CN115533101A - Preparation method of powder metallurgy high-speed steel - Google Patents
Preparation method of powder metallurgy high-speed steel Download PDFInfo
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- CN115533101A CN115533101A CN202211069289.3A CN202211069289A CN115533101A CN 115533101 A CN115533101 A CN 115533101A CN 202211069289 A CN202211069289 A CN 202211069289A CN 115533101 A CN115533101 A CN 115533101A
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- 229910000997 High-speed steel Inorganic materials 0.000 title claims abstract description 72
- 238000004663 powder metallurgy Methods 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 55
- 239000010410 layer Substances 0.000 claims abstract description 49
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 46
- 239000010959 steel Substances 0.000 claims abstract description 46
- 238000005242 forging Methods 0.000 claims abstract description 43
- 230000006698 induction Effects 0.000 claims abstract description 30
- 239000002344 surface layer Substances 0.000 claims abstract description 29
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 27
- 239000002131 composite material Substances 0.000 claims abstract description 23
- 238000007872 degassing Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000010791 quenching Methods 0.000 claims abstract description 20
- 230000000171 quenching effect Effects 0.000 claims abstract description 20
- 238000000137 annealing Methods 0.000 claims abstract description 19
- 230000000750 progressive effect Effects 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims description 80
- 239000002245 particle Substances 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 238000011049 filling Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 238000000280 densification Methods 0.000 abstract 1
- 150000001247 metal acetylides Chemical class 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 12
- 238000007873 sieving Methods 0.000 description 9
- 238000001887 electron backscatter diffraction Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 229910001103 M42 high speed steel Inorganic materials 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 230000007423 decrease Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000004308 accommodation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/18—Hardening; Quenching with or without subsequent tempering
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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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
- C21D1/32—Soft annealing, e.g. spheroidising
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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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/34—Methods of heating
- C21D1/42—Induction heating
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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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
- C21D2221/00—Treating localised areas of an article
- C21D2221/10—Differential treatment of inner with respect to outer regions, e.g. core and periphery, respectively
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Abstract
The invention discloses a preparation method of powder metallurgy high-speed steel. Arranging high-speed steel powder with different grain size ranges in a composite sheath which is formed by sleeving a plurality of sheaths from outside to inside according to the grain size from large to small, and then performing degassing treatment and hot isostatic pressing densification on the sheaths; firstly, carrying out rapid inner layer spheroidizing annealing at a lower temperature, and then carrying out surface layer induction annealing at a higher temperature; and performing discontinuous progressive radial forging on the annealed steel ingot, and then performing induction step quenching. By adopting the method, the powder metallurgy high-speed steel can obtain a structure with double gradients of grain size and carbide size.
Description
Technical Field
The invention relates to a preparation method of high-speed steel, in particular to a preparation method of powder metallurgy high-speed steel.
Background
The high-speed steel has the advantages of high hardness, good red hardness, high wear resistance and the like, and is widely applied to manufacturing high-speed cutting tools and the like. In order to ensure the performance requirement, a large amount of carbon and alloy elements are added into the high-speed steel to form a large amount of hard and stable alloy carbide. The traditional high-speed steel production process is a casting and forging process: smelting → casting into electrode bar → electroslag remelting → high temperature cogging → forging → rolling → annealing. The high-speed steel produced by the process is easy to generate the problems of coarse primary carbide, uneven distribution, zonal structure segregation and other structure quality, and can not meet the strict requirements of high-end precision cutters on the structure quality.
In the powder metallurgy process, the extremely high cooling speed is obtained through liquid drop atomization, and the problem of element segregation can be effectively solved. The atomized powder is further formed into a block material through hot isostatic pressing, and then the density of the material is further improved by utilizing hot working. The powder metallurgy technology can solve the problem of the structure quality of the traditional cast-forged high-speed steel, and is suitable for preparing high-end precision cutters.
However, in the actual service process of the cutting tool, the requirements for the mechanical properties of different positions of the material are greatly different: the surface of the cutter has severe friction with a processed workpiece, and higher hardness and wear resistance are required; the requirement on the wear resistance of the interior of the cutter is not high, but better impact resistance is required. Obviously, the powder metallurgy high-speed steel with uniform structure can not meet the requirements of gradient performance on the surface and the inside of the cutter.
Patent CN111014704A discloses a method for preparing powder metallurgy tool and die steel, mixing powders with different particle sizes according to a certain proportion and then loading into a sheath, and controlling the mixing proportion of the powders with different particle sizes to effectively reduce the porosity. However, it cannot realize a texture structure with a double gradient of grain size and carbide size.
Patent CN113714497A discloses a method for preparing gradient powder metallurgy high-speed steel, which achieves different hardness, toughness and wear resistance of the core and the surface, and improves the matching of the materials of each part by the tissue interface, however, the patent needs to prepare the powders with different chemical compositions and properties in advance, and needs to convey the powders with different chemical compositions and properties into a container for sintering through a special device. In addition, although the device can realize the accurate conveying of the left inner core gradient powder, the right inner core gradient powder and the outer core gradient powder, and the accurate conveying of the upper inner core gradient powder, the lower inner core gradient powder and the outer core gradient powder, thereby realizing the compression molding. However, it cannot achieve a texture structure with a double gradient of grain size and carbide size.
Disclosure of Invention
The invention aims to: the invention aims to provide a preparation method of powder metallurgy high-speed steel with the characteristics of double-gradient distribution of grain size and carbide size.
The technical scheme is as follows: the preparation method of the powder metallurgy high-speed steel comprises the following steps:
(1) Arranging high-speed steel powder in a composite sheath consisting of mutually nested sheaths from outside to inside in the order of the particle size from large to small;
(2) Removing the inner layer sheath, degassing the outer layer sheath, and performing hot isostatic pressing to obtain a steel ingot with gradient powder grain size;
(3) Carrying out inner spheroidizing annealing on the steel ingot, and then carrying out surface induction annealing to obtain an annealed steel ingot with a gradient structure, wherein the size of carbide is gradually reduced from the surface layer to the inner layer;
(4) And carrying out discontinuous progressive radial forging on the annealed steel ingot, and carrying out graded quenching to obtain the high-speed steel with the grain size gradually increasing from the surface to the inside and the gradient structure.
Wherein, in the step (1), the high-speed steel powder is sieved into powder with different grain diameters; the particle size ranges of the high-speed steel powder obtained by screening are respectively from large to small: 275 μm or more, 225 to 275 μm, 200 to 250 μm, 175 to 225 μm, 150 to 200 μm, 125 to 175 μm, 75 to 125 μm, 100 μm or less.
Wherein, in the step (1), the diameter difference of the adjacent sheaths is 50-150 mm.
In the step (2), the outer-layer sheath is an outermost-layer sheath; the hot isostatic pressing temperature is 1000-1100 ℃, the pressure is 80-120 MPa, and the time is 2-6 h.
Wherein in the step (3), the temperature of the inner layer spheroidizing annealing is 1050-1120 ℃, and the time is 2-4 h; the heating rate of the inner layer spheroidizing annealing is 15-50 ℃/min. Under the condition of the temperature rise rate, the spheroidization effect of the carbide of the inner layer is improved, and the carbide gradient is formed.
Wherein, in the step (3), the temperature of the surface layer induction annealing is 1120-1180 ℃, and the time is 1-2 h. The surface layer induction annealing enables a target heating temperature area to be limited in the surface layer area, which is beneficial to improving the spheroidizing effect of the surface layer carbide and avoiding coarsening the size of the inner layer carbide to form a carbide gradient.
In the step (4), the discontinuous and progressive radial forging refers to that the loading direction is along the radial direction of the steel ingot, and the loading mode is discontinuous and progressive; the forging frequency is 90-150 times/min, and the forging reduction per minute is 3-10 mm.
In the step (4), the induction heating graded quenching temperature is firstly increased to 700-900 ℃ and is kept for 0.5-2 h, then is increased to 1180-1220 ℃, is kept for 5-15 min and is then quenched. The induction staged quenching limits the target heating temperature area to the surface layer area, refines the surface layer grain size, and is beneficial to avoiding coarsening of the inner layer grain size and forming grain gradient.
The invention principle is as follows: according to the invention, high-speed steel powder is arranged in a composite sheath formed by concentric sheaths from outside to inside according to the order of the particle size range from large to small, the sheaths are subjected to degassing treatment for many times, and then hot isostatic pressing is carried out, so that the powder metallurgy high-speed steel ingot with low oxygen content, compact structure and gradient distribution of powder particle size is obtained, and a material foundation is laid for obtaining a double-gradient structure subsequently; then, carrying out graded annealing, namely, firstly utilizing inner layer spheroidizing annealing in a lower temperature range to decompose and spheroidize carbides with smaller size and lower stability formed by small-particle-size powder particles in the core part of the steel ingot, and then utilizing surface layer induction annealing in a higher temperature range to decompose and spheroidize carbides with larger size and higher stability formed by large-particle-size powder particles in the surface layer of the steel ingot, so as to obtain a gradient structure with the carbide size gradually reduced from the surface layer to the inside; controlling forging frequency and radial rolling reduction through discontinuous progressive radial forging to ensure that a gradient structure of a steel ingot can be transmitted to a forged material; the forging material is heat treated by induction staged quenching, and the forging material is made to obtain a gradient structure with the grain size gradually increasing from the surface to the inside by utilizing the surface skin effect and the surface-core cooling speed stage difference.
Has the beneficial effects that: compared with the prior art, the invention has the following remarkable effects: (1) The powder metallurgy high-speed steel structure with the characteristic that the size of the matrix crystal grains and the size of the carbide are distributed in double gradients can be obtained, namely, the size of the carbide is gradually reduced from the surface of the steel to the inside of the steel, and the size of the matrix crystal grains is gradually increased. (2) The gradient structure of the invention can realize the gradient mechanical property of the powder high-speed steel: close to the surface, large-size carbides guarantee high wear resistance, and small-size matrix grains guarantee high hardness, so that the surface has excellent wear resistance; close to the interior, the small-size carbide has small fracture tendency when loaded, and the large-size matrix crystal grains have strong dislocation accommodation capacity, so that the interior has better impact toughness.
Drawings
FIG. 1 is an SEM and EBSD picture of the high speed steel structure of example 1;
FIG. 2 is an SEM and EBSD picture of the high speed steel structure of example 2;
FIG. 3 is an SEM and EBSD picture of the high speed steel structure of example 3;
FIG. 4 is an SEM and EBSD picture of the high speed steel structure of example 4;
FIG. 5 is an SEM and EBSD picture of the high speed steel structure of example 5;
FIG. 6 is an SEM and EBSD picture of the high speed steel structure of example 6;
FIG. 7 is an SEM photograph of the high speed steel structure of comparative example 1;
FIG. 8 is an SEM photograph of the structure of a high-speed steel of comparative example 2;
FIG. 9 is an EBSD map of the high speed steel structure of comparative example 3;
FIG. 10 is an EBSD map of the high-speed steel structure of comparative example 4.
Detailed Description
The present invention is described in further detail below.
Example 1
A preparation method of powder metallurgy high-speed steel comprises the following steps:
(1) Sieving M42 high-speed steel powder into powder with different particle size ranges of more than 275 microns, 225-275 microns, 200-250 microns, 175-225 microns, 150-200 microns, 125-175 microns, 75-125 microns and less than 100 microns;
(2) Sequentially arranging the powder in a composite sheath formed by concentrically sheathing sheaths with diameters of 100, 150, 200, 250, 300, 350, 400 and 450mm from outside to inside according to the order of the particle size range from large to small, and then removing the inner sheath and only keeping the outermost sheath;
(3) Vibrating the composite sheath for degassing, and then circularly performing degassing treatment of vacuumizing and nitrogen filling for 4 times;
(4) Hot isostatic pressing the sheath at 1000 ℃, wherein the pressure is 80MPa, and the time is 6h;
(5) Rapidly heating the hot isostatic pressing steel ingot to 1050 ℃ at a speed of 50 ℃/min, heating for 4h, then heating to 1120 ℃ by utilizing induction heating, and heating for 2h;
(6) Carrying out discontinuous progressive radial forging on the annealed steel ingot, wherein the forging frequency is 90 times/min, and the forging reduction per minute is 10mm;
(7) And (3) heating the billet steel to 700 ℃ by induction heating, preserving heat for 2h, then heating to 1180 ℃, preserving heat for 15min, and quenching to obtain the high-speed steel.
In all drawings of the present application, (a) is a surface layer and (b) is an inner layer. As can be seen from FIG. 1, the surface layer has an average grain size of about 4.2 μm, the carbides have an average grain size of about 4.9 μm, the inner layer has an average grain size of about 10.2 μm, and the carbides have an average grain size of about 2.7 μm, and a gradient structure is formed in which the carbide size gradually decreases from the surface layer to the inner layer and the grain size gradually increases from the surface to the inside.
Example 2
A preparation method of powder metallurgy high-speed steel comprises the following steps:
(1) Sieving M42 high-speed steel powder into powder with different particle size ranges of more than 275 microns, 225-275 microns, 200-250 microns, 175-225 microns, 150-200 microns, 125-175 microns, 75-125 microns, less than 100 microns and the like;
(2) Sequentially arranging the powder in a composite sheath formed by concentrically sheathing sheaths with the diameters of 100 mm, 250 mm, 400 mm, 550 mm, 700 mm, 850 mm, 1000 mm and 1150mm from outside to inside according to the order of the particle size range from large to small, removing the sheath at the inner layer, and only reserving the sheath at the outermost layer;
(3) Vibrating the composite sheath for degassing, and then circularly performing degassing treatment of vacuumizing and nitrogen filling for 5 times;
(4) Hot isostatic pressing the ladle sleeve at 1100 ℃, wherein the pressure is 120MPa, and the time is 2h;
(5) Rapidly heating the hot isostatic pressing steel ingot to 1120 ℃ at a speed of 15 ℃/min, heating for 2h, then heating to 1180 ℃ by utilizing induction heating, and heating for 1h;
(6) Carrying out discontinuous progressive radial forging on the annealed steel ingot, wherein the forging frequency is 150 times/min, and the forging reduction per minute is 3mm;
(7) And (3) heating the steel billet to 900 ℃ by induction heating, preserving heat for 0.5h, then heating to 1220 ℃, preserving heat for 5min, and quenching to obtain the high-speed steel.
As can be seen from FIG. 2, the average size of the grains of the surface layer is about 3.9 μm, the average size of the carbides is about 4.7 μm, the average size of the grains of the inner layer is about 10.5 μm, the average size of the carbides is about 2.3 μm, and a gradient structure is formed in which the size of the carbides decreases from the surface layer to the inner layer and the size of the grains increases from the surface to the inner portion
Example 3
A preparation method of powder metallurgy high-speed steel comprises the following steps:
(1) Sieving TPM558 high-speed steel powder into powder with different particle size ranges of more than 275 microns, 225-275 microns, 200-250 microns, 175-225 microns, 150-200 microns, 125-175 microns, 75-125 microns and less than 100 microns;
(2) Sequentially arranging the powder in a composite sheath formed by concentrically sheathing sheaths with diameters of 100, 200, 300, 400, 500, 600, 700 and 800mm from outside to inside according to the order of the particle size range from large to small, removing the inner sheath and only keeping the outermost sheath;
(3) Vibrating the composite sheath for degassing, and then circularly performing degassing treatment of vacuumizing and nitrogen filling for 3 times;
(4) Hot isostatic pressing the sheath at 1050 ℃, wherein the pressure is 100MPa, and the time is 4h;
(5) Rapidly heating the hot isostatic pressing steel ingot to 1080 ℃ at a speed of 15 ℃/min, heating for 3h, then heating to 1160 ℃ by utilizing induction heating, and heating for 1h;
(6) Carrying out discontinuous progressive radial forging on the annealed steel ingot, wherein the forging frequency is 100 times/min, and the forging reduction per minute is 8mm;
(7) And (3) heating the steel billet to 800 ℃ by induction heating, preserving heat for 1h, then heating to 1220 ℃, preserving heat for 5min, and quenching to obtain the high-speed steel.
As can be seen from FIG. 3, the average size of the grains of the surface layer is about 3.8 μm, the average size of the carbides is about 5.1 μm, the average size of the grains of the inner layer is about 9.7 μm, and the average size of the carbides is about 2.4 μm, forming a gradient structure in which the size of the carbides decreases from the surface layer to the inner layer and the size of the grains increases from the surface to the inside.
Example 4
A preparation method of powder metallurgy high-speed steel comprises the following steps:
(1) Sieving TPM558 high speed steel powder into powder of 275-275 micron size, 225-275 micron size, 200-250 micron size, 175-225 micron size, 150-200 micron size, 125-175 micron size, 75-125 micron size and below 100 micron size;
(2) Sequentially arranging the powder in a composite sheath formed by concentrically sheathing sheaths with diameters of 100 mm, 200 mm, 300 mm, 400 mm, 500 mm, 600 mm, 700 mm and 800mm from outside to inside according to the order of the particle size range from large to small, removing the sheath at the inner layer, and only reserving the sheath at the outermost layer;
(3) Vibrating the composite sheath for degassing, and then circularly performing degassing treatment of vacuumizing and nitrogen filling for 5 times;
(4) Hot isostatic pressing the clad at 1050 ℃, wherein the pressure is 110MPa, and the time is 5h;
(5) Rapidly heating the hot isostatic pressing steel ingot to 1100 ℃ at a speed of 15 ℃/min for 3h, then heating to 1170 ℃ by using induction heating, and heating for 1h;
(6) Carrying out discontinuous progressive radial forging on the annealed steel ingot, wherein the forging frequency is 120 times/min, and the forging reduction per minute is 6mm;
(7) And (3) heating the steel billet to 800 ℃ by induction heating, preserving heat for 1h, then heating to 1200 ℃, preserving heat for 10min, and quenching to obtain the high-speed steel.
As can be seen from FIG. 4, the surface layer has an average grain size of about 4.3 μm, the carbides have an average grain size of about 5.1 μm, the inner layer has an average grain size of about 11.5 μm, and the carbides have an average grain size of about 2.4 μm, and a gradient structure is formed in which the carbide size gradually decreases from the surface layer to the inner layer and the grain size gradually increases from the surface to the inside.
Example 5
A preparation method of powder metallurgy high-speed steel comprises the following steps:
(1) Screening TPM380 high speed steel powder into powder of 275 micron over, 225-275 micron, 200-250 micron, 175-225 micron, 150-200 micron, 125-175 micron, 75-125 micron and 100 micron below different grain size range;
(2) Sequentially arranging the powder in a composite sheath formed by concentrically sheathing sheaths with diameters of 100, 200, 300, 400, 500, 600, 700 and 800mm from outside to inside according to the order of the particle size range from large to small, removing the inner sheath and only keeping the outermost sheath;
(3) Vibrating the composite sheath for degassing, and then circularly performing degassing treatment of vacuumizing and nitrogen filling for 3 times;
(4) Hot isostatic pressing the sheath at 1050 ℃, wherein the pressure is 110MPa, and the time is 3h;
(5) Rapidly heating the hot isostatic pressing steel ingot to 1100 ℃ at a speed of 15 ℃/min, heating for 2h, then heating to 1180 ℃ by utilizing induction heating, and heating for 1h;
(6) Carrying out discontinuous progressive radial forging on the annealed steel ingot, wherein the forging frequency is 110 times/min, and the forging reduction per minute is 7mm;
(7) And (3) heating the billet steel to 800 ℃ by induction heating, preserving heat for 1h, then heating to 1190 ℃, preserving heat for 12min, and quenching to obtain the high-speed steel.
As can be seen from FIG. 5, the surface layer has an average grain size of about 4.5 μm, the carbides have an average grain size of about 4.6 μm, the inner layer has an average grain size of about 10.9 μm, and the carbides have an average grain size of about 2.5 μm, and a gradient structure is formed in which the carbide size gradually decreases from the surface layer to the inner layer and the grain size gradually increases from the surface to the inside.
Example 6
A preparation method of powder metallurgy high-speed steel comprises the following steps:
(1) Sieving M42 high-speed steel powder into powder with different particle size ranges of more than 275 microns, 225-275 microns, 200-250 microns, 175-225 microns, 150-200 microns, 125-175 microns, 75-125 microns and less than 100 microns;
(2) Sequentially arranging the powder in a composite sheath formed by concentrically sheathing sheaths with diameters of 100 mm, 200 mm, 300 mm, 400 mm, 500 mm, 600 mm, 700 mm and 800mm from outside to inside according to the order of the particle size range from large to small, removing the sheath at the inner layer, and only reserving the sheath at the outermost layer;
(3) Hot isostatic pressing the clad at 1050 ℃, wherein the pressure is 100MPa, and the time is 4h;
(4) Rapidly heating the hot isostatic pressing steel ingot to 1050 ℃ at a speed of 15 ℃/min, heating for 4h, then heating to 1120 ℃ by utilizing induction heating, and heating for 2h;
(5) Carrying out discontinuous progressive radial forging on the annealed steel ingot, wherein the forging frequency is 100 times/min, and the forging reduction per minute is 7mm;
(6) And (3) heating the steel billet to 800 ℃ by induction heating, preserving heat for 1h, then heating to 1180 ℃, preserving heat for 15min, and quenching to obtain the high-speed steel.
As can be seen from FIG. 6, the surface layer crystal grains have an average size of about 3.9 μm, the carbides have an average size of about 5.1 μm, the inner layer crystal grains have an average size of about 9.8 μm, and the carbides have an average size of about 2.3 μm, and a gradient structure is formed in which the carbide size gradually decreases from the surface layer to the inner layer and the crystal grain size gradually increases from the surface to the inside.
Comparative example 1
A preparation method of powder metallurgy high-speed steel comprises the following steps:
(1) Sieving the TFM5610 high-speed steel powder into powder with different particle size ranges of more than 275 microns, 225-275 microns, 200-250 microns, 175-225 microns, 150-200 microns, 125-175 microns, 75-125 microns and less than 100 microns;
(2) Sequentially arranging the powder in a composite sheath formed by concentrically sheathing sheaths with diameters of 100 mm, 200 mm, 300 mm, 400 mm, 500 mm, 600 mm, 700 mm and 800mm from outside to inside according to the order of the particle size range from large to small, removing the sheath at the inner layer, and only reserving the sheath at the outermost layer;
(3) Vibrating the composite sheath for degassing, and then circularly performing degassing treatment of vacuumizing and nitrogen filling for 4 times;
(4) Hot isostatic pressing the clad at 1050 ℃, wherein the pressure is 100MPa, and the time is 4h;
(5) Slowly heating the hot isostatic pressing steel ingot to 1050 ℃ at the speed of 5 ℃/min, heating for 4h, then heating to 1120 ℃ by utilizing induction heating, and heating for 2h;
(6) Carrying out discontinuous progressive radial forging on the annealed steel ingot, wherein the forging frequency is 100 times/min, and the forging reduction per minute is 7mm;
(7) And (3) heating the steel billet to 800 ℃ by induction heating, preserving heat for 1h, then heating to 1180 ℃, preserving heat for 15min, and quenching to obtain the high-speed steel.
As can be seen from FIG. 7, in this comparative example, since the temperature increase rate of the inner layer spheroidizing annealing in step (5) was slow, the spheroidizing effect of the carbide of the inner layer was not good, and a carbide gradient was not obtained.
Comparative example 2
A preparation method of powder metallurgy high-speed steel comprises the following steps:
(1) Sieving M42 high-speed steel powder into powder with different particle size ranges of more than 275 microns, 225-275 microns, 200-250 microns, 175-225 microns, 150-200 microns, 125-175 microns, 75-125 microns and less than 100 microns;
(2) Sequentially arranging the powder in a composite sheath formed by concentrically sheathing sheaths with diameters of 100 mm, 200 mm, 300 mm, 400 mm, 500 mm, 600 mm, 700 mm and 800mm from outside to inside according to the order of the particle size range from large to small, removing the sheath at the inner layer, and only reserving the sheath at the outermost layer;
(3) Vibrating the composite sheath for degassing, and then circularly performing degassing treatment of vacuumizing and nitrogen filling for 4 times;
(4) Hot isostatic pressing the sheath at 1050 ℃, wherein the pressure is 100MPa, and the time is 4h;
(5) Rapidly heating the hot isostatic pressing steel ingot to 1120 ℃ at a speed of 15 ℃/min, and heating for 4h;
(6) Carrying out discontinuous progressive radial forging on the annealed steel ingot, wherein the forging frequency is 100 times/min, and the forging reduction per minute is 7mm;
(7) And (3) heating the steel billet to 800 ℃ by induction heating, preserving heat for 1h, then heating to 1180 ℃, preserving heat for 15min, and quenching to obtain the high-speed steel.
As can be seen from fig. 8, in the comparative example, without the step annealing, the carbides of the surface layer and the inner layer are similar in size, and a carbide gradient is not obtained.
Comparative example 3
A preparation method of powder metallurgy high-speed steel comprises the following steps:
(1) Sieving M42 high-speed steel powder into powder with different particle size ranges of more than 275 microns, 225-275 microns, 200-250 microns, 175-225 microns, 150-200 microns, 125-175 microns, 75-125 microns and less than 100 microns;
(2) Sequentially arranging the powder in a composite sheath formed by concentrically sheathing sheaths with diameters of 100 mm, 200 mm, 300 mm, 400 mm, 500 mm, 600 mm, 700 mm and 800mm from outside to inside according to the order of the particle size range from large to small, removing the sheath at the inner layer, and only reserving the sheath at the outermost layer;
(3) Vibrating the composite sheath for degassing, and then circularly performing degassing treatment of vacuumizing and nitrogen filling for 4 times;
(4) Hot isostatic pressing the sheath at 1050 ℃, wherein the pressure is 100MPa, and the time is 4h;
(5) Rapidly heating the hot isostatic pressing steel ingot to 1050 ℃ at a speed of 15 ℃/min, heating for 4h, then heating to 1120 ℃ by utilizing induction heating, and heating for 2h;
(6) Carrying out conventional forging on the annealed steel ingot;
(7) And (3) heating the steel billet to 800 ℃ by induction heating, preserving heat for 1h, then heating to 1180 ℃, preserving heat for 15min, and quenching to obtain the high-speed steel.
As can be seen from fig. 9, in this comparative example, in which the conventional forging method was used, the surface layer and the inner layer had similar grain sizes, and no grain gradient was obtained.
Comparative example 4
A preparation method of powder metallurgy high-speed steel comprises the following steps:
(1) Sieving M42 high-speed steel powder into powder with different particle size ranges of more than 275 microns, 225-275 microns, 200-250 microns, 175-225 microns, 150-200 microns, 125-175 microns, 75-125 microns and less than 100 microns;
(2) Sequentially arranging the powder in a composite sheath formed by concentrically sheathing sheaths with diameters of 100, 200, 300, 400, 500, 600, 700 and 800mm from outside to inside according to the order of the particle size range from large to small, removing the inner sheath and only keeping the outermost sheath;
(3) Vibrating the composite sheath for degassing, and then circularly performing degassing treatment of vacuumizing and nitrogen filling for 4 times;
(4) Hot isostatic pressing the clad at 1050 ℃, wherein the pressure is 100MPa, and the time is 4h;
(5) Rapidly heating the hot isostatic pressing steel ingot to 1050 ℃ at a speed of 15 ℃/min, heating for 4h, then heating to 1120 ℃ by utilizing induction heating, and heating for 2h;
(6) Carrying out discontinuous progressive radial forging on the annealed steel ingot, wherein the forging frequency is 100 times/min, and the forging reduction per minute is 7mm;
(7) And (3) quenching the steel billet by adopting a conventional salt bath quenching process after heat preservation for 10min at 1200 ℃ to obtain the high-speed steel.
As can be seen from fig. 10, in the present comparative example, using the conventional quenching method, the surface layer and the inner layer have grain sizes close to each other, and no grain gradient is obtained.
Claims (10)
1. The preparation method of the powder metallurgy high-speed steel is characterized by comprising the following steps of:
(1) Arranging high-speed steel powder in a composite sheath consisting of mutually nested sheaths from outside to inside according to the sequence of the particle sizes from large to small;
(2) Removing the inner layer sheath, degassing the outer layer sheath, and performing hot isostatic pressing to obtain a steel ingot with gradient powder particle size;
(3) Carrying out inner-layer spheroidizing annealing on the steel ingot, and then carrying out surface layer induction annealing to obtain an annealed steel ingot with a gradient structure, wherein the size of carbide is gradually reduced from the surface layer to the inner layer;
(4) And performing discontinuous progressive radial forging on the annealed steel ingot, and performing graded quenching to obtain the high-speed steel with a gradient structure, wherein the grain size of the high-speed steel gradually increases from the surface to the inside.
2. The method for preparing powder metallurgy high-speed steel according to claim 1, wherein in the step (3), the temperature of inner layer spheroidizing annealing is 1050-1120 ℃ and the time is 2-4 h.
3. The method for preparing powder metallurgy high-speed steel according to claim 1, wherein in the step (3), the temperature rise rate of the inner layer spheroidizing annealing is 15-50 ℃/min.
4. The method for preparing powder metallurgy high-speed steel according to claim 1, wherein the surface induction annealing temperature is 1120-1180 ℃ and the time is 1-2 hours.
5. The method for preparing powder metallurgy high-speed steel according to claim 1, wherein in the step (4), the frequency of the discontinuous progressive radial forging is 90 to 150 times/min, and the forging reduction per minute is 3 to 10mm.
6. The method for preparing powder metallurgy high-speed steel according to claim 1, wherein in the step (4), the induction heating and stage quenching process comprises the following steps: firstly heating to 700-900 ℃ and preserving heat for 0.5-2 h, then heating to 1180-1220 ℃, preserving heat for 5-15 min and then quenching.
7. The method for preparing powder metallurgy high-speed steel according to claim 1, wherein in the step (2), the hot isostatic pressing temperature is 1000-1100 ℃, the pressure is 80-120 MPa, and the time is 2-6 h.
8. The method for preparing the powder metallurgy high-speed steel according to the claim 1, wherein in the step (1), the grain size of the high-speed steel powder ranges from large to small: 275 μm or more, 225 to 275 μm, 200 to 250 μm, 175 to 225 μm, 150 to 200 μm, 125 to 175 μm, 75 to 125 μm, 100 μm or less.
9. The method for preparing powder metallurgy high-speed steel according to claim 1, wherein in the step (1), the diameter difference between adjacent sheaths is 50 to 150mm.
10. The method for preparing powder metallurgy high-speed steel according to claim 1, wherein in the step (2), the degassing process comprises the following steps: and performing vacuum and nitrogen filling on the outer layer sheath circulation.
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