CN111394640A - Iron-nickel gas valve alloy and preparation method thereof - Google Patents
Iron-nickel gas valve alloy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an iron-nickel gas valve alloy, which comprises the following components in percentage by weight: c: 0.03-0.15%, less than or equal to 0.50% of Si, less than or equal to 0.50% of Mn, 20-28% of Cr, Ni: 25-35%, S is less than or equal to 0.040%, P is less than or equal to 0.040%, Mo: 0.30-1.20%, V is less than or equal to 0.80%, Cu is less than or equal to 0.50%, Al: 1.20-2.50%, Ti: 2.00-3.00%, Nb: 0.20-1.00 percent of Ce, less than or equal to 0.012 percent of Zr, less than or equal to 0.05 percent of Zr, and the balance of Fe and inevitable impurities. Aiming at the defect of low hardness of the existing iron-nickel alloy aging treatment, Cr and Ni elements are used as main matrix solid solution strengthening elements and precipitation dispersion strengthening phases such as Al, Ti, Mo, V, Nb and the like are adopted by adjusting component elements, so that the iron-nickel alloy with high temperature performance similar to NCF751 at 750 ℃ and higher hardness than the common iron-nickel alloy can be prepared.
Description
Technical Field
The invention relates to structural steel for cold forging, in particular to an iron-nickel gas valve alloy and a preparation method thereof.
Background
With the rapid development of the automobile industry in China in recent years, the emission standard of automobiles is continuously improved, and the emission standard is improved from the national V to the national VI standard. In order to reduce the emission concentration, oil and gas in an engine must be fully combusted, particularly the general application of a vortex supercharging technology, the combustion temperature of the engine is generally increased, more strict requirements are put on the material of an exhaust valve, the service temperature of the exhaust valve is high (650 plus 850 ℃), the pressure bearing capacity of a valve disc and a neck part of the air valve is high, and the high-temperature gas corrosion is serious, so that the common austenite valve steel (21-4N and 21-4NWNb) cannot bear, even if the hollow valve technology of 21-4NWNb is adopted.
At present, Inconel751 and Nimonic80A are materials with better high-temperature performance than austenitic gas valve steel in the gas valve alloy standard in the world, and due to the high alloy content and high manufacturing cost of the alloys, economic gas valve alloy research is carried out in various countries. For example, a more used Fe — Ni alloy (3015) is available abroad, and the percentage composition is as follows: c is less than or equal to 0.08
P≤0.015、Ni30-30.5、Cr13.5-15.5、Ti2.30-2.90、Al1.6-2.20、
Mn is less than or equal to 0.50, Si is less than or equal to 0.50, MoO.40-1.0 and Nb0.40-0.90. However, the Fe-Ni alloy has weak points, the alloy has low hardness after aging treatment, and the valve is produced to improve the hardness. And hard alloy surfacing on the conical surface of the valve is required.
The publication number is CN1453458A, and the invention name is: a diesel oil double-metal exhaust valve of a diesel locomotive and a manufacturing method thereof are disclosed, wherein the patent comprises the following components: 0.04-0.15%, Si: 0.40-1.20%, Mn: 0.50-1.0%, Cr: 20-24%, Ni: 38-40%, Ti: 2.5-3.0%, Al: 0.60-1.20%, Nb: 0.40-1.20%, V: 0.01-0.20%, W: 0.60-0.80%.
The publication number is CN105543713A, and the invention name is: a microalloyed high-strength oxidation-resistant iron-nickel alloy air valve steel material and a preparation method thereof, which disclose the following components: c: 0.02 to 0.10%, Mn: 0.20-1.0%, Cr: 14-20%, Ni: 25-36%, Ti: 1.9-3.0%, Al: 0.50-2.60%, Nb: 0.40-0.70%, No: 0.70-1.20%.
The related patents of the iron-nickel alloy relate to the application field of engine valves, in CN1453458A, the content of nickel is 38-40%, the cost is higher, the cost of added W is high, and certain solid solution strengthening exists, but W can form particularly hard and particularly stable carbide to influence the machinability of the material; in CN105543713A, the Cr content is 14-20% and relatively low, and the Cr content is poor in oxidation resistance and corrosion resistance, so that the high hardness, the toughness and the corrosion resistance are difficult to achieve, and the Cr content is well matched with the low cost.
Disclosure of Invention
The invention aims to provide an iron-nickel gas valve alloy and a preparation method thereof, wherein through the adjustment of component elements, chromium and nickel elements are used as main matrix solidifying elements and precipitation dispersion strengthening phases such as aluminum, titanium, molybdenum, vanadium, niobium and the like are adopted, the iron-nickel gas valve alloy has high temperature performance similar to Inconel751 at 750 ℃, the hardness of the material is higher after aging heat treatment, the alloy can not be subjected to surfacing welding, and the high temperature corrosion resistance is more ideal.
In order to achieve the above object, the present invention adopts the following technical solutions.
In one aspect, an iron-nickel valve alloy comprises, by weight:
c: 0.03-0.15%, less than or equal to 0.50% of Si, less than or equal to 0.50% of Mn, 20-28% of Cr, Ni: 25-35%, S is less than or equal to 0.040%, P is less than or equal to 0.040%, Mo: 0.30-1.20%, V is less than or equal to 0.80%, Cu is less than or equal to 0.50%, Al: 1.20-2.50%, Ti: 2.00-3.00%, Nb: 0.20-1.00 percent of Ce, less than or equal to 0.012 percent of Zr, less than or equal to 0.05 percent of Zr, and the balance of Fe and inevitable impurities.
In another aspect, a method for preparing an iron-nickel gas valve alloy comprises the following steps:
s1, proportioning according to chemical components of a gas valve alloy, smelting in a vacuum induction furnace, and then casting into a steel ingot;
s2, placing the steel ingot serving as a consumable electrode in an electroslag remelting device for electroslag remelting, washing liquid metal into a water-cooled crystallizer through slag bath slag, and solidifying the liquid metal into the steel ingot again;
s3, heating the steel ingot to the temperature of 1000-1200 ℃, and preserving heat for 2-4 hours, wherein the initial forging temperature is more than or equal to 1000 ℃, and the final forging temperature is more than or equal to 950 ℃;
s4, polishing the forged blank, then heating and rolling the polished forged blank on a wire rod continuous rolling mill to form a disc circle with a required size, and straightening and polishing the disc circle into a bright silver rod after solution treatment.
In S4, the heating and rolling are specifically: the heating temperature of the forging stock in a wire heating furnace is 1000-1150 ℃, the heating time is more than or equal to 2.5 hours, the rolling speed is controlled to be less than or equal to 30m/s, the finish rolling temperature is controlled to be more than or equal to 850 ℃, and the forging stock is cooled by water after being rolled.
In S4, the solution treatment specifically includes: the heat treatment solid solution temperature is controlled to be 900-1150 ℃, and the aging temperature is controlled to be 650-800 ℃.
By adopting the iron-nickel gas valve alloy and the preparation method thereof, aiming at the defect of low hardness of the existing iron-nickel alloy aging treatment, Cr and Ni elements are taken as main matrix solid solution strengthening elements and precipitation dispersion strengthening phases such as Al, Ti, Mo, V, Nb and the like through the adjustment of component elements, so that the iron-nickel gas valve alloy which has high temperature performance similar to NCF751 at 750 ℃ and higher hardness than the common iron-nickel alloy can be prepared.
Detailed Description
The iron-nickel gas valve alloy comprises the following components in percentage by weight: c: 0.03-0.15%, less than or equal to 0.50% of Si, less than or equal to 0.50% of Mn, 20-28% of Cr, Ni: 25-35%, S is less than or equal to 0.040%, P is less than or equal to 0.040%, Mo: 0.30-1.20%, V is less than or equal to 0.80%, Cu is less than or equal to 0.50%, Al: 1.20-2.50%, Ti: 2.00-3.00%, Nb: 0.20-1.00 percent of Ce, less than or equal to 0.012 percent of Zr, less than or equal to 0.05 percent of Zr, and the balance of Fe and inevitable impurities.
The design principle of the components of the invention is as follows:
carbon is an indispensable element in steel. Carbon is a high-strength carbide-forming element in steel while enlarging the austenite phase region. The strengthening effect of carbon in steel is closely related to the composition and structure of the carbide formed, and the strengthening effect is also temperature dependent. With increasing temperature, the strengthening effect is reduced due to the aggregation of carbides. The increase in carbon content in the steel also reduces the plasticity and weldability of the steel. Therefore, the carbon content in general heat-resistant steel is controlled to be in a low range except for steel with high strength requirement. In addition, carbon may be used as a grain boundary strengthening element. Carbon in the heat-resistant steel is precipitated in the form of carbide in the aging process, the mechanical property is improved by forming the carbide, and the granular discontinuous carbide precipitated in the grain boundary prevents the sliding along the crystal and the crack propagation, so that the service life can be prolonged, and the lasting plasticity and the toughness can be improved.
Chromium is a main element for resisting high-temperature oxidation and high-temperature corrosion in the heat-resistant steel, and can improve the heat strength of the heat-resistant steel. When the chromium content in the steel is high enough, a compact Cr2O3 film can be formed on the surface of the steel, the oxide film can prevent the diffusion of corrosive gases such as oxygen, sulfur, nitrogen and the like into the steel to a certain extent, can also prevent the outward diffusion of metal ions, and can also form a spinel type composite oxide film with good protection in a certain temperature range, for example, a NiO.Cr2O3 composite oxide film is formed on the surface of heat-resistant steel containing Ni and Cr, so that the high-temperature oxidation resistance of the steel is enhanced. Most of Cr in the matrix is dissolved in the matrix except a small amount of Cr forms carbide with C, and solid solution strengthening is generated. In addition, since chromium has a high melting point (1903 ℃), it has excellent creep resistance.
The silicon is a beneficial element for resisting high-temperature corrosion in the heat-resistant steel, and the performance of the heat-resistant steel working at room temperature can be improved by adding a small amount of silicon into the heat-resistant steel, at high temperature, a layer of SiO2 film with good protection and compactness is formed on the surface of the silicon-containing heat-resistant steel, and the joint alloying of the silicon and the aluminum has obvious effect of improving the high-temperature oxidation resistance of the steel, but along with the increase of the silicon content, some phases (such as sigma phase and L aves phase) harmful to the mechanical properties of the alloy can appear in a matrix, so that the alloy performance is sharply reduced.
Sulfur in the heat-resistant alloy segregates to grain boundaries or phase boundaries, and weakens the grain boundaries and the phase boundaries, thereby becoming channels for crack generation and propagation. Sulfur in steel forms eutectic with iron to generate hot brittleness, which can cause hot cracking, hot breaking and other adverse effects, so a deoxidizer and a desulfurizer are usually added in the smelting process to reduce the harmful effect of sulfur.
Molybdenum is a ferrite-forming element. Research shows that molybdenum and chromium are effective alloy elements for improving the pitting corrosion performance of stainless steel, and the molybdenum has a particularly prominent effect. Molybdenum can promote the passivation of stainless steel, improve the corrosion resistance, and particularly has the function of preventing pitting corrosion tendency. Molybdenum is added into chromium and nickel stainless steel, so that the corrosion resistance and the corrosion and wear resistance of the stainless steel can be improved. By using the solid solution strengthening method, the molybdenum can improve the strength of the austenitic stainless steel and the tempering resistance of the martensitic stainless steel. In addition, molybdenum can also improve the hardenability, high temperature strength, and creep resistance of the steel.
Nickel can effectively expand and maintain the austenite phase region at normal temperature. If the alloy contains more than 25 percent of Ni, the alloy can obtain a single austenite structure at normal temperature. In addition, Ni can form a gamma' precipitation strengthening phase with Al, Ti, Nb and other elements, thereby improving the strength of the material.
Phosphorus generally has a detrimental effect on the mechanical properties of the superalloy. However, in the late 80 s of the last century, researchers found that phosphorus in appropriate amounts was beneficial to the creep and durability properties of some superalloys. The proper amount of phosphorus can improve the creep resistance of the high-temperature alloy, reduce the steady-state creep rate and prolong the second-stage creep time. And the phosphorus content has no obvious influence on the room temperature and high temperature performance of the heat-resistant alloy. The strengthening effect of phosphorus on grain boundaries is shown as follows: phosphorus atoms are segregated in a grain boundary, the bonding relation between main elements of the grain boundary is changed, a certain atomic group is formed, the interatomic bonding force is increased, the grain boundary strength is improved, or the form of a grain boundary precipitated phase is changed, one or two mechanisms act together, and the durability and the creep property of the high-temperature alloy are improved. The segregation of phosphorus to the grain boundaries promotes nucleation of grain boundary phases and produces precipitate phases, mainly the M23C6 and M3B2 phases. The document reports that the phosphorus content of about 0.016 percent reaches the most appropriate grain boundary precipitation state, and the grain boundary slippage and the nucleation and growth of grain boundary cracks are powerfully prevented.
In addition, for Nb added into the high-temperature alloy, Nb is mainly dissolved in a gamma 'phase (Ni3AITi), Nb enters the gamma' phase, so that the quantity of the gamma 'phase is increased, the strength and the solubility are improved, the diffusion rate of other elements in the gamma' phase is reduced, the particle growth rate and the conversion tendency to η phase are reduced, the content of Nb is increased, the content of Ti in the gamma 'phase is reduced, the formation tendency of η phase is reduced, the stability of the gamma' phase is improved, and in addition, the Nb can promote grain refinement.
The titanium has low solubility in the heat-resistant steel, and has the main function that the titanium and supersaturated carbon dissolved in the matrix can form high-strength and high-hardness carbide TiC, and TiC particles can play a good precipitation hardening effect when being uniformly distributed on the matrix. In addition, titanium in gamma prime precipitation hardening alloys can significantly improve the reverse domain boundary energy of the gamma prime phase, strengthening the cutting mechanism and causing strengthening effect.
Aluminum is a harmful element in conventional steel grades, but can improve the oxidation resistance of the alloy in heat-resistant alloy. The principle of the oxidation resistance of aluminum is similar to that of chromium, and a layer of Al 203 film with high density is formed on the surface layer of the alloy to prevent corrosive gas from invading into the alloy matrix. Further, aluminum is also an important basic constituent element of the precipitation hardening phase γ '(Ni 3AITi), and as the content of aluminum increases, the amount of the γ' phase also increases, enhancing the precipitation strengthening effect. Al added into the high-temperature alloy enters a gamma solid solution partially, and most of the Al with 80 percent and Ni form Ni3Al to perform precipitation strengthening. And secondly, the solubility of each element in the gamma ' phase is changed by adding Al, and the quantity of Al and Ni entering the gamma ' phase is increased along with the increase of the Al content, so that the quantity of the gamma ' phase is further increased, and the strengthening effect is improved.
The iron-nickel gas valve alloy can be prepared by the following preparation method, which comprises the following steps:
s1, proportioning according to chemical components of a gas valve alloy, smelting in a vacuum induction furnace, and then casting into a steel ingot;
s2, placing the steel ingot serving as a consumable electrode in an electroslag remelting device for electroslag remelting, washing liquid metal into a lower water-cooled crystallizer through a slag layer of a slag pool, and re-solidifying into a steel ingot of 1.5-2.0 tons;
s3, heating the steel ingot to the temperature of 1000-1200 ℃, and preserving heat for 2-4 hours, wherein the initial forging temperature is more than or equal to 1000 ℃, the final forging temperature is more than or equal to 950 ℃, and the size of the forging stock is 8-9m in a 160-square mode;
s4, polishing the forged blank, then heating and rolling the polished forged blank on a wire rod continuous rolling mill to form a disc circle with a required size, and straightening and polishing the disc circle into a bright silver rod after solution treatment.
In S4, the heating and rolling are specifically: the heating temperature of the forging stock in a wire heating furnace is 1000-1150 ℃, the heating time is more than or equal to 2.5 hours, the rolling speed is controlled to be less than or equal to 30m/s, the finish rolling temperature is controlled to be more than or equal to 850 ℃, and the forging stock is cooled by water after being rolled.
In S4, the solution treatment specifically includes: the heat treatment solid solution temperature is controlled to be 900-1150 ℃, and the aging temperature is controlled to be 650-800 ℃.
Because the austenite structure of the material precipitates carbide phase in steel ingot solidification and subsequent cooling at the temperature of 1000-1150 ℃, and dissolves the precipitated phase in the matrix as much as possible in plastic deformation to obtain single-phase structure, the preparation is provided for later aging precipitation to precipitate uniform and fine strengthening phase, and the aging at the temperature of 650-800 ℃ is carried out to precipitate strengthening phase with a certain quantity in the alloy matrix, such as gamma' phase, so as to achieve the maximum strengthening effect of the alloy.
Specific examples are as follows:
table 1 shows the chemical analysis components (wt%) of examples 1 to 3
Table 2 shows the mechanical properties of 5hAC at 750 ℃ in example 1
Table 3 shows the aging Performance test of examples 1 to 3
Heat treatment System | HRC | Metallography, scanning (gamma'% and size) | |
Example 1 | 970℃12minWQ+760℃3hAC | 34.8 | |
Example 2 | 970℃12minWQ+760℃6hAC | 35.7 | |
Example 3 | 970℃12minWQ+760℃10hAC | 37.6 | Grade 9 grain size |
As shown in the table above, the component chromium (Cr) of the invention is higher, Ni is low, thus the cost is relatively lower, and the oxidation resistance and the corrosion resistance are better, and then Al, Ti, Mo, V, Nb and the like are added to precipitate dispersion strengthening, the alloy has the strength which is higher than HRC35 and is higher than the hardness of other iron-nickel alloys, and the rotary bending fatigue limit at 700 ℃ is 430MPa, the high-temperature yield strength at 700 ℃ is 750MPa, and is equivalent to the nickel-based alloy NCF 751.
It should be understood by those skilled in the art that the above embodiments are only for illustrating the present invention and are not to be used as a limitation of the present invention, and that changes and modifications to the above described embodiments are within the scope of the claims of the present invention as long as they are within the spirit and scope of the present invention.
Claims (4)
1. An iron-nickel gas valve alloy, characterized by comprising, in weight percent:
c: 0.03-0.15%, less than or equal to 0.50% of Si, less than or equal to 0.50% of Mn, 20-28% of Cr, Ni: 25-35%, S is less than or equal to 0.040%, P is less than or equal to 0.040%, Mo: 0.30-1.20%, V is less than or equal to 0.80%, Cu is less than or equal to 0.50%, Al: 1.20-2.50%, Ti: 2.00-3.00%, Nb: 0.20-1.00 percent of Ce, less than or equal to 0.012 percent of Zr, less than or equal to 0.05 percent of Zr, and the balance of Fe and inevitable impurities.
2. The method of making an iron-nickel gas valve alloy as set forth in claim 1, including the steps of:
s1, proportioning according to chemical components of a gas valve alloy, smelting in a vacuum induction furnace, and then casting into a steel ingot;
s2, placing the steel ingot serving as a consumable electrode in an electroslag remelting device for electroslag remelting, washing liquid metal into a water-cooled crystallizer through slag bath slag, and solidifying the liquid metal into the steel ingot again;
s3, heating the steel ingot to the temperature of 1000-1200 ℃, and preserving heat for 2-4 hours, wherein the initial forging temperature is more than or equal to 1000 ℃, and the final forging temperature is more than or equal to 950 ℃;
s4, polishing the forged blank, then heating and rolling the polished forged blank on a wire rod continuous rolling mill to form a disc circle with a required size, and straightening and polishing the disc circle into a bright silver rod after solution treatment.
3. The method according to claim 2, wherein in S4, the heating and rolling are specifically: the heating temperature of the forging stock in a wire heating furnace is 1000-1150 ℃, the heating time is more than or equal to 2.5 hours, the rolling speed is controlled to be less than or equal to 30m/s, the finish rolling temperature is controlled to be more than or equal to 850 ℃, and the forging stock is cooled by water after being rolled.
4. The method according to claim 2, wherein in S4, the solution treatment is specifically: the heat treatment solid solution temperature is controlled to be 900-1150 ℃, and the aging temperature is controlled to be 650-800 ℃.
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