CN115786632A - Manufacturing method of nitrogen-containing corrosion-resistant plastic die steel forged material - Google Patents
Manufacturing method of nitrogen-containing corrosion-resistant plastic die steel forged material Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a manufacturing method of a nitrogen-containing corrosion-resistant plastic die steel forged material, which solves the problem of nitrogen increase in the production of high-nitrogen corrosion-resistant plastic die steel, breaks through the production bottleneck of the processing technology of large-size forged materials and improves the internal and surface quality of steel. Specifically, smelting by adopting an electric furnace, LF and VD is adopted to enable the nitrogen content to reach the maximum dissolubility under normal pressure, and the addition amount of the later-stage nitriding alloy material is reduced; nitrogen is blown into the furnace for pressurization in the remelting process of the pressurized electroslag furnace, and a nitriding alloy material is added to meet the control requirement of nitrogen in the components. The hot working and annealing heat treatment of the 'fast forging machine' solves the production process of large-size forged materials, and further fills the blank of the production process of high-nitrogen corrosion-resistant plastic die steel forged materials. The invention has the following advantages: the smelting process realizes high nitrogen content and high purity; the hot working and annealing treatment make the steel material have high mechanical property, high isotropy and structure uniformity.
Description
Technical Field
The invention belongs to the technical field of steel material forging production, and particularly relates to a manufacturing method of a nitrogen-containing corrosion-resistant plastic die steel forging material; comprises the whole production processes of smelting, hot working and heat treatment of the high-nitrogen corrosion-resistant plastic die steel with the nitrogen content of 0.25-0.45 percent.
Background
The necessary performances of the corrosion-resistant plastic die steel in the manufacture of the die include wear resistance, corrosion resistance and polishing property. The design or proportion of alloy components is the most main factor influencing the performance of the steel, wherein carbon is an important constituent element in the corrosion-resistant plastic die steel, and the excessive carbon content can form carbide with chromium, thereby increasing the segregation tendency, and reducing the polishing performance and the corrosion resistance. The problems can be well solved by adopting high-nitrogen alloying and replacing carbon with nitrogen, and the alloy is one of important development directions of the corrosion-resistant plastic die steel at present. The high nitrogen corrosion resistant plastic die steel belongs to martensitic stainless steel, and the strengthening effect of nitrogen in martensitic stainless steel mainly includes martensitic stainless steel phase transformation strengthening, precipitation strengthening, solid solution strengthening and the like. In terms of corrosion resistance, nitrogen can retard the dissolution of chromium in steel and improve the stability of a passive film, and in addition, the internationally recognized calculation method for the pitting corrosion resistance equivalent of stainless steel is PRE = Cr% +3.3Mo% +16N%, and the influence degree of nitrogen on the pitting corrosion resistance of stainless steel is very large. The polishing performance is the most important index of the corrosion-resistant plastic die steel, and the structure segregation can be obviously reduced after nitrogen alloying is adopted, so that more excellent structure uniformity and polishing performance are obtained. Factors influencing the solubility of nitrogen in molten steel include alloy components, temperature and pressure, and in the actual production of the high-nitrogen corrosion-resistant plastic die steel, the alloy components and the temperature are fixed, but the pressure is increased to realize the effective method for increasing the nitrogen. Nowadays, there are many smelting methods for high nitrogen steel, such as pressurized induction smelting, pressurized electroslag remelting, powder metallurgy, etc., and because of the limitations of nitrogen increasing equipment, technology and capacity, the smelting and processing of high nitrogen steel are generally carried out in laboratories, and the industrialized stable continuous production, especially the smelting of large steel ingots, cannot be realized. The hot working process of the high-nitrogen corrosion-resistant plastic die steel is more researched in a laboratory by methods such as thermal simulation. In the actual production process, the problems of surface quality, internal structure, performance and the like in the hot working process of large-size high-nitrogen corrosion-resistant plastic die steel are not verified in practice. Therefore, the production process of the high-nitrogen corrosion-resistant plastic die steel in the future not only needs to solve the problem of nitrogen increase, but also needs to break through the production bottleneck of the processing process of large-size forged materials and improve the internal and surface quality of steel.
Disclosure of Invention
The invention discloses a manufacturing method of a nitrogen-containing corrosion-resistant plastic die steel forging material, namely a production process for producing a large-size forging material by adopting smelting of an electric furnace, LF, VD and a pressurized electroslag furnace, hot working of a rapid forging machine and annealing heat treatment, and further filling the blank of the production process of the high-nitrogen corrosion-resistant plastic die steel forging material; wherein the smelting process aims at realizing high nitrogen content and high purity; the goal of hot working and annealing is to provide high mechanical properties, high isotropy and structural homogeneity to the steel.
In order to realize the purpose, the technical scheme is as follows: the electric furnace + LF + VD' is adopted for the primary smelting, so that the nitrogen content is enabled to reach the maximum dissolubility under normal pressure while the deoxidation effect and good purity of the molten steel are ensured, and the addition of the later-stage nitriding alloy material is reduced; nitrogen is blown into the furnace for pressurization in the remelting process of the pressurized electroslag furnace, and a nitriding alloy material is added to meet the control requirement of nitrogen in the components. The nitride alloy material is selected from silicon nitride and chromium nitride, and is added according to the nitrogen increasing proportion of 70 percent and 30 percent respectively; in the aspect of hot working, an electroslag ingot is subjected to homogenization treatment, a 35MN rapid forging machine is utilized for multi-directional deformation, and proper rolling reduction and finish forging temperature are controlled so as to ensure the surface quality of forged steel and improve the uniformity, mechanical property and isotropy of a structure; and a cooling process after forging and a proper annealing treatment process are matched to obtain a uniform spherical pearlite structure, so that good structure preparation is provided for heat treatment of the die.
The specific process steps are as follows:
1. electric furnace + LF + VD smelting process
(1) Raw materials are selected from pig iron, scrap steel and alloy materials containing iron, chromium, molybdenum, vanadium and other elements;
(2) charging scrap and pig iron into an electric furnace → feeding electricity → blowing oxygen → adding slag → full melting → sampling → tapping with phosphorus not more than 0.007%;
(3) after electric furnace tapping and slag skimming → LF furnace in-place adding slag materials such as lime and the like → electrifying → adding deoxidizer → sampling → adding alloy materials to adjust components → hanging out after the components are qualified;
(4) after the ladle is put into the VD tank, the pressure of argon gas blowing is not more than 100Pa → 10mi n-20 mi n is kept → the VD tank is uncovered → nitrogen gas is blown (the flow of nitrogen gas is calculated according to the design target of nitrogen in the electrode blank) → sampling → supplementing ferrochrome nitride → adjusting the temperature of feed electricity → tapping casting the electrode blank; the specification of the electrode blank is phi 470 mm-phi 600mm.
2. The remelting process of the pressurized electroslag furnace comprises the following steps:
(1) preparation work: performing roller milling treatment on the surface of the electrode blank, removing the iron oxide scale on the surface, and cutting the steel seed bottom pad; cleaning the electroslag furnace body and surrounding dust and impurities, and ensuring the sealing effect; checking the normal operation of a pressure pipeline and a feeding system of the pressurized electroslag furnace; a crystallizer with phi 750mm or phi 930mm is used, and 30 kg-50 kg of silicon nitride is added into one of two alloy feeders above the pressurized electroslag furnace, and 50 kg-100 kg of chromium nitride is added into the other alloy feeder.
(2) Feeding electricity for arc striking, entering a slagging stage, wherein the time is 1.0-2 h, and the melting rate is 610-900 kg/h; and after 10min of slagging is started, filling nitrogen into the furnace to increase the pressure in the furnace, setting the pressure to be 10-15 bar, and after the pressure reaches a set value, simultaneously adding two nitride alloy materials of silicon nitride and chromium nitride into the furnace by an alloy feeder at the rates of 2-6 kg/h and 3-10 kg/h respectively, thereby realizing the aim of 0.25-0.45 percent of nitrogen in the steel.
(3) And in the normal smelting stage, parameters such as the pressure in the furnace, the adding speed of the nitriding alloy material, the melting speed and the like are kept stable.
(4) And in the filling stage, the pressure in the furnace is kept stable at 10.0-15.0 bar.
(5) The electroslag ingot is 750mm or 930mm in diameter, and the electroslag ingot is cooled for 10-24 hr before being sent to the processing plant.
3. The hot processing technology comprises the following steps:
(1) homogenizing and diffusing the steel ingot at 1200-1260 ℃, and keeping the temperature for 15-30 h to homogenize the element segregation in the steel ingot.
(2) After diffusion treatment, the temperature is reduced to 1180-1200 ℃ for forging production, the finish forging temperature is controlled to be not lower than 980 ℃, cracks are prevented from being generated due to temperature reduction, and the surface quality of steel is ensured.
(3) Multi-fire-time and multi-direction forging is adopted, one fire time, a clamp handle is pressed, and the surface is lightly pressed by the rolling reduction of 50 mm-80 mm, so that the surface of the steel ingot is flat; second heating, upsetting and lightly pressing the surface with a rolling reduction of 50-80 mm, flattening surface wrinkles caused by upsetting, and improving the isotropy of the steel; drawing out after three times of fire, controlling the drawing-out reduction amount to be 60-150 mm, and controlling the finish forging temperature to be not lower than 1000 ℃ during drawing-out.
(4) Can realize the stable production of large-size forged materials with the thickness of 100 mm-500 mm and the width of 300 mm-900 mm.
4. Annealing heat treatment process:
after forging, the steel is cooled in an air cooling or air cooling mode, and after the temperature is reduced to 100-300 ℃, the steel is loaded in a furnace for annealing treatment; the annealing temperature is 810-890 ℃, and the heat preservation time is 20-45 h; then cooling to 200-400 ℃ at a cooling speed of 20-50 ℃/h, and discharging to obtain uniform spherical pearlite structure.
Description of the invention points:
the invention firstly provides a method for manufacturing a large-specification corrosion-resistant plastic die steel forging material containing 0.25-0.45% of nitrogen by adopting the processes of 'electric furnace + LF + VD + pressurized electroslag furnace + forging + annealing'. The method is limited by equipment capacity, the high-nitrogen corrosion-resistant plastic die steel produced at home and abroad has smaller specification and higher cost, and the production of large-size high forging materials only stays on theoretical analysis.
The smelting, processing and heat treatment method designed by the invention is verified by industrial production practice. The nitrogen increase in the steel needs two smelting processes: (1) the smelting ingredients of 'electric furnace + LF + VD' are not added with ferrosilicon for one-time nitrogen increase, and the nitrogen in the molten steel reaches the maximum dissolving amount under normal pressure by using methods of nitrogen blowing and chromium nitride adding while the purity of the molten steel is ensured; (2) and (2) secondary nitrogen increase, adopting 'pressurized electroslag' remelting and smelting, continuously adding silicon nitride and chromium nitride alloy materials in the smelting process, wherein the silicon nitride provides 70% of nitrogen increase amount, the chromium nitride provides 30% of nitrogen increase amount, controlling the pressure in the furnace to be 10.0 bar-15.0 bar, and dissolving nitrogen in the nitrogen nitride alloy materials into the molten steel to realize secondary nitrogen content increase.
Theories and practices prove that the hot working process of the high-nitrogen corrosion-resistant plastic die steel has a narrow hot working interval and is easy to crack after the temperature is reduced, so that the heating temperature, the finish forging temperature and the single-pass reduction of forging are cooperatively controlled in the forging process, and the internal and surface quality of a forged material is ensured; controlled forging and cooling of steel, and reasonable spheroidizing annealing process to obtain homogeneous pearlite structure, and provides excellent structure preparation for quenching and tempering heat treatment of mold.
Compared with the prior art, the invention has the following advantages:
(1) compared with the patent of the invention of 'a method for smelting high-nitrogen die steel by using a vacuum induction furnace and a pressurized electroslag furnace' (patent number 202111489598.1), the method mainly realizes nitrogen increase by nitrogen blowing in the smelting process of an electric furnace + LF + VD, is twice of the nitrogen increase amount in the smelting process of the vacuum induction furnace, and is simple and easy to realize. The consumption of alloy nitride materials such as chromium nitride, silicon nitride and the like is reduced in the later period, the cost is reduced, and the uniformity and the qualification rate of nitrogen in large steel ingots are improved.
(2) The added nitride alloy material is remelted by the pressurized electroslag, so that the steel obtains higher nitrogen content. The stable control of the production process parameters of the large steel ingot improves the uniformity of the distribution of nitrogen elements in the steel, and the nitrogen accurately reaches the target; under the protection of nitrogen with enough pressure, the nitrogen in the molten pool is prevented from escaping, the oxygen content and the impurity content of the steel ingot are reduced, and the purity is further improved; compared with the invention patent of 'a method for smelting high-nitrogen die steel by a vacuum induction furnace and a pressurized electroslag furnace' (patent number 202111489598.1), the method not only meets the requirement of low silicon in the component design of the corrosion-resistant plastic die steel, but also reduces the cost. The electric furnace, LF, VD and pressurized electroslag furnace are jointly smelted, so that the nitrogen uniformity is better than that of other smelting modes, and the industrial production of large-size steel ingots is facilitated.
(3) The homogenization process, the forging heating temperature and the controlled forging air cooling process in the hot working process are controlled, and compared with other hot working modes, the method has better structure uniformity, mechanical property, isotropy and surface quality.
(4) Compared with other high-nitrogen corrosion-resistant plastic die steel production processes, the whole set of industrial production process of 'electric furnace + LF + VD + pressurized electroslag furnace + forging + annealing' has the characteristics of high nitrogen content, high quality, high efficiency, low energy consumption, large product size and the like.
Drawings
FIG. 1 is a distribution diagram of the positions of the chemical components and the microstructure of a forged material finished product;
FIG. 2 shows an annealed microstructure of the head center of a 30Cr14MoN0.4 finished product;
FIG. 3 30Cr14MoN0.4 annealed microstructure at the position of 1/4 diagonal line of the head of the finished product;
FIG. 4 shows an annealed microstructure at the corner of the head of a finished product of 30Cr14MoN0.4;
FIG. 5 shows an annealed microstructure at the center of the head of a finished product of 20Cr13Ni MoN0.25;
FIG. 6 is an annealed microstructure at a position 1/4 of a diagonal line of a head of a finished product of 20Cr13Ni MoN0.25;
FIG. 7 annealed microstructures of 20Cr13Ni MoN0.25 as the corner positions of the head of the finished product;
FIG. 8 shows an annealed microstructure at the center of the head of a finished product of 30Cr15MoN0.45;
FIG. 9 shows an annealed microstructure at a position 1/4 of a diagonal line of a head of a finished product material 30Cr 15MoN0.45;
FIG. 10 shows an annealed microstructure at corner positions of the head of a 30Cr15MoN0.45 finished product;
the figures are as follows: 1-the corner of the head of the forging material, 2-the 1/4 part of the diagonal line of the head of the forging material, 3-the center of the head of the forging material, 4-the corner of the tail of the forging material, 5-the 1/4 part of the diagonal line of the tail of the forging material, 6-the center of the tail of the forging material, 7-the height direction of the forging material, 8-the width direction of the forging material and 9-the length direction of the forging material.
Detailed Description
The following examples are provided to illustrate the present invention in detail with reference to the accompanying drawings.
According to the technical scheme, the following three preferable examples are provided.
Example 1
Smelting and casting an electrode blank with the diameter of 470mm by an electric furnace and LF and VD, remelting an electroslag ingot with the diameter of 750mm by a pressurized electroslag furnace, producing a forged flat steel with the finished product specification of 260mm multiplied by 610mm (thickness multiplied by width) by a 35MN fast forging machine, and annealing the forged steel. The target steel grade was 30Cr14MoN0.4, and the alloy composition and final product target values are shown in Table 1.
TABLE 1
The method comprises the steps of performing electric furnace smelting according to target components and process requirements of steel grades and according to a batching target in a table 2.
TABLE 2
Smelting by adopting an electric furnace of 30t, and selecting scrap steel, pig iron, ferrochrome, electrolytic manganese, ferromolybdenum and the like as ingredients; oxygen is blown after full melting, temperature measurement and sampling are carried out after 1000kg of slag is added and 30mi n is carried out, and the analysis P is 0.005 percent.
Thirdly, measuring the temperature of 1573 ℃ before the LF station after slagging off, adding 300kg of lime and 50kg of aluminum-calcium slag, and adding 50kg of electrolytic manganese; after the alloy is put in place, the alloy is electrified to adjust the temperature, and 30kg of deoxidizing agent such as aluminum powder and carburant are added at the same time.
And after the color of the protective slag turns white, measuring the temperature, sampling and analyzing all elements, continuously adding alloy materials according to the analysis result, and adjusting the components to be qualified.
Fifthly, turning to a VD station after slagging off of the LF furnace, starting a VD pump for degassing, keeping the argon flow at 40L/min-60L/min, keeping the pressure at 67Pa, and keeping the pressure at 15 min.
Sixthly, blowing nitrogen gas 110m after uncovering 3 Blowing argon gas 5 min, sampling and analyzing nitrogen to be 0.167%, heating by supplying electricity, adding 270kg of chromium nitride, sampling and analyzing all elements to reach target values, wherein nitrogen is0.184%, 0.0018% oxygen, 0.18% silicon; and (4) lifting the steel ladle to a casting station, and casting the electrode blank with the diameter of 470 mm.
And (4) carrying out surface roll milling treatment after annealing of the electrode blank, removing iron oxide scales on the surface, and cutting a bottom pad.
And adopt 15t to pressurize electroslag furnace to remelt, check out the apparatus to operate well before producing; and remelting an electroslag ingot with the diameter of 750mm by using an electrode blank with the diameter of 470 mm.
The pressure of the nitrogen gas is increased after the self-supporting slagging starts to be 12 min, and the pressure is increased to 10bar after 20 min; the melting rate is 658 kg/h-670 kg/h, the adding rate of silicon nitride is 4.8 kg/h-4.9 kg/h, and the adding rate of chromium nitride is 8.3 kg/h-8.4 kg/h.
The method is characterized in that the method enters a normal smelting stage, the pressure is 9.9-10.5 bar, the temperature difference of cooling water is 7.2-7.7 ℃, and the alloy material adding rate and other smelting parameters are stable.
The electrode begins to enter a filling stage when the weight of the electrode is 264kg, the total filling time is 1h24mn, and the pressure in the filling stage is maintained at about 10.0 bar.
Stopping filling, stopping power supply and releasing pressure, cooling the electroslag ingot in a crystallizer for 1.5h, cooling the electroslag ingot cover after stripping for 12h, and heating the electroslag ingot cover in a forging plant after cooling.
The temperature of the selection diffusion treatment is 1220 ℃, and the heat preservation is carried out for 20h; after the diffusion is finished, cooling to 1190 ℃, preserving the heat for 2 hours, and carrying out forging production; lightly pressing the surface of the steel ingot by 60mm rolling reduction for one fire time, and pressing a clamp handle; upsetting for two times, wherein the height ratio of the front part to the rear part is 2:1, slightly pressing the surface with 60mm of rolling reduction after upsetting; drawing out for three times, wherein the rolling reduction of the first 4 times is 100-120 mm, the rolling reduction of the second 6 times is 60-80 mm, and chamfering is carried out in the process to prevent the corners from cracking; drawing out the fiber for four times with the rolling reduction of 40 mm-80 mm; drawing out and shaping for five times; the reburning temperature of each fire is 1190 ℃, and the final forging temperature is not lower than 1023 ℃ when drawing out; the specification of the forged finished product is 260mm multiplied by 610mm.
Cooling the forged steel to 212 ℃ in air, loading the forged steel into an annealing furnace, keeping the temperature of 870 ℃ for 30h, cooling to 310 ℃ at a cooling rate of not more than 30 ℃/h, discharging and cooling in air.
The chemical compositions of the forged material are analyzed by sampling from different positions of the cross sections of the head part and the tail part of the annealed forged material (see figure 1), and the analysis results are shown in a table 3 and list main control elements and easily burnt elements; from the result, nitrogen elements at different positions of the head and the tail of the forging material are uniformly distributed, and other elements meet the target control requirement.
TABLE 3
The microstructure (500 times) of the forged product after the water-in-oil annealing, which is obtained by sampling and observing the center of the head (figure 2), the diagonal line 1/4 (figure 3) and the side (figure 4) of the forged product, is spherical pearlite and is uniformly distributed.
Example 2
Smelting and casting an electrode blank with the diameter of 600mm by an electric furnace plus LF plus VD, remelting an electroslag ingot with the diameter of 930mm by a pressurized electroslag furnace, producing a forged flat steel with the specification of a finished product of 300mm multiplied by 870mm (thickness multiplied by width) by a 35MN fast forging machine, and annealing the forged steel. The target steel grade was 20Cr13Ni MoN0.25, and the alloy composition and the target product value are shown in Table 4.
TABLE 4
The method comprises the steps of performing electric furnace smelting according to target components and process requirements of steel grades and according to a batching target in a table 5.
TABLE 5
Smelting by adopting an electric furnace of 30t, and selecting scrap steel, pig iron, ferrochrome, nickel plates, electrolytic manganese, ferromolybdenum and the like as ingredients; blowing oxygen after full melting, adding 1000kg of slag, 30mi n, measuring temperature and sampling, and analyzing that P is 0.006%.
Thirdly, measuring the temperature of 1570 ℃ after slagging off and before an LF station, adding 420kg of lime and 80kg of aluminum-calcium slag, and adding 70kg of electrolytic manganese; after the alloy is put in place, the alloy materials such as ferrochrome and the like are added, and 60kg of deoxidizing agent such as aluminum powder and 20kg of carburant are added.
And after the color of the protective slag turns white, measuring the temperature, sampling and analyzing all elements, continuously adding electrolytic manganese, ferromolybdenum and nickel plate alloy materials according to the analysis result, and adjusting the components to be qualified.
Fifthly, turning to a VD station after slagging off of the LF furnace, starting a VD pump for degassing, keeping the argon flow at 40L/min-60L/min, keeping the pressure at 67Pa, and keeping the pressure at 15 min.
Sixthly, blowing nitrogen gas 80m after uncovering the cover 3 Argon gas is blown to 5 min, the nitrogen content is 0.135 percent through sampling analysis, 300kg of chromium nitride is added after the temperature is raised through power supply, and the total elements reach the target value through sampling analysis, wherein the nitrogen content is 0.163 percent, the oxygen content is 0.0020 percent, and the silicon content is 0.17 percent; and (4) hoisting the steel ladle to a casting station, and casting the electrode blank with the diameter of 600mm.
And (4) carrying out surface roll milling treatment after annealing of the electrode blank, removing iron oxide scales on the surface, and cutting a bottom pad.
And adopt 15t to pressurize electroslag furnace to remelt, check out the apparatus to operate well before producing; and remelting an electroslag ingot with the diameter of 930mm by using an electrode blank with the diameter of 600mm.
The pressure of the nitrogen gas is increased after 20min of the self-supporting slagging, and the pressure is increased to 12bar after 20 min; the melting rate is 835 kg/h-848 kg/h, the adding rate of silicon nitride is 2.2 kg/h-7.7 kg/h, and the adding rate of chromium nitride is 3.9 kg/h-4.0 kg/h.
The method is characterized in that the method enters a normal smelting stage, the pressure is 11.8-12.3 bar, the temperature difference of cooling water is 7.3-7.7 ℃, and the alloy material adding rate and other smelting parameters are stable.
The electrode blank begins to enter a filling stage when the weight of the electrode blank is remained 310kg, the total filling time is 1h24mi n, and the pressure in the filling stage is maintained to be about 10.0 bar.
After filling, power is cut off to release pressure, the electroslag ingot is cooled in a crystallizer for 2h, the electroslag ingot is cooled in a cover for 15h after stripping, and the cover is cooled and then sent to a forging plant for heating.
The temperature of the selection diffusion treatment is 1220 ℃, and the heat preservation is carried out for 25h; after diffusion is finished, cooling to 1190 ℃, preserving heat for 3 hours, and carrying out forging production; lightly pressing the surface of the steel ingot by 60mm of rolling reduction for one fire, and pressing a clamp handle by the end of a bottom pad; and (3) secondary fire upsetting, wherein the height ratio of the front part to the rear part is 2:1, slightly pressing the surface by 60mm pressing 5 lower weight after upsetting; drawing out for three times, wherein the rolling reduction of the first 6 times is 100-150 mm, the rolling reduction of the second 6 times is 60-80 mm, and chamfering is carried out in the process to prevent the corners from cracking; drawing out the fiber for four times with the rolling reduction of 40 mm-80 mm; drawing out the long part for five to six times with the rolling reduction of 40-80 mm, and shaping; the reburning temperature of drawing out each fire is 1190 ℃, and the final forging temperature is not lower than 1015 ℃; the specification of the forged finished product is 260mm multiplied by 870mm.
Cooling the forged steel to 260 ℃ in air, loading into an annealing furnace, keeping the temperature of 870 ℃ for 35h, cooling to 300 ℃ at the cooling rate of not more than 30 ℃/h, discharging and air cooling.
The chemical compositions of the forged material are analyzed by sampling from different positions of the cross sections of the head part and the tail part of the annealed forged material (see figure 1), and the analysis results are shown in table 6, wherein main control elements and easily burnt elements are listed; from the result, nitrogen elements at different positions of the head and the tail of the forging material are uniformly distributed, and other elements meet the target control requirement.
TABLE 6
The microstructure (500 times) of the forged product after the water/water annealing was sampled and observed at the center of the head (FIG. 5), the 1/4 diagonal (FIG. 6) and the side (FIG. 7), and the annealed structure was spherical pearlite and was uniformly distributed.
Example 3
Smelting and casting an electrode blank with the diameter of 470mm by an electric furnace and LF and VD, remelting an electroslag ingot with the diameter of 750mm by a pressurized electroslag furnace, producing a forged flat steel with the specification of 305mm multiplied by 610mm (thickness multiplied by width) by a 35MN fast forging machine, and annealing the forged steel. The target steel grade was 30Cr15MoN0.45, and the alloy composition and the target product values are shown in Table 7.
TABLE 7
The method comprises the steps of performing electric furnace smelting according to target components and process requirements of steel grades and according to a batching target in a table 8.
TABLE 8
Smelting by adopting an electric furnace of 30t, and selecting scrap steel, pig iron, ferrochrome, electrolytic manganese, ferromolybdenum and the like as ingredients; blowing oxygen after full melting, adding 1000kg of slag, 30mi n, measuring temperature and sampling, and analyzing that P is 0.006%.
Thirdly, measuring the temperature of 1573 ℃ after slagging off and before an LF station, adding 350kg of lime and 60kg of aluminum-calcium slag, and adding 60kg of electrolytic manganese; after the alloy is put in place, the alloy materials such as ferrochrome and the like are added, and 30kg of aluminum powder deoxidizer and 30kg of carburant are added in batches.
And after the color of the protective slag turns white, measuring the temperature, sampling and analyzing all elements, continuously adding electrolytic manganese, ferromolybdenum and nickel plate alloy materials according to the analysis result, and adjusting the components to be qualified.
Fifthly, turning to a VD station after slagging off of the LF furnace, starting a VD pump for degassing, keeping the argon flow at 40L/min-60L/min, keeping the pressure at 67Pa, and keeping the pressure at 15 min.
Sixthly, blowing 130m of nitrogen after uncovering 3 Argon gas is blown to 5 min, the nitrogen content is 0.181% by sampling analysis, 200kg of chromium nitride is added after the temperature is raised by power supply, and the total elements reach the target value by sampling analysis, wherein the nitrogen content is 0.196%, the oxygen content is 0.0023%, and the silicon content is 0.22%; and (4) hoisting the steel ladle to a casting station, and casting the electrode blank with the diameter of 470 mm.
And carrying out surface roll milling treatment after annealing of the electrode blank, removing iron oxide scales on the surface, and cutting a bottom pad.
And adopt 15t to pressurize electroslag furnace to remelt, check out the apparatus to operate well before producing; and remelting an electroslag ingot with the diameter of 750mm by using an electrode blank with the diameter of 470 mm.
The pressure of the nitrogen gas is increased after the self-skin slagging is started to be 20min, and the pressure is increased to be 10bar after 20 min; the melting rate is 716 kg/h-730 kg/h, the adding rate of silicon nitride is 5.13 kg/h-5.2 kg/h, and the adding rate of chromium nitride is 8.9 kg/h-9.0 kg/h.
And entering a normal smelting stage after 80 min of slagging, wherein the pressure and the cooling water pressure are 9.8-10.3 bar, the current is 13-16 KA, the voltage is 60-66V, the temperature difference of the cooling water is 7.2-7.8 ℃, and various parameters in the smelting process are stable.
The electrode blank begins to enter a filling stage when the weight of the electrode blank is 200kg, the total filling time is 1h15mi n, and the pressure in the filling stage is maintained at about 10.0 bar.
Stopping filling, stopping power supply and releasing pressure, cooling the electroslag ingot in a crystallizer for 1.5h, cooling the electroslag ingot cover after stripping for 12h, and heating the electroslag ingot cover in a forging plant after cooling.
The temperature of the selection diffusion treatment is 1220 ℃, and the heat preservation is carried out for 20h; after the diffusion is finished, cooling to 1190 ℃, preserving the heat for 2 hours, and carrying out forging production; lightly pressing the surface of the steel ingot by 60mm of rolling reduction for one time, and pressing a clamp handle by the end of a bottom pad; upsetting for two times, wherein the height ratio of the front part to the rear part is 2:1, slightly pressing the surface by 60mm pressing 5 lower weight after upsetting; drawing out for three times, wherein the rolling reduction of the first 4 times is 100-150 mm, the rolling reduction of the second 6 times is 60-80 mm, and chamfering is carried out in the process to prevent the corners from cracking; drawing out the fiber for four times with the rolling reduction of 40 mm-80 mm; drawing out the long part with five fire times, wherein the rolling reduction is 40-80 mm, and shaping; the reburning temperature of drawing out each fire is 1190 ℃, and the final forging temperature is not lower than 1010 ℃; the specification of the forged finished product is 300mm multiplied by 810mm.
The steel after the self-feedback forging is air-cooled to 260 ℃ and then is loaded into an annealing furnace, the temperature rise speed is 50 ℃/h, the temperature is raised to 870 ℃ and is kept for 30h, then the temperature is reduced to 300 ℃ at the temperature reduction speed of not more than 130 ℃/h, and the steel is discharged from the furnace and air-cooled.
The chemical compositions of the forged material are analyzed by sampling from different positions of the cross sections of the head and the tail of the annealed forged material (see figure 1), and the analysis results are shown in a table 9 and list main control elements and easily burnt elements; from the result, nitrogen elements at different positions of the head and the tail of the forging material are uniformly distributed, and other elements all meet the target control requirement.
TABLE 9
Watch 9 (continuation)
The microstructure (500 times) of the forged product after the water/water annealing was sampled and observed at the head center (FIG. 8), the diagonal line 1/4 (FIG. 9) and the side (FIG. 10), and the annealed structure was spherical pearlite and was uniformly distributed.
Claims (2)
1. The manufacturing method of the nitrogen-containing corrosion-resistant plastic die steel forging material is characterized by comprising the steps of 'electric furnace + LF + VD + pressurized electroslag furnace + forging + annealing';
the smelting process of 'electric furnace + LF + VD' ensures the deoxidation effect and good purity of molten steel, simultaneously enables the nitrogen content to reach the maximum dissolubility under normal pressure, and reduces the adding amount of later-stage nitriding alloy materials;
according to the 'pressurized electroslag furnace' remelting process, nitrogen is blown into the furnace in the remelting process to be pressurized, a nitrided alloy material is added to meet the control requirement of nitrogen in the components, and the nitrided alloy material is selected from silicon nitride and chromium nitride and is added according to the nitrogen increasing proportion of 70% and 30% respectively;
in the forging hot processing technology, an electroslag ingot is subjected to homogenization treatment, a 35MN rapid forging machine is used for multi-directional deformation, and the appropriate rolling reduction and finish forging temperature are controlled, so that the surface quality of a forged steel material is ensured, and the uniformity, mechanical property and isotropy of a structure are improved;
the annealing heat treatment process comprises the following steps: and a cooling process after forging and a proper annealing treatment process are matched to obtain a uniform spherical pearlite structure, so that good structure preparation is provided for heat treatment of the die.
2. The method of manufacturing a nitrogen-containing corrosion resistant die steel forging according to claim 1,
the specific process steps of smelting by the electric furnace, LF and VD are as follows:
(1) raw materials are selected from pig iron, scrap steel and alloy materials containing iron, chromium, molybdenum, vanadium and other elements;
(2) charging scrap and pig iron into an electric furnace → feeding electricity → blowing oxygen → adding slag → full melting → sampling → tapping with phosphorus not more than 0.007%;
(3) after electric furnace tapping and slag skimming → LF furnace in-place adding slag materials such as lime and the like → electrifying → adding deoxidizer → sampling → adding alloy materials to adjust components → lifting the components out after the components are qualified;
(4) after the ladle is put into the VD tank, the pressure of argon blowing gas is not more than 100Pa → the pressure is kept for 10min to 20min → the VD tank is uncovered → nitrogen blowing (the flow of nitrogen blowing is calculated according to the design target of nitrogen in the electrode blank) → sampling → supplementing ferrochrome nitride → adjusting the temperature for power supply → tapping and casting the electrode blank; the specification of the electrode blank is phi 470 mm-phi 600mm;
the remelting specific process of the pressurized electroslag furnace comprises the following steps:
(1) preparation work: performing roller milling treatment on the surface of the electrode blank, removing the iron oxide scale on the surface, and cutting the steel seed bottom pad; cleaning the electroslag furnace body and surrounding dust and impurities, and ensuring the sealing effect; checking the normal operation of a pressure pipeline and a feeding system of the pressurized electroslag furnace; using a crystallizer with phi 750mm or phi 930mm, and adding 30 kg-50 kg of silicon nitride into one of two alloy feeders above the pressurized electroslag furnace, and adding 50 kg-100 kg of chromium nitride into the other alloy feeder;
(2) feeding electricity for arc striking, entering a slagging stage, wherein the time is 1.0-2 h, and the melting rate is 610-900 kg/h; after 10min after slagging begins, filling nitrogen into the furnace to increase the pressure in the furnace, setting the pressure to be 10-15 bar, and after the pressure reaches a set value, simultaneously adding two nitride alloy materials of silicon nitride and chromium nitride into the furnace by an alloy feeder at the rates of 2-6 kg/h and 3-10 kg/h respectively to achieve the aim of 0.25-0.45% of nitrogen in steel;
(3) in the normal smelting stage, parameters such as the pressure in the furnace, the adding speed of the nitriding alloy material, the melting speed and the like are kept stable;
(4) keeping the pressure in the furnace to be 10.0-15.0 bar stable in the filling stage;
(5) the electroslag ingot is 750mm phi or 930mm phi, and the electroslag ingot is cooled for 10 to 24 hours and then is sent to a processing plant;
the forging hot working comprises the following specific process steps:
(1) carrying out homogenization diffusion treatment on the steel ingot at 1200-1260 ℃, wherein the heat preservation time is 15-30 h, so that the element segregation in the steel ingot is homogenized;
(2) after diffusion treatment, cooling to 1180-1200 ℃ for forging production, controlling the finish forging temperature to be not lower than 980 ℃, preventing the temperature from reducing and generating cracks, and ensuring the surface quality of steel;
(3) multi-fire-time and multi-direction forging is adopted, one fire time, a clamp handle is pressed, and the surface is lightly pressed by the rolling reduction of 50 mm-80 mm, so that the surface of the steel ingot is flat; second heating, upsetting and lightly pressing the surface with a rolling reduction of 50-80 mm, flattening surface wrinkles caused by upsetting, and improving the isotropy of the steel; drawing out after three times of fire, wherein the drawing-out reduction amount is controlled to be 60-150 mm, and the finish forging temperature is controlled to be not lower than 1000 ℃ during drawing out;
(4) can realize the stable production of large-size forged materials with the thickness of 100 mm-500 mm and the width of 300 mm-900 mm;
the annealing heat treatment comprises the following specific process steps:
after forging, the steel is cooled in an air cooling or air cooling mode, and after the temperature is reduced to 100-300 ℃, the steel is loaded in a furnace for annealing treatment; the annealing temperature is 810-890 ℃, and the heat preservation time is 20-45 h; then cooling to 200-400 ℃ at a cooling speed of 20-50 ℃/h, and discharging to obtain uniform spherical pearlite structure.
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| CN114318109A (en) * | 2021-12-08 | 2022-04-12 | 抚顺特殊钢股份有限公司 | Method for smelting high-nitrogen die steel by using vacuum induction furnace and pressurized electroslag furnace |
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| SU1261964A1 (en) * | 1985-03-11 | 1986-10-07 | Институт проблем литья АН УССР | Method of producing nitrogen-containing die steel |
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