CN114351046A - Rare earth hot work die steel and preparation method thereof - Google Patents
Rare earth hot work die steel and preparation method thereof Download PDFInfo
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Abstract
The invention provides rare earth hot work die steel and a preparation method thereof. The rare earth hot work die steel comprises the following components: c, Mn, Si, S, P, Cr, Mo, V, Al, La and Ce, and the balance of Fe. The preparation method comprises the steps of smelting, refining, VD vacuum degassing, tempering and the like. The invention has the advantages that: 1. re is added on the basis of alloy containing Cr, Mo, Si, V and the like, La and Ce are specifically added, the component configuration of Cr, V, Mo and the like is further optimized, and solid solution strengthening and secondary hardening mechanism promotion and reinforcement are adopted, so that the die steel prepared from the rare earth has the characteristics of high strength, high toughness, high thermal stability and the like, the service life of a die can be prolonged, the production rhythm is accelerated, and a large number of application requirements are met; 2. tests show that the service life of the conventional H13 hot work die steel is only 3000-4000 times, and the rare earth hot work die steel provided by the invention is 8000-10000 times.
Description
Technical Field
The invention relates to the technical field of rare earth steel.
In particular to rare earth hot work die steel and a preparation method thereof.
Background
The hot working die is taken as important basic process equipment, is mainly used for forging and die-casting molding of solid metal, and is widely applied to the fields of automobile industry, mechanical manufacturing and the like. The hot working die bears complex thermal-mechanical load action in the working process, the service life of the hot working die is generally low, the production cost and the production rhythm of a forge piece are directly influenced, and the economic benefit of an enterprise is further seriously influenced. The cost of the hot forging die accounts for 8-15% of the production cost at abroad, and the cost of the hot forging die is up to 30-40% at home. To meet the development requirements of modern manufacturing industry, the Chinese die industry society emphasizes the importance of die reliability and service life. The main factors influencing the reliability and the service life of the die comprise the structural design of the die, the processing and manufacturing process, the selection of the material of the die, the heat treatment process, the surface strengthening, the lubrication, the use and the maintenance and the like. Among the many factors of mold failure, failure due to improper mold materials and mold heat treatment processes accounts for about 80%. Therefore, higher requirements are put on material selection and optimization of the mold material.
Disclosure of Invention
The invention provides rare earth hot work die steel and a preparation method thereof aiming at the defects of short service life and poor thermal stability of the existing widely used H13 hot work die steel, so as to achieve the characteristics of high strength, high toughness, high thermal stability and the like, thereby achieving the purposes of prolonging the service life of the die, accelerating the production rhythm and obtaining a large amount of application requirements.
The aim of the invention is achieved by the following technical measures:
the rare earth hot work die steel is characterized by comprising the following components: c, Mn, Si, S, P, Cr, Mo, V, Al, La and Ce, and the balance of Fe.
The specific optimization scheme is that the rare earth hot work die steel is characterized in that: the composition comprises the following components in percentage by mass:
c: 0.35-0.45%, Mn: 0.38% -0.44%, Si: 0.20-0.40%, S is less than or equal to 0.003%, P is less than or equal to 0.012%, Cr: 5.0% -5.50%, Mo: 2.0% -2.20%, V: 0.55-0.65%, Al: 0.025% -0.045%, La: 0.0045-0.0060%, Ce: 0.0010 to 0.015 percent, and the balance of Fe.
The specific optimization scheme is that the rare earth hot work die steel is characterized in that: the composition comprises the following components in percentage by mass:
c: 0.38% -0.42%, Mn: 0.38% -0.42%, Si: 0.25-0.30%, S is less than or equal to 0.003%, P is less than or equal to 0.010%, Cr: 5.1% -5.3%, Mo: 2.08% -2.14%, V: 0.56-0.58%, Al: 0.028% -0.040%, La: 0.0049% -0.0055%, Ce: 0.0011 to 0.014 percent and the balance of Fe.
The specific optimization scheme is that the rare earth hot work die steel is characterized in that: the composition comprises the following components in percentage by mass:
c: 0.39-0.41%, Mn: 0.38% -0.40%, Si: 0.24-0.38%, S is less than or equal to 0.003%, P is less than or equal to 0.010%, Cr: 5.25% -5.28%, Mo: 2.1% -2.14%, V: 0.56-0.58%, Al: 0.030-0.036%, La: 0.0050-0.0054%, Ce: 0.0012 to 0.013 percent and the balance of Fe.
The preparation method of the rare earth hot work die steel is characterized by comprising the following steps: the method comprises the following steps:
step one, smelting in an electric arc furnace EAF;
step two, refining white slag in an LF furnace;
step three, VD vacuum degassing;
step four, pouring an electrode blank under the argon protective atmosphere;
fifthly, cutting an electrode blank riser by flame;
step six, grinding and processing the electrode blank to manufacture a consumable electrode;
seventhly, electroslag remelting under the protection of argon gas:
step eight, carrying out high-temperature diffusion annealing on the electroslag ingot;
step nine, forging;
step ten, annealing;
step eleven, performing a melting detection performance test;
step twelve, flaw detection;
thirteen, semi-finishing;
step fourteen, tempering;
in the quenching and tempering process, the austenitizing homogenization temperature is 1030 ℃;
then, a graded quenching mode is adopted: the austenitized die material is quickly cooled to 370-420 ℃, and then is cooled to room temperature after heat preservation for 5-10 minutes; then heating to 565 ℃, preserving heat according to 1min/mm and then cooling by air;
the tempering times are three to four;
fifteen, physical and chemical inspection;
sixthly, handing over and checking.
In the first step and the seventh step, the adopted arc striking agent base stock is prepared by steel scraps without Ti components through decontamination, baking and air cooling;
before use, the arc striking agent is prepared from arc striking agent base material and pseudo-ginseng slag at a ratio of 5:1, and the pseudo-ginseng slag is Al2O3With CaF2Prepared according to the proportion of 3: 7;
when in use, the arc striking agent is paved into the furnace bottom.
95% of the commercially available arc-striking agents contain Ti, and the Ti in the traditional Ti-containing arc-striking agents can be prevented from polluting molten steel through the operation.
A specific optimization scheme, wherein in the seventh step, the size of the arc striking agent base material is 20-30 mm in length and 10-15 mm in width.
A specific optimization scheme is characterized in that in the first step and the seventh step, the adopted arc striking agent base material is prepared from the steel scraps of the rare earth hot-working die steel through the following steps:
a1, removing rust, oil stains, cooling liquid and iron scale on the surface of steel scraps to remove dirt;
a2, baking at 480 +/-20 ℃ for 2 hours;
a3, air cooling to prepare the arc striking agent.
A specific optimization scheme, in the third step, when the free oxygen [ O ] in the steel is less than or equal to 5ppm and the FeO in the refining slag is less than or equal to 0.5 percent, carrying out VD vacuum degassing treatment on the molten steel; according to La: ce = 3:7, packaging the mixed rare earth into a clean steel pipe, and then pressing the steel pipe filled with the rare earth into molten steel by adopting a pressing method, wherein:
la in the steel pipe: 0.0045-0.0060%, Ce: 0.0010 to 0.015 percent, and pressing the steel pipe to a position below 450 to 550mm of the liquid steel surface;
or La: 0.0049% -0.0055%, Ce: 0.0011 to 0.014 percent, and pressing the steel pipe to the position of 455 to 475mm below the molten steel surface.
In the smelting process, the beneficial effects of the rare earth elements can be fully exerted by the operation, and the strength, toughness and thermal stability indexes of the steel are improved.
A specific optimization scheme, in the ninth step, carrying out high-temperature diffusion annealing treatment on the electroslag ingot before forging, wherein the high-temperature diffusion temperature is 1260 ℃, and the diffusion time is 30 hours;
during forging, the forging is carried out by adopting a deformation mode of three-time upsetting and drawing, wherein the first-fire heating temperature is 1260 ℃, the second-fire heating temperature is 1220 ℃, and the third-fire heating temperature is 1190 ℃, wherein the upsetting ratio is more than or equal to 2, and the total forging ratio is more than or equal to 5.
The high-temperature diffusion annealing can improve segregation to prevent the segregation from reducing the toughness and other properties, the large-forging-ratio forging can effectively break the cast structure, the closed metal solidification defect and the uniform structure of the steel ingot, and the comprehensive properties of the hot-work die steel, such as strength, toughness, thermal stability and the like, are improved.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the advantages that:
1. re is added on the basis of alloy containing Cr, Mo, Si, V and the like, La and Ce are specifically added, the component configuration of Cr, V, Mo and the like is further optimized, and solid solution strengthening and secondary hardening mechanism promotion and reinforcement are adopted, so that the die steel prepared from the rare earth has the characteristics of high strength, high toughness, high thermal stability and the like, the service life of a die can be prolonged, the production rhythm is accelerated, and a large number of application requirements are met;
2. tests show that the service life of the conventional H13 hot work die steel is only 3000-4000 times, and the rare earth hot work die steel provided by the invention is 8000-10000 times.
The invention is further described with reference to the following figures and detailed description.
Drawings
FIG. 1 is a schematic structural view of a structure after thermal refining of the present invention.
FIG. 2 is a schematic structural view of the macroscopic morphology of the inclusion of the present invention.
FIG. 3 is an index of various non-metallic inclusions in Table 1 according to the present invention.
Detailed Description
Example 1: the rare earth hot-work die steel comprises the following components in percentage by mass:
C:0.35%~0.45%,Mn:0.38%~0.44%,Si:0.20%~0.40%,S≦0.003%,P≦0.012%,Cr:5.0%~5.50%,Mo:2.0%~2.20%,V:0.55%~0.65%,Al:0.025%~0.045%,La:0.0045%~0.0060%,Ce:0.0010%~0.015%。
tests prove that the rare earth hot work die steel provided by the invention has the service life of 8000-10000 times, which is only 3000-4000 times compared with the conventional H13 hot work die steel, and the service life of the die is obviously prolonged.
Example 2: as a preferred embodiment of the invention, the rare earth hot-work die steel comprises the following components in percentage by mass:
C:0.38%~0.42%,Mn:0.38%~0.42%,Si:0.25%~0.30%,S≦0.003%,P≦0.010%,Cr:5.1%~5.3%,Mo:2.08%~2.14%,V:0.56%~0.58%,Al:0.028%~0.040%,La:0.0049%~0.0055%,Ce:0.0011%~0.014%。
tests prove that the rare earth hot work die steel provided by the invention has the service life of 8500-9000 times, is only 3000-4000 times compared with the conventional H13 hot work die steel, and obviously prolongs the service life of the die.
Example 3: as a preferred embodiment of the invention, the rare earth hot-work die steel comprises the following components in percentage by mass:
C:0.39%~0.41%,Mn:0.38%~0.40%,Si:0.24%~0.38%,S≦0.003%,P≦0.010%,Cr:5.25%~5.28%,Mo:2.1%~2.14%,V:0.56%~0.58%,Al:0.030%~0.036%,La:0.0050%~0.0054%,Ce:0.0012%~0.013%。
tests prove that the rare earth hot-work die steel provided by the invention has the service life of 8800 to 9600 times, which is only 3000 to 4000 times longer than the conventional H13 hot-work die steel, and the service life of the die is obviously prolonged.
Example 4: the preparation method of the rare earth hot work die steel provided by the invention comprises the following steps:
step 1, smelting by an EAF (electric arc furnace);
step 2, refining the white slag in the LF furnace;
step 3, VD vacuum degassing;
when the free oxygen [ O ] in the steel is less than or equal to 5ppm and the (FeO) in the refining slag is less than or equal to 0.5%, carrying out VD vacuum degassing treatment on the molten steel;
according to La: ce = 3:7, preparing mixed rare earth, packaging into a clean steel tube, wherein,
La:0.0045%~0.0060%, Ce:0.0010%~0.015%;
pressing La and Ce rare earth alloy packaged in a clean steel tube below the surface of molten steel by adopting a press-in method
Adding the molten steel into the molten steel in a mode of 450-550 mm, and simultaneously properly increasing the flow of bottom blowing argon to ensure that the liquid level of the molten steel is not exposed;
step 4, pouring an electrode blank under the argon protective atmosphere;
step 5, cutting an electrode blank riser by flame;
step 6, grinding the electrode blank to manufacture a consumable electrode;
and 7, electroslag remelting under the protection of argon:
in the electroslag remelting process, the scraps made of the same material are used as an electroslag remelting arc-striking agent base material, and the arc-striking agent base material is processed into a size with the length of 20-30 mm and the width of 10-15 mm;
the metal chip arc striking agent base stock and pseudo-ginseng slag (30% Al2O3+70% CaF2) are prepared into electroslag remelting arc striking agent according to the proportion and are paved at the bottom of a slag furnace, and the paving amount is the same as the specification of a crystallizer;
step 8, carrying out high-temperature diffusion heating on the electroslag ingot;
step 9, forging: forging in a deformation mode of three-time upsetting and drawing;
step 10, annealing;
step 11, performance test;
step 12, ultrasonic flaw detection;
step 13, semi-finishing;
step 14, tempering;
in the quenching and tempering process, the austenitizing homogenization temperature is 1030 ℃;
then, a graded quenching mode is adopted: the austenitized die material is quickly cooled to 370-420 ℃, and then is cooled to room temperature after heat preservation for 5-10 minutes; then heating to 565 ℃, preserving heat according to 1min/mm and then cooling by air;
the tempering times are three to four;
step 15, physical and chemical detection;
and step 16, checking.
Tests prove that the rare earth hot work die steel provided by the invention has the service life of 8000-10000 times, which is only 3000-4000 times compared with the conventional H13 hot work die steel, and the service life of the die is obviously prolonged.
Example 5: the preparation method of the rare earth hot work die steel provided by the invention comprises the following steps:
electric Arc Furnace (EAF) smelting → LF furnace refining → VD vacuum degassing → argon protection pouring of electrode blank → electrode flame cutting riser → electrode blank grinding → argon protection electroslag remelting → electroslag ingot high temperature diffusion annealing → forging → annealing → melting inspection performance test → rough machining → flaw detection → semi-finishing → tempering → physicochemical inspection → inspection.
In the smelting process, after carbon control and oxygen control, tapping pre-deoxidation and refining are carried out at the end point of an electric furnace, when the free oxygen [ O ] in steel is less than or equal to 5ppm and the (FeO) in slag is less than or equal to 0.5 percent, after VD vacuum degassing treatment is carried out on molten steel, mixed rare earth of 0.0045 percent of La and 0.015 percent of Ce is added, and then the mixed rare earth is added into the molten steel in a mode of pressing the mixed rare earth into the position which is 450-550 mm below the liquid level, particularly, the effect of pressing the mixed rare earth into the position which is 500mm below the liquid level of the molten steel is optimal, and meanwhile, the flow of bottom blowing argon is increased to ensure that the liquid level of the molten steel is not exposed.
In the smelting process, the scraps of the high-quality rare earth hot-work die steel are used as an arc-striking agent base material for electroslag remelting, and the arc-striking agent base material is processed into a size with the length of 25-35 mm and the width of 10-15 mm. The arc striking agent base material and the pseudo-ginseng slag are mixed according to the mass ratio of 5:1, spreading the electroslag remelting arc striking agent at the bottom of the electroslag remelting furnace, wherein the spreading amount is matched with the specification of a crystallizer.
High-temperature diffusion annealing is adopted before the forging process, the diffusion heating temperature is 1260 ℃, and the high-temperature diffusion time is 30 hours. And (3) eliminating the band segregation by adopting a high-temperature homogenization technology. To avoid serious zonal segregation, high temperature diffusion is used to eliminate and reduce. Even if the technical measures of low melting speed and strong water cooling are adopted in the electroslag remelting process, an electroslag ingot has certain composition and structure segregation, and if long-time high-temperature diffusion annealing treatment is not adopted before forging, the strip segregation of a forged piece is serious, and the toughness index of the material can be obviously reduced.
In the forging process, a deformation mode of three times of upsetting and drawing is adopted, and cogging reduction is increased. And drawing and forming are carried out after integral upsetting, the total upsetting ratio is 3.6, and the total forging ratio (drawing-out ratio) is 5.8. The forging temperature is gradually reduced in the two-fire and three-fire upsetting-drawing processes, wherein the first-fire heating temperature is 1260 ℃, the second-fire heating temperature is 1220 ℃, and the third-fire heating temperature is 1190 ℃.
In the quenching and tempering process, the austenitizing homogenization temperature is 1030 ℃;
then, a graded quenching mode is adopted: the austenitized die material is quickly cooled to 370-420 ℃, and then is cooled to room temperature after heat preservation for 5-10 minutes; then heating to 565 ℃, preserving heat according to 1min/mm and then cooling by air;
the number of tempering is three to four.
Example 6: it differs from example 1 in that:
when the free oxygen [ O ] in the steel is less than or equal to 5ppm and the (FeO) in the refining slag is less than or equal to 0.5%, carrying out VD vacuum degassing treatment on the molten steel; according to La: ce = 3:7, preparing mixed rare earth, and packaging into a clean steel tube, wherein the ratio of La: 0.0049% -0.0055%, Ce: 0.0011 to 0.014 percent; la and Ce rare earth alloy packaged in a clean steel tube is pressed into the liquid steel surface by adopting a pressing-in method and is added into the liquid steel in a mode of 455-475 mm, and meanwhile, the flow of bottom blowing argon is properly increased to ensure that the liquid steel surface is not exposed.
By using the rare earth hot work die steel and the preparation method thereof provided by the invention, 1 electroslag ingot is smelted by an electric furnace and electroslag smelting method, and one bar with the diameter of 300mm is machined after forging. Ultrasonic flaw detection was carried out according to SEP 1921, and defects such as shrinkage cavities, cracks, white spots, delamination, and voids affecting the use were not found in the interior. The indexes of various non-metallic inclusions are shown in figure 3: table 1 shows the indexes of various non-metallic inclusions, the macroscopic morphology of the inclusions is shown in fig. 2, and the structure after the quenching and tempering is shown in fig. 1. As shown in figures 1, 2 and 3, the rare earth hot work die steel has the characteristics of high strength, high toughness, high thermal stability and the like, and tests prove that the rare earth hot work die steel provided by the invention has the service life of 8000-10000 times, which is only 3000-4000 times longer than that of the conventional H13 hot work die steel, so that the service life of the die is obviously prolonged, the production rhythm is accelerated, and a large number of application requirements are obtained.
While one embodiment of the present invention has been described in detail, the description is only a preferred embodiment of the present invention and should not be taken as limiting the scope of the invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (10)
1. The rare earth hot work die steel is characterized by comprising the following components: c, Mn, Si, S, P, Cr, Mo, V, Al, La and Ce, and the balance of Fe.
2. The rare earth hot work die steel according to claim 1, characterized in that: the composition comprises the following components in percentage by mass:
c: 0.35-0.45%, Mn: 0.38% -0.44%, Si: 0.20-0.40%, S is less than or equal to 0.003%, P is less than or equal to 0.012%, Cr: 5.0% -5.50%, Mo: 2.0% -2.20%, V: 0.55-0.65%, Al: 0.025% -0.045%, La: 0.0045-0.0060%, Ce: 0.0010 to 0.015 percent, and the balance of Fe.
3. The rare earth hot work die steel according to claim 1, characterized in that: the composition comprises the following components in percentage by mass:
c: 0.38% -0.42%, Mn: 0.38% -0.42%, Si: 0.25-0.30%, S is less than or equal to 0.003%, P is less than or equal to 0.010%, Cr: 5.1% -5.3%, Mo: 2.08% -2.14%, V: 0.56-0.58%, Al: 0.028% -0.040%, La: 0.0049% -0.0055%, Ce: 0.0011 to 0.014 percent and the balance of Fe.
4. The rare earth hot work die steel according to claim 1, characterized in that: the composition comprises the following components in percentage by mass:
c: 0.39-0.41%, Mn: 0.38% -0.40%, Si: 0.24-0.38%, S is less than or equal to 0.003%, P is less than or equal to 0.010%, Cr: 5.25% -5.28%, Mo: 2.1% -2.14%, V: 0.56-0.58%, Al: 0.030-0.036%, La: 0.0050-0.0054%, Ce: 0.0012 to 0.013 percent and the balance of Fe.
5. The preparation method of the rare earth hot work die steel is characterized by comprising the following steps: the method comprises the following steps:
step one, smelting in an electric arc furnace EAF;
step two, refining white slag in an LF furnace;
step three, VD vacuum degassing;
step four, pouring an electrode blank under the argon protective atmosphere;
fifthly, cutting an electrode blank riser by flame;
step six, grinding and processing the electrode blank to manufacture a consumable electrode;
seventhly, electroslag remelting under the protection of argon gas:
step eight, carrying out high-temperature diffusion annealing on the electroslag ingot;
step nine, forging;
step ten, annealing;
step eleven, performing a melting detection performance test;
step twelve, flaw detection;
thirteen, semi-finishing;
step fourteen, tempering;
in the quenching and tempering process, the austenitizing homogenization temperature is 1030 ℃;
then, a graded quenching mode is adopted: the austenitized die material is quickly cooled to 370-420 ℃, and then is cooled to room temperature after heat preservation for 5-10 minutes; then heating to 565 ℃, preserving heat according to 1min/mm and then cooling by air;
the tempering times are three to four;
fifteen, physical and chemical inspection;
sixthly, handing over and checking.
6. The method for producing a rare earth hot work die steel according to claim 5, characterized in that: in the first step and the seventh step, the adopted arc striking agent base material is prepared by steel scraps without Ti components through decontamination, baking and air cooling;
before use, the arc striking agent is prepared from arc striking agent base material and pseudo-ginseng slag at a ratio of 5:1, and the pseudo-ginseng slag is Al2O3With CaF2Prepared according to the proportion of 3: 7;
when in use, the arc striking agent is paved into the furnace bottom.
7. The method for producing a rare earth hot work die steel according to claim 6, characterized in that: in the seventh step, the size of the base material of the arc striking agent is 20 mm-30 mm in length and 10 mm-15 mm in width.
8. The method for producing a rare earth hot work die steel according to claim 6 or 7, characterized in that: in the first step and the seventh step, the adopted arc striking agent base material is prepared from the steel scraps of the rare earth hot-working die steel by the following steps:
a1, removing rust, oil stains, cooling liquid and iron scale on the surface of steel scraps to remove dirt;
a2, baking at 480 +/-20 ℃ for 2 hours;
a3, air cooling to prepare the arc striking agent.
9. The method for producing a rare earth hot work die steel according to claim 5, characterized in that: in the third step, when the free oxygen [ O ] in the steel is less than or equal to 5ppm and the FeO in the refining slag is less than or equal to 0.5 percent, carrying out VD vacuum degassing treatment on the molten steel; according to La: ce = 3:7, packaging the mixed rare earth into a clean steel pipe, and then pressing the steel pipe filled with the rare earth into molten steel by adopting a pressing method, wherein:
la in the steel pipe: 0.0045-0.0060%, Ce: 0.0010 to 0.015 percent, and pressing the steel pipe to a position below 450 to 550mm of the liquid steel surface;
or La: 0.0049% -0.0055%, Ce: 0.0011 to 0.014 percent, and pressing the steel pipe to the position of 455 to 475mm below the molten steel surface.
10. The method for producing a rare earth hot work die steel according to claim 5, characterized in that: step nine, before forging, carrying out high-temperature diffusion annealing treatment on the electroslag ingot, wherein the high-temperature diffusion temperature is 1260 ℃, and the diffusion time is 30 hours;
during forging, the forging is carried out by adopting a deformation mode of three-time upsetting and drawing, wherein the first-fire heating temperature is 1260 ℃, the second-fire heating temperature is 1220 ℃, and the third-fire heating temperature is 1190 ℃, wherein the upsetting ratio is more than or equal to 2, and the total forging ratio is more than or equal to 5.
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