CN108588462B - Preparation method of complex phase co-strengthening hard alloy material - Google Patents
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Abstract
The invention discloses a preparation method of a complex phase co-strengthening hard alloy material, which comprises the steps of obtaining tungsten carbide-based pre-alloy powder and titanium carbonitride-based pre-alloy powder through pre-alloying treatment, uniformly mixing the two powders with cobalt powder, performing secondary atomization drying granulation, then performing compression molding in a cold press, and finally sintering in a high-temperature vacuum tube furnace to finally obtain the complex phase co-strengthening hard alloy material.
Description
Technical Field
The invention relates to the technical field of alloy preparation, in particular to a preparation method of a complex phase co-strengthening hard alloy material.
Background
The contradiction between strength and toughness is a fatal defect of the traditional hard alloy material, and limits the new industrial popularization of the hard alloy. The commonly adopted methods such as powder pre-alloying, binder phase component transformation, heat treatment and the like have limited effect on improving the problem of toughness and toughness contradiction. Therefore, it is important to develop a new method for improving the toughness of cemented carbide.
Through reasonable structural design, the performance advantages of the strength component and the toughness component of the hard alloy are fully exerted, and the method is a key means for solving the contradiction problem of the toughness.
Disclosure of Invention
The invention provides a preparation method of a complex phase co-strengthening hard alloy material, aiming at the current situation of the research and development field that the common means is difficult to solve the problem of the obdurability of the hard alloy.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a complex phase co-strengthening hard alloy material comprises the following steps:
1) respectively placing tungsten carbide powder, nickel trinickel aluminide powder, titanium carbonitride powder and nickel powder in a high-energy ball mill, and performing pre-alloying treatment to obtain two kinds of pre-alloyed powder;
2) atomizing, drying and granulating the two pre-alloyed powders, and uniformly mixing the prepared tungsten carbide-based spherical powder, titanium carbonitride-based spherical powder and cobalt powder in a slow three-dimensional vortex mixer;
3) carrying out secondary atomization drying granulation on the mixed powder, filling the mixed powder into a cold pressing die, and carrying out compression molding in a four-column single-shaft cold press;
4) and (4) conveying the blank into a high-temperature vacuum tube furnace for sintering to finally obtain the complex phase co-strengthening hard alloy material.
As a further improvement of the invention, in the step 1), the mass ratio of the tungsten carbide powder to the nickel trinickel aluminide powder to the nickel powder is (9.1-9.5): 1; the mass ratio of the titanium carbonitride powder to the nickel powder is (9.1-9.5): 1.
as a further improvement of the invention, in the step 1), the rotation speed of the ball mill for the pre-alloying treatment is 480-550 r/min, and the ball-material ratio is (2.2-2.7): 1, the ball milling tank and the grinding ball are made of hard alloy.
As a further improvement of the invention, in the step 2), the mass ratio of the tungsten carbide-based spherical powder, the titanium carbonitride-based spherical powder and the cobalt powder is (5.1-5.4): (3.4-4.2): 1.
as a further improvement of the invention, in the step 2) and the step 3), the rotation speed of an atomizer of the atomizing and drying granulator is 22000-25000 r/min, the temperatures of an air inlet and an air outlet are 210 ℃ and 80 ℃ respectively, the particle size of the dried powder is 80-120 mu m, and the rotation speed of the three-dimensional vortex mixer is 30 r/min.
As a further improvement of the invention, in the step 3), the cold-pressing forming pressure is 220-260 MPa, and the pressure is maintained for 3 minutes.
As a further improvement of the invention, in the step 4), the sintering temperature is 1410 ℃, the temperature is maintained for 0.5 hour, the temperature rising/reducing rate is 5 ℃/min, and the argon protection is carried out.
The forming agent is SBS, and the adding amount is 2% of the mixed powder.
Compared with the prior art, the invention has the following characteristics and advantages:
the invention firstly carries out pre-alloying treatment to obtain tungsten carbide-based pre-alloy powder and titanium carbonitride-based pre-alloy powder, then uniformly mixes the two powders with cobalt powder, carries out secondary atomization, drying and granulation, then carries out compression molding in a cold press, and finally carries out sintering in a high-temperature vacuum tube furnace; wherein, the tungsten carbide-based pre-alloy powder obtained by the pre-alloying method is used as a toughness component, the titanium carbonitride-based pre-alloy powder is used as a strength component, and the two components are respectively granulated to ensure the purity of the two componentsThe net property. The cobalt powder is used as an interface component to improve the affinity of tough two phases, and cobalt, nickel aluminide and tungsten carbide can form a topological close-packed structure and a WC-Co solid solution and form the solid solution with titanium carbonitride to strengthen a phase interface; the secondary atomization drying granulation can improve the formability of the mixed powder and ensure the compactness of the cold-pressed blank. The bending strength of the complex phase co-strengthening hard alloy prepared by the invention is more than 4762MPa, and the impact toughness is more than 17.6J cm2。
Further, in the process of preparing the complex phase co-strengthening hard alloy material, in order to solve the problem that the existing methods such as powder pre-alloying, binder phase component transformation, heat treatment and the like are difficult to effectively solve the toughness contradiction, the invention adopts a complex phase component and structure optimization method to research the relationship between the mass ratio of tungsten carbide, nickel aluminide, titanium carbonitride and nickel, the technological parameters of atomization, drying and granulation, the technological parameters of cold press molding and the toughness of the hard alloy, namely: for the complex phase co-strengthening hard alloy, the optimal mass ratio of tungsten carbide, nickel aluminide, titanium carbonitride and nickel, the technological parameters of atomization, drying and granulation and the technological parameters of cold press molding, which have higher strength and toughness, are kept. The method has the advantages of high component control precision, strong process stability and repeatability, and capability of realizing the strengthening and toughening of the hard alloy.
Detailed Description
The invention relates to a preparation method of a complex phase co-strengthening hard alloy material, which comprises the following steps:
(1) tungsten carbide powder, nickel trinickel aluminide powder, titanium carbonitride powder and nickel powder are respectively mixed according to the mass ratio (8.9-9.3): 1 and (9.1-9.5): 1, placing the powder in a high-energy ball mill, and carrying out pre-alloying treatment to obtain two pre-alloyed powders. The rotating speed of the ball mill is 480-550 revolutions per minute, and the ball-material ratio is (2.2-2.7): 1, the ball milling tank and the grinding ball are made of hard alloy;
(2) atomizing, drying and granulating the two kinds of pre-alloyed powder, wherein the rotating speed of an atomizer is 22000-25000 r/min, the temperatures of an air inlet and an air outlet are 210 ℃ and 80 ℃, respectively, the particle size of the dried powder is 80-120 mu m, and the prepared tungsten carbide-based and titanium carbonitride-based spherical powder and cobalt powder are mixed according to the mass percentage (5.1-5.4): (3.4-4.2): 1, uniformly mixing in a low-speed three-dimensional vortex mixer at the rotating speed of 30 revolutions per minute;
(3) carrying out secondary atomization drying granulation on the mixed powder, filling the mixed powder into a cold pressing die, and carrying out compression molding in a four-column single-shaft cold press, wherein the cold pressing molding pressure is 220-260 MPa, and the pressure is maintained for 3 minutes;
(4) and (3) conveying the blank into a high-temperature vacuum tube furnace for sintering to finally obtain the complex phase co-strengthening hard alloy material, wherein the sintering temperature is 1410 ℃, the heat preservation time is 0.5 hour, the heating/cooling rate is 5 ℃/min, and the argon protection is performed.
The high temperature strength of the complex phase co-strengthened cemented carbide prepared in the following examples is shown in table 1.
Example 1
(1) Respectively mixing tungsten carbide powder, nickel trinickel aluminide powder, titanium carbonitride powder and nickel powder according to the mass ratio of 8.9: 1 and 9.1: 1, placing the powder in a high-energy ball mill, and carrying out pre-alloying treatment to obtain pre-alloy powder. The rotating speed of the ball mill is 540 r/m, the ball-material ratio is 2.5: 1, the ball milling tank and the grinding ball are made of hard alloy;
(2) atomizing, drying and granulating the two kinds of pre-alloyed powder, wherein the rotating speed of an atomizer is 22000 r/min, the temperatures of an air inlet and an air outlet are respectively 210 ℃ and 80 ℃, the particle size of the dried powder is 90 mu m, and the prepared tungsten carbide-based and titanium carbonitride-based spherical powder and cobalt powder are mixed according to the mass percentage of 5.2: 4.0: 1, uniformly mixing in a low-speed three-dimensional vortex mixer at the rotating speed of 30 revolutions per minute;
(3) carrying out secondary atomization drying granulation on the mixed powder, filling the mixed powder into a cold pressing die, and carrying out compression molding in a four-column single-shaft cold press, wherein the cold pressing molding pressure is 250MPa, and the pressure is maintained for 3 minutes;
(4) and (3) conveying the blank into a high-temperature vacuum tube furnace for sintering to finally obtain the complex phase co-strengthening hard alloy material, wherein the sintering temperature is 1410 ℃, the heat preservation time is 0.5 hour, the heating/cooling rate is 5 ℃/min, and the argon protection is performed.
Example 2
(1) Respectively mixing tungsten carbide powder, nickel trinickel aluminide powder, titanium carbonitride powder and nickel powder according to the mass ratio of 9.1: 1 and 9.2: 1, placing the powder in a high-energy ball mill, and carrying out pre-alloying treatment to obtain pre-alloy powder. The rotating speed of the ball mill is 480 revolutions per minute, the ball-material ratio is 2.8: 1, the ball milling tank and the grinding ball are made of hard alloy;
(2) atomizing, drying and granulating the two kinds of pre-alloyed powder, wherein the rotating speed of an atomizer is 24000 r/min, the temperatures of an air inlet and an air outlet are respectively 210 ℃ and 80 ℃, the particle size of the dried powder is 80 mu m, and the prepared tungsten carbide-based and titanium carbonitride-based spherical powder and cobalt powder are mixed according to the mass percentage of 5.4: 4.1: 1, uniformly mixing in a low-speed three-dimensional vortex mixer at the rotating speed of 30 revolutions per minute;
(3) carrying out secondary atomization drying granulation on the mixed powder, filling the mixed powder into a cold pressing die, and carrying out compression molding in a four-column single-shaft cold press, wherein the cold pressing molding pressure is 260MPa, and the pressure is maintained for 3 minutes;
(4) and (3) conveying the blank into a high-temperature vacuum tube furnace for sintering to finally obtain the complex phase co-strengthening hard alloy material, wherein the sintering temperature is 1410 ℃, the heat preservation time is 0.5 hour, the heating/cooling rate is 5 ℃/min, and the argon protection is performed.
Example 3
(1) Respectively mixing tungsten carbide powder, nickel trinickel aluminide powder, titanium carbonitride powder and nickel powder according to the mass ratio of 9.3: 1 and 9.3: 1, placing the powder in a high-energy ball mill, and carrying out pre-alloying treatment to obtain pre-alloy powder. The rotating speed of the ball mill is 500 r/m, the ball-material ratio is 2.7: 1, the ball milling tank and the grinding ball are made of hard alloy;
(2) atomizing, drying and granulating the two pre-alloyed powders, wherein the rotating speed of an atomizer is 25000 r/min, the temperatures of an air inlet and an air outlet are respectively 210 ℃ and 80 ℃, the particle size of the dried powder is 120 mu m, and the prepared tungsten carbide-based and titanium carbonitride-based spherical powder and cobalt powder are mixed according to the mass percentage of 5.2: 3.6: 1, uniformly mixing in a low-speed three-dimensional vortex mixer at the rotating speed of 30 revolutions per minute;
(3) carrying out secondary atomization drying granulation on the mixed powder, filling the mixed powder into a cold pressing die, and carrying out compression molding in a four-column single-shaft cold press, wherein the cold pressing molding pressure is 240MPa, and the pressure is maintained for 3 minutes;
(4) and (3) conveying the blank into a high-temperature vacuum tube furnace for sintering to finally obtain the complex phase co-strengthening hard alloy material, wherein the sintering temperature is 1410 ℃, the heat preservation time is 0.5 hour, the heating/cooling rate is 5 ℃/min, and the argon protection is performed.
Example 4
(1) Respectively mixing tungsten carbide powder, nickel trinickel aluminide powder, titanium carbonitride powder and nickel powder according to the mass ratio of 9.0: 1 and 9.4: 1, placing the powder in a high-energy ball mill, and carrying out pre-alloying treatment to obtain pre-alloy powder. The rotating speed of the ball mill is 510 revolutions per minute, the ball-material ratio is 2.3: 1, the ball milling tank and the grinding ball are made of hard alloy;
(2) atomizing, drying and granulating the two kinds of pre-alloyed powder, wherein the rotating speed of an atomizer is 23000 r/min, the temperatures of an air inlet and an air outlet are respectively 210 ℃ and 80 ℃, the particle size of the dried powder is 120 mu m, and the prepared tungsten carbide-based and titanium carbonitride-based spherical powder and cobalt powder are mixed according to the mass percentage of 5.2: 4.2: 1, uniformly mixing in a low-speed three-dimensional vortex mixer at the rotating speed of 30 revolutions per minute;
(3) carrying out secondary atomization drying granulation on the mixed powder, filling the mixed powder into a cold pressing die, and carrying out compression molding in a four-column single-shaft cold press, wherein the cold pressing molding pressure is 260MPa, and the pressure is maintained for 3 minutes;
(4) and (3) conveying the blank into a high-temperature vacuum tube furnace for sintering to finally obtain the complex phase co-strengthening hard alloy material, wherein the sintering temperature is 1410 ℃, the heat preservation time is 0.5 hour, the heating/cooling rate is 5 ℃/min, and the argon protection is performed.
The performance parameters of the complex phase co-strengthening hard alloy materials prepared in the embodiments 1-4 are shown in table 1:
TABLE 1
As can be seen from the table, the bending strength of the complex phase co-strengthening hard alloy prepared by the invention is more than 4762MPa, and the impact toughness is more than 17.6 J.cm2。
Example 5
(1) Respectively mixing tungsten carbide powder, nickel trinickel aluminide powder, titanium carbonitride powder and nickel powder according to the mass ratio of 9.0: 1 and 9.1: 1, placing the powder in a high-energy ball mill, and carrying out pre-alloying treatment to obtain pre-alloy powder. The rotating speed of the ball mill is 510 revolutions per minute, the ball-material ratio is 2.4: 1, the ball milling tank and the grinding ball are made of hard alloy;
(2) atomizing, drying and granulating the two kinds of pre-alloyed powder, wherein the rotating speed of an atomizer is 24000 r/min, the temperatures of an air inlet and an air outlet are respectively 210 ℃ and 80 ℃, the particle size of the dried powder is 100 mu m, and the prepared tungsten carbide-based and titanium carbonitride-based spherical powder and cobalt powder are mixed according to the mass percentage of 5.4: 4.2: 1, uniformly mixing in a low-speed three-dimensional vortex mixer at the rotating speed of 30 revolutions per minute;
(3) carrying out secondary atomization drying granulation on the mixed powder, filling the mixed powder into a cold pressing die, and carrying out compression molding in a four-column single-shaft cold press, wherein the cold pressing molding pressure is 260MPa, and the pressure is maintained for 3 minutes;
(4) and (3) conveying the blank into a high-temperature vacuum tube furnace for sintering to finally obtain the complex phase co-strengthening hard alloy material, wherein the sintering temperature is 1410 ℃, the heat preservation time is 0.5 hour, the heating/cooling rate is 5 ℃/min, and the argon protection is performed.
Example 6
(1) Respectively mixing tungsten carbide powder, nickel trinickel aluminide powder, titanium carbonitride powder and nickel powder according to the mass ratio of 9.3: 1 and 9.2: 1, placing the powder in a high-energy ball mill, and carrying out pre-alloying treatment to obtain pre-alloy powder. The rotating speed of the ball mill is 495 r/min, the ball-material ratio is 2.6: 1, the ball milling tank and the grinding ball are made of hard alloy;
(2) atomizing, drying and granulating the two kinds of pre-alloyed powder, wherein the rotating speed of an atomizer is 23000 r/min, the temperatures of an air inlet and an air outlet are respectively 210 ℃ and 80 ℃, the particle size of the dried powder is 110 mu m, and the prepared tungsten carbide-based and titanium carbonitride-based spherical powder and cobalt powder are mixed according to the mass percentage of 5.4: 4.2: 1, uniformly mixing in a low-speed three-dimensional vortex mixer at the rotating speed of 30 revolutions per minute;
(3) carrying out secondary atomization drying granulation on the mixed powder, filling the mixed powder into a cold pressing die, and carrying out compression molding in a four-column single-shaft cold press, wherein the cold pressing molding pressure is 220MPa, and the pressure is maintained for 3 minutes;
(4) and (3) conveying the blank into a high-temperature vacuum tube furnace for sintering to finally obtain the complex phase co-strengthening hard alloy material, wherein the sintering temperature is 1410 ℃, the heat preservation time is 0.5 hour, the heating/cooling rate is 5 ℃/min, and the argon protection is performed.
Example 7
(1) Respectively mixing tungsten carbide powder, nickel trinickel aluminide powder, titanium carbonitride powder and nickel powder according to the mass ratio of 9.3: 1 and 9.5: 1, placing the powder in a high-energy ball mill, and carrying out pre-alloying treatment to obtain pre-alloy powder. The rotating speed of the ball mill is 550 revolutions per minute, and the ball-material ratio is 2.7: 1, the ball milling tank and the grinding ball are made of hard alloy;
(2) atomizing, drying and granulating the two pre-alloyed powders, wherein the rotating speed of an atomizer is 25000 r/m, the temperatures of an air inlet and an air outlet are respectively 210 ℃ and 80 ℃, the particle size of the dried powder is 120 mu m, and the prepared tungsten carbide-based and titanium carbonitride-based spherical powder and cobalt powder are mixed according to the mass percentage of 5.4: 4.2: 1, uniformly mixing in a low-speed three-dimensional vortex mixer at the rotating speed of 30 revolutions per minute;
(3) carrying out secondary atomization drying granulation on the mixed powder, filling the mixed powder into a cold pressing die, and carrying out compression molding in a four-column single-shaft cold press, wherein the cold pressing molding pressure is 260MPa, and the pressure is maintained for 3 minutes;
(4) and (3) conveying the blank into a high-temperature vacuum tube furnace for sintering to finally obtain the complex phase co-strengthening hard alloy material, wherein the sintering temperature is 1410 ℃, the heat preservation time is 0.5 hour, the heating/cooling rate is 5 ℃/min, and the argon protection is performed.
Example 8
(1) Respectively mixing tungsten carbide powder, nickel trinickel aluminide powder, titanium carbonitride powder and nickel powder according to the mass ratio of 8.9: 1 and 9.1: 1, placing the powder in a high-energy ball mill, and carrying out pre-alloying treatment to obtain pre-alloy powder. The rotating speed of the ball mill is 480 revolutions per minute, the ball-material ratio is 2.2: 1, the ball milling tank and the grinding ball are made of hard alloy;
(2) atomizing, drying and granulating the two kinds of pre-alloyed powder, wherein the rotating speed of an atomizer is 22000 r/min, the temperatures of an air inlet and an air outlet are respectively 210 ℃ and 80 ℃, the particle size of the dried powder is 80 mu m, and the prepared tungsten carbide-based and titanium carbonitride-based spherical powder and cobalt powder are mixed according to the mass percentage of 5.1: 3.4: 1, uniformly mixing in a low-speed three-dimensional vortex mixer at the rotating speed of 30 revolutions per minute;
(3) carrying out secondary atomization drying granulation on the mixed powder, filling the mixed powder into a cold pressing die, and carrying out compression molding in a four-column single-shaft cold press, wherein the cold pressing molding pressure is 220MPa, and the pressure is maintained for 3 minutes;
(4) and (3) conveying the blank into a high-temperature vacuum tube furnace for sintering to finally obtain the complex phase co-strengthening hard alloy material, wherein the sintering temperature is 1410 ℃, the heat preservation time is 0.5 hour, the heating/cooling rate is 5 ℃/min, and the argon protection is performed.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (4)
1. The preparation method of the complex phase co-strengthening hard alloy material is characterized by comprising the following steps:
1) respectively placing tungsten carbide powder, nickel trinickel aluminide powder, titanium carbonitride powder and nickel powder in a high-energy ball mill, and performing pre-alloying treatment to obtain two kinds of pre-alloyed powder;
2) atomizing, drying and granulating the two pre-alloyed powders, and uniformly mixing the prepared tungsten carbide-based spherical powder, titanium carbonitride-based spherical powder and cobalt powder in a slow three-dimensional vortex mixer;
3) carrying out secondary atomization drying granulation on the mixed powder, filling the mixed powder into a cold pressing die, and carrying out compression molding in a four-column single-shaft cold press;
4) sending the blank into a high-temperature vacuum tube furnace for sintering to finally obtain a complex phase co-strengthening hard alloy material;
in the step 1), the mass ratio of the tungsten carbide powder to the nickel trinickel aluminide powder is (8.9-9.3): 1; the mass ratio of the titanium carbonitride powder to the nickel powder is (9.1-9.5): 1;
in the step 2), the mass ratio of the tungsten carbide-based spherical powder, the titanium carbonitride-based spherical powder and the cobalt powder is (5.1-5.4): (3.4-4.2): 1;
in the step 3), cold-pressing molding pressure is 220-260 MPa, and pressure is maintained for 3 minutes;
in the step 4), the sintering temperature is 1410 ℃, the temperature is kept for 0.5 hour, the temperature rising/reducing rate is 5 ℃/min, and the argon protection is carried out.
2. The preparation method of the complex-phase co-strengthening hard alloy material as claimed in claim 1, wherein in the step 1), the rotation speed of a ball mill for pre-alloying treatment is 480-550 r/min, and the ball-to-material ratio is (2.2-2.7): 1, the ball milling tank and the grinding ball are made of hard alloy.
3. The preparation method of the complex-phase co-strengthening hard alloy material as claimed in claim 1, wherein in the step 2) and the step 3), the rotation speed of an atomizer of an atomization drying granulator is 22000-25000 r/min, the temperatures of an air inlet and an air outlet are 210 ℃ and 80 ℃ respectively, the particle size of the dried powder is 80-120 μm, and the rotation speed of a three-dimensional vortex mixer is 30 r/min.
4. The method for preparing the complex phase co-strengthening hard alloy material as claimed in claim 1, wherein the forming agent is SBS, and the adding amount is 2% of the mass of the mixed powder.
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