CN109554628B - Preparation method of graphene composite high-speed tool steel - Google Patents

Preparation method of graphene composite high-speed tool steel Download PDF

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CN109554628B
CN109554628B CN201811407391.3A CN201811407391A CN109554628B CN 109554628 B CN109554628 B CN 109554628B CN 201811407391 A CN201811407391 A CN 201811407391A CN 109554628 B CN109554628 B CN 109554628B
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tool steel
speed tool
graphene
powder
graphene composite
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CN109554628A (en
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张海平
曹振
王旭东
李炯利
郭建强
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AECC Beijing Institute of Aeronautical Materials
Beijing Graphene Technology Research Institute Co Ltd
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AECC Beijing Institute of Aeronautical Materials
Beijing Graphene Technology 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
    • C22C38/24—Ferrous alloys, e.g. steel alloys containing chromium with vanadium
    • 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/18—Hardening; Quenching with or without subsequent tempering
    • 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
    • C21D8/005—Modifying the physical properties by deformation combined with, or followed by, heat treatment of ferrous alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • C22C33/0278—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%
    • 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%
    • 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
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • 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
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium 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
    • C22C38/30—Ferrous alloys, e.g. steel alloys containing chromium with cobalt

Abstract

The invention relates to a preparation method of graphene composite high-speed tool steel, which comprises the following steps: providing a mixed solution, wherein the mixed solution comprises a volatile organic solvent, graphene powder and high-speed tool steel powder; drying the mixed solution to obtain mixed powder; loading the dried mixed powder into a sheath, vacuumizing and degassing, and sealing the sheath; carrying out hot isostatic pressing treatment on the sealed sheath loaded with the mixed powder, wherein the hot isostatic pressing temperature is 950-1300 ℃, so that the mixed powder forms graphene composite high-speed tool steel; and separating the graphene steel composite high-speed tool steel from the sheath.

Description

Preparation method of graphene composite high-speed tool steel
Technical Field
The invention relates to the technical field of high-speed tool steel materials, in particular to a preparation method of graphene composite high-speed tool steel.
Background
The high-speed tool steel is mainly used for preparing high-speed cutting tools, such as drill bits, milling cutters, band saws and the like, and has the characteristics of high red hardness, good wear resistance, high strength and the like. The rapid development of modern manufacturing industry requires high speed tool steels to have better performance and stability, thereby improving the machining efficiency and machining precision thereof. In recent years, the quality, production technology and other aspects of domestic and foreign high-speed tool steel have been rapidly developed, and the development of high-speed tool steel also promotes the development of industrial products towards upgrading, individuation and high added value. However, the performance of the existing high-speed tool steel can only meet the cutting requirements of common materials, and for high-performance parts, the strength and hardness of the existing high-speed tool steel are still not high enough, and the toughness is low, so that the processing requirements of the high-performance parts cannot be met.
Disclosure of Invention
Based on the above, it is necessary to provide a method for preparing graphene composite high-speed tool steel, aiming at the problem of how to improve the mechanical properties of the high-speed tool steel.
The invention provides a preparation method of graphene composite high-speed tool steel, which comprises the following steps:
providing a mixed solution, wherein the mixed solution comprises a volatile organic solvent, graphene powder and high-speed tool steel powder;
drying the mixed solution to obtain mixed powder;
loading the dried mixed powder into a sheath, vacuumizing and degassing, and sealing the sheath;
carrying out hot isostatic pressing treatment on the sealed sheath loaded with the mixed powder, wherein the hot isostatic pressing temperature is 950-1300 ℃, so that the mixed powder forms a composite material green body; and
and separating the composite material blank from the sheath.
In one embodiment, the hot isostatic pressing is performed at a temperature of 1050 ℃ to 1200 ℃.
In one embodiment, the mass fraction of the graphene powder in the graphene composite high-speed tool steel is 0.01-2%.
In one embodiment, the sheet diameter of the graphene powder is 3-40 μm.
In one embodiment, the particle size of the high-speed tool steel powder is 10-70 μm.
In one embodiment, the step of drying comprises:
stirring the mixed solution at 40-50 ℃ until part of the volatile organic solvent is removed to form slurry; and
and drying the slurry in vacuum, and completely removing the volatile organic solvent in the slurry.
In one embodiment, the step of vacuum degassing comprises:
vacuumizing the sheath loaded with the mixed powder until the vacuum degree in the sheath is less than or equal to 1.0 x 10-2Pa; and
and heating the ladle sleeve loaded with the mixed powder under the vacuum degree, wherein the heating temperature is 400-600 ℃.
In one embodiment, the heating time is 2 hours to 10 hours.
In one embodiment, the preparation method of the graphene composite high-speed tool steel further comprises the following steps: and a step of performing low-temperature ball milling on the dried mixed powder between the drying treatment step and the vacuumizing degassing treatment step, wherein the temperature of the low-temperature ball milling is-80 ℃ to-160 ℃.
In one embodiment, the preparation method of the graphene composite high-speed tool steel further comprises the step of machining the composite material blank.
In one embodiment, the organic solvent is absolute ethanol.
In one embodiment, the high-speed tool steel powder body comprises iron elements, non-graphite carbon elements and other elements, and the mass fraction of the non-graphite carbon elements in the graphene composite high-speed tool steel is 1.4-1.8%.
In one embodiment, the other elements include the following elements in the graphene composite high-speed tool steel by mass fraction:
Cr:4.0％～5.0％；
V:4.0％～5.5％；
Mo:1.5％～2.5％；
Co:7.5％～8.2％；
W:10.2％～12％；
Mn:≤0.3％；
Si:≤0.6％。
in one embodiment, the high-speed tool steel powder is obtained by crushing a steel material, or is a mixture of elementary powders of constituent elements of the high-speed tool steel.
According to the preparation method of the graphene composite high-speed tool steel, the graphene and high-speed tool steel powder are mechanically mixed, vacuum pumped and subjected to hot isostatic pressing to prepare the graphene composite high-speed tool steel. By the hot isostatic pressing method, under the simultaneous action of high temperature and high pressure, the graphene and the high-speed tool steel powder are solidified and formed, so that the combination of the graphene and the high-speed tool steel powder matrix is realized, the problems that the graphene is easy to agglomerate and cannot be uniformly dispersed in the matrix and the high-temperature interface reaction is caused are solved, the process steps are simplified, and the oxidation degree of the graphene in the multi-step process is avoided. The temperature of hot isostatic pressing is controlled to be 950-1300 ℃, so that the graphene and the high-speed tool steel material are firmly combined, a good combination interface is formed between the graphene and steel elements, and the graphene composite high-speed tool steel with high mechanical property is formed.
The graphene composite high-speed tool steel can be applied to common cutting materials such as cutters, drill bits, band saws and the like, can also be applied to heavy-duty mechanical tools and precision punching tools made of high-strength materials, and is longer in service life.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below by way of examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a preparation method of graphene composite high-speed tool steel, which comprises the following steps:
s10, providing a mixed solution, wherein the mixed solution comprises a volatile organic solvent, graphene powder and high-speed tool steel powder;
s20, drying the mixed solution to obtain mixed powder;
s30, loading the dried mixed powder in a sheath for vacuum-pumping degassing treatment and sealing the sheath;
s40, carrying out hot isostatic pressing treatment on the sealed capsule loaded with the mixed powder, wherein the hot isostatic pressing temperature is 950-1300 ℃, so that the mixed powder forms a composite material green body;
s50, separating the composite material blank from the sheath.
According to the embodiment of the invention, the graphene composite high-speed tool steel is prepared by mechanically mixing, vacuum pumping and hot isostatic pressing treatment of graphene and high-speed tool steel powder. By the hot isostatic pressing method, under the simultaneous action of high temperature and high pressure, the graphene and the high-speed tool steel powder are solidified and formed, so that the combination of the graphene and the high-speed tool steel powder matrix is realized, the problems that the graphene is easy to agglomerate, cannot be uniformly dispersed in the matrix and can not react at a high-temperature interface are solved, the process steps are simplified, and the problem of graphene oxidation in a multi-step process is solved. The temperature of hot isostatic pressing is controlled to be 950-1300 ℃, so that the graphene and the high-speed tool steel material are firmly combined, a good combination interface is formed between the graphene and steel elements, and the graphene composite high-speed tool steel with high mechanical property is formed.
The high-speed tool steel powder can be powder of single substances of all constituent elements or powder obtained by crushing corresponding steel. The high-speed tool steel powder takes iron which accounts for more than 70% of the total mass of the graphene composite high-speed tool steel as a basic element, takes tungsten, molybdenum, chromium, vanadium and cobalt as main alloy elements, and comprises non-graphite carbon elements and high-carbon high-alloy steel of other doped elements. And calculating the use amount of each component element forming the high-speed tool steel powder according to the mass fraction of each component element in the graphene composite high-speed tool steel. In the graphene composite high-speed tool steel, the mass fraction of the non-graphite carbon element can be 1.4-1.8%, and preferably 1.6-1.7%; the mass fraction of the main alloy elements can be as follows: 10.2 to 12 percent of W, 1.5 to 2.5 percent of Mo, 4 to 5 percent of Cr, 4 to 5.5 percent of V and 7.5 to 8.2 percent of Co; the graphene composite high-speed tool steel can also comprise or not comprise Mn, Si or other alloy elements with lower content, preferably, Mn is less than or equal to 0.3 percent, and Si is less than or equal to 0.6 percent.
The mass ratio of the graphene powder to the high-speed tool steel powder is 0.01: 99.9-1: 49, namely the mass fraction of the graphene powder in the graphene composite high-speed tool steel is 0.01-2%. The graphene is original graphene, namely graphene which is not oxidized or connected with functional groups, the number of layers of the graphene can be 1-8, preferably 1-3, and the smaller the number of layers of the graphene is, the better the mechanical property of the formed graphene composite high-speed tool steel is. Preferably, in the graphene composite high-speed tool steel, the mass fraction of the graphene is 0.05-0.5%.
The particle size of the high-speed tool steel powder can be 10-70 mu m, the sheet size of the graphene powder is 3-40 mu m, and the range of the sheet size is more beneficial to uniform mixing between the steel powder and the graphene powder and improvement of the mechanical property of the graphene composite high-speed tool steel through mutual matching.
In step S10, the graphene powder and the high-speed tool steel powder are mixed in the volatile organic solvent in a uniformly dispersed manner, and the graphene powder in the mixed powder after the volatile organic solvent is volatilized is uniformly mixed in the high-speed tool steel powder.
In an embodiment, the step of providing the mixed liquid may include:
s12, mixing the graphene powder and the high-speed tool steel powder in a dry state to form first mixed powder;
and S14, mixing the first mixed powder with the volatile organic solvent.
The volatile organic solvent can be selected from volatile solvents which do not affect the properties of the graphene powder and the high-speed tool steel powder, and comprises at least one of organic solvents such as ethanol, diethyl ether and acetone, preferably, the components of the mixed solution contain no water, and the volatile organic solvent is absolute ethyl alcohol.
In step S12, the graphene powder and the high-speed tool steel powder may be uniformly mixed by a mechanical mixing method. Preferably, the graphene powder and the high-speed tool steel powder are uniformly mixed through a V-shaped powder mixer. The powder mixing time can be determined according to the particle sizes and the types of the graphene powder and the high-speed tool steel powder. In one embodiment, the powder mixing time may be 4 hours to 10 hours.
In step S14, the first mixed powder and the volatile organic solvent may be stirred to form the mixed solution.
In step S20, the drying process may be performed by heating the mixed solution at a temperature of 25 to 50 ℃. In an embodiment, the step S20 and the step S14 may be performed simultaneously, and the process steps may be simplified by heating the mixed solution during stirring to volatilize the volatile organic solvent.
Preferably, the drying process may include: stirring the mixed solution at 40-50 ℃ until part of the volatile organic solvent is removed to form slurry, wherein the content of the volatile organic solvent in the slurry is preferably 5-20% of the total weight of the slurry; and carrying out vacuum drying on the slurry to completely remove the volatile organic solvent in the slurry. Through the drying treatment, the surface of the high-speed tool steel powder can be prevented from being oxidized in the heating and drying process in the long-time aerobic environment. In one embodiment, the temperature of the vacuum drying may be 80 ℃ to 100 ℃.
In step S30, the step of vacuum degassing may include:
s32, vacuumizing the sheath loaded with the mixed powder until the vacuum degree in the sheath is less than or equal to 1.0 x 10-2Pa; and
s34, heating the coating loaded with the mixed powder under the vacuum degree, wherein the heating temperature is 400-600 ℃.
The step of firstly vacuumizing and then performing heat treatment is favorable for ensuring the thoroughness of vacuumizing and degassing treatment and avoiding the property of the mixed powder from being influenced in the process, and the graphene is prevented from being oxidized by the step of heating treatment.
In one embodiment, the heating time of step S34 is 2 hours to 10 hours.
In an embodiment, the method may further include: and ball-milling the mixed powder after the drying treatment between the drying treatment step and the vacuumizing degassing treatment step. Ball milling is carried out before the vacuumizing treatment step, so that the particle size of the mixed powder is smaller, and thorough degassing is facilitated. Meanwhile, the particle size of the mixed powder is reduced, so that the reduction of the interface distance between graphene and steel elements in the hot isostatic pressing is facilitated, and the mechanical property of the graphene composite high-speed tool steel is improved. The ball milling process is preferably low-temperature ball milling, and the low-temperature ball milling can not only uniformly mix the graphene powder and the high-speed tool steel powder, but also form interface combination between the graphene powder and the high-speed tool steel powder, so that the mechanical property of the graphene composite high-speed tool steel is further improved. Preferably, the temperature of the low-temperature ball milling can be-80 ℃ to-160 ℃.
In step S40, the mixed powder is loaded into the sealed sheath, and the sheath loaded with the mixed powder is subjected to high temperature while applying pressure equivalent to each other, so that the mixed powder is sintered and densified under the action of high temperature and high pressure to form the graphene composite high-speed tool steel. The material of the sheath may be selected from metal or glass. The pressurizing medium can adopt inert gases such as nitrogen, argon and the like.
Preferably, the hot isostatic pressing temperature may be 1050 ℃ to 1200 ℃. The pressure of the hot isostatic pressing can be 120MPa to 200 MPa. The hot isostatic pressing treatment time may be 2 hours to 5 hours. The temperature, the pressure and the time are matched with each other, so that the graphene steel composite material formed by hot isostatic pressing is more uniform in overall density, more compact in material and better in mechanical property.
Preferably, the preparation method of the graphene composite high-speed tool steel may further include: s60, separating the composite material blank from the sheath, and then carrying out mechanical processing and heat treatment on the composite material blank. The machining and heat treatment includes one or more of isothermal forging, rolling and quenching and tempering heat treatment.
In one embodiment, the machining comprises isothermal forging of the composite body at a temperature of 900 ℃ to 1200 ℃ at a forging rate of 0.005mm/min to 0.02 mm/min. The graphene composite high-speed tool steel can be shaped through isothermal forging, and the precision and the quality of the graphene composite high-speed tool steel are improved.
In an embodiment, the machining may further include the step of rolling the composite body, and the rolling temperature may be 1000 ℃ to 1200 ℃. In one embodiment, the thickness of the rolled blank may be 1.5mm to 30 mm. The rolling thickness can be determined according to the specific application of the graphene composite high-speed tool steel.
In an embodiment, the machining further includes quenching and tempering the composite material blank, where the quenching temperature is 1150-1200 ℃, the tempering temperature may be 500-600 ℃, and the tempering frequency may be 2-3 times. The quenching and tempering heat treatment can further improve the hardness and the wear resistance of the workpiece, so that the graphene composite high-speed tool steel can obtain better comprehensive mechanical properties.
The embodiment of the invention also provides graphene high-speed tool steel which can be prepared by the preparation method, the graphene high-speed tool steel comprises a high-speed tool steel matrix and graphene compounded with the high-speed tool steel matrix, the high-speed tool steel matrix comprises an iron element, a non-graphite carbon element and other elements, and the other elements comprise Cr, V, Mo, Co and W; the graphene composite high-speed tool steel comprises the following components in percentage by mass:
0.01% -2% of graphene;
1.4 to 1.8 percent of non-graphite carbon element;
Cr 4％～5％；
V 4％～5.5％；
Mo 1.5％～2.5％；
Co 7.5％～8.2％；
W 10.2％～12％。
according to the graphene composite high-speed tool steel provided by the embodiment of the invention, the two-dimensional nano material graphene with the mass fraction of 0.01% -2% and the high-speed tool steel matrix containing specific elements are uniformly compounded, and the graphene has a unique two-dimensional honeycomb crystal structure and extremely high bond strength, so that the graphene composite high-speed tool steel has high mechanical properties, particularly high bending strength, hardness and impact toughness.
Furthermore, not only the mass fraction of graphene affects the mechanical properties of the composite steel, but also the mass fraction of each element in the steel matrix of the high-speed tool affects the mechanical properties of the composite steel, for example, Cr promotes the growth of grains, which leads to the increase of brittleness of the steel, and W inhibits the growth of grains and has the function of grain refinement, thereby avoiding the embrittlement of the steel. According to the embodiment of the invention, the comprehensive mechanical properties of the graphene composite high-speed tool steel are more excellent by controlling the proportion of various elements in the matrix of the graphene and the high-speed tool steel.
In one embodiment, in the graphene composite high-speed tool steel, the other elements further comprise Mn and Si, wherein the mass fraction of Mn is less than or equal to 0.3%, and the mass fraction of Si is less than or equal to 0.6%.
The bending strength of the graphene composite high-speed tool steel can reach 3800-4500 Mpa, the hardness of the graphene composite high-speed tool steel can reach 70-80 HRC, and the impact toughness of the graphene composite high-speed tool steel can reach 70J/cm2～90J/cm2。
Example 1
The raw materials comprise 1000 g of graphene powder and powder of elements capable of forming high-speed tool steel, wherein 2 g of graphene, 16 g of amorphous carbon, 47 g of Cr, 18 g of Mo, 49 g of V, 110 g of W, 80 g of Co, 6 g of Si, 3 g of Mn and the balance of Fe. The average diameter of the powder of each element simple substance constituting the high-speed tool steel is 50 μm.
Putting the graphene powder and the elemental substance powder into a V-shaped powder mixer for mixing for 8 hours;
dispersing the mixed powder into absolute ethyl alcohol, drying the mixture into slurry under mechanical stirring at 40 ℃, transferring the slurry into a vacuum drying oven for complete drying treatment, and obtaining mixed powder at the drying temperature of 100 ℃;
the dried mixed powder is put into a cylindrical steel sheath and vacuumized until the vacuum pressure is 1 multiplied by 10-2After Pa, heating to 600 ℃, preserving heat for 2h, cooling to room temperature, and welding a steel sheath for sealing;
carrying out hot isostatic pressing treatment on the sealed steel ladle sleeve for 2 hours under the conditions that the temperature is 1200 ℃ and the pressure is 160MPa, and solidifying the mixed powder into a composite steel material;
removing the steel sheath outside the hot isostatic pressed composite steel, and then carrying out isothermal forging at 1180 ℃ at a forging rate of 0.01 mm/min;
rolling the isothermal forged composite steel at 1150 ℃;
quenching the rolled composite steel at 1180 ℃, and then tempering for 1h multiplied by 3 times at 550 ℃.
The mechanical properties of the prepared graphene steel composite high-speed tool steel were measured, and the results are shown in table 1.
Example 2
Basically the same as the preparation method of example 1, except that the average diameter of the powder of each element simple substance constituting the high-speed tool steel in the raw material is less than 10 μm.
The mechanical properties of the prepared graphene composite high-speed tool steel were measured, and the results are shown in table 1. As can be seen from table 1, the steel material prepared in example 1 has better properties in terms of bending strength, hardness, impact toughness and the like than example 2, and it is demonstrated that controlling the grain size in a proper range is beneficial to enhancing the mechanical properties of the graphene composite high-speed tool steel.
Example 3
The raw materials and the preparation method are basically the same as those of the example 1, except that the mixed powder is dispersed in absolute ethyl alcohol and then is directly and thoroughly dried under mechanical stirring at 100 ℃ in an open environment to obtain the mixed powder.
The mechanical properties of the prepared graphene composite high-speed tool steel were measured, and the results are shown in table 1. As can be seen from table 1, the steel material prepared in example 3 has lower properties than example 1 due to a certain degree of oxidation of graphene during the drying process of example 3.
Example 4
The raw materials and the preparation method are basically the same as those of the example 1, except that the mixed powder after drying treatment is subjected to low-temperature ball milling before sheathing, the temperature of the low-temperature ball milling is-120 ℃, and the ball milling time is 6 hours.
The mechanical properties of the prepared graphene steel composite high-speed tool steel were measured, and the results are shown in table 1 below. As can be seen from Table 1, low temperature ball milling is advantageous in improving the mechanical properties of high speed tool steels.
Example 5
The raw materials and the preparation method are basically the same as those of the example 1, except that the mixed powder after drying treatment is ball-milled at normal temperature before sheathing, the ball-milling temperature is 25 ℃, and the ball-milling time is 6 hours.
The mechanical properties of the prepared graphene steel composite high-speed tool steel were measured, and the results are shown in table 1 below.
As can be seen from Table 1, graphene is oxidized to a certain extent during the normal-temperature ball milling process, which is not favorable for improving the mechanical properties of the high-speed tool steel.
Comparative example 1
The preparation method is basically the same as that of example 1, except that graphene is not added to the raw materials.
The mechanical properties of the prepared graphene steel composite high-speed tool steel were measured, and the results are shown in table 1 below.
Comparative example 2
The same raw materials as those in example 1, except that a cold isostatic pressing process is adopted, and the preparation method comprises the following steps:
specifically, a steel sheath sealed with mixed powder is prepared by the same steps and under the same conditions as those of the embodiment 1, and the steel sheath is subjected to cold isostatic pressing treatment at 25 ℃ under the pressure of 300MPa for 10 min; the resulting composite steel was sintered at 1150 ℃ for 2 hours, and then subjected to the same isothermal forging, rolling, quenching and tempering steps as in example 1.
The mechanical properties of the prepared graphene steel composite high-speed tool steel were measured, and the results are shown in table 1 below.
Comparative example 3
The same raw materials as in example 1, except that the pressure forming and high temperature sintering processes were used.
Specifically, the same procedure as in example 1 was used to prepare a mixed powder under the same conditions.
And (3) putting the mixed powder into a cylindrical die, compacting the mixed powder by using a 2000T press, and keeping the pressure for 10 min. And heating the pressed and formed blank to 1150 ℃, sintering, keeping the temperature for 2 hours to obtain a composite steel, and then carrying out isothermal forging, rolling, quenching and tempering steps which are the same as those of the embodiment 1.
The mechanical properties of the prepared graphene steel composite high-speed tool steel were measured, and the results are shown in table 1 below.
Comparative example 4
Essentially the same procedure as for example 1 was followed except that the hot isostatic pressing temperature was 850 ℃.
The mechanical properties of the prepared graphene composite high-speed tool steel were measured, and the results are shown in table 1.
Comparative example 5
The same preparation method as in example 1 was repeated except that the mass of Cr in the raw material was increased to 100 g and the amount of Fe was decreased to 10% by mass.
The mechanical properties of the prepared graphene steel composite high-speed tool steel were measured, and the results are shown in table 1 below.
Comparative example 6
The same preparation method as in example 1 was repeated except that the mass of W in the raw material was reduced to 50 g and the corresponding amount of Fe was increased to make the mass fraction of W5%.
The mechanical properties of the prepared graphene steel composite high-speed tool steel were measured, and the results are shown in table 1 below.
TABLE 1
Graphene composite high-speed tool steel Bending strength Hardness of Impact toughness α k
Example 1 4000MPa 72HRC 88J/cm2
Example 2 3450MPa 67HRC 48J/cm2
Example 3 3560MPa 68HRC 50J/cm2
Example 4 4050MPa 73HRC 90J/cm2
Example 5 3550MPa 68HRC 50J/cm2
Comparative example 1 2900MPa 60HRC 39J/cm2
Comparative example 2 3100MPa 65HRC 42J/cm2
Comparative example 3 3230MPa 64HRC 41J/cm2
Comparative example 4 3010MPa 64HRC 40J/cm2
Comparative example 5 2800MPa 59HRC 38J/cm2
Comparative example 6 3055MPa 61HRC 44J/cm2
As can be seen from Table 1, the steel prepared in the examples is better than the steel prepared in the comparative examples in mechanical properties such as bending strength, hardness and impact toughness, and the addition of graphene, the consolidation forming process, the hot isostatic pressing temperature and the element mass fraction ratio are key factors influencing the mechanical properties of the steel, and the graphene composite high-speed tool steel is beneficial to having excellent mechanical properties, especially higher bending strength, hardness and impact toughness by comprehensively controlling the key factors.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (12)

1. The preparation method of the graphene composite high-speed tool steel is characterized by comprising the following steps:
providing a mixed solution, wherein the mixed solution is composed of a volatile organic solvent, graphene powder and high-speed tool steel powder, the high-speed tool steel powder is composed of iron elements, non-graphite carbon elements and other elements, the mass fraction of the non-graphite carbon elements in the graphene composite high-speed tool steel is 1.4% -1.8%, and the other elements in the graphene composite high-speed tool steel account for the following mass fractions: 4.0 to 5.0 percent of Cr; v is 4.0 to 5.5 percent; 1.5 to 2.5 percent of Mo; 7.5 to 8.2 percent of Co; 10.2 to 12 percent of W; mn is less than or equal to 0.3 percent; si is less than or equal to 0.6 percent;
drying the mixed solution to obtain mixed powder;
loading the dried mixed powder into a sheath, vacuumizing and degassing, and sealing the sheath;
carrying out hot isostatic pressing treatment on the sealed sheath loaded with the mixed powder, wherein the hot isostatic pressing temperature is 950-1300 ℃, so that the mixed powder forms a composite material green body; and
and separating the composite material blank from the sheath.
2. The method for preparing the graphene composite high-speed tool steel according to claim 1, wherein the hot isostatic pressing temperature is 1050 ℃ to 1200 ℃.
3. The preparation method of the graphene composite high-speed tool steel according to claim 1, wherein the graphene powder accounts for 0.01-2% of the graphene composite high-speed tool steel in mass percentage.
4. The method for preparing the graphene composite high-speed tool steel according to claim 1, wherein the sheet diameter of the graphene powder is 3-40 μm.
5. The method for preparing the graphene composite high-speed tool steel according to claim 1, wherein the particle size of the high-speed tool steel powder is 10-70 μm.
6. The method for preparing the graphene composite high-speed tool steel according to claim 1, wherein the drying treatment step comprises:
stirring the mixed solution at 40-50 ℃ until part of the volatile organic solvent is removed to form slurry; and
and drying the slurry in vacuum, and completely removing the volatile organic solvent in the slurry.
7. The method for preparing the graphene composite high-speed tool steel according to claim 1, wherein the step of vacuumizing and degassing treatment comprises the following steps:
vacuumizing the sheath loaded with the mixed powder until the vacuum degree in the sheath is less than or equal to 1.0 x 10-2Pa; and
and heating the ladle sleeve loaded with the mixed powder under the vacuum degree, wherein the heating temperature is 400-600 ℃.
8. The method for preparing the graphene composite high-speed tool steel according to claim 7, wherein the heating time is 2 to 10 hours.
9. The method for preparing the graphene composite high-speed tool steel according to claim 1, further comprising: and a step of performing low-temperature ball milling on the dried mixed powder between the drying treatment step and the vacuumizing degassing treatment step, wherein the temperature of the low-temperature ball milling is-80 ℃ to-160 ℃.
10. The method for preparing the graphene composite high-speed tool steel according to claim 1, further comprising the step of machining the composite material blank.
11. The method for preparing the graphene composite high-speed tool steel according to claim 1, wherein the organic solvent is absolute ethyl alcohol.
12. The method for producing the graphene composite high-speed tool steel according to claim 1, wherein the high-speed tool steel powder is obtained by crushing a steel material or is a mixture of elemental powders of constituent elements of the high-speed tool steel.
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