CN112251686B - Ultrahigh-strength nanocrystalline 4Cr5MoWSi die steel and preparation method thereof - Google Patents
Ultrahigh-strength nanocrystalline 4Cr5MoWSi die steel and preparation method thereof Download PDFInfo
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 55
- 239000010959 steel Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 33
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 10
- 230000032683 aging Effects 0.000 claims abstract description 8
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 4
- 238000005242 forging Methods 0.000 claims description 5
- 230000006698 induction Effects 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000003723 Smelting Methods 0.000 claims 1
- BULVZWIRKLYCBC-UHFFFAOYSA-N phorate Chemical compound CCOP(=S)(OCC)SCSCC BULVZWIRKLYCBC-UHFFFAOYSA-N 0.000 claims 1
- 238000005498 polishing Methods 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 10
- 238000007254 oxidation reaction Methods 0.000 abstract description 10
- 239000002159 nanocrystal Substances 0.000 abstract description 3
- 239000002707 nanocrystalline material Substances 0.000 abstract 1
- 239000002055 nanoplate Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 25
- 239000011651 chromium Substances 0.000 description 11
- 239000000203 mixture Substances 0.000 description 11
- 238000000034 method Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 8
- 229910052804 chromium Inorganic materials 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 229910052750 molybdenum Inorganic materials 0.000 description 7
- 229910052721 tungsten Inorganic materials 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000011161 development Methods 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000007769 metal material Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
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- 238000002474 experimental method Methods 0.000 description 2
- 238000005098 hot rolling Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000010274 multidirectional forging Methods 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910001563 bainite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 230000004584 weight gain Effects 0.000 description 1
- 235000019786 weight gain Nutrition 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium with molybdenum or tungsten
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/005—Modifying the physical properties by deformation combined with, or followed by, heat treatment of ferrous alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/24—Ferrous alloys, e.g. steel alloys containing chromium with vanadium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/26—Ferrous alloys, e.g. steel alloys containing chromium with niobium or tantalum
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D2201/00—Treatment for obtaining particular effects
- C21D2201/03—Amorphous or microcrystalline structure
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Abstract
The invention relates to the technical field of materials, in particular to nanocrystalline 4Cr5MoWSi die steel and a preparation method thereof. The die steel comprises the following chemical components (in weight percent): c is 0.34-0.42; 4.2-5.8 parts of Cr; w is 0.6-1.4; 0.6 to 1.4 parts of Mo; 0.03 to 0.05 Nb; 0.01 to 0.03 percent of Ce; 0.4 to 0.8 percent of Si; v is 0.2 to 0.4; the balance being Fe. The preparation method of the die steel comprises the following steps: (1) keeping the temperature at 1020-1100 ℃ for a period of time, and rapidly cooling to room temperature to obtain a nano-batten precursor; (2) the temperature of the nano-plate precursor is 800-880 ℃, and the strain rate is 0.5-2 s‑1The total strain amount is more than or equal to 70 percent, so that the precursor of the nano-lath is converted into a nano-crystal structure; (3) and (3) aging the nanocrystalline material for 4 hours at 440-480 ℃, and rapidly cooling to room temperature after aging. The nanocrystalline die steel prepared by the invention has ultrahigh strength, good plasticity and toughness and high-temperature oxidation resistance, and is suitable for preparing various high-end dies.
Description
Technical Field
The invention relates to the technical field of materials, in particular to high-strength nanocrystalline 4Cr5MoWSi die steel and a preparation method thereof.
Background
With the rapid development of economy and society, the performance of the traditional die steel is gradually difficult to meet the requirements of people, and the development of novel die steel materials with higher performance is urgently needed. Attempts have been made to improve the hardness and wear resistance of die steel materials by further increasing the carbon and chromium content. However, as the strength of the material is improved, the plasticity and the toughness of the material are obviously reduced, and the bottleneck problem can not be solved properly all the time, so that the development of the traditional die steel material is in a stagnation state for a long time.
Compared with a coarse-grain steel material, the nano-grain steel material has excellent comprehensive mechanical properties such as higher strength and plasticity, larger fatigue strength and the like, and simultaneously has good high-temperature oxidation resistance, so that the nano-grain steel material is very attractive in practical application, and a new way for developing and preparing the nano-grain die steel opens up a new way for optimizing the performance of the traditional die steel.
At present, the preparation of bulk nanocrystalline metal materials is mainly achieved by a large plastic deformation (SPD) method. Common large plastic deformation methods comprise Equal Channel Angular Pressing (ECAP), accumulative composite rolling (ARB), Multidirectional Forging (MF), High Pressure Torsion (HPT) and the like, all of which need high-power equipment and expensive dies, and the prepared material has smaller size and cannot meet the requirement of large-scale industrial production. Therefore, the invention provides novel nanocrystalline die steel and a preparation method thereof, the preparation of the nanocrystalline die steel can be realized through conventional hot rolling deformation, and new foundation and opportunity are brought to the development of the traditional die steel material.
Disclosure of Invention
The invention aims to provide nanocrystalline die steel, and in order to achieve the aim, the technical scheme of the invention is as follows:
the nanocrystalline 4Cr5MoWSi die steel comprises the following chemical components in percentage by weight: c is 0.34-0.42; 4.2-5.8 parts of Cr; w is 0.6-1.4; 0.6 to 1.4 parts of Mo; 0.03 to 0.05 Nb; 0.01 to 0.03 percent of Ce; 0.4 to 0.8 percent of Si; v is 0.2 to 0.4; the balance being Fe. Some preferred elements are: c: 0.38 to 0.41; cr: 5.0 to 5.6; w: 1.0 to 1.3; mo: 1.0 to 1.3; si: 0.6 to 0.8.
The preparation method of the nanocrystalline die steel comprises the following steps: a vacuum induction furnace is adopted to obtain a raw material ingot, and the ingot is polished and then is subjected to cogging forging and finish forging at the temperature of more than 1100 ℃ to form a blank.
Preserving the temperature of the blank obtained by the finish forging processing at 1020-1100 ℃ for a period of time, and rapidly cooling to room temperature to obtain a nano-lath precursor; thermally deforming the obtained nano-lath precursor to obtain a nano-crystal structure; and carrying out aging treatment on the nanocrystalline structure to finally obtain the nanocrystalline die steel.
As a preferred technical scheme:
and (3) keeping the temperature of the blank at 1020-1100 ℃ for a period of time, wherein the heat preservation time t is (2.8-3.8) Dmin, wherein D is the effective thickness of the sample, and the unit is millimeter mm.
The cooling rate of the rapid cooling is 10-80 ℃/s.
The nano-batten precursor has the strain rate of 0.5-2.0 s at the temperature of 800-880 DEG C-1Is thermally deformed within the range of (1), and the total strain amount is 70% or more. Preferably: the thermal deformation temperature is 810-840 ℃, and the strain rate is 0.6-1.2 s-1The total strain amount is 90% or more.
The microstructure of the material prepared by the method is a nanocrystalline structure, and the grain size is 30-90 nm.
The invention has the beneficial effects that:
(1) different from the situation of the prior art, the nanocrystalline iron and steel material provided by the invention can realize the preparation of nanocrystalline die steel through conventional thermal deformation without depending on high-power equipment and expensive dies.
(2) The bulk nanocrystalline metal material prepared by the method is not limited by size, and compared with the prior art, the bulk nanocrystalline metal material with larger size can be prepared, so that the requirement of large-scale industrial production is met.
(3) The method can obviously improve the comprehensive mechanical property of the die steel, and the obtained nanocrystalline die steel has ultrahigh strength and good plasticity and toughness and is suitable for preparing various high-end dies. Under the conditions of optimized alloy components (C content is 0.38-0.41; Cr content is 5.0-5.6; W content is 1.0-1.3; Mo content is 1.0-1.3; Si content is 0.6-0.8) and thermal deformation (thermal deformation temperature is 810-840 ℃, strain rate is 0.6-1.2 s)-1And the total strain is more than or equal to 90 percent), the tensile strength of the prepared nanocrystalline die steel is as high as 1800-2200 MPa, the elongation is 10-15 percent, and the Vickers hardness is 540-610.
(4) The nanocrystalline die steel prepared by the method has excellent high-temperature oxidation resistance.
Drawings
FIG. 1 TEM photograph of a nanostring precursor.
FIG. 2 is a TEM photograph of the structure of the nanocrystal formed by thermally deforming the precursor of the nano-lath.
Detailed Description
In order to make the purpose, technical solution and effect of the present application clearer and clearer, the present application is further described in detail below with reference to the accompanying drawings and examples.
The invention provides novel nanocrystalline die steel, which comprises the chemical components of 0.34-0.42 of C; 4.2-5.8 parts of Cr; w is 0.6-1.4; 0.6 to 1.4 parts of Mo; 0.03 to 0.05 Nb; 0.01 to 0.03 percent of Ce; si:0.4 to 0.8; 0.2-0.4V, and the balance Fe.
Please refer to fig. 1-2. FIG. 1 shows the nano-slab precursor formed by rapidly cooling the material of example 8 of the present invention, and it can be seen from the TEM tissue photograph that the width of the slab is between 15 nm and 42 nm. FIG. 2 shows the structure of the nano-scale crystals formed by thermal deformation of the nano-slab precursor of example 8 of the present invention, and it can be seen from the TEM photograph that the crystal grain size is between 30 nm and 75 nm.
The present application will now be illustrated and explained by means of several groups of specific examples and comparative examples, which should not be taken to limit the scope of the present application.
Example (b): examples 1 to 9 are die steels smelted in the chemical composition range provided by the present invention, in which the contents of C, Cr, W, Mo, and Si elements are gradually increased, and the corresponding preparation processes are also appropriately adjusted within the technical parameter range specified by the present invention. The size of the prepared bulk nanocrystalline metal material is 150 multiplied by 800 multiplied by 10 mm.
Comparative example: the chemical compositions of C, Cr, W, Mo and Si in comparative example 1 are all lower than the lower limit of the chemical composition range provided by the invention, and the chemical compositions of C, Cr, W, Mo and Si in comparative example 9 are all higher than the upper limit of the chemical composition range provided by the invention, and the effect of the change of the chemical compositions of C, Cr, W, Mo and Si on the preparation of the nanocrystalline die steel is illustrated by comparing with example 1 and example 9 respectively. Comparative example 2, in which the amount of strain is below the lower limit of the amount of strain provided by the present invention, illustrates the effect of the amount of strain on the production of nanocrystalline die steel by comparison with example 2. The effect of strain rate on nanocrystalline die steel production is illustrated by comparing the strain rate of comparative example 3, which is above the upper limit of the strain rate provided by the present invention, and the strain rate of comparative example 4, which is below the lower limit of the strain rate provided by the present invention, with example 3 and example 4, respectively. Comparative example 5 slow cooling to room temperature after heat treatment illustrates the effect of cooling rate after heat treatment on nanocrystalline die steel production by comparison with example 5. Comparative example 6, in which the heat treatment temperature is lower than the lower limit of the heat treatment temperature provided by the present invention, illustrates the effect of the heat treatment temperature on the preparation of nanocrystalline die steel by comparison with example 6. Comparative example 7, in which the heat distortion temperature is higher than the upper limit of the heat distortion temperature provided by the present invention, and comparative example 8, in which the heat distortion temperature is lower than the lower limit of the heat distortion temperature provided by the present invention, illustrates the influence of the heat distortion temperature on the preparation of the nanocrystalline die steel by comparing with example 7 and example 8, respectively. In addition, the invention also shows that the nanocrystalline die steel provided by the invention has good comprehensive mechanical property and high-temperature oxidation resistance by comparing with the commercially widely-used 5CrMnMo die steel.
TABLE 1 chemical composition, Heat treatment Process and Hot Rolling Process of example and comparative materials
1. Hardness test
The hardness of the materials of the examples and comparative examples were tested. The Vickers hardness of the material after 4h ageing at 460 ℃ was measured using a HTV-1000 type durometer. Before testing, the sample surface was polished. The sample was a thin sheet with dimensions of 10mm diameter and 2mm thickness. The test loading force is 9.8N, the pressurizing duration is 15s, and the hardness value is automatically calculated by measuring the diagonal length of the indentation through computer hardness analysis software. The final hardness values were averaged over 15 points and three replicates were selected for each set of samples.
2. Tensile Property test
The room temperature tensile mechanical properties of the aged comparative and example materials were tested using an Instron model 8872 tensile tester at a tensile rate of 0.5 mm/min. Before testing, a lathe is adopted to process the material into standard tensile samples with the thread diameter of 10mm, the gauge length of 5mm and the gauge length of 30mm, three parallel samples are taken from each group of heat treatment samples, and the mechanical properties obtained by the experiment comprise tensile strength, yield strength and elongation, and the results are shown in table 2.
3. Grain size statistics
The material was characterized using a Transmission Electron Microscope (TEM) and the grain size of the material was counted using a line cut. The preparation method of the TEM sample comprises the following steps: firstly, manually grinding and thinning a sample to be less than 40 mu m by using No. 2000 abrasive paper, and preparing the sample by using a punching machine
A sheet of (a); and then, thinning the sample by adopting a Tenupol-5 chemical double-spraying thinning instrument, wherein the double-spraying liquid is 6% perchloric acid, 30% butanol and 64% methanol, and the double-spraying thinning temperature is-25 ℃. And (3) observing the double-sprayed thinned sample by using a TECNAI20 transmission electron microscope, wherein the working voltage during TEM observation is 200kV, and the alpha and beta angle rotation ranges are +/-30 degrees by using a double-inclined magnetic sample table. Drawing parallel fixed-length straight lines on the TEM picture, and calculating the grain size of the material according to the number of the fixed-length straight lines passing through the grains.
4. High temperature oxidation resistance test
The test is carried out according to the test steps specified in the national standard GB/T13303-1991 method for measuring the oxidation resistance of steel, the material is oxidized for 1000 hours in the air at 500 ℃ and 600 ℃, and the weight gain of the oxidized material is measured, so as to evaluate the high temperature oxidation resistance of the material.
TABLE 2 structural characteristics and mechanical properties after aging of the materials of the examples and comparative examples
As can be seen from the results in Table 2, examples 1 to 9 are all nanocrystalline structures, which make them have high strength, good plasticity and large hardness. In the chemical composition range specified by the invention, as the chemical composition content of C, Cr, W, Mo and Si is increased, the grain size of the material is gradually reduced, the strength and the hardness of the material are improved, and the elongation and the reduction of area are gradually reduced.
In comparative example 1, the contents of C, Cr, W, Mo and Si elements are all lower than the lower limit of the chemical composition range specified in the present invention, a bainite structure is obtained after rapid cooling, and a nanocrystalline structure cannot be obtained by performing thermal deformation with the precursor as an original structure. The comparative example 9, in which the contents of C, Cr, W, Mo, and Si elements are higher than the chemical composition range defined in the present invention, obtained a ferrite structure after rapid cooling and also failed to obtain a nanocrystalline structure after hot deformation.
The strain of comparative example 2 is small, and the structure of the nano-lath is still formed after deformation, so that the preparation of the nano-crystalline structure cannot be realized.
Comparative example 3 has a large strain rate and fails to realize the preparation of a nanocrystalline structure. Comparative example 4 has a small strain rate, and the grains are coarsened during thermal deformation, so that the preparation of the nanocrystalline structure cannot be achieved.
Comparative example 5 was slowly cooled to room temperature after heat treatment, and comparative example 6 was at a lower heat treatment temperature, which made their precursors non-lath structures of the nano-scale provided by the present invention, and thus none of them could achieve the preparation of nanocrystalline structure.
The temperature ranges for hot deformation of the nano-lath precursors of comparative examples 7 and 8 are outside the range provided by the present invention, and the preparation of the nanocrystalline structure cannot be achieved.
Compared with the 5CrMnMo die steel widely used in commerce at present, the novel nanocrystalline 4Cr5MoWSi die steel provided by the invention not only has higher strength and hardness, but also has better plasticity and toughness than the traditional die steel material.
As can be seen from the results in Table 3, the oxidation gain of the experiments of examples 1 to 9 at 500 ℃ and 600 ℃ is lower than that of comparative examples 1 to 9 and commercial 5CrMnMo die steel, which shows that the nanocrystalline 4Cr5MoWSi die steel provided by the invention has good high-temperature oxidation resistance.
TABLE 3 Oxidation weighting of the materials of the examples and comparative examples
The above description is only for the purpose of illustrating embodiments of the present application and is not intended to limit the scope of the present application, and all modifications of equivalent structures and equivalent processes, which are made by the contents of the specification and the drawings of the present application or are directly or indirectly applied to other related technical fields, are also included in the scope of the present application.
Claims (7)
1. The ultrahigh-strength nanocrystalline 4Cr5MoWSi die steel is characterized in that: the die steel comprises the following chemical components in percentage by weight: c is 0.34-0.42; 4.2-5.8 parts of Cr; w is 0.6-1.4; 0.6 to 1.4 parts of Mo; 0.03 to 0.05 Nb; 0.01 to 0.03 percent of Ce; 0.4 to 0.8 percent of Si; v is 0.2 to 0.4; the balance being Fe;
the preparation method of the die steel comprises the following steps:
smelting by adopting a vacuum induction furnace to obtain a raw material ingot; polishing the cast ingot, cogging and forging at the temperature of more than 1100 ℃, and finish forging to obtain a blank, keeping the temperature of the blank at 1020-1100 ℃ for a period of time, and rapidly cooling to room temperature to obtain a nano-strip precursor; the nano-batten precursor has the strain rate of 0.5-2.0 s at the temperature of 800-880 DEG C-1Thermal deformation is carried out within the range of (1), the total strain amount is more than or equal to 70 percent, and a nanocrystalline structure is obtained; and (4) carrying out aging treatment on the nanocrystalline structure to finally obtain the nanocrystalline 4Cr5MoWSi die steel.
2. The ultra-high strength nanocrystalline 4Cr5MoWSi mold steel according to claim 1, characterized in that: c, according to weight percentage: 0.38 to 0.41; cr: 5.0 to 5.6; w: 1.0 to 1.3; mo: 1.0 to 1.3; si: 0.6 to 0.8.
3. According to claimThe ultrahigh-strength nanocrystalline 4Cr5MoWSi die steel required by claim 1 is characterized in that: keeping the temperature at 1020-1100 ℃ for a period of timet=(2.8~3.8)Dmin, wherein,Dthe effective thickness of the sample is in mm, and the sample is rapidly cooled to room temperature after heat preservation is finished so as to obtain the nano-lath precursor.
4. The ultra-high strength nanocrystalline 4Cr5MoWSi mold steel according to claim 1 or 3, characterized in that: the cooling rate of the rapid cooling is 10-80 ℃/s.
5. The ultra-high strength nanocrystalline 4Cr5MoWSi mold steel according to claim 1, characterized in that: the aging temperature is 440-480 ℃, and the aging time is 3-5 h.
6. The ultra-high strength nanocrystalline 4Cr5MoWSi mold steel according to claim 1, characterized in that: the thermal deformation temperature is 810-840 ℃, and the strain rate is 0.6-1.2 s-1The total strain amount is 90% or more.
7. The ultra-high strength nanocrystalline 4Cr5MoWSi mold steel according to claim 5 or 6, characterized in that: the microstructure of the prepared material is nanocrystalline, and the grain size is 30-90 nm; the tensile strength of the material is as high as 1800-2200 MPa, the elongation is 10-15%, and the reduction of area is more than 45%.
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