CN111663068B - HfC modified WC-Co composite material with nearly equal particle size, and preparation method and application thereof - Google Patents
HfC modified WC-Co composite material with nearly equal particle size, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an HfC modified WC-Co composite material with a nearly equal particle size, and a preparation method and application thereof, wherein the composite material comprises the following substances in percentage by mass: 87.1-88.0 wt% of WC, 11.0-12.0 wt% of Co, 0.9-1.1 wt% of HfC, and the balance of inevitable impurities, wherein the initial particle size of the HfC is 0.7-0.8 μm, and the initial particle size of the WC is 0.7-0.9 μm. The method comprises the following steps: putting WC, Co and HfC powder weighed in proportion into a ball milling tank containing hard alloy grinding balls, and carrying out wet ball milling to prepare ball milling slurry; drying the ball-milling slurry to remove the solvent, and sieving to obtain composite powder with the particle size of less than or equal to 75 mu m; the composite powder is put in a mould to be pretreated at high temperature in a vacuum furnace, and then is sintered, cured and formed by adopting discharge plasma. The application is in a cutter material or a mould material. The WC-Co composite material prepared by the invention has the advantages of fine and uniform grain size, high hardness of more than 91HRA and bending strength of about 3000MPa, and is suitable for being used as a high-performance cutter material or a die material.
Description
Technical Field
The invention relates to the field of hard alloy and powder metallurgy, in particular to a HfC modified WC-Co composite material with a nearly equal particle size, a preparation method and application thereof.
Background
Tungsten carbide-cobalt (WC-Co) hard alloy has a series of excellent performances such as high strength, high hardness, high elastic modulus, high thermal conductivity, high temperature resistance, corrosion resistance and the like, so that the tungsten carbide-cobalt (WC-Co) hard alloy is widely applied to the industrial fields such as metal cutting processing, rock drilling and mining, forming dies, wear-resistant parts and the like.
Domestic and foreign researches show that the mechanical property of the WC-Co hard alloy can be effectively improved by refining the crystal grains of the WC-Co hard alloy. The sintering temperature of the traditional WC-Co hard alloy is generally between 1100 ℃ and 1600 ℃, WC crystal grains can be dissolved and separated out in a liquid phase in the temperature range, particularly when the hard alloy is sintered at the temperature above the temperature of the liquid phase generated by Co melting, the WC crystal grains obviously grow up, even the WC crystal grains abnormally grow up to form thick crystal grains, and the WC crystal grains can grow into the large crystal grains in a crystal grain rotating and combining mode even if the solid phase sintering is carried out at the temperature lower than the liquid phase forming temperature. However, the presence of coarse grains can lead to deterioration of the mechanical properties of the cemented carbide, thereby limiting the use of cemented carbides.
At present, the method for inhibiting the growth of WC crystal grains is mainly to add a crystal grain growth inhibitor, such as TiC, VC and Cr, into WC-Co hard alloy3C2Carbide or composite carbide such as TaC and NbC. There is no consensus on the mechanism of the inhibitor to refine the WC grains, but the following three can be basically classified: (1) the inhibitor can be adsorbed on the surface of the tungsten carbide particles to reduce the surface energy of the tungsten carbide, thereby reducing the dissolution speed of the tungsten carbide in a high-temperature liquid phase and the solubility of the tungsten carbide particles in the liquid phase, and effectively controlling the continuous growth process of tungsten carbide grains in the sintering process; (2) the inhibitor can be dissolved in Co in a solid manner, so that the solubility of W in Co is reduced, and the process of recrystallization of fine tungsten carbide particles through a liquid phase is hindered; (3) the inhibitor is partially polymerized along the WC/WC interface, so that the migration of the tungsten carbide interface is blocked, and further, the tungsten carbide particles are prevented from being aggregated and grown.
The grain size of the grain growth inhibitor adopted by the WC-Co hard alloy is generally 3-5 times or even higher than that of WC, so that the grain growth inhibitor is beneficial to relatively uniform distribution of a small amount of added inhibitor at a WC/WC grain interface, and the inhibition effect of the grain growth inhibitor on WC in the sintering process is fully exerted. Such a large difference in particle size generally corresponds to a large difference in grain size, and therefore, the grain growth inhibitor added to the WC cemented carbide suppresses the growth of WC grains, but causes a decrease in toughness of the WC — Co cemented carbide. In addition, the grain size of the grain growth inhibitor is mostly nano-scale, and agglomeration is easy to occur, so that the grain growth inhibitor is difficult to really realize uniform dispersion distribution in WC-Co alloy, and is not favorable for fully exerting the inhibition effect on the growth of WC grains, thereby reducing the improvement effect on the structure performance of the hard alloy.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects of the prior art, the invention aims to provide a WC-Co composite material modified by HfC with a near-equal grain diameter, which has fine and uniform grains, high hardness and high bending strength, the invention also aims to provide a preparation method of the WC-Co composite material modified by HfC with a near-equal grain diameter, which reduces the sintering preparation cost and improves the sintering preparation efficiency, and the invention also aims to provide a WC-Co composite material modified by HfC with a near-equal grain diameter, which is applied to a cutter material or a die material.
The technical scheme is as follows: the invention relates to a HfC modified WC-Co composite material with a nearly equal particle size, which comprises the following substances in percentage by mass: 87.1 to 88.0wt% of WC, 11.0 to 12.0wt% of Co, 0.9 to 1.1wt% of HfC, and the balance of unavoidable impurities, wherein the initial particle size of HfC is 0.7 to 0.8 μm, and the initial particle size of WC is 0.7 to 0.9 μm. The HfC can reduce the sharpness of WC crystal grains, make the WC crystal grains deformed and inhibit the growth of the WC crystal grains.
The preparation method of the HfC modified WC-Co composite material with the approximate equal grain diameter comprises the following steps:
(1) putting WC, Co and HfC powder weighed in proportion into a ball milling tank containing hard alloy grinding balls, and carrying out wet ball milling, wherein a ball milling medium is cyclohexane, so as to prepare ball milling slurry; the ball milling medium is cyclohexane, so that excessive oxygen can be prevented from being sucked;
(2) drying the ball-milling slurry to remove the solvent, and sieving to obtain composite powder with the particle size of less than or equal to 75 mu m;
(3) placing the composite powder in a mold, and performing high-temperature pretreatment in a vacuum furnace with the vacuum degree of not more than 1x10-3Pa, the heating rate is 10-30 ℃/min, the pretreatment temperature is 1250-1350 ℃, the heat preservation time is 60-90 min, then, the sintering and curing molding is carried out by adopting discharge plasma, the sintering pressure is 30-50 MPa, the vacuum degree is less than or equal to 6Pa, the heating rate is 50-200 ℃/min, the sintering temperature is 1100-1200 ℃, and the heat preservation time is 10-20 min, so that the WC-Co composite material containing HfC is obtained.
The HfC modified WC-Co composite material with the approximate equal grain diameter is applied to a cutter material or a die material, and has the advantages of fine and uniform grain size, high hardness of more than 91HRA and bending strength of about 3000 MPa.
Has the advantages that: compared with the prior art, the invention has the following remarkable characteristics:
1. the prepared WC-Co composite material has fine and uniform grain size, high hardness of more than 91HRA and bending strength of about 3000MPa, and is suitable for being used as a high-performance cutter material or a die material;
2. according to the invention, HfC with a grain diameter nearly equal to that of WC is added into WC containing 11.0-12.0 wt% of Co, so that the problem of discontinuous structure grain size caused by mismatching of the grain diameter of the traditional grain growth inhibitor and the grain diameter of WC is avoided; the particle sizes of the initial HfC and the initial WC are 0.7-0.8 mu m and 0.7-0.9 mu m respectively, the submicron powder is easier to disperse compared with the nanoscale powder, the self agglomeration of the HfC and the WC powder can be avoided, the HfC is beneficial to the uniform dispersion distribution of the HfC in WC-Co and the uniform dispersion distribution of the WC in Co, and the cost of raw materials is obviously lower than that of the corresponding nanopowder;
3. after 0.9-1.1 wt% of HfC with nearly equal particle size is added into WC-Co, the WC crystal grains are refined by utilizing the inhibiting effect of HfC with lower content and particle size of 0.7-0.8 mu m on the growth of WC crystal grains, so that the hardness of the WC composite material is improved, the weakening effect of HfC with lower hardness on the hardness of the WC composite material is inhibited, and the toughness of the WC-Co composite material is improved by utilizing the good interface combination of HfC and Co;
4. the WC-Co composite material is prepared by adopting a method combining vacuum pretreatment and spark plasma sintering technologies, so that on one hand, the vacuum pretreatment is facilitated to promote the uniform distribution of Co among WC crystal grains and the wetting among WC-Co, on the other hand, the spark plasma sintering technology is utilized to realize the rapid sintering densification and inhibit the growth of crystal grains at a lower temperature, and the organization and the performance of the WC-Co composite material are further improved while the sintering preparation cost is reduced and the sintering preparation efficiency is improved.
Drawings
FIG. 1 is a back scattering scanning electron microscope image of a WC-Co composite material modified by doping HfC with a nearly equal particle size obtained in example 1 of the invention;
FIG. 2 is a graph showing the grain size distribution of the WC-Co composite material modified by doping HfC with a nearly equal grain size obtained in example 1 of the present invention;
FIG. 3 is a back scattering scanning electron microscope image of the WC-Co composite material modified by doping HfC with nearly equal particle size obtained in example 2 of the invention;
FIG. 4 is a scanning electron microscope image of secondary electrons of the WC-Co composite material modified by doping HfC with nearly equal particle size obtained in example 3 of the invention;
FIG. 5 is a graph of hardness and mechanical properties of WC-Co-HfC cemented carbide according to the present invention.
Detailed Description
In the following examples, the starting materials were all available as received.
Example 1
The WC-Co composite material modified by doping HfC with nearly equal grain diameter and the preparation method thereof are prepared by the following steps:
(1) pouring 88.0g of WC (grain size 08 μm, purity > 99.9%, Xiamen Jinlu Co., Ltd.), 1.0g of HfC (grain size 0.7 μm, Nanjing Youtian Metal technology Co., Ltd.), 11.0g of Co (grain size 0.8 μm, Xiamen Jinlu Co., Ltd.) into a 250ml cemented carbide pot, and adding cyclohexane as a solvent (the volume of the obtained mixed slurry does not exceed 2/3 of the volume of the ball mill pot) to obtain a mixed slurry; and (3) placing the ball milling tank filled with the mixed slurry on a planetary ball mill for wet ball milling (the rotating speed is 250r/min, and the ball milling time is 24 hours) to obtain ball milling slurry.
(2) And (3) putting the ball-milled slurry into a vacuum drying oven, vacuumizing and drying until the residual amount of the solvent is less than or equal to 1%, taking out the dried powder, grinding and sieving to obtain the composite powder with the particle size of less than or equal to 75 microns.
(3) 34.0g of composite powder was charged into the inner diameter
And outer diameter
In the cylindrical graphite die, the powder, the female die and the punch are separated by graphite paper for demolding, and the graphite die filled with the composite powder is put into a vacuum furnace for pretreatment. The pretreatment parameters are as follows: the atmosphere is high vacuum (less than or equal to 1x 10)-3Pa), rate of temperature rise: 20 deg.C/min at 1300 deg.CThe temperature is 60 min.
(4) Taking out the pretreated graphite mold filled with the composite powder, and coating a layer of graphite felt with the thickness of 10mm outside the female mold to reduce heat radiation loss; and placing the graphite mold filled with the composite powder in a discharge plasma sintering furnace for sintering to obtain the WC-Co composite material doped with the HfC particles. The sintering parameters are as follows: the sintering atmosphere is low vacuum (less than or equal to 6Pa), the sintering pressure is 30MPa, the heating rate is 100 ℃/min, the sintering temperature is 1175 ℃, and the heat preservation time is 10 min.
The density of the WC-Co composite material doped with HfC prepared by the embodiment is 97.6%, the average grain diameter is 0.81 μm (the grain diameter is counted by adopting Nanomeasurer by 300 grains), the hardness is 92.5HRA, and the bending strength is 3094MPa (three-point bending).
The back scattering scanning electron microscope image of the WC-Co composite material modified by the doped HfC having a nearly equal particle size prepared in this embodiment is shown in fig. 1, and it can be seen from the microstructure image that the particle sizes of most of the grains are not greatly different, and the microstructure is relatively uniform. The grain size distribution graph is shown in fig. 2, according to the statistical result of the grain sizes, it can be seen that most of the grain sizes are 0.3-1.2 micrometers, and a few of the grain sizes are in the micrometer level, and compared with the material added with the nanometer level particles, the grain sizes of the material are more continuous. The average grain size is 0.81 mu m, and no significant growth occurs and the grain size is kept smaller than the primary grain size of 0.7-0.9.
Example 2
The WC-Co composite material modified by doping HfC with nearly equal grain diameter and the preparation method thereof are prepared by the following steps:
(1) pouring 87.9g of WC (particle size 0.7 μm, purity > 99.9%, Xiamen Jinlu Co., Ltd.), 1.1g of HfC (particle size 0.8 μm, Nanjing Youtian Metal technology Co., Ltd.), 11.0g of Co (particle size 0.8 μm, Xiamen Jinlu Co., Ltd.) into a 250ml cemented carbide pot, and adding cyclohexane as a solvent (the volume of the obtained mixed slurry does not exceed 2/3 of the volume of the ball mill pot) to obtain a mixed slurry; and (3) placing the ball milling tank filled with the mixed slurry on a planetary ball mill for wet ball milling (the rotating speed is 250r/min, and the ball milling time is 24 hours) to obtain ball milling slurry.
Step (2) is the same as in example 1;
(3) 34.0g of composite powder was charged into the inner diameter
And outer diameter
In the cylindrical graphite die, the powder, the female die and the punch are separated by graphite paper for demolding, and the graphite die filled with the composite powder is put into a vacuum furnace for pretreatment. The pretreatment parameters are as follows: the atmosphere is high vacuum (less than or equal to 1x 10)-3Pa), rate of temperature rise: 10 ℃/min, 1350 ℃ and 60min of heat preservation time.
(4) Taking out the pretreated graphite mold filled with the composite powder, and coating a layer of graphite felt with the thickness of 10mm outside the female mold to reduce heat radiation loss; and placing the graphite mold filled with the composite powder in a discharge plasma sintering furnace for sintering to obtain the WC-Co composite material doped with the HfC particles. The sintering parameters are as follows: the sintering atmosphere is low vacuum (less than or equal to 6Pa), the sintering pressure is 50MPa, the heating rate is 200 ℃/min, the sintering temperature is 1100 ℃, and the heat preservation time is 20 min.
The density of the WC-Co composite material doped with HfC prepared by the embodiment is 97.2%, the average grain diameter is 0.84 μm (the grain diameter is counted by adopting Nanomeasurer by 300 grains), the hardness is 92.0HRA, and the bending strength is 2767MPa (three-point bending).
A back scattering scanning electron microscope image of the material prepared in this example is shown in fig. 3, and the obtained structure is different from that of example 1 due to different contents and particle sizes of the used HfC.
Example 3
The WC-Co composite material modified by doping HfC with nearly equal grain diameter and the preparation method thereof are prepared by the following steps:
(1) pouring 87.1g of WC (particle size 0.9 μm, purity > 99.9%, Xiamen Jinlu Co., Ltd.), 0.9g of HfC (particle size 0.8 μm, Nanjing Youtian Metal technology Co., Ltd.), 12.0g of Co (particle size 0.8 μm, Xiamen Jinlu Co., Ltd.) into a 250ml cemented carbide pot, and adding cyclohexane as a solvent (the volume of the obtained mixed slurry does not exceed 2/3 of the volume of the ball mill pot) to obtain a mixed slurry; and (3) placing the ball milling tank filled with the mixed slurry on a planetary ball mill for wet ball milling (the rotating speed is 250r/min, and the ball milling time is 24 hours) to obtain ball milling slurry.
Step (2) is the same as in example 1;
(3) 34.0g of composite powder was charged into the inner diameter
And outer diameter
In the cylindrical graphite die, the powder, the female die and the punch are separated by graphite paper for demolding, and the graphite die filled with the composite powder is put into a vacuum furnace for pretreatment. The pretreatment parameters are as follows: the atmosphere is high vacuum (less than or equal to 1x 10)-3Pa), rate of temperature rise: 30 ℃/min, 1250 ℃ and the heat preservation time of 90 min.
(4) Taking out the pretreated graphite mold filled with the composite powder, and coating a layer of graphite felt with the thickness of 10mm outside the female mold to reduce heat radiation loss; and placing the graphite mold filled with the composite powder in a discharge plasma sintering furnace for sintering to obtain the WC-Co composite material doped with the HfC particles. The sintering parameters are as follows: the sintering atmosphere is low vacuum (less than or equal to 6Pa), the sintering pressure is 30MPa, the heating rate is 50 ℃/min, the sintering temperature is 1200 ℃, and the heat preservation time is 15 min.
The density of the WC-Co composite doped with HfC prepared in this example is 97.8%, the average grain size is 0.98um (300 grain diameters counted by Nanomeasurer), the hardness is 91.6HRA, and the bending strength is 2656MPa (three-point bending).
The secondary electron scanning electron microscope picture of the material prepared in example 3 is shown in fig. 4, and it can be seen that there are individual, coarse, plate-like WC grains, because in this example the amount of HfC added is small, and part of the WC grains are not inhibited by the HfC particles, resulting in abnormal growth of part of the grains. However, as a whole, under the suppression effect of HfC, the grain size in the structure is not greatly different except for individual coarse grains, the entire structure is more uniform, and the grain size is more continuous.
The hardness and bending strength of the composite materials obtained in examples 1, 2 and 3 are summarized in FIG. 5, and it can be seen that the composite material obtained by the method of the present invention has high hardness of 91HRA or more and bending strength of about 3000MPa, and is suitable for use as a high-performance cutter material or a mold material.
Claims (7)
1. A preparation method of a WC-Co composite material modified by HfC with a nearly equal particle size is characterized by comprising the following steps:
(1) putting WC, Co and HfC powder weighed in proportion into a ball milling tank containing hard alloy grinding balls, and carrying out wet ball milling to prepare ball milling slurry;
(2) drying the ball-milling slurry to remove the solvent, and sieving to obtain composite powder with the particle size of less than or equal to 75 mu m;
(3) placing the composite powder in a mould to carry out high-temperature pretreatment in a vacuum furnace, and then sintering, curing and molding by adopting discharge plasma to obtain a WC-Co composite material containing HfC;
the approximate-equal-particle-size HfC modified WC-Co composite material comprises the following substances in percentage by mass: 87.1-88.0 wt% of WC, 11.0-12.0 wt% of Co, 0.9-1.1 wt% of HfC, and the balance of inevitable impurities, wherein the initial particle size of HfC is 0.7-0.8 mm, and the initial particle size of WC is 0.7-0.9 mm.
2. The preparation method of the near-uniform-particle-size HfC modified WC-Co composite material as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (1), the ball milling medium is cyclohexane.
3. The preparation method of the near-uniform-particle-size HfC modified WC-Co composite material as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (3), the vacuum degree of the high-temperature pretreatment is less than or equal to 1x10-3Pa。
4. The preparation method of the near-isoparticle-size HfC modified WC-Co composite material as claimed in claim 3, wherein the preparation method comprises the following steps: in the step (3), the temperature rise rate of the high-temperature pretreatment is 10-30 ℃/min, the pretreatment temperature is 1250-1350 ℃, and the heat preservation time is 60-90 min.
5. The preparation method of the near-uniform-particle-size HfC modified WC-Co composite material as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (3), the sintering pressure of the spark plasma sintering is 30-50 MPa.
6. The preparation method of the near-uniform-particle-size HfC modified WC-Co composite material as claimed in claim 5, wherein the preparation method comprises the following steps: in the step (3), the vacuum degree of the spark plasma sintering is less than or equal to 6 Pa.
7. The preparation method of the near-uniform-particle-size HfC modified WC-Co composite material as claimed in claim 6, wherein the preparation method comprises the following steps: in the step (3), the temperature rise rate of the spark plasma sintering is 50-200 ℃/min, the sintering temperature is 1100-1200 ℃, and the heat preservation time is 10-20 min.
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|---|---|---|---|---|
| CN101186981A (en) * | 2007-12-21 | 2008-05-28 | 北京工业大学 | High-intensity high-tenacity super fine crystal WC-10Co hard alloy preparation method |
| CN110106423A (en) * | 2019-06-13 | 2019-08-09 | 河源市全诚硬质合金有限公司 | A kind of preparation process of Talide |
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