CN105603330B - The antifatigue Valve Steel Bar Wire Product of fine grain and its manufacturing method - Google Patents

The antifatigue Valve Steel Bar Wire Product of fine grain and its manufacturing method Download PDF

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CN105603330B
CN105603330B CN201610033981.9A CN201610033981A CN105603330B CN 105603330 B CN105603330 B CN 105603330B CN 201610033981 A CN201610033981 A CN 201610033981A CN 105603330 B CN105603330 B CN 105603330B
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temperature
valve steel
antifatigue
refining
pickling
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CN105603330A (en
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莫燕
王东哲
吴畏
刘海定
张志国
万红
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Chongqing Materials Research Institute Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/54—Ferrous alloys, e.g. steel alloys containing chromium with nickel with boron
    • 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
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/004—Heat treatment of ferrous alloys containing Cr and Ni
    • 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
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/005—Heat treatment of ferrous alloys containing Mn
    • 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
    • C21D8/06—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/48—Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working

Abstract

The present invention relates to the antifatigue air valve Steel material of fine grain, the material elements such as including Ni, Cr, Ti, Al, Mo, Nb, Mn, C, B, Mg, Zr, N, Y, Fe.Invention passes through crystal grain thinning, improve Valve Steel plasticity, using the cold-drawing process of simple and effective, further crystal grain thinning, improve about 6 10% plasticity index, be conducive to the molding of valve electricity pier, this Valve Steel is made to disclosure satisfy that high intensity and repeatedly antifatigue requirement Scouring Condition under of the valve under 780 950 DEG C of high temperature harshness working environments.Experiments verify that material at high temperature rotary bending fatigue function admirable of the present invention；High temperature creep can be shown that there is material of the present invention enough creep strengths to fail to prevent air-stop gate.

Description

The antifatigue Valve Steel Bar Wire Product of fine grain and its manufacturing method
Technical field
The invention belongs to Material Field, the antifatigue Valve Steel Bar Wire Product of more particularly to a kind of fine grain and its manufacturing method.
Background technology
Valve Steel refers exclusively to the alloy material for manufacturing engine charge, air bleeding valve, need in high temperature, high pressure, height wash away, be high Work under the conditions of burn into high-frequency, since operating condition is severe, to the plasticity of material, fatigue behaviour, elevated temperature strength, thermohardening, Wearability, corrosion resistance etc. require very high so that the manufacture of Valve Steel and production are with very strong professional.In the life of Valve Steel During production, due to Valve Steel hardness height itself, the features such as plasticity is low, and processing hardening is apparent, make the production and processing of Valve Steel compared with For difficulty.
Valve Steel production at present mainly through rolling, being dissolved, uncoiling, aligning, polishing be air valve section bar.Due in production process Middle rolling blank dimensional tolerance is larger, and especially its circularity is far from meeting valve production requirement.Usual solution is to increase Add billet size, increase final pass surface stock removal, this has been resulted in, and utilization rate of raw materials is relatively low, and production cost is high to be lacked Point.Especially to small dimension (Φ≤8mm) material, on the one hand, since finishing temperature limits, hot-roll forming is extremely difficult, surface matter Amount is poor, on the other hand, grinding allowance need to be further increased, to ensure dimensional tolerance and surface quality.Solve having for blank circularity One of efficacious prescriptions method is to carry out warm drawing, however this technological requirement drawing equipment has heating function, while must strictly carry out Temperature controls, the ageing treatment that otherwise will cause Valve Steel, aggravates product hardening, increases valve molding difficulty.In this context, Cold-drawing process shows huge potentiality since equipment requirement is low, small investment, circularity are good in terms of steel sectional material of air valve preparation. But it should also be mentioned that the characteristics of due to air valve Steel material itself, cold-drawing process is two big difficult it is still necessary to overcome：Plasticity is low, Pass deformation cannot be too big, is otherwise easily broken in drawing process；Processing hardening is apparent, need to repeatedly be tempered to eliminate processing Internal stress, energy consumption is big, and working hour is long.
Invention content
The object of the present invention is to provide a kind of high-strength, antioxidant iron-nickel alloy air valve Steel material of microalloying and preparations Method.The present invention improves Valve Steel plasticity, using the cold-drawing process of simple and effective, further refinement is brilliant by crystal grain thinning Grain improves about 6-10% plasticity index, is conducive to the molding of valve electricity pier, this Valve Steel is made to disclosure satisfy that valve at 780-950 DEG C High intensity and the antifatigue requirement under Scouring Condition repeatedly under high temperature harshness working environment.Experiments verify that material of the present invention High Temperature Rotating fatigue property is excellent；High temperature creep can be shown that there is material of the present invention enough creep strengths to prevent gas Door failure.
The technical scheme is that：
A kind of antifatigue air valve Steel material of fine grain, the weight percentage of the material each component are：Ni 25.0- 36.0%；Cr 14.0-20.0%；Ti 1.9-3.0%；Al 0.5-2.6%；Mo 0.7-1.2%；Nb 0.4-0.7%；Mn 0.2-1.0%；C 0.02-0.1%；B 0.003-0.015%；Mg 0.01-0.3%；Zr 0.001-0.04%；N 0.01- 0.1%；Y 0.001-0.05%；Surplus be Fe and impurity, wherein the total amount of impurity be≤0.1%, the impurity for Cu, Si, S, P, respective weight percentage are Cu≤0.01%；Si≤0.1%；S≤0.005%；P≤0.002%,.
Preferable technical solution is that the weight percentage of material each component of the present invention is：Ni 32.5%；Cr 14.55%；Ti 2.86%；Al 1.75%；Mo 0.77%；Nb 0.56%；Mn 0.36%；C 0.027%；B 0.0073%；Mg 0.042%；Zr 0.03%；N 0.08%；Y 0.03%；Surplus is Fe and impurity.
The preparation method of the antifatigue air valve Steel material of fine grain, there is following steps：
1) electrode bar is prepared
Proportioning according to the above-mentioned antifatigue air valve Steel material of fine grain takes the proportioning of each component to take each component, drying；It will Ni, Cr, Fe, Nb, C are warming up to aniseed thawing, then carry out first time refining, refine power as aniseed under vacuum condition 500kw, refining time 60min, refining latter stage vacuum degree≤3Pa；Ti, Al, Mo, B, Zr, N, Y conduct are added in argon gas atmosphere Small powder is warming up to small powder thawing；Vacuum degree≤3Pa carries out second and refines, refines power 500kw, refining time 50min；Essence After refining, Mg, Mn are added in, stirs 5min, temperature adjustment is 1500~1600 DEG C, is cast into electrode bar；
2) electroslag remelting
It is CaF by slag system proportioning2：Al2O3：CaO：MgO=65：15:12:8 electroslag slag charge melts, described in step 1) Electrode bar puts remelting in slag charge into, obtains ESR ingot；
3) hammer cogging
1100-1180 DEG C of heat preservation 2-3h of ESR ingot that step 3) obtains, 1000-1050 DEG C of starting forging temperature, multi-pass tempering, 830-960 DEG C of final forging temperature, is swaged into square billet；
4) hot rolling
Square billet hot rolling, 1080-1150 DEG C of start rolling temperature, 830-960 DEG C of holding temperature, 880-980 DEG C of finishing temperature, rolling For round billet；
5) softening heat treatment
Round billet holding temperature is 1050 DEG C, soaking time 1-2h, water cooling to room temperature；
6) soda boiling, pickling
Round billet after softening heat treatment, at 480-550 DEG C, boils 0.5-1h with soda boiling liquid；Pickle room temperature pickling 20- 40min；
7) cold drawing
Round billet drawing through step 6) soda boiling, pickling, drawing speed 12m/min, pass deformation 10-15% are total to become Shape amount is 30-60%；
8) solid solution, ageing treatment
It will be dissolved by the wire and rod of cold drawing, the antifatigue air valve Steel material of fine grain obtained after ageing treatment, Middle solution treatment is：1050-1100 DEG C of heat preservation 1-2h, water cooling or oil cooling；Ageing treatment is 720-760 DEG C of heat preservation 4-16h.
When the step 1) aniseed all melts, vacuum degree≤20Pa, refining period vacuum degree≤3Pa.
During the step 2) remelting, electrode bar is controlled with crystallizer packing ratio in 0.5-0.8, melting current 6-10kA, Remelting voltage is 40-60V.
Step 6) soda boiling liquid NaOH：Mass ratio=60 of NaCl:40, H in pickling2SO4：HNO3：HF：H2The mass ratio of O is =15:20:10:55.
Crystal grain refinement is the effective means that can improve material plasticity and improve intensity, while to fatigue of materials performance It is highly beneficial thus advantageous to the production and comprehensive performance of Valve Steel.The present invention is by adding the elements such as Zr, N, Y, conducive to this hair Bright Valve Steel crystal grain refinement improves its plasticity while air valve hardness of steel is ensured.The present invention prepares circularity using cold-drawing process Valve Steel good, dimensional accuracy is high, total deformation degree are up to 50%, and processing hardening improves, and are not required between drawing passes by softening heat Processing, energy saving and working hour improve yield rate 8%, especially suitable for the Valve Steel of the present invention, especially small dimension (diameter Φ≤12, it is more excellent be Φ≤8mm) Valve Steel Bar Wire Product production.
The present invention improves Valve Steel plasticity by crystal grain thinning.The micro alloying elements such as Zr, N and Y are added in steel, Conducive to crystal grain refinement.
Wherein Zr easily forms carbide, plays solution strengthening effect, while can hinder crystal boundary migration, crystal grain thinning.Zr contents In 0.001-0.04%, Zr lower limits are 0.001% for control, and preferred upper limit control is 0.03%；
N primarily forms nitride, such as TiN, and nitride is high with alloy substrate mismatch, can reduce ingot casting dendrite distance, Reduce macro-grain size, carbide size is made to become smaller, is more evenly distributed, while can also make base phase stabilizer, play solution strengthening Effect.N content control is controlled in 0.01-0.1%, the preferred upper limit 0.08%.
Y is easy to O in smelting process and has an effect, and forms oxide particle, on the one hand has the function of deoxygenation, the opposing party The dispersed oxide phase stability that face is formed is good, plays the role of intercrystalline strengthening, while crystal grain thinning, improves Valve Steel plasticity, But too high levels can form YAl with Al2, it is enriched in crystal boundary, it is prone to which cleavage fracture deteriorates alloy property, thus its content Control is controlled in 0.001-0.05%, the preferred upper limit 0.03%.
The present invention uses the cold-drawing process of simple and effective, and further crystal grain thinning makes this Valve Steel disclosure satisfy that valve High intensity, antifatigue requirement under high temperature harshness working environment.Its manufacturing method is to carry out softening heat treatment to hot-rolled profile, To eliminate hot rolling hardening；Soda boiling pickling processes are carried out, to remove the oxide skin of surface attachment；It carries out lime white coating, dry Roasting processing, covers lubrication in order to which lubricant buries；Cold drawing processing is carried out, to obtain moderate finite deformation amount and preferable circularity, same to time control Grinding allowance processed；Dynamic recrystallization treatment is carried out, to eliminate crystal grain deformation and processing hardening；Uncoiling, aligning, polishing processing are carried out, Obtain Valve Steel finished product.Trimmed size Φ≤12mm, pass deformation >=15%, total deformation >=50%.
Specific embodiment
Proportioning, takes each component of the present invention, material of the present invention is prepared as follows as described in table 1：
1 chemical component table of table (wt%)
Note：Comparative example is commercially available air valve steel alloy material Ni 30.
1) electrode bar is prepared
Above-mentioned each component is taken according to proportioning described in table 1, is dried and is kept the temperature 4h in 200 DEG C and preheated, dry steam.By Ni, Cr, Fe, Nb, C are packed into furnace crucible as aniseed, vacuumize power transmission, are continuously improved with vacuum degree, slowly promote power transmission power. After vacuum degree is better than 20Pa, power is increased to 650kw until all thawings of whole aniseed, then carry out first time refining, essence Downlink power 500kw, refining time 60min, refining latter stage vacuum degree are better than 3Pa.It is added in argon gas atmosphere after refining small Expect Ti, Al, Mo, B, Zr, N, Y, increased wattage to 650kw makes small powder all melt again, when vacuum degree is better than carrying out the after 3Pa Double refining refines power 500kw, refining time 50min.After refining, Mg, Mn are added in, stirs 5min, then sampling point Analysis, temperature adjustment is 1500~1600 DEG C after ingredient qualification, is cast into 200 electrode bars of Φ.Electrode bar surface need to carry out sand milling finishing, To remove descale.Vacuum breaker, all kinds of material do not add in whole process in batches, at times, to ensure that good degassing, decontamination are imitated Fruit.
2) electroslag remelting
By electroslag slag charge, (slag system matches CaF2：Al2O3：CaO：MgO=65:15:12:8) electric arc slugging, with preparing Electrode bar carries out electroslag remelting.Electrode bar is controlled with crystallizer packing ratio in 0.5-0.8, and melting current control is in 6-10kA, weight Molten voltage control is in 40-60V.Electroslag slag charge can further desulfurization dephosphorization, by objectionable impurities content control in extremely low level
3) hammer cogging
ESR ingot hammer cogging, at 1100-1180 DEG C, soaking time is controlled in 2-3h for holding temperature control, opens forging temperature 1000-1050 DEG C of degree, 830-960 DEG C of final forging temperature are swaged into Φ 95mm round billets, and centre can multi-pass tempering.Again through common forging 45 45mm square billets finally are swaged into, so that subsequent hot rolled is used.
4) hot rolling
Hot rolling heat holding temperature is consistent with forging holding temperature.880-980 DEG C of finishing temperature of 1080-1150 DEG C of start rolling temperature； Rolling specs are required according to final products size, can be Φ 16,15.... until minimum Φ 8.
5) softening heat treatment
The purpose of softening heat treatment is to eliminate processing hardening caused by hot rolling, drawing process, in favor of material of the present invention Be again deformed.Softening heat treatment holding temperature is 1050 DEG C, and soaking time 1-2h, the type of cooling is water cooling.
6) soda boiling, pickling
Soda boiling formula is NaOH：NaCl=60:40,480-550 DEG C of soda boiling temperature, soda boiling time 0.5-1h；Pickling formula For H2SO4：HNO3：HF：H2O=15:20:10:55, room temperature pickling, pickling time 20-40min.
7) cold drawing
Drawing speed 12m/min, pass deformation control are controlled in 10-15%, total deformation in 30-60%, obtain line Bar.Intermediate View drawing sclerotic conditions increase a softening heat treatment process.
8) solid solution, ageing treatment
It will be dissolved by the wire and rod of cold drawing, the high-strength, antioxidant iron nickel of microalloying obtained after ageing treatment Alloy air valve Steel material, wherein solution treatment are：1050-1100 DEG C of heat preservation 1-2h, water cooling or oil cooling；Ageing treatment is 720- 760 DEG C of heat preservation 4-16h.
9) aligning, scale blanking, polishing
Product is aligned after service check qualification, scale blanking, and length is controlled in 3-4m, and it is coarse to polish rear surface It spends Ra and is better than 2.0 μm.
The specification of Φ 8.0mm is made with wire and rod of the present invention, does following measuring and calculating and experiment：
If direct hot-roll forming, it is contemplated that the factors such as circularity, surface defect, it is hot rolled after billet size need to be relaxed to Φ 8.6mm could be polished as Φ 8.0mm finished products, grinding rate：
According to hot rolling+cold drawing molding, billet size only needs Φ 8.2mm, you can polishes as Φ 8.0mm finished products, grinding Rate：
It can be seen that yield rate about 8% can be improved using the wire and rod method of material preparation of the present invention.
With reference to influence of the drawing deformation amount to material property, the rolling of blank of the embodiment of the present invention is Φ 12.0mm, compared Φ 8.0mm are after same softening heat treatment for example, plasticity index and grain size such as table 2.
Plasticity index after 2 softening heat treatment of table
Material Elongation percentage/% The contraction percentage of area/% Grain size/grade
Embodiment (Φ 12.0) 40 66 9.0
Comparative example (Φ 8.0) 32 54 7.5
Embodiment (12.0 cold drawings of Φ to Φ 8.2) 46 73 10.0
As a result：It is shown in Table 2.Rolled-section is from Φ 12.0mm points of 4 passages in embodiment, respectively cold drawing to Φ 10.7, 9.7th, 8.9 and 8.2mm, without sofening treatment between each passage, each pass deformation is respectively 20.5%, 17.8%, 15.8%th, 15.1%, total deformation 53.3%.Then pass through with the same softening heat treatment of comparative example, measure its elongation percentage and disconnected Face shrinking percentage, by cold drawing, the crystal grain of embodiment is further refined, and plasticity index further improves.Meanwhile the present invention In the material, the micro alloying elements such as Zr, N, Y make grain size increase by 1.5 grades, and plasticity index is apparently higher than comparative example.
With reference to valve operation condition, solid-solution and aging heat treatment is carried out to Valve Steel, tests its room-temperature mechanical property such as table 3.
Mechanical property after 3 solid-solution and aging heat treatment of table
As a result：Valve Steel good mechanical performance of the present invention, meanwhile, Zr, N, the microalloying of Y element and cold-drawn are pulled out at technique Reason, not only makes crystal grain refinement, also enhances mechanical property, plasticity index greatly improves.
After the present embodiment, comparative example are carried out identical solid-solution and aging heat treatment, implement under the conditions of 750 DEG C, 150 MPa Creep rupture is tested, and implements High Temperature Rotating crooked fatigue experiment under the conditions of 800 DEG C, 250MPa, and experimental result is shown in Table 4.
4 high-temerature creep of table and rotary bending fatigue experiment
As a result：The creep Resisting fractre time showing of the present embodiment under experimental conditions is longer than comparative example, at high temperature Excellent.Due to the high temperature of valve operation condition, high frequency characteristics, the fatigue behaviour of air valve Steel material is even more important.By comparing It is found that the present embodiment is compared to comparative example, fatigue strength higher, high-temperature behavior is more excellent.
In conclusion Valve Steel wire and rod room temperature of the present invention, having excellent high-temperature strength, pass through Zr, N, the microalloying of Y element And process is pulled out in cold-drawn, is refined crystal grain, mechanical property enhancing, especially plasticity index greatly improves, fatigue fracture Number increases, and fatigue behaviour is excellent, can slow down crackle, increases the valve operation service life, and compared to common hot-roll forming skill Art lumber recovery higher, it is highly beneficial in terms of improving engine performance, saving cost.

Claims (6)

1. a kind of antifatigue air valve Steel material of fine grain, it is characterised in that：The weight percentage of the material each component is：Ni 25.0-36.0%；Cr 14.0-20.0%；Ti 1.9-3.0%；Al 0.5-2.6%；Mo 0.7-1.2%；Nb 0.4- 0.7%；Mn 0.2-1.0%；C 0.02-0.1%；B 0.003-0.015%；Mg 0.01-0.3%；Zr 0.001- 0.04%；N 0.01-0.1%；Y 0.001-0.05%；Surplus is Fe and impurity, and the wherein total amount of impurity is≤0.1%, institute Impurity is stated as Cu, Si, S, P, respective weight percentage is Cu≤0.01%；Si≤0.1%；S≤0.005%；P≤ 0.002%；The air valve Steel material is made using following preparation method：
1) electrode bar is prepared
Proportioning according to the antifatigue air valve Steel material of the fine grain takes each component, drying；Using Ni, Cr, Fe, Nb, C as big Expect, aniseed thawing is warming up under vacuum condition, then carries out first time refining, refine power 500kw, refining time 60min, it is smart Refine latter stage vacuum degree≤3Pa；Ti, Al, Mo, B, Zr, N, Y are added in argon gas atmosphere as small powder, is warming up to small powder thawing；Very Reciprocal of duty cycle≤3Pa carries out second and refines, refines power 500kw, refining time 50min；After refining, Mg, Mn are added in, is stirred 5min is mixed, temperature adjustment is 1500~1600 DEG C, is cast into electrode bar；
2) electroslag remelting
It is CaF by slag system proportioning2：Al2O3：CaO：MgO=65：15:12:8 electroslag slag charge fusing, the electrode described in step 1) Stick puts remelting in slag charge into, obtains ESR ingot；
3) hammer cogging
1100-1180 DEG C of heat preservation 2-3h of ESR ingot that step 3) obtains, 1000-1050 DEG C of starting forging temperature, multi-pass tempering, finish-forging 830-960 DEG C of temperature, is swaged into square billet；
4) hot rolling
Square billet hot rolling, 1080-1150 DEG C of start rolling temperature, 830-960 DEG C of holding temperature, 880-980 DEG C of finishing temperature are rolled as circle Base；
5) softening heat treatment
Round billet holding temperature is 1050 DEG C, soaking time 1-2h, water cooling to room temperature；
6) soda boiling, pickling
Round billet after softening heat treatment, at 480-550 DEG C, boils 0.5-1h with soda boiling liquid；Pickle room temperature pickling 20-40min；
7) cold drawing
Round billet drawing through step 6) soda boiling, pickling, drawing speed 12m/min, pass deformation 10-15%, total deformation For 30-60%；
8) solid solution, ageing treatment
It will be dissolved by the wire and rod of cold drawing, the antifatigue air valve Steel material of fine grain obtained after ageing treatment, wherein solid Molten processing is：1050-1100 DEG C of heat preservation 1-2h, water cooling or oil cooling；Ageing treatment is 720-760 DEG C of heat preservation 4-16h.
2. material according to claim 1, it is characterised in that：The weight percentage of the material each component is：Ni 32.5%；Cr 14.55%；Ti 2.86%；Al 1.75%；Mo 0.77%；Nb 0.56%；Mn 0.36%；C 0.027%；B 0.0073%；Mg 0.042%；Zr 0.03%；N 0.08%；Y 0.03%；Surplus is Fe and impurity.
3. the preparation method of the antifatigue air valve Steel material of fine grain, which is characterized in that have following steps：
1) electrode bar is prepared
Proportioning according to the antifatigue air valve Steel material of fine grain described in claims 1 or 2 takes each component, drying；By Ni, Cr, Fe, Nb, C are warming up to aniseed thawing, then carry out first time refining as aniseed under vacuum condition, refine power 500kw, essence Refine time 60min, refining latter stage vacuum degree≤3Pa；Ti, Al, Mo, B, Zr, N, Y are added in argon gas atmosphere as small powder, is risen Temperature to small powder melts；Vacuum degree≤3Pa carries out second and refines, refines power 500kw, refining time 50min；Refining terminates Afterwards, Mg, Mn are added in, stirs 5min, temperature adjustment is 1500~1600 DEG C, is cast into electrode bar；
2) electroslag remelting
It is CaF by slag system proportioning2：Al2O3：CaO：MgO=65：15:12:8 electroslag slag charge fusing, the electrode described in step 1) Stick puts remelting in slag charge into, obtains ESR ingot；
3) hammer cogging
1100-1180 DEG C of heat preservation 2-3h of ESR ingot that step 3) obtains, 1000-1050 DEG C of starting forging temperature, multi-pass tempering, finish-forging 830-960 DEG C of temperature, is swaged into square billet；
4) hot rolling
Square billet hot rolling, 1080-1150 DEG C of start rolling temperature, 830-960 DEG C of holding temperature, 880-980 DEG C of finishing temperature are rolled as circle Base；
5) softening heat treatment
Round billet holding temperature is 1050 DEG C, soaking time 1-2h, water cooling to room temperature；
6) soda boiling, pickling
Round billet after softening heat treatment, at 480-550 DEG C, boils 0.5-1h with soda boiling liquid；Pickle room temperature pickling 20-40min；
7) cold drawing
Round billet drawing through step 6) soda boiling, pickling, drawing speed 12m/min, pass deformation 10-15%, total deformation For 30-60%；
8) solid solution, ageing treatment
It will be dissolved by the wire and rod of cold drawing, the antifatigue air valve Steel material of fine grain obtained after ageing treatment, wherein solid Molten processing is：1050-1100 DEG C of heat preservation 1-2h, water cooling or oil cooling；Ageing treatment is 720-760 DEG C of heat preservation 4-16h.
4. according to the method described in claim 3, it is characterized in that：When the step 1) aniseed all melts, vacuum degree≤ 20Pa, refining period vacuum degree≤3Pa.
5. according to the method described in claim 3, it is characterized in that：During the step 2) remelting, electrode bar is filled with crystallizer Than controlling in 0.5-0.8, melting current 6-10kA, remelting voltage is 40-60V.
6. according to the method described in claim 3, it is characterized in that：Step 6) soda boiling liquid NaOH：Mass ratio=60 of NaCl: 40, H in pickling2SO4：HNO3：HF：H2The mass ratio of O is=15:20:10:55.
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