CN101302599A - Niobium microalloyed high strength hot work die steel and preparation thereof - Google Patents
Niobium microalloyed high strength hot work die steel and preparation thereof Download PDFInfo
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Abstract
The invention relates to niobium microalloyed high-strength hot working die steel, belonging to the alloy steel manufacturing process technical field. The compositions by weight percentage of the steel are: 0.3 to 0.6 percent of C, 0.1 to 0.5 percent of Si, 0.1 to 0.5 percent of Mn, 4.0 to 6.5 percent of Cr, 1.0 to 3.5 percent of Mo, 0.4 to 1.4 percent of V, 0.02 to 0.10 percent of Nb, less than 0.03 percent of P, less than 0.03 percent of S, and the balance being Fe. The process for preparing the hot working die steel comprises the following steps of: batching, smelting, secondary refining and electroslag remelting; homogenizing the mixture for 5 to 10 hours at a temperature of between 1210 and 1300 DEG C, and forging, annealing, quenching and tempering the mixture; heating up the mixture to a temperature of between 1000 and 1100 DEG C for austenization, after performing 'step heating' at a temperature of 650 DEG C and at a temperature of 800 DEG C, then performing secondary tempering to the processed mixture, and finally acquiring the hot working die steel. The die steel has the advantages of good thermal resistance, good thermal stability and good thermal fatigue performance.
Description
Technical field
The present invention relates to a kind of niobium microalloyed high strength hot work die steel and preparation method thereof, this die steel has high strength and high thermal stability, has good toughness and thermal fatigue property simultaneously concurrently, belongs to the steel alloy manufacturing process technology field.
Background technology
In the hot-work die steel field, the steel grade of domestic present widespread use has 5CrNiMo, 5CrMnMo, 3Cr2W8V and H13 steel.Because the particularity on work condition of hot-work die steel is also just very strict to the performance requriements of hot-work die steel.5CrNiMo and 5CrMnMo cause subsiding and the thermal wear under shock stress, thermal fatigue of working portion of die easily because its heat resistance is lower, and it is bigger to be not suitable for manufacturing dimension, the hot-work die that working temperature is higher.The 3Cr2W8V thermohardening is better, but its thermal fatigue resistance is poor, and mould often produces inefficacy because of be full of cracks takes place.The thermostability of H13 steel is not ideal enough, and use temperature can not be above 600 ℃.Therefore, the hot-work die steel of exploitation with high heat-intensity, high thermal stability and good thermal fatigue property has crucial meaning.
At present, niobium adds to as micro alloying element and has obtained in the structure iron very using widely and obtaining effect preferably, and the application of niobium in mould steel rarely has report.Because niobium has effects such as crystal grain thinning, precipitation strength and prevention grain growth, therefore, attempt in hot-work die steel that vanadium with the niobium instead of part carries out the reinforcement of steel and heat resistance and thermal fatigue property that malleableize improves steel are new ways.
The patent No. application in 1985 is 85100822, in the patent of patent " hot-work die steel " by name, the niobium add-on of 4Cr3Mo2NiVNb is 0.3%; The patent No. application in 2000 is 00117148.8, in the patent of patent " a kind of interalloy chromium series hot die steel " by name, the niobium add-on is 0.15%～0.3%; In addition, show in the document that the niobium add-on was less than 0.01% o'clock, the mechanical property of steel can not be significantly improved.In the process of Nb-microalloying, crucial problem is to control well the add-on of niobium.The niobium add-on is crossed at most and produce more macrobead pseudoeutectic carbide easily in the process of solidification of molten steel, has a strong impact on the impelling strength of steel, add-on very little, DeGrain then.The niobium add-on of steel of the present invention adopts 0.02%～0.1%, and the result shows that the heat resistance of steel, thermostability and thermal fatigue property are significantly improved, and a spot of pseudoeutectic carbide that forms can be eliminated by the method for high-temperature homogenization.
Under such technical background, the present invention has developed this by the method for Nb-microalloying and has had high heat-intensity, high thermal stability, has the good toughness and the hot-work die steel of thermal fatigue property simultaneously concurrently.This hot-work die steel not only can replace normal steels such as 3Cr2W8V and H13 steel under some occasion, fill a vacancy under the working conditions that can also be difficult to be competent at the steel grade of some current widespread use, as be used for precision forging die, forge the difficult part of forging such as stainless steel, valve.
Summary of the invention
The purpose of this invention is to provide a kind of high heat-intensity that has, the niobium microalloyed high strength hot work die steel of high thermal stability and good thermal fatigue property.
Another object of the present invention provides a kind of preparation method of niobium microalloyed high strength hot work die steel.
Hot-work die steel of the present invention is characterised in that to have following composition and weight percent:
C 0.3～0.6％， Si 0.1～0.5％，
Mn 0.1～0.5％， Cr 4.0～6.5％，
Mo 1.0～3.5％， V 0.4～1.4％，
Nb 0.02～0.10％， P ＜0.03％，
S＜0.03%, the Fe surplus.
The preparation method of above-mentioned niobium microalloyed high strength hot work die steel is characterized in that this method has following technological process and step:
A. melting and external refining: carry out electrosmelting or induction melting by above-mentioned alloying element proportioning, then carry out external refining;
B. esr: can carry out electroslag remelting before forging for demanding steel, common steel ingot then can directly forge after melting and refining,
C. high temperature homogeneity: at the macrobead pseudoeutectic carbide of niobium, the employing temperature is that 1210～1300 ℃ high temperature homogeneity technology is eliminated it, and the homogeneity time is 5～10h, to reach even as-cast structure, reduce segregation, eliminate the purpose of the pseudoeutectic carbide of niobium;
D. forge: above-mentioned steel ingot is forged processing in 1100～900 ℃ of temperature ranges;
E. annealing: annealing temperature is 820～860 ℃, and soaking time is 6～10h, cold speed of cooling＜100 of stove ℃/h;
F. the tempering heat treatment of quenching: adopt two sections preheating methods, carry out at 650 ℃, 800 ℃ " staged heating ", at 650 ℃ of insulation 1～5h, 800 ℃ of insulation 1～5h, then be heated to 1000～1100 ℃ and carry out austenitizing, insulation 1～5h (decide according to scantling and rate of heating above-mentioned concrete heat-up time in each stage), employing oil quenching or shrend; Carry out 600～650 ℃ of double temperings subsequently, each tempering time is 2～6h, thereby the niobium element of steel grade is effectively distributed.The niobium element solid solution of distribution 35～45% is in austenite; Distribute 55～65% niobium element Nb (C, N) in, thereby play the effect that stops grain growth, crystal grain thinning; The niobium element of distribution 5～10% is separated out from martensite in the process of secondary hardening, thereby plays the effect of dispersion-strengthened.
The theoretical foundation of its composition design of hot-work die steel of the present invention is as described below:
Main alloying element is Nb, Mo, V, Cr in the hot-work die steel of the present invention.Gap such as NbC or NbN intermediate phase can " pinning " on austenite grain boundary, stop austenite crystal to be grown up by separating out pinning mechanism, the solid solution niobium can produce intensive and pull the ability that crystal boundary moves because atomic radius is more much bigger than iron.Therefore, add the effect that an amount of niobium element can play crystal grain thinning and precipitation strength, thereby improve the intensity and the antifatigue softening performance of steel.The raising of molybdenum content can increase Mo
2The motivating force that C and MoC carbide form delays Mo
2C and MoC are to Mo
23C
6Change, thereby further improve the hot strength and the thermostability of material.And the raising of molybdenum content can increase the solubility product of Nb (C, N) in austenite, and a large amount of Nb is remained in the sosoloid, so that disperse is separated out in the ferrite of low-temperature transformation, produces higher precipitation strength effect.Add V element and the obvious age hardening effect can in the process of high tempering, occur, and reduce the superheated susceptivity of steel.The Cr solid solution helps to improve the stability of supercooled austenite in austenite, solid solution helps to improve martensitic resistance to tempering in martensite.
In addition, because the alloy degree that hot-work die steel of the present invention adopts is higher, therefore consider suitably to improve carbon content, to match with the high alloy degree.The high-carbon high-alloy degree has good effect for the heat resistance, thermostability and the thermal fatigue property that improve steel, but also can bring some adverse influences simultaneously, as forming macrobead pseudoeutectic carbide etc.For these disadvantageous effects, the present invention considers to adopt supporting thermal treatment process to be eliminated, as high-temperature homogenization.The result shows, adopt thermal treatment process of the present invention that hot-work die steel of the present invention is handled, can reduce the effect that reach high heat-intensity, high thermal stability and high thermal fatigue property under the situation of unfavorable factor effectively, this is the unusual part of the present invention just also.
Description of drawings
Fig. 1 is microstructure observation and the EDX analysis chart of hot-work die steel of the present invention (being called for short SDH8Nb) before and after the high temperature homogeneity.
(a) SDH8Nb as-cast microstructure before the high temperature homogeneity
(b) the pseudoeutectic carbide is eliminated back SDH8Nb as-cast microstructure
(c) SDH8Nb as-cast structure SEM observes before the high temperature homogeneity
(d) (c) 1. EDX energy spectrum analysis figure among the figure
Fig. 2 be hot-work die steel of the present invention (be called for short SDH8Nb) under 620 ℃ of conditions with the correlated thermostability figure of H13 steel.
Fig. 3 is the thermal fatigue property comparison diagram of hot-work die steel of the present invention (being called for short SDH8Nb) and H13 steel.
(a) thermal fatigue property of SDH8Nb
(b) thermal fatigue property of H13
Embodiment
Now specific embodiments of the invention are described in down.
In this example, adopt the moiety and the weight percent thereof of hot-work die steel as follows:
C?0.46％，Si?0.26％，Mn?0.45％，?Cr?4.48％，?Mo 2.88％，
V 0.56%, Nb 0.063% P 0.015%, and S 0.015%, the Fe surplus.
In the present embodiment, the technological process and the step of hot-work die steel are as follows:
A. induction melting: by above-mentioned alloying element proportioning melting in medium-frequency induction furnace, smelting temperature then is cast into Φ 80mm steel ingot and air cooling greater than 1500 ℃;
B. esr: above-mentioned steel ingot is put in the esr device as consumable electrode, carries out secondary refining; Utilize electric current to melt consumable electrode steel alloy mother metal by the electroslag layer heat that has a resistance, liquid metal is frozen into the about 70kg steel ingot of Φ 160mm more again with in the water mold of molten drop form below the slag blanket of slag bath falls to;
C. high temperature homogeneity: at the macrobead pseudoeutectic carbide of niobium, carry out the high temperature homogeneity at 1250 ℃ and handle, the homogeneity time is 6h, cold speed of cooling＜100 of stove ℃/h; To reach even as-cast structure, reduce segregation, eliminate the purpose of the pseudoeutectic carbide of niobium;
D. forge: above-mentioned steel ingot is forged in 1100～900 ℃ of temperature ranges, and draw out is square stock and the Φ 18mm of 60mm * 60mm;
E. annealing: the bar of 60mm * 60mm square stock and Φ 18mm is put into process furnace together anneal, annealing temperature is 830 ℃, and soaking time is 8h, and stove is chilled to 300 ℃ of left and right sides air coolings then, cold speed of cooling＜100 of stove ℃/h;
F. the tempering of quenching: adopt two sections preheating methods, carry out at 650 ℃, 800 ℃ " staged heating ", at 650 ℃ of insulation 2h, at 800 ℃ of insulation 2h, then be heated to 1060 ℃ and carry out austenitizing, insulation 1h, carry out 610 ℃ of double temperings behind the oil quenching, each tempering 2h.
Heat stability test: adopt the thermal treatment process of 1060 ℃ of+610 ℃ of double temperings that quench that hot-work die steel of the present invention is handled, adopt the thermal treatment process of 1100 ℃ of+600 ℃ of double temperings that quench that the H13 steel is handled, the two hardness all is adjusted to about 51.5HRC.Be incubated 2h, 4h, 6h, 9h, 12h, 15h, 20h respectively at 620 ℃.
Implementation result: hot-work die steel of the present invention (be called for short SDH8Nb) heat resistance is good, Heat stability is good, and under 20 hours conditions of 620 ℃ of insulations, the high 5HRC of hardness ratio H13 steel; This material is after circulation under 700 ℃ of conditions 3000 times, and crackle is still tiny and be net distribution, and thermal fatigue property is good.
The effect of high temperature homogeneity: the microstructure of SDH8Nb is shown in accompanying drawing 1 (a) before the high temperature homogeneity, as seen there is oarse-grained pseudoeutectic carbide in the place, grain boundary in the steel, analyze as can be known through SEM observation and EDX, this carbide is mainly the carbide of Nb, V, Mo, shown in accompanying drawing 1 (c), (d).Because the solid solubility temperature of Nb, V is higher, generally between 1150 ℃～1300 ℃, therefore, the present invention considers under the unlikely local little molten situation that causes steel, improve the temperature of homogeneity as far as possible, thereby more Nb, V are solidly soluted in the matrix, finally selected 1250 ℃ to carry out the high temperature homogeneity.After insulation under 1250 ℃ of conditions, the microstructure of SDH8Nb is shown in accompanying drawing 1 (b), and the result shows, macrobead pseudoeutectic carbide behind the high-temperature homogenization in the steel is basically eliminate, can reach uniform formation, reduce segregation, eliminate the purpose of pseudoeutectic carbide.
Performance test:
Quenching hardness: 60.9HRC
Tempered-hardness: 52.0HRC
Room temperature notched bar impact strength: 25J/cm
2(specimen size is 7mm * 10mm * 55mm, opens U type breach, and U type groove is opened on the plane of 10mm * 55mm)
Thermostability:
Carry out the thermostability simultaneous test of hot-work die steel of the present invention and H13 steel under 620 ℃ of conditions, test-results as shown in Figure 2.By accompanying drawing 2 as seen, when under 620 ℃ of conditions, carrying out heat stability test, after 600 ℃ of tempered H13 of 1100 ℃ of quench hots steel insulation 20 hours, hardness has been low to moderate below the 35HRC, and hot-work die steel of the present invention quenches after 610 ℃ of tempering insulations 20 hours through temperature in 1060 ℃, but than the high 5HRC of H13, thermostability obviously is better than the H13 steel to hardness.
Thermal fatigue property:
After circulation under 700 ℃ of conditions 3000 times, the thermal fatigue surface topography (as shown in Figure 3) of observing hot-work die steel of the present invention and H13 steel as seen, long thick crackle has appearred in the surface of H13 steel, is the cracking state, the crackle of hot-work die steel of the present invention is then more tiny, is netted.According to formula D=Ds * Dd, Ds=A * W/L, Dd=P * d
Max/ d
5A, it is as shown in table 1 that utilization thermal fatigue damage factor software for calculation calculates the two thermal fatigue damage factor.Wherein, Ds is a surface factor, and Dd is a depth factor, and A is the crackle area percentage, and W is the wideest crack size, and L is the crackle total length, and P is the crack depth area percentage, d
MaxBe the deep torn grain degree of depth, d
5ABe crackle the last 5 mean depth.Damage factor by the visible hot-work die steel of the present invention of table 1 only is 1/2 of a H13 steel, and this has shown that more fully hot-work die steel of the present invention has the thermal fatigue property better than H13 steel.
The thermal fatigue damage factor contrast table of table 1SDH8Nb and H13 steel
Claims (2)
1. niobium microalloyed high strength hot work die steel, the chemical ingredients and the weight percent that it is characterized in that this steel are: C 0.3～0.6%, Si 0.1～0.5%, and Mn 0.1～0.5%, and Cr 4.0～6.5%, Mo 1.0～3.5%, V 0.4～1.4%, and Nb 0.02～0.10%, P＜0.03%, S＜0.03%, the Fe surplus.
2. preparation method who is used for as claims 1 described niobium microalloyed high strength hot work die steel is characterized in that this method has following technological process and step:
1) press the chemical ingredients and the weight percent of niobium microalloyed high strength hot work die steel: C 0.3～0.6%, Si 0.1～0.5%, and Mn 0.1～0.5%, and Cr 4.0～6.5%, Mo 1.0～3.5%, V 0.4～1.4%, and Nb 0.02～0.10%, P＜0.03%, S＜0.03%, the Fe surplus, batching, melting and external refining, esr then;
2) high temperature homogeneity: the homogeneity temperature is 1210～1300 ℃, and the homogeneity time is 5～10h; Forge then, annealing: annealing temperature is 820～860 ℃, and soaking time is 6～10h, cold speed of cooling＜100 of stove ℃/h;
3) Q-tempering thermal treatment: adopt two sections preheating methods, at 650 ℃ of insulation 1～5h, 800 ℃ of insulation 1～5h then are heated to 1000～1100 ℃ and carry out austenitizing, and insulation 1～5h adopts oil quenching or shrend; Carry out 600～650 ℃ of double temperings subsequently, each tempering time is 2～6h.
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