[CAMP-ISIJ (The Iron and Steel Institute of Japan) such as Hayashi, 11 (1998): 1031] earlier shrend behind the 0.05%C-2.0%Mn steel austenitizing is obtained martensite, 1 road rolls down 50% after 640 ℃ of insulations, and reheat to 640 ℃ depresses 50% or 80%.The result shows that the sample of the direction unanimity that twice are rolling forms along the fibrous grain structure of rolling direction elongation; The sample at the rolling 90 ° of angles of having overturn, second road, total reduction has formed the equiax crystal of 1 μ m, and total reduction has formed the sub-micron crystal that waits of average grain size 0.77 μ m.
Use gross distortion also can obtain the ferrous materials of mean sizes less than 0.2 μ m in conjunction with phase-change method.For example, the disclosed a kind of 7mm Plate Steel that uses composition as C:0.05～0.35, Mn＜1.0, Si＜0.30, Cr＜3.0, Mo＜1.0, V＜0.30 of Chinese patent application CN1272554, obtain low-carbon lath martensite, tempering lath martensite or lower bainite Preparedness Directorate by thermal treatment, the width requirement of lath is controlled at below the 0.5 μ m; Then, at multi-pass below 720 ℃ or single pass warm-rolling or cold rolling, total reduction requires greater than 65%; At last, 550～720 ℃ of recrystallization annealings 1.5～24 hours.The result can obtain the steel plate of grain-size less than 50nm.Use similar approach, at first 1000 ℃ of SS400 steel test plate (panel) insulations that 2mm is thick 0.5 hour, shrend obtained the low-carbon lath martensite tissue to Tsuji etc. [Scr.Mater., 46 (2002): 305] then, and corresponding original austenite grain diameter is 200 μ m.Then, test plate (panel) is cold rolling 50%, 200～700 ℃ of annealing 0.5 hour, finally obtain the super fine organization that crystal grain diameter is about 0.18 μ m again.But, when matrix phase crystal grain so tiny (mean sizes is below 0.2 μ m), deadly defect-plasticity unstable can appear on the contrary, promptly after surrender, has only very little work-hardening effect, thereby cause low even stretch percentage elongation and high yield strength ratio (yield strength often is higher than 0.9 with the ratio of tensile strength) [Journal of Materials Science Letters such as Jingtianfu, 16 (1997): 485, Scr.Mater. such as Tsuji, 46 (2002): 305].Therefore, the ferrous materials that matrix phase crystal grain is too tiny is not only made difficulty or manufacturing cost height, and has serious defective and application limitation.In sum, among the preparation method of existing various sub-micron grain steel, some does not possess technical scale production; Some then implements to exist the difficulty that is difficult to overcome in technical scale production, too complicated as manufacturing process, apparatus and process is required too high and original blank thickness is had certain requirement and rests on non-productive stage.
Summary of the invention
In view of the technical problem of existing sub-micron grain steel in the manufacture view existence, the objective of the invention is to have the soft steel or the low alloy steel steel plate manufacture method of sub-micron grain, can utilize conventional mill, the soft steel that obtains or the grain-size of low alloy steel are submicron order, be that crystal grain diameter is in 1.0 μ m～0.1 mu m range, sub-micron grain is distributed in surface of steel plate to the full thickness of slab cross section at thickness of slab center, has favorable tissue stability simultaneously, and crystal grain is difficult for growing up; And productivity height, adaptability are strong.
For achieving the above object, sub-micron grain soft steel of the present invention or low alloy steel steel plate manufacture method comprise the steps:
A. austenitizing is handled: with original steel billet material at Ac
3The above insulation of temperature certain hour makes the complete austenitizing of steel billet material;
B. hot rolling: be higher than Ar
3Carry out hot rolling under the temperature, the accumulation draught is 40～90%;
C. cooling fast: cool off fast after the hot rolling, to 600 ℃ of temperature ranges to room temperature;
D. warm-rolling or cold rolling: carry out warm-rolling or cold rolling at 600 ℃ to the temperature range of room temperature, the accumulation draught is more than 40%;
E. after the rolling end, can cool off immediately or be incubated certain hour and organize adjustment, and then cool off or roll bending.
Wherein, Ac
3Be the starting temperature of perlite to austenitic transformation, Ar
3Be the starting temperature of austenite to perlitic transformation.
In the above-mentioned steps, the treatment stage of the austenitizing of step a, at first with a certain temperature of steel billet material on Ac3, so that complete austenitizing.Both the slab material can be reheated to above-mentioned temperature range, also continuously cast bloom directly can be cooled to the said temperature interval, maybe will be cooled to the said temperature interval through the slab after the roughing.For fear of AUSTENITE GRAIN COARSENING, temperature should not be too high; Simultaneously, select rational soaking time to guarantee austenitic homogenizing and to suppress austenite crystal and grow up.
Step b carries out hot rolling to blank, with further crystal grain thinning.In the operation of rolling, more than Tnr (Tnr is the non-recrystallization temperature of austenite), then dynamic recrystallization can take place in crystal grain as temperature, and austenite crystal is by refinement.Hot-rolled temperature is under Tnr and at Ar
3On the time, roll the back austenite crystal and be elongated owing to recrystallize does not take place, and remain unchanged in the process of cooling more than transformation temperature; But can take place after being cooled under the transformation temperature to change mutually, still can impel crystal grain to obtain refinement.Above-mentioned hot rolled finishing temperature should be at Ar
3More than the transformation temperature, be lower than Ar as finishing temperature
3, can endanger final plasticity of steel plate and toughness, also can increase the load of milling train.
Hot rolling both can be carried out by single pass, also can divide some passages to carry out.But rolling pass can influence the degree of refinement of crystal grain.When dynamic recrystallization temperature province (more than the Tnr) is rolling, the number of times that dynamic recrystallization takes place is many more, and the austenite crystal refinement is good more.Therefore, multi-pass is rolling continuously is suitable, but need take all factors into consideration all influence factors that exist in the operation of rolling, to determine the number of times of best continuous rolling passage.Generally, continuous 1～4 passage is rolling is ideal.
Draught also is the important factor that influences degree of grain refinement in the course of hot rolling.When rolling at recrystallization temperature zone (more than the Tnr), too little as draught per pass, can not produce dynamic recrystallization.And work as at non-recrystallization temperature zone (Tnr～Ar
3) rolling, not enough as the accumulation draught, the austenite crystal deflection is little, thereby influences the degree of refinement of crystal grain after the phase transformation.Therefore for obtaining the crystal grain of good refinement, draught per pass must be enough big with the accumulation draught in the operation of rolling: draught per pass should be greater than 20%, and the accumulation draught is 40～90%.
Need cooling fast after hot rolling finishes, speed of cooling should be greater than 50 ℃/s.At this moment, contain a kind of in mutually of martensitic phase or bainite in the microstructure of steel at least; The composition of microstructure depends on chemical constitution, hot rolling technology and the process for cooling subsequently of steel.Usually, after above-mentioned hot rolling and quick cooling, obtain the microstructure of micron order (being that crystal grain diameter is more than 1.0 μ m) grain-size.
Above-mentioned micron crystalline grain steel plate still needs to do to the temperature range of room temperature at 600 ℃ further rolling, and the accumulation draught needs more than 40%.In the operation of rolling, dynamic recrystallization may take place in the crystal grain of gross distortion; Perhaps, also recrystallize may take place, and then obtain the sub-micron grain steel plate in subsequent process and subsequent heat treatment.In the rolling process and heat treatment process, the cementite (size is less than 0.2 μ m) that the small and dispersed of formation distributes can improve the nucleation rate of recrystallize and hinder moving of crystal boundary, plays the crystal grain thinning effect.Also can improve simultaneously the stability of microstructure, significantly suppress growing up of sub-micron grain.
The warm-rolling of steps d or cold rollingly both can carry out by single pass also can divide some passages to carry out.In view of temperature is lower, be to reduce using the excessive demand of rolling equipment, adopt that continuous multi-pass is rolling to suit.But the accumulation draught must be more than 40%.
The rolling both can cool off or roll bending after finishing immediately, also can keep certain hour under a certain temperature, organized adjustment, and then cooled off or roll bending.
Through the steel plate that above-mentioned steps obtains, can also utilize thermal treatment process to be for further processing, to obtain even more ideal comprehensive mechanical performance; But thermal treatment temp should not surpass 600 ℃, and soaking time should not be above 1.5 hours.
Beneficial effect of the present invention is compared with existing ultra-fine grain steel preparation method,
1. the crystal grain general diameter of the steel matrix phase of existing method preparation is a micron order, and the crystal grain diameter of the steel matrix phase of the present invention's preparation is at 1.0 μ m～0.2 mu m range; Simultaneously, the matrix of the steel plate of the present invention preparation also exists in mutually diameter that disperse distributes to stop grain growth, improve degree of grain refinement and improve structure stability less than the cementite particle (size is less than 0.2 μ m) of 0.2 μ m.
2. manufacture method of the present invention, at first utilize the hot rolling preliminary crystal grain thinning of fast cold technology and obtain desirable microstructure, hot-rolled temperature scope with broad, and other prior art is usually because require relatively harsher to the hot rolled temperature range, often in the operation of rolling, influenced grain refining, so can need other assisted heating device owing to the temperature reduction is too fast.The present invention has then broken through this restriction.
3. manufacture method of the present invention, behind the fast cold junction bundle of hot rolling, just directly carry out warm-rolling or cold rollingly can obtain the sub-micron grain steel plate to the ambient temperature scope at 600 ℃, and need not to carry out other art breading (as thermal treatment), method is simple; And relaxed requirement to microstructure in the slab before warm-rolling or the cold-rolling process.
4. can be connected combination after the manufacture method of the present invention, 600 ℃ and following temperature warm-rolling with roll bending technology and carry out, can significantly improve production efficiency.
5. manufacture method of the present invention can obtain the mean diameter of crystal grain on surface to the full thickness of slab cross section of heart portion all at the submicron order steel plate; Simultaneously, the sub-micron grain that is obtained has favorable tissue stability, and the grain growth tendency is little.
Description of drawings
Fig. 1 organizes along steel plate sample central section, rolling direction plate vertical section electron scanning micrograph for embodiment of the invention EX3.
Fig. 2 is parallel to rolling surface direction steel plate sample central section transmission electron microscope photo for embodiment of the invention EX3 group.
Fig. 3 organizes along steel plate sample central section, rolling direction plate vertical section electron scanning micrograph for embodiment of the invention EX4.
Embodiment
The chemical ingredients of the steel plate of embodiment E X1～8 is referring to table 1, and technological parameter is referring to table 2.In the sampling of steel plate thickness of slab center, use scanning electronic microscope (SEM) and transmission electron microscope (TEM) to analyze, observe the grain size and the pattern thereof of sub-micron grain steel plate.
Because the sub-micron grain size of the steel plate of the inventive method preparation becomes big along the thickness of slab direction gradually by surface to heart portion, that is: closely surface crystal grain is thinner, and the thickness of slab central section is thicker; So the embodiment of this patent is in these steel plate thickness of slab center samplings, the size of observing sub-micron grain steel plate heart portion crystal grain emphatically.Grain-size adopts the resection in the stereoscopic metallography to measure thickness of slab central section average grain diameter size measuring last row that the results are shown in Table 2.
Fig. 1 has provided the SEM photo of embodiment E X3 group sample, and the white particle that disperse distributes among the figure is a cementite, and the cementite particle diameter is all less than 0.2 μ m; As seen, each regional crystal grain all has in various degree elongation along rolling direction, is fibrous.Simultaneously, exist the tiny cementite particle of the size of disperse distribution in the steel plate less than 0.2 μ m.Yet, use tem observation, also include little crystal grain in these fibrous crystal grain, as shown in Figure 2, these crystal grain all are the equiax crystal that forms in preparation process.
Fig. 3 has provided the SEM photos (white particle of disperse distribution is cementite among the figure) of steel plate (EX4 the organizes sample) tissue that uses 550 ℃ of insulations of employing that manufacture method of the present invention prepares, also further subsequent heat treatment technology acquisition in 1 hour.Therefrom find out: after 550 ℃ of insulations annealing in 1 hour, the mean diameter of steel plate crystal grain increases to 0.70 μ m by 0.40 μ m of rolling attitude, still remains on submicron-scale; And be equiax crystal.Equally, exist the tiny cementite particle of the size of disperse distribution in the steel plate less than 0.2 μ m.As seen, the submicron superfine crystal particle of the present invention's acquisition has extraordinary structure stability.
In sum, manufacture method of the present invention not only has good grain refining effect, and formed crystal grain tiny, even, stablize.
Table 1
| Alloy species | The chemical ingredients numbering | Chemical ingredients (wt%) | ||||||||||||
| C | Si | Mn | S | P | Ni | Cr | Mo | Cu | Nb | Ti | V | Al | ||
| Soft steel | A | 0.18 | ＜0.03 | 0.70 | 0.005 | 0.011 | 0.02 | ＜0.02 | -- | 0.02 | ＜0.01 | 0.001 | 0.01 | 0.035 |
| Low alloy steel | B | 0.084 | 0.21 | 1.53 | 0.005 | 0.018 | 0.21 | 0.02 | -- | 0.22 | 0.041 | 0.02 | 0.062 | -- |
| Low alloy steel | C | 0.07 | 0.31 | 0.31 | 0.004 | 0.082 | 0.11 | 0.6 | 0.46 | 0.24 | 0.02 | 0.002 | -- | 0.02 |
The parameter of table 2 embodiment and test result thereof
| The embodiment group number | The chemical ingredients numbering | Sotck thinkness (mm) | Hot rolling technology | Warm-rolling or cold-rolling process | Thermal treatment process | Steel plate thickness (mm) | Average crystal grain diameter (μ m) | ||||||||||
| Rolling temperature (℃) | Soaking time (min) | Accumulation draught (%) | Passage | The type of cooling | Rolling temperature (℃) | Soaking time (min) | Accumulation draught (%) | Passage | The type of cooling | Holding temperature (℃) | Soaking time (min) | The type of cooling | |||||
| EX1 | A | 15.7 | 900 | 25 | 50 | 1 | Water-cooled | 500 | 25 | 74 | 4 | Water-cooled | -- | -- | -- | 2.5 | 0.40 |
| EX2 | A | 15.7 | 900 | 25 | 72 | 3 | Water-cooled | 500 | 25 | 58 | 3 | Water-cooled | -- | -- | -- | 1.8 | 0.50 |
| EX3 | A | 15.7 | 1000 | 20 | 52 | 1 | Water-cooled | 500 | 30 | 81 | 4 | Batch | -- | -- | -- | 1.5 | 0.40 |
| EX4 | A | 15.7 | 1000 | 20 | 52 | 1 | Water-cooled | 500 | 30 | 81 | 4 | Water-cooled | 550 | 60 | Water-cooled | 1.5 | 0.70 |
| EX5 | A | 15.7 | 1000 | 23 | 54 | 1 | Water-cooled | Room temperature | 30 | 60 | 11 | Air cooling | -- | -- | -- | 2.8 | 0.40 |
| EX6 | B | 15 | 1000 | 30 | 80 | 1 | Water-cooled | 500 | 30 | 45.3 | 1 | Water-cooled | -- | -- | -- | 1.64 | 0.60 |
| EX7 | B | 15 | 1000 | 30 | 80 | 1 | Water-cooled | 500 | 30 | 45.3 | 1 | Water-cooled | 450 | 60 | Water-cooled | 1.64 | 0.80 |
| EX8 | C | 14 | 1000 | 25 | 48 | 1 | Water-cooled | 600 | 35 | 73 | 3 | Air-cooled | -- | -- | -- | 2.1 | 0.50 |
Claims (9)
1. have the manufacture method of the soft steel or the low alloy steel steel plate of sub-micron grain, comprise the steps:
A. austenitizing is handled: with original steel billet material at Ac
3The above insulation of temperature certain hour makes the complete austenitizing of steel billet material;
B. hot rolling: be higher than Ar
3Carry out hot rolling under the temperature, the accumulation draught is 40～90%;
C. cooling fast: cool off fast after the hot rolling, to 600 ℃ of temperature ranges to room temperature;
D. warm-rolling or cold rolling: carry out warm-rolling or cold rolling at 600 ℃ to the temperature range of room temperature, the accumulation draught is more than 40%;
E. after the rolling end, cool off immediately or be incubated certain hour after cool off again or roll bending.
2. the manufacture method with soft steel or low alloy steel steel plate of sub-micron grain according to claim 1 is characterized in that heat-treat after above-mentioned steps is finished, thermal treatment temp is lower than 600 ℃ again, and soaking time is no more than 1.5 hours.
3. the manufacture method with soft steel or low alloy steel steel plate of sub-micron grain according to claim 1 is characterized in that, hot rolling technology is that single pass or continuous some passages are carried out among the described step b.
4. the manufacture method with soft steel or low alloy steel steel plate of sub-micron grain according to claim 3 is characterized in that hot rolling technology is that continuous 1～4 passage is rolling among the described step b.
5. according to claim 1 or 3 or 4 described manufacture method with soft steel or low alloy steel steel plate of sub-micron grain, it is characterized in that hot rolling technology single pass draught is greater than 20% among the described step b, the accumulation draught is 40～90%.
6. the manufacture method with soft steel or low alloy steel steel plate of sub-micron grain according to claim 1 is characterized in that described step c speed of cooling is greater than 50 ℃/s.
7. the manufacture method with soft steel or low alloy steel steel plate of sub-micron grain according to claim 1 is characterized in that, in the described steps d warm-rolling or cold rolling be that single pass carries out, or divide some passages to carry out.
8. the manufacture method with soft steel or low alloy steel steel plate of sub-micron grain according to claim 1 is characterized in that, in the described steps d warm-rolling or cold rolling be that continuous multi-pass is rolling.
9. according to claim 1 or 7 or 8 described manufacture method, it is characterized in that the accumulation draught of warm-rolling or cold-rolling process is more than 40% in the described steps d with soft steel or low alloy steel steel plate of sub-micron grain.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101619383B (en) * | 2009-08-05 | 2011-06-29 | 吉林诺亚机电科技有限公司 | Novel thermal forming method of high-strength steel plate stamping part |
| CN101671772B (en) * | 2009-09-29 | 2011-05-04 | 燕山大学 | Method for preparing ultra-fine grained ferrite and nano-carbide low-carbon steel plate |
| CN102071299B (en) * | 2010-11-09 | 2012-10-03 | 燕山大学 | Method for preparing high-performance nanocrystalline spring steel sheet |
| CN102703665B (en) * | 2012-05-25 | 2013-10-02 | 燕山大学 | Preparation method of nano-structure strip martensitic ultra-high-strength steel plate |
| CN102703837B (en) * | 2012-05-25 | 2014-05-14 | 燕山大学 | Nano-structured lath martensite steel and preparation method thereof |
| CN103343207B (en) * | 2013-07-11 | 2015-01-07 | 东北大学 | Method for enhancing strength of low-carbon and medium-carbon steel through nano carbide precipitation |
| CN103468906A (en) * | 2013-09-17 | 2013-12-25 | 北京科技大学 | Process for preparing 2000 MPa nano-scale bainitic steel through low temperature rolling |
| CN107201436B (en) * | 2017-05-08 | 2018-07-31 | 武汉钢铁有限公司 | A kind of process producing Thin Specs medium carbon steel |
| CN110241364B (en) * | 2019-07-19 | 2021-03-26 | 东北大学 | High-strength plastic nano/submicron crystal cold-rolled 304 stainless steel strip and preparation method thereof |
| CN114622074B (en) * | 2022-05-12 | 2022-08-05 | 中北大学 | Austenitic stainless steel, heat treatment process thereof and application of heat treatment process |
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