CN114713819A - Superfine tungsten carbide coated high-speed steel composite powder and preparation method thereof - Google Patents
Superfine tungsten carbide coated high-speed steel composite powder and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a superfine tungsten carbide coated high-speed steel composite powder and a preparation method thereof, wherein the preparation method comprises the following steps: making the high-speed steel powder body in a fluidized state in a protective atmosphere; mixing high-speed steel particles, a tungsten source and reaction gas to carry out vapor deposition; and (4) carrying out gas-solid separation to obtain the superfine tungsten carbide coated high-speed steel composite powder. The superfine tungsten carbide coated high-speed steel composite powder is prepared by the method, the tungsten carbide coated high-speed steel composite powder realizes the uniform distribution of tungsten carbide on a microscale, the size of the tungsten carbide is refined, and the performance of powder metallurgy high-speed steel can be obviously improved.
Description
Technical Field
The invention belongs to the field of powder metallurgy of steel alloy, relates to a preparation method of coated high-speed steel composite powder, and particularly relates to ultrafine tungsten carbide coated high-speed steel composite powder and a preparation method thereof.
Background
The high-speed steel has the characteristics of high hardness, high wear resistance, high heat resistance and excellent toughness and toughness matching, and is mainly used for manufacturing metal cutting tools, extrusion dies and the like. Tungsten-based high-speed steel is a main high-speed steel material, and commonly used tungsten-based high-speed steels such as W18Cr4V, W6Mo5Cr4V2 and the like have excellent wear resistance associated with a large amount of high-hardness carbides contained in the structure thereof. In order to avoid carbide segregation and refine carbide caused by smelting method production, powder metallurgy high-speed steel appeared after 60 years of 20 th century. The powder metallurgy preparation process is to prepare the high-speed steel by utilizing metal powder through a certain forming process and finally through a proper sintering mode. The structure segregation generated in the smelting and solidification process is limited to the size of one powder particle, and the problem of macrosegregation in the whole high-speed steel is perfectly solved. The structure of the powder metallurgy high-speed steel is fine and dispersed carbides which are uniformly distributed in a matrix, macrostructure segregation is successfully eliminated and crystal grains are refined by utilizing a powder metallurgy mode, so that the service life of the high-speed tool steel is obviously prolonged. Meanwhile, the limitation of the traditional casting high-speed steel on the alloy content is thoroughly broken through by the powder metallurgy mode, so that the preparation of high-alloy-content tool steel with higher performance becomes possible.
The powder metallurgy high-speed steel is rapidly developed since the advent, gradually embodies the strong advantages of the powder metallurgy high-speed steel, and is compared with the traditional high-speed steel: (1) organization aspect: no alloy element segregation, fine and dispersed carbide, and no structural anisotropy caused by hot working due to powder metallurgy forming. (2) Mechanical properties: the high-speed steel has three main characteristics of high hardness, high toughness and high red hardness, and the addition amount of alloy elements can be increased due to the powder metallurgy preparation mode, so that the hardness of the high-speed steel is further improved, and the hardness after heat treatment can reach 67-70 HRC. In particular, addition of a large amount of W or the like promotes further improvement in red hardness, and 4 to 5HRC can be improved as compared with M2 high-speed steel. The structure refinement and segregation elimination can greatly improve the toughness of the powder high-speed steel, and the bending strength can also be obviously improved. (3) The preparation method comprises the following steps: the improvement of the structure enables the hot processing performance to be better, and compared with hard alloy, the hot processing performance is higher in cost performance, higher in cost advantage and good in grinding performance, because carbides of high-speed steel produced by a powder metallurgy process are uniformly dispersed and distributed in the structure. In contrast, carbides in traditional cast high-speed steel are easy to agglomerate, and the interaction of large carbides and a blade during grinding can cause edge breaking, so that the grinding performance of the high-speed steel can be improved by a powder metallurgy processing mode. (4) The service performance is as follows: mainly embodied in that the service life is prolonged, the cutting machine can be applied to high-speed cutting, and the yield is higher. The powder metallurgy high-speed steel is greatly improved in the aspects of structure, mechanical property and the like, the service performance is further greatly improved due to the high alloy content and the uniform and fine structure, and the service life of the high-speed steel is obviously prolonged due to the high hardness and the excellent initial property. In summary, the use of powder metallurgy in the production of high speed steel has prompted further development of tool materials. Further, powder metallurgy high-speed steel plays a significant role in high-quality cutting tools because of its excellent mechanical properties, no segregation, and fine structure.
However, the high-speed steel is used as the eutectic carbide tool steel, wherein the content of the alloying elements such as W, Mo, V, Cr and the like reaches more than 17 percent, the composition change range of the internal alloy carbide is large,these alloying elements form a large amount of eutectic carbides, which are mainly classified as M in high speed tool steels2C、M6C、M23C6And the like, which have a decisive influence on the structure and properties of high-speed steel. Wherein M is2C and M6The C two carbides are fishbone-shaped and harmful to performance, and the main component of the C two carbides is WC. Due to the composition segregation in the powder preparation process, W is combined with the C element added in the melt, and M is formed in the preparation process2C and M6The problem of large WC particles caused by the coarse mesh carbide of C causes local stress concentration in the material to cause cracks, and the processing performance, the mechanical property and the service life are seriously influenced. Therefore, how to obtain a dispersed fine tungsten carbide reinforced structure is a key problem for improving the performance and the service life of the powder metallurgy high-speed steel.
Disclosure of Invention
Aiming at the problems of performance decline, short service life and the like caused by the fact that the tungsten carbide structure is thick, the nanoscale tungsten carbide reinforcing phase is uniformly coated on the surface of the high-speed steel powder, the superfine tungsten carbide coated high-speed steel composite powder is prepared, the uniform dispersion distribution and the fine structure of the reinforcing phase tungsten carbide are realized from the powder source, and the mechanical property and the service life of the composite powder are greatly improved.
The invention aims to provide the superfine tungsten carbide coated high-speed steel composite powder and the preparation method thereof, and the preparation method ensures the uniform distribution of tungsten carbide and high-speed steel powder materials on a microscale, so as to improve the mechanical property of high-speed steel devices.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a preparation method of tungsten carbide coated high-speed steel composite powder, which comprises the following steps:
(1) screening the high-speed steel powder, placing the obtained high-speed steel powder with the particle size of 1-30 micrometers in a fluidized bed reactor, then discharging inert gas through an inert gas discharge port of the fluidized bed reactor, and exhausting internal air to ensure that the high-speed steel powder is in a fluidized state in a protective atmosphere.
(2) Tungsten source (WCl)6) Preheating to 275-347 ℃ outside a fluidized bed reactor, mixing a tungsten source and a carrier gas (Ar) in a mixer (the tungsten source is in a gas-liquid mixed state of atomized liquid drops), heating the fluidized bed reactor to 600-900 ℃, simultaneously introducing the tungsten source into the fluidized bed reactor in which the high-speed steel powder in the step (1) is positioned at a gas speed of 5-500 mL/min under the load of the carrier gas, and simultaneously introducing a reaction gas of an alkyne compound into the fluidized bed reactor at a gas speed of 75-500 mL/min, wherein the mixing time of the fluidized high-speed steel powder, the tungsten source and the reaction gas is 1-150 min, and the flow ratio of the tungsten source to the reaction gas is 1: 1-1: 10. the tungsten source of the present invention is entirely involved in the reaction, and the reaction gas is excessive, so the ratio of the total tungsten source to the high-speed steel powder is such that the content of tungsten carbide in the final product is 1 to 18 wt% (preferably 9 wt.% to 18 wt.%), which is converted to the tungsten source.
(3) And (3) after the mixing time in the step (2) is over, cooling the materials in the fluidized bed, and then carrying out gas-solid separation to obtain the product of the superfine tungsten carbide coated high-speed steel composite powder.
In the invention, the fluidization state in the step (1) not only enables the high-speed steel powder to be uniformly distributed in the fluidized bed reactor, but also provides a kinetic foundation for subsequent full reaction, and simultaneously exhausts the air in the fluidized bed reactor, thereby preventing oxygen in the air from being introduced into the high-speed steel powder in the form of impurities.
Preferably, the high-speed steel powder is W6Mo5Cr4V2 high-speed steel powder (the components comprise 0.15-0.40 wt% of Mn, less than or equal to 0.030 wt% of S, less than or equal to 0.030 wt% of P, 3.80-4.40 wt% of Cr, less than or equal to 0.30 wt% of Ni, 1.75-2.20 wt% of V, 4.50-5.50 wt% of Mo, 5.50-6.75 wt% of W, and Fe and inevitable impurities as matrix).
Preferably, the gas in the protective atmosphere in step (1) comprises any one or a combination of two of nitrogen and 2 gases in argon.
In the invention, the protective atmosphere can not only keep the high-speed steel powder in a fluidized state, but also isolate oxygen in the environment, thereby facilitating the subsequent controllable coating of tungsten carbide.
Preferably, the tungsten source in step (2) is WCl6，WCl6The preheating temperature is between 275 ℃ and 347 ℃, and can be, for example, 275 ℃, 290 ℃, 300 ℃, 310 ℃, 320 ℃, 330 ℃, 347 ℃, but is not limited to the values listed, and other values not listed in the range of values are equally applicable. WCl6After preheating, the mixed gas is formed with carrier gas and enters a fluidized bed reactor. Wherein, the carrier gas is the same as the protective atmosphere in the step (1).
Preferably, the gas flow rate of the tungsten source and carrier gas mixer in step (2) is 50mL/min-500mL/min, such as 50mL/min, 100mL/min, 150mL/min, 200mL/min, 300mL/min, 400mL/min, 500mL/min, but not limited to the values listed, and other values not listed in the range are equally applicable.
Preferably, the reaction gas in step (2) is acetylene, and the acetylene and the carrier gas form a mixed gas to enter the fluidized bed reactor. Wherein, the carrier gas is selected to be the same as the protective atmosphere in the step (1).
Preferably, the flow rate of the reaction gas and carrier gas mixer in step (2) is 75mL/min-500mL/min, such as 75mL/min, 100mL/min, 150mL/min, 200mL/min, 250mL/min, 300mL/min, 350mL/min, 400mL/min, 500mL/min, but not limited to the values listed, and other values not listed in this range are equally applicable.
Preferably, the temperature of the mixing in step (2) is 600 ℃ to 900 ℃, for example 600 ℃, 700 ℃, 800 ℃, 830 ℃, 850 ℃, 880 ℃, 900 ℃, but is not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, the mixing time in step (2) is 1min or more, for example, 1min, 5min, 10min, 15min, 20min, 30min, 40min, 50min, 60min, 120min, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
Preferably, the gas-solid separation method in step (3) includes any one of gravity settling and centrifugal settling. Wherein the gravity settling process comprises the steps of closing the carrier gas, the fluidized gas and the reaction gas, and standing for 30 minutes to realize gas-solid separation.
In another aspect, the invention provides the ultra-fine tungsten carbide coated high-speed steel composite powder prepared by the preparation method in the first aspect, wherein the tungsten carbide coated high-speed steel composite powder has a tungsten carbide coating layer with a mass fraction of 1-18 wt% (preferably 9-18 wt%).
The tungsten carbide coated high-speed steel composite powder is combined with a fluidized bed process technology through a chemical vapor deposition principle, a tungsten carbide shell is uniformly coated on the surface of the high-speed steel powder, the uniform distribution of the high-speed steel powder and a tungsten carbide material is realized on the powder scale, meanwhile, the fine tungsten carbide is dispersed and distributed, the mechanical property of the high-speed steel material is ensured, and the service life of a high-speed steel product is prolonged.
In a third aspect, the invention provides a sintering method of superfine tungsten carbide coated high-speed steel, which specifically comprises the following steps:
i, preparing the superfine tungsten carbide coated high-speed steel composite powder by adopting the preparation method of the superfine tungsten carbide coated high-speed steel composite powder.
And II, placing the superfine tungsten carbide coated high-speed steel composite powder prepared in the step I into a mold, placing the mold into a sintering furnace for cold press forming, wherein the pressure of the cold press forming is 18-22 MPa (preferably 20MPa), and keeping the pressure for 12-18 min (preferably 15 min).
And III, raising the temperature in the sintering furnace to 1180-1250 ℃ (preferably 1200 ℃), increasing the pressure of the die to 28-35 MPa (preferably 30MPa), and sintering for 50-80 min (preferably 60 min).
And IV, cooling the material sintered in the step III to 908-922 ℃ (916 ℃ is preferred), preserving the temperature for 50-80 min (60 min is preferred), cooling the material to room temperature in a furnace, and taking out the material to obtain the product of the superfine tungsten carbide coated high-speed steel.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, a tungsten source, reaction gas and fluidized high-speed steel powder with specific granularity are subjected to vapor deposition and fluidized reaction under specific conditions at specific temperature to combine, the size and the shape of the surface ultrafine tungsten carbide are determined by the proportion of the tungsten source and the reaction gas, and the coating amount is determined by the reaction time, so that the state of fine size and uniform dispersion distribution of the tungsten carbide (realized by vapor deposition) is realized from the source of powder, the excellent mechanical property of the high-speed steel product is ensured, and the service life of the high-speed steel product is greatly prolonged.
According to the invention, by setting the flow rate of the tungsten source and the flow rate of the reaction gas and reasonably setting parameters such as particle size, proportion and the like of the raw materials, the finally prepared composite powder has excellent mechanical properties, controllable coating amount and low cost, and is easy for large-scale batch production.
Drawings
FIG. 1 is an SEM image of the tungsten carbide coated high-speed steel composite powder prepared by the preparation method provided in example 1.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a preparation method of tungsten carbide coated high-speed steel composite powder, which comprises the following steps:
(1) the high-speed steel powder with the grain diameter of 1-30 mu m is in a fluidized state in the protective atmosphere of the fluidized bed reactor.
(2) On the basis of continuously performing the step (1), synchronously introducing a tungsten source and reaction gas into a fluidized bed reactor, mixing with high-speed steel powder at the mixing temperature of 700 ℃ for 60min, introducing 70ml of gas at the tungsten source temperature of 300 ℃, and introducing 60ml of reaction gas.
(3) And (4) after the reaction is finished, carrying out gas-solid separation to obtain the tungsten carbide coated high-speed steel composite powder.
Fig. 1 is an SEM image of the tungsten carbide coated high-speed steel composite powder obtained by the preparation method provided in this embodiment, and it can be seen from fig. 1 that the surface of the high-speed steel powder body is uniformly coated with fine tungsten carbide particles.
The tungsten carbide content of the tungsten carbide coated high-speed steel composite powder obtained by the preparation method provided by the embodiment is 10 wt.%.
Example 2
The embodiment provides a preparation method of tungsten carbide coated high-speed steel composite powder, which comprises the following steps:
(1) the high-speed steel powder with the grain diameter of 1-30 mu m is in a fluidized state in the protective atmosphere of the fluidized bed reactor.
(2) On the basis of continuously performing the step (1), synchronously introducing a tungsten source and reaction gas into a fluidized bed reactor, mixing with high-speed steel powder at the mixing temperature of 850 ℃ for 90min, introducing 80ml of gas at the tungsten source temperature of 200 ℃, and introducing 150ml of reaction gas.
(3) And (4) after the reaction is finished, carrying out gas-solid separation to obtain the tungsten carbide coated high-speed steel composite powder.
The tungsten carbide content of the tungsten carbide coated high-speed steel composite powder obtained by the preparation method provided by the embodiment is 15 wt.%. The microstructure of the obtained tungsten carbide coated high-speed steel alloy powder is similar to that of the embodiment 1, and therefore, the description thereof is omitted.
Example 3
The embodiment provides a preparation method of tungsten carbide coated high-speed steel composite powder, which comprises the following steps:
(1) the high-speed steel powder with the grain diameter of 1-30 mu m is in a fluidized state in the protective atmosphere of the fluidized bed reactor.
(2) On the basis of continuously performing the step (1), synchronously introducing a tungsten source and reaction gas into a fluidized bed reactor, mixing with high-speed steel powder at the mixing temperature of 900 ℃ for 120min, introducing the tungsten source at the temperature of 330 ℃ at the gas introduction speed of 90ml, and introducing the reaction gas at the gas introduction speed of 100 ml.
(3) And (4) after the reaction is finished, carrying out gas-solid separation to obtain the tungsten carbide coated high-speed steel composite powder.
The tungsten carbide content of the tungsten carbide coated high-speed steel composite powder obtained by the preparation method provided by the embodiment is 18 wt.%. And the microstructure of the obtained tungsten carbide coated high-speed steel alloy powder is similar to that of the tungsten carbide coated high-speed steel alloy powder in the embodiment 1, so that the detailed description is omitted.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. The preparation method of the superfine tungsten carbide coated high-speed steel composite powder is characterized by comprising the following steps of:
(1) screening the high-speed steel powder, placing the obtained high-speed steel powder with the particle size of 1-30 micrometers in a fluidized bed reactor, then discharging inert gas through an inert gas discharge port of the fluidized bed reactor, and exhausting internal air to ensure that the high-speed steel powder is in a fluidized state in a protective atmosphere;
(2) preheating a tungsten source to 275-347 ℃ outside a fluidized bed reactor, mixing the tungsten source with a carrier gas in a mixer, heating the fluidized bed reactor to 600-900 ℃, simultaneously introducing the tungsten source into the fluidized bed reactor in which the high-speed steel powder in the step (1) is located at a gas rate of 5-500 mL/min under the load of the carrier gas, and simultaneously introducing a reaction gas into the fluidized bed reactor at a gas rate of 75-500 mL/min, wherein the reaction gas is an alkyne compound, the mixing time of the fluidized high-speed steel powder, the tungsten source and the reaction gas is 1-150 min, and the flow ratio of the tungsten source to the reaction gas is (1: 1) - (1: 10);
(3) and (3) after the mixing time in the step (2) is over, cooling the materials in the fluidized bed, and then carrying out gas-solid separation to obtain the product of the superfine tungsten carbide coated high-speed steel composite powder.
2. The method for preparing the superfine tungsten carbide coated high-speed steel composite powder according to claim 1, wherein the chemical components of the high-speed steel powder in the step (1) comprise the following components in percentage by mass: mn: 0.15-0.40 wt%, S is less than or equal to 0.030 wt%, P is less than or equal to 0.030 wt%, Cr: 3.80-4.40 wt%, Ni less than or equal to 0.30 wt%, V: 1.75-2.20 wt%, Mo: 4.50-5.50 wt%, W: 5.50-6.75 wt%; the matrix is Fe and inevitable impurities, and the carrier gas in the step (2) is the same as the inert gas in the step (1).
3. The method for preparing the superfine tungsten carbide coated high-speed steel composite powder according to claim 1 or 2, wherein the inert gas in the step (1) is one or two of nitrogen and argon, and the inert gas discharge port is arranged at the bottom of the fluidized bed reactor.
4. The method for preparing the superfine tungsten carbide coated high-speed steel composite powder according to any one of claims 1 to 3, wherein in the step (2), a tungsten source and a reaction gas are respectively and independently introduced into a fluidized bed reactor in a protective atmosphere in which the high-speed steel powder is located under the load of a carrier gas.
5. The method for preparing the superfine tungsten carbide coated high-speed steel composite powder according to any one of claims 1 to 3, wherein the mixing time in the step (2) is 10-150 min; the tungsten source in the step (2) is WCl6(ii) a The preheating temperature of the tungsten source in the step (2) is 278-345 ℃.
6. The method for preparing the ultra-fine tungsten carbide coated high-speed steel composite powder according to any one of claims 1 to 3, wherein the alkyne compound in the step (2) is acetylene.
7. The method for preparing the ultra-fine tungsten carbide coated high-speed steel composite powder according to any one of claims 1 to 3, wherein the gas-solid separation method in the step (3) is any one of gravity settling and centrifugal settling.
8. The superfine tungsten carbide coated high-speed steel composite powder is characterized by being prepared by the preparation method of any one of claims 1 to 7.
9. The ultrafine tungsten carbide coated high-speed steel composite powder according to claim 8, wherein the mass fraction of tungsten carbide in the tungsten carbide coated high-speed steel composite powder is 1-18 wt.% (preferably 9-18 wt.%).
10. A sintering method of superfine tungsten carbide coated high-speed steel is characterized by comprising the following steps:
i, preparing the ultra-fine tungsten carbide coated high-speed steel composite powder by the method for preparing the ultra-fine tungsten carbide coated high-speed steel composite powder according to any one of claims 1 to 7;
II, placing the superfine tungsten carbide coated high-speed steel composite powder prepared in the step I into a mold, placing the mold into a sintering furnace for cold press forming, wherein the pressure of the cold press forming is about 18-22 MPa, and keeping the pressure for 12-18 min;
III, raising the temperature in the sintering furnace to 1180-1250 ℃, increasing the pressure of a die to 28-35 MPa, and sintering for 50-80 min;
and IV, cooling the material sintered in the step III to 908-922 ℃, preserving heat for 50-80 min, then cooling the material in a furnace to room temperature, and taking out the material to obtain the product of the superfine tungsten carbide coated high-speed steel.
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