CN114686783B - High-elasticity-modulus age-hardening high-speed steel material and preparation method thereof - Google Patents

High-elasticity-modulus age-hardening high-speed steel material and preparation method thereof Download PDF

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CN114686783B
CN114686783B CN202210256814.6A CN202210256814A CN114686783B CN 114686783 B CN114686783 B CN 114686783B CN 202210256814 A CN202210256814 A CN 202210256814A CN 114686783 B CN114686783 B CN 114686783B
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speed steel
ball milling
steel material
age
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CN114686783A (en
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谢丰伟
康希越
陈帅鹏
张乾坤
陈豫章
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Changsha Sharpen Advanced Materials Co ltd
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    • C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
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Abstract

The invention discloses a high-elasticity modulus age-hardening high-speed steel material and a preparation method thereof, wherein the high-speed steel material comprises the following components in percentage by mass: co:15 to 30 percent; total amount of Mo and W: 10-20%, wherein the content of W is less than 10%; cr:2 to 5 percent; ni:1 to 4 percent; v:1 to 3 percent; mn:1 to 2 percent; nb:0.5 to 1 percent; n:0.5 to 1 percent, and the balance of Fe and inevitable impurities. According to the invention, cr, V, ni and a non-metallic element N are added for solid solution strengthening, and nitride strengthening particles are added to synergistically obtain the high-elasticity-modulus age-hardening high-speed steel material. The elastic modulus of the age-hardening high-speed steel material provided by the invention can be improved by 10-20%, and other mechanical properties are synchronously improved.

Description

High-elasticity-modulus age-hardening high-speed steel material and preparation method thereof
Technical Field
The invention relates to the technical field of powder metallurgy, in particular to the field of powder metallurgy ferrous materials, and especially relates to a high-elasticity-modulus age-hardening high-speed steel material and a preparation method thereof.
Background
Titanium alloys and superalloys play an indispensable role in the aerospace industry, and the demand is increasing. However, it is typically a difficult-to-machine material, mainly due to low thermal conductivity and high chemical activity, resulting in a less efficient machining process, low surface finish and high tool consumption. At present, the machining tools of titanium alloy and high-temperature alloy are often selected from traditional carbide high-speed steel tools and coating hard alloy tools. When the former is selected for processing, the hardness of the cutting edge material is rapidly reduced due to the restriction of the hot hardness, and the cutting edge material is softened and plastically deformed to be incapable of keeping sharpness and is rapidly worn. If a hard alloy cutter is selected, a high-sharpness thin cutting edge is difficult to prepare due to low toughness; and the oxidation resistance is poor, oxidation abrasion and collapse easily occur under high-speed cutting, and the surface coating is damaged to cause rapid abrasion of the cutter.
Therefore, an Fe-Co-Mo age-hardening high-speed steel which can overcome the above-mentioned disadvantages is produced. The age hardening high-speed steel is a material which generates a fine and dispersed intermetallic compound second phase in situ in a matrix through aging so as to carry out strong hardening on the material, has the advantages of high hardness, higher toughness, large heat conductivity coefficient, excellent tempering resistance, high thermal hardness, high processing stability, good processing performance and the like, and is considered to be a cutting tool material more suitable for processing difficult-to-process materials. However, the elastic modulus of the high-speed steel is 10% -15% lower than that of the traditional powder high-speed steel, the rigidity is lower when the high-speed steel is made into a cutting tool material with a certain sectional area, the stability in service is not high, and the high-speed steel is easy to deform, so that the elastic modulus of the high-speed steel needs to be improved urgently. In the prior art, a composite material is mainly formed by adding high-modulus ceramic particles, so that the particles are uniformly dispersed in a matrix, and the overall elastic modulus is increased. In the field of steel materials, tiB is mainly generated in situ by Ti and B elements 2 The reinforcing particles thereby increase the modulus of elasticity. T isif the addition amount of i is too low, the enhancement effect is not obvious, if the content of Ti is too high, the subsequent processing performance of the material is adversely affected, and if the price of titanium is too high, the cost is increased, so that the large-range application is limited. Therefore, a method for improving the elastic modulus without reducing the performance of the material is needed, which has low cost and is suitable for industrial large-scale production.
Disclosure of Invention
In view of the deficiencies of the prior art, it is an object of the present invention to devise and develop a Fe-Co-Mo/W based high elastic modulus age-hardening high speed steel material which synergistically increases the overall elastic modulus by adding various high melting point metallic elements such as Cr, V, ni and non-metallic element N for solution strengthening and adding nitride reinforcing particles;
the invention also aims to provide a preparation method of the high-elasticity modulus age hardening high-speed steel material, which is characterized in that pure metal powder such as Fe powder, co powder, mo powder, W powder, cr powder and the like and metal nitride powder are uniformly mixed by ball milling by using a powder metallurgy method and are sequentially subjected to processes such as press forming, vacuum sintering, heat treatment and the like to prepare the high-elasticity modulus age hardening high-speed steel material.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention relates to a high-elasticity-modulus age-hardening high-speed steel material which is composed of a steel matrix, and intermetallic compounds and nitrides which are dispersedly distributed in the steel matrix, wherein the nitrides are vanadium nitride and manganese nitride, N element is dissolved in the steel matrix, and the mass fraction of the N element in the high-speed steel material is 0.5-1%.
The invention provides a high-elasticity modulus age hardening high-speed steel material, which comprises metal nitride and matrix solid solution nitrogen, wherein the uniform distribution of the high-modulus metal nitride can improve the elastic modulus of the material, and the solid solution nitrogen can strongly stabilize austenite and enlarge the phase region of the austenite, thereby improving the mechanical property, improving the strength, not reducing the plasticity, and improving the corrosion resistance of the material.
According to the preferable scheme, the high-speed steel material comprises the following components in percentage by mass: co:15 to 30 percent; total amount of Mo and W: 10-20%, wherein the content of W is less than 10%; cr:2 to 5 percent; ni:1 to 4 percent; v:1 to 3 percent; mn:1 to 2 percent; nb:0.5 to 1 percent; n:0.5 to 1 percent, and the balance of Fe and inevitable impurities.
Further preferably, the high-speed steel material comprises the following components in percentage by mass: co:21 to 25 percent; 10 to 12 percent of Mo and 4 to 6 percent of W; cr:3 to 4 percent; ni:2 to 3 percent; v:2 to 3 percent; mn:1 to 2 percent; nb:0.6 to 0.7 percent; n:0.6 to 0.8 percent, and the balance of Fe and inevitable impurities.
The invention relates to a preparation method of a high-elasticity modulus age-hardening high-speed steel material, which comprises the following steps: preparing pure cobalt, pure molybdenum, pure chromium, pure nickel, pure tungsten, pure niobium, pure iron, pure vanadium nitride and manganese nitride according to a designed proportion to obtain mixed powder, ball-milling the mixed powder, carbon black and a forming agent in a nitrogen atmosphere to obtain a mixture, pressing and forming, pre-sintering in a vacuum environment, then sintering at a high temperature in the nitrogen atmosphere to obtain a sintered blank, and carrying out solution treatment and aging treatment on the sintered blank twice to obtain the high-strength high-elasticity modulus high-speed steel.
Preferably, all of the starting powders used are commercially high purity powders.
Preferably, the addition amount of the carbon black is 0.1-0.6% of the mass of the mixed powder. In the present invention, carbon black is added to cause a carbon-oxygen reaction with adsorbed oxygen during sintering, so that on the one hand, the impurity oxygen content of the material is reduced, and on the other hand, the carbon-oxygen reaction exposes fresh atoms on the powder surface to increase the sintering driving force.
Preferably, the forming agent is at least one selected from paraffin, PEG and PVB, and the adding amount of the forming agent is 3-6% of the mass of the mixed powder.
In a preferable scheme, the ball milling medium is absolute ethyl alcohol, hard alloy balls are used as the milling balls, the ball-material ratio is (4-7): 1, the ball milling rotation speed is 240-340 r/min, and the ball milling time is 48-72h.
In a preferable scheme, the ball milling adopts intermittent ball milling, each ball milling is carried out for 10-15h, air cooling is carried out for 20-40min, and the pressure in a ball milling tank is 0.2-0.4MPa during the ball milling.
According to the invention, a ventilating ball milling tank is adopted for ball milling operation, nitrogen is intermittently and circularly introduced in the ball milling process, on one hand, excessive oxidation of mixed powder during ball milling can be prevented, on the other hand, partial nitrogen molecules can be adsorbed and decomposed in the ball milling process, and then nitrogen atoms are diffused into a powder matrix, so that mixed powder with high nitrogen content is obtained to supplement nitrogen, and thus on the one hand, the nitrogen content in solid solution in a steel matrix can be increased, and on the other hand, the solid solubility of nitrogen in austenite is limited, so that the solid solution of nitrogen in added vanadium nitride and manganese nitride can be reduced, the vanadium nitride and manganese nitride still exist in the form of a hard second phase, and the elastic modulus is improved.
In the actual operation process, before ball milling, nitrogen is firstly introduced for 10-15min to discharge air in the ball milling tank, then the nitrogen is continuously introduced, the micro-positive pressure formed in the ball milling tank is 0.2-0.4MPa, each ball milling time is 10-15h, the ball milling and the introduction of the nitrogen are stopped, air cooling is carried out for 20-40min, the overhigh temperature in the ball milling tank is avoided, and the oxidation is further reduced. According to the operation of the invention, not only nitrogen can be introduced to the maximum extent, but also the introduction of excessive oxygen impurities can be avoided during the ball milling process.
In the actual operation process, the ball mill can adopt a roller ball mill or a planetary ball mill which is well known to those skilled in the art, and the roller ball mill is preferably adopted for ball milling because the roller ball mill has a large discharge amount during mixing.
Preferably, the pressure of the compression molding is 100-200 MPa, and the dwell time is 20-30 s.
The pressure of the press forming is controlled within the range, the density of a finished product obtained finally by sintering is highest, the performance is optimal, and if the pressure is too high, the density of a pressed compact is too high, so that the degassing in the sintering process is difficult, and the density is reduced; too low a compaction pressure results in a green compact with too low a strength, which is not only detrimental to green compact transfer operations, but also difficult to fully densify. The compaction pressure is controlled within the above range, at which the green density is about half the theoretical density.
Preferably, the procedure of the pre-sintering is as follows: heating to 100-200 deg.C, maintaining for 1-2h, heating to 300-600 deg.C, maintaining for 4-6h, heating to 850-1050 deg.C, maintaining for 1-3h, heating at 2-8 deg.C/min, and vacuum degree less than 0.01Pa.
The sintering is carried out in a vacuum environment, and a heat-preservation platform at 100-200 ℃ is used for removing water vapor and other gases adsorbed by a pressed compact; the heat preservation platform with the temperature of 300-600 ℃ is used for removing the forming agent in the pressed compact; before 850 ℃, a blank body has certain density and enough degassing channels are reserved by setting the time of a heat preservation platform and the heating rate (2-8 ℃/min); the 850-1050 ℃ heat preservation platform is used for fully carrying out the carbon-oxygen reaction, realizing the activation of the powder surface to promote the sintering densification,
in a preferable scheme, the high-temperature sintering temperature is 1300-1450 ℃, the high-temperature sintering time is 2-3h, and the vacuum is 1-5kPa. And finally densifying through high-temperature sintering, and simultaneously introducing nitrogen partial pressure during the high-temperature sintering, so that the loss of N can be further reduced, and the solid solution of nitrogen in the added vanadium nitride and manganese nitride can be reduced.
In a preferable scheme, the temperature of the first solution treatment is 1230-1280 ℃, the time of the first solution treatment is 10-15min, the temperature of the first aging treatment is 700-800 ℃, the time of the first aging treatment is 1-3h, the temperature of the second solution treatment is 1140-1190 ℃, and the time of the second solution treatment is 15-20 min; the temperature of the second aging treatment is 550-750 ℃, and the time of the second aging treatment is 1-4h.
According to the invention, after the obtained compact body is sintered, an optimized structure is obtained without conventional thermal deformation (such as hot forging and rolling) processing, the risk that the elastic modulus is reduced due to the fact that the nitride particle size is damaged and even the nitride particles are decomposed and denitrified in the thermal deformation process is avoided, the uniform dispersion precipitation of precipitated phases is regulated and controlled directly through two-stage solid solution-aging treatment, fine grains are obtained at the same time, and the high-elasticity-modulus age-hardening carbon-free high-speed steel material is finally obtained.
In addition, the invention adopts two-stage solid solution-aging treatment, wherein the first time is high-temperature solid solution and high-temperature aging, and the second time is semi-solid solution and preset temperature aging. The first high-temperature solid solution aims at completely dissolving precipitated phases which are in a net-shaped uneven distribution and are used for age hardening high-speed steel in a sintering state into a matrix in a solid solution mode, and because higher temperature brings higher nucleation energy, more nucleation sites exist in subsequent high-temperature aging, and the precipitated phases can be precipitated uniformly at one time. The second semi-solid solution treatment aims at re-dissolving most precipitated phases generated after the first high-temperature aging into a matrix, and leaving a small amount of larger precipitated phases, wherein the larger precipitated phases are generally micron-sized and can serve as wear-resistant phases of materials and simultaneously prevent grains from excessively growing, and can serve as nucleation sites for re-aging precipitation; thus, the precipitated phase is uniformly dispersed and precipitated in the aging process of the second preset temperature. Through two-stage solid solution-aging treatment, the precipitation phase ratio can be regulated and controlled to be uniform dispersion precipitation, and the damage of thermal deformation treatment is avoided. Because the strength and the plasticity of the material are generally in a negative correlation relationship, and the elastic modulus is insensitive to the change of subsequent treatment and environment, the high-modulus age-hardening carbon-free high-speed steel material with different strong plasticity combinations can be obtained by regulating and controlling the solution-aging heat treatment.
Principles and advantages
The high-speed steel material provided by the invention has metal nitrides and matrix solid-solution nitrogen, the elastic modulus of the material can be improved by the uniform distribution of the high-modulus metal nitrides, and meanwhile, the solid-solution nitrogen can strongly stabilize austenite and enlarge the phase region of the austenite, so that the mechanical property is improved, the plasticity is not reduced while the strength is improved, and the corrosion resistance of the material can also be improved.
Of course, besides N element, the invention also regulates and controls other element compositions to obtain a steel matrix with specific performance and controllably obtain intermetallic compounds with reinforcing effect which are dispersed in the steel matrix, thereby obtaining the age-hardening high-speed steel material with high elastic modulus under the synergistic action of the metal nitride: specifically, the components of the invention are as follows:
the Cr element is an important metal element in the present invention. Cr is an element added in the present invention in the largest amount, about 2 to 5%, in addition to the basic components of Fe, co, mo, and W. Cr is a ferrite stabilizing element and reduces an austenite phase region, and the addition of Cr can neutralize the influence of the stable austenite phase region of N element, so that the alpha → gamma transition temperature of the material is stabilized in a certain range. Meanwhile, cr enhances the elastic modulus of the matrix through solid solution strengthening, improves the hardenability, and is beneficial to enhancing the oxidation resistance and the corrosion resistance of the steel.
Ni is also an important metal element in the invention, and has synergistic effect with Cr, the elastic modulus is enhanced mainly by solid solution strengthening, but the content of Ni is too high to reduce M obviously s Accordingly, the content is limited to 1 to 4% in the present invention.
The V element is introduced through pure element powder and vanadium nitride. In the invention, the V element is controlled to be 1-3%, and the V has high melting point, can improve hardenability and microstructure besides the solid solution strengthening effect, and can not weaken the grinding performance.
The Mn element has the functions of regulating the microstructure of a steel matrix and eliminating thermal embrittlement caused by trace sulfur, thereby improving the hot workability. In addition, 0.5-1% of Nb element is added for refining grains and improving the hardening capacity.
The preparation method comprises the steps of ball-milling and uniformly mixing pure metal powder such as Fe powder, co powder, mo powder, W powder, cr powder and the like and metal nitride powder by adopting a powder metallurgy method, and sequentially performing the processes of press forming, vacuum sintering, heat treatment and the like.
The invention overcomes the defects of the prior art, and provides a new feasible scheme for improving the elastic modulus of age-hardening high-speed steel by using the alloying principle and high-modulus nitride particles to jointly enhance the elastic modulus through component design. The age hardening high-speed steel prepared by the invention has the advantages that the elastic modulus can be improved by 10-20%, and other mechanical properties are synchronously improved.
The preparation scheme of the invention does not need to be subjected to complex smelting treatment and also does not need to be subjected to hot working treatment such as forging, rolling and the like. Short process flow, convenient operation, high production efficiency and lower cost, and can be applied to industrial production.
Drawings
FIG. 1 is a scanning electron microscope picture of the high elastic modulus age-hardened high speed steel of example 1 of the present invention after heat treatment.
Detailed Description
For better understanding of the present invention, the following detailed description will be given of the technical solutions and effects of the present invention through specific embodiments. The present invention includes, but is not limited to, the following examples.
Example 1
The high-elasticity modulus age-hardening high-speed steel material comprises the following chemical components in percentage by mass: co:21 percent; mo:10 percent; w:4 percent; cr:3 percent; ni:2 percent; v:2 percent; mn:2 percent; nb:0.6 percent; n:0.8%, the balance being Fe and unavoidable impurities. Wherein the N element is introduced by adding manganese nitride and vanadium nitride powder and ball milling and introducing nitrogen. The preparation method comprises the following steps:
1) Mixing pure metal Fe powder, co powder, mo powder, W powder, cr powder, ni powder, V powder, nb powder, mnN powder, VN powder and 0.4wt% of carbon black according to a designed proportion in a ball mill for 60 hours. Introducing nitrogen for 15min to exhaust air before ball milling, maintaining micro positive pressure (0.3 MPa) in the ball milling tank, stopping ball milling every 15h, introducing nitrogen, and cooling the ball milling tank for 30min. Carrying out negative pressure drying, granulating and vacuum packaging on the mixed powder after ball milling;
2) Pressing and forming the powder obtained in the step 1) under the pressure of 150MPa and the pressure maintaining time of 25s, and performing vacuum sintering and partial pressure sintering in nitrogen atmosphere on the green compact. Wherein the vacuum sintering stage: the temperature is kept at 150 ℃ for 1h to remove water vapor and other gases, at 450 ℃ for 4h to remove the forming agent, and at 950 ℃ for 2h to be used for fully carrying out the carbon-oxygen reaction. The temperature was maintained at a maximum temperature of 1350 ℃ for 2h while introducing nitrogen gas for partial pressure sintering with a vacuum degree of 2Kpa maintained for final densification.
3) Sequentially carrying out solid solution treatment at 1250 ℃ for 15min and aging treatment at 750 ℃ for 3h on the sintered blank sample obtained in the step 2); (2) solution treatment at 1150 ℃ for 15min and aging treatment at 600 ℃ for 2h; (3) and (4) carrying out subsequent treatment such as machining and the like to obtain the high-modulus age-hardening high-speed steel material.
The elastic modulus of the high-modulus age-hardening high-speed steel obtained in the embodiment is 246GPa, and other mechanical property data are shown in Table 1.
Example 2
The high-elasticity modulus age-hardening high-speed steel material comprises the following chemical components in percentage by mass: co:25 percent; mo:12 percent; w:5 percent; cr:3 percent; ni:2 percent; v:2 percent; mn:2 percent; nb:0.6 percent; n:0.8%, the balance being Fe and unavoidable impurities. Wherein the N element is introduced by adding manganese nitride and vanadium nitride powder and ball milling and introducing nitrogen. The preparation method comprises the following steps:
1) Pure metal Fe powder, co powder, mo powder, W powder, cr powder, ni powder, V powder, nb powder, mnN powder, VN powder and 0.4wt% of carbon black are mixed uniformly in a ball mill for 72 hours. Introducing nitrogen for 15min to exhaust air before ball milling, maintaining the micro-positive pressure (0.4 MPa) in the ball milling tank, stopping ball milling every 15h, introducing nitrogen, and cooling the ball milling tank for 30min. Carrying out negative pressure drying, granulating and vacuum packaging on the mixed powder after ball milling;
2) Pressing and forming the powder obtained in the step 1) under the pressure of 150MPa and the pressure maintaining time of 25s, and performing vacuum sintering and partial pressure sintering in nitrogen atmosphere on the green compact. Wherein the vacuum sintering stage: the temperature is kept at 150 ℃ for 1h to remove water vapor and other gases, at 450 ℃ for 4h to remove the forming agent, and at 950 ℃ for 2h to be used for fully carrying out the carbon-oxygen reaction. The temperature was held at 1380 ℃ for 2h while introducing nitrogen for partial pressure sintering at a vacuum of 2.5Kpa for final densification.
3) Sequentially carrying out solution treatment on the sintered blank sample obtained in the step 2) at 1260 ℃ for 15min and aging treatment at 800 ℃ for 3h; (2) solution treatment at 1150 ℃ for 15min and aging treatment at 600 ℃ for 2h; (3) and (4) carrying out subsequent treatment such as machining and the like to obtain the high-modulus age-hardening high-speed steel material.
The elastic modulus of the high-modulus age-hardening high-speed steel obtained in the embodiment is 249GPa, and other mechanical property data are shown in Table 1.
Example 3
The high-elasticity modulus age-hardening high-speed steel material comprises the following chemical components in percentage by mass: co:21 percent; mo:10 percent; w:4 percent; cr:4 percent; ni:3 percent; v:3 percent; mn:2 percent; nb:0.7 percent; n:0.8%, the balance being Fe and unavoidable impurities. Wherein the N element is introduced by adding manganese nitride and vanadium nitride powder and ball milling and introducing nitrogen. The preparation method comprises the following steps:
1) Mixing pure metal Fe powder, co powder, mo powder, W powder, cr powder, ni powder, V powder, nb powder, mnN powder, VN powder and 0.4wt% of carbon black according to a designed proportion in a ball mill for 65 hours. Introducing nitrogen for 15min to exhaust air before ball milling, maintaining micro positive pressure (0.3 MPa) in the ball milling tank, stopping ball milling every 15h, introducing nitrogen, and cooling the ball milling tank for 30min. Carrying out negative pressure drying, granulating and vacuum packaging on the mixed powder after ball milling;
2) Pressing and forming the powder obtained in the step 1) under the pressure of 150MPa and the pressure maintaining time of 25s, and performing vacuum sintering and partial pressure sintering in nitrogen atmosphere on the green compact. Wherein the vacuum sintering stage: keeping the temperature at 150 ℃ for 1h to remove water vapor and other gases, keeping the temperature at 450 ℃ for 4h to remove the forming agent, and keeping the temperature at 950 ℃ for 2h to be used for fully carrying out the carbon-oxygen reaction. The temperature was maintained at a maximum temperature of 1320 ℃ for 2h while nitrogen was introduced for partial pressure sintering with a vacuum of 2Kpa maintained for final densification.
3) Sequentially carrying out solution treatment at 1250 ℃ for 15min and aging treatment at 700 ℃ for 3h on the sintered blank sample obtained in the step 2); (2) solution treatment at 1150 ℃ for 15min and aging treatment at 610 ℃ for 2h; (3) and (4) carrying out subsequent treatment such as machining and the like to obtain the high-modulus age-hardening high-speed steel material.
The elastic modulus of the high-modulus age-hardening high-speed steel obtained in the embodiment is 245GPa, and other mechanical property data are shown in Table 1.
Example 4
The high-elasticity modulus age-hardening high-speed steel material comprises the following chemical components in percentage by mass: co:21 percent; mo:10 percent; w:4 percent; cr:3 percent; ni:2 percent; v:2 percent; mn:2 percent; nb:0.6 percent; n:0.8%, the balance being Fe and unavoidable impurities. Wherein the N element is introduced by adding manganese nitride and vanadium nitride powder and ball milling and introducing nitrogen. The preparation method comprises the following steps:
1) Pure metal Fe powder, co powder, mo powder, W powder, cr powder, ni powder, V powder, nb powder, mnN powder, VN powder and 0.4wt% of carbon black are mixed uniformly in a ball mill for 72 hours. Introducing nitrogen for 15min to exhaust air before ball milling, maintaining micro positive pressure (0.3 MPa) in the ball milling tank, stopping ball milling every 15h, introducing nitrogen, and cooling the ball milling tank for 30min. Carrying out negative pressure drying, granulating and vacuum packaging on the mixed powder after ball milling;
2) Pressing and forming the powder obtained in the step 1) under the pressure of 150MPa and the pressure maintaining time of 25s, and performing vacuum sintering and partial pressure sintering in nitrogen atmosphere on the green compact. Wherein the vacuum sintering stage: the temperature is kept at 150 ℃ for 1h to remove water vapor and other gases, at 450 ℃ for 4h to remove the forming agent, and at 950 ℃ for 2h to be used for fully carrying out the carbon-oxygen reaction. The temperature is maintained at the maximum temperature of 1400 ℃ for 2h, and nitrogen is introduced for partial pressure sintering while the vacuum degree is kept at 2Kpa for final densification.
3) Sequentially carrying out solution treatment at the temperature of 1) for 15min and aging treatment at the temperature of 750 ℃ for 3h on the sintered blank sample obtained in the step 2); (2) solution treatment at 1140 ℃ for 15min and aging treatment at 550 ℃ for 2h; (3) and (4) carrying out subsequent treatment such as machining and the like to obtain the high-modulus age-hardening high-speed steel material.
The elastic modulus of the high-modulus age-hardening carbon-free high-speed steel obtained in the embodiment is 247GPa, and other mechanical property data are shown in Table 1.
Example 5
The high-elasticity modulus age hardening high-speed steel material is characterized by comprising the following chemical components in percentage by mass: co:21 percent; mo:10 percent; w:4 percent; cr:3 percent; ni:2 percent; v:2 percent; mn:2 percent; nb:0.6 percent; n:0.6%, the balance being Fe and unavoidable impurities. Wherein the N element is introduced by adding manganese nitride and vanadium nitride powder and ball milling and introducing nitrogen. The preparation method comprises the following steps:
1) Mixing pure metal Fe powder, co powder, mo powder, W powder, cr powder, ni powder, V powder, nb powder, mnN powder, VN powder and 0.4wt% of carbon black according to a designed proportion in a ball mill uniformly, wherein the ball milling time is 48h. Introducing nitrogen for 15min to exhaust air before ball milling, maintaining the micro-positive pressure (0.2 MPa) in the ball milling tank, stopping ball milling every 15h, introducing nitrogen, and cooling the ball milling tank for 30min. Carrying out negative pressure drying, granulating and vacuum packaging on the mixed powder after ball milling;
2) Pressing and forming the powder obtained in the step 1) under the pressure of 200MPa for 25s of pressure maintaining time, and performing vacuum sintering and nitrogen atmosphere partial pressure sintering on a pressed blank. Wherein the vacuum sintering stage: the temperature is kept at 150 ℃ for 1h to remove water vapor and other gases, at 450 ℃ for 4h to remove the forming agent, and at 950 ℃ for 2h to be used for fully carrying out the carbon-oxygen reaction. The temperature was maintained at the maximum temperature of 1300 ℃ for 2h while introducing nitrogen for partial pressure sintering with a vacuum degree of 1Kpa maintained for final densification.
3) Sequentially carrying out solid solution treatment at 1250 ℃ for 15min and aging treatment at 750 ℃ for 3h on the sintered blank sample obtained in the step 2); (2) solution treatment at 1150 ℃ for 15min and aging treatment at 600 ℃ for 2h; (3) and (4) carrying out subsequent treatment such as machining and the like to obtain the high-modulus age-hardening high-speed steel material.
The elastic modulus of the high-modulus age-hardening high-speed steel obtained in the embodiment is 241GPa, and other mechanical property data are shown in Table 1.
Comparative example 1
The comparative example 1 is Fe-Co-Mo/W high-speed steel without other metal elements and nitrogen elements, and comprises the following chemical components in percentage by mass: co:21 percent; mo:10%, W:4 percent, and the balance of Fe and inevitable impurities. The rest is the same as in example 1. The elastic modulus of the age-hardened high-speed steel obtained by the comparative example is 223GPa, and the other mechanical property data are shown in Table 1.
Comparative example 2
Compared with the embodiment 1, nitrogen is not introduced into the components, namely the mass ratio of the components is Co:21 percent; mo:10 percent; w:4 percent; cr:3 percent; ni:2 percent; v:2 percent; nb:0.6 percent; the remainder being Fe and unavoidable impurities, the remaining preparation steps being the same as in example 1. The elastic modulus of the age-hardened high-speed steel obtained by the comparative example is 232GPa, and the other mechanical property data are shown in Table 1.
Comparative example 3
The composition of the age-hardened high-speed steel provided by the comparative example is Co:21 percent; mo:10 percent; w:4 percent; v:1 percent; mn:2 percent; n:0.8%, the balance being Fe and unavoidable impurities. In the comparative example, only in the process of preparing raw materials, alloying element powder except for the Fe-Co-Mo/W matrix, namely Cr powder, ni powder and Nb powder, is not added, the rest is the same as that in the example 1, the elastic modulus of the age-hardened high-speed steel obtained in the comparative example is 239GPa, and the other mechanical property data are shown in the table 1.
Comparative example 4
Comparative example 4, the other conditions were the same as in example 1 except that no nitrogen gas was introduced during the ball milling.
Comparative example 5
In comparative example 5, the other conditions were the same as in example 1 except that the first-order solution-aging treatment, i.e., solution treatment at 1150 ℃ for 15min and aging treatment at 600 ℃ for 2 hours, was employed.
Table 1: elastic modulus, hardness, flexural strength and impact toughness data for examples and comparative examples
Figure BDA0003548929860000111
According to the data listed in Table 1, compared with the comparative example 1 (original age-hardened high-speed steel), the elasticity modulus of the five examples of the invention is greatly improved, and simultaneously the hardness, the bending strength and the impact toughness are slightly improved; comparative examples 1, 2 and 3 show that the enhancement by metal elements such as Cr, ni, nb, etc. alone or the enhancement by nitride particles and solid-solution N element alone have a certain elastic modulus-improving effect, but not as strong as the synergistic enhancement effect of the two shown in the examples.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the present invention.

Claims (6)

1. A preparation method of a high-elasticity modulus age hardening high-speed steel material is characterized by comprising the following steps: the method comprises the following steps: preparing pure cobalt, pure molybdenum, pure chromium, pure nickel, pure tungsten, pure niobium, pure iron, pure vanadium nitride and pure manganese nitride according to a designed proportion to obtain mixed powder, performing ball milling on the mixed powder, carbon black and a forming agent in a nitrogen atmosphere to obtain a mixture, performing compression molding, pre-sintering in a vacuum environment, then sintering at a high temperature in the nitrogen atmosphere to obtain a sintered blank, and performing solution treatment and aging treatment on the sintered blank twice to obtain the high-strength high-elasticity-modulus high-speed steel;
the pre-sintering procedure comprises the following steps: firstly heating to 100-200 ℃, preserving heat for 1-2h, then heating to 300-600 ℃, preserving heat for 4-6h, then heating to 850-1050 ℃, preserving heat for 1-3h, wherein the heating rate is 2-8 ℃/min, and the vacuum degree is less than 0.01Pa;
the temperature of the first solid solution treatment is 1230-1280 ℃, the time of the first solid solution treatment is 10-15min, the temperature of the first aging treatment is 700-800 ℃, the time of the first aging treatment is 1-3h, the temperature of the second solid solution treatment is 1140-1190 ℃, and the time of the second solid solution treatment is 15-20min; the temperature of the second time aging treatment is 550-750 ℃, and the time of the second time aging treatment is 1-4h;
the high-speed steel material comprises the following components in percentage by mass: co:15 to 30 percent; total amount of Mo and W: 10 to 20 percent, wherein the W content is less than 10 percent; cr:2 to 5 percent; ni:1 to 4 percent; v:1 to 3 percent; mn:1 to 2 percent; nb:0.5 to 1 percent; n:0.5 to 1 percent, and the balance of Fe and inevitable impurities;
the high-speed steel material is composed of a steel matrix, and intermetallic compounds and nitrides which are dispersedly distributed in the steel matrix, wherein the nitrides are vanadium nitride and manganese nitride, N element is solid-dissolved in the steel matrix, and the mass fraction of the N element in the high-speed steel material is 0.5-1%.
2. The method for preparing a high-elastic modulus age-hardening high-speed steel material according to claim 1, characterized in that: the adding amount of the carbon black is 0.1 to 0.6 percent of the mass of the mixed powder;
the forming agent is selected from at least one of paraffin, PEG and PVB, and the addition amount of the forming agent is 3-6% of the mass of the mixed powder.
3. The method for preparing a high-elastic modulus age-hardening high-speed steel material according to claim 1, characterized in that: the ball milling medium is absolute ethyl alcohol, the grinding ball is a hard alloy ball, the ball material ratio is (4-7) to 1, the ball milling rotation speed is 240-340r/min, and the ball milling time is 48-72h.
4. The method for preparing a high-elastic modulus age-hardening high-speed steel material according to claim 1, characterized in that: the ball milling adopts intermittent ball milling, each ball milling lasts for 10-15h, air cooling is carried out for 20-40min, and the pressure in a ball milling tank is 0.2-0.4MPa during ball milling.
5. The method for preparing a high-elastic modulus age-hardening high-speed steel material according to claim 1, characterized in that: the pressure of the compression molding is 100 to 200MPa, and the dwell time is 20 to 30s.
6. The method for preparing the high-elasticity-modulus age-hardening high-speed steel material according to claim 1, characterized by comprising the following steps of: the high-temperature sintering temperature is 1300-1450 ℃, the high-temperature sintering time is 2-3h, and nitrogen is introduced to keep the vacuum at 1-5kPa.
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