CN115074592A - High-temperature-resistant high-toughness hard alloy material for die and preparation method thereof - Google Patents
High-temperature-resistant high-toughness hard alloy material for die and preparation method thereof Download PDFInfo
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- B22F9/00—Making metallic powder or suspensions thereof
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Abstract
The invention discloses a high-temperature-resistant high-toughness hard alloy material for a die and a preparation method thereof, wherein the high-temperature-resistant high-toughness hard alloy material comprises the following materials in parts by weight: 85-89 parts of tungsten carbide, 10-14 parts of cobalt, 0.5-0.8 part of vanadium carbide, 5-10 parts of rhenium-molybdenum-nickel alloy powder, 5-10 parts of hafnium carbide, 1-3 parts of chromium carbide, 2-8 parts of graphite oxide, 2-5 parts of titanium carbide, 6-10 parts of tantalum carbide and 10-15 parts of iron, mixing the materials, performing ball milling, spray drying, sieving to obtain granules, and then performing compression molding on the granules to obtain a green compact; and placing the pressed compact into a sintering furnace for sintering, and then naturally cooling to room temperature to obtain the hard alloy material. The hard alloy particles obtained by the invention are uniformly distributed, have the advantages of high toughness and high temperature resistance, and also have certain corrosion resistance, and the bending strength, the hardness and the service life of the hard alloy particles are obviously improved.
Description
Technical Field
The invention relates to the technical field of hard alloy, in particular to a high-temperature-resistant high-toughness hard alloy material for a die and a preparation method thereof.
Background
The hard alloy is an alloy material prepared from a hard compound of refractory metal and bonding metal through a powder metallurgy process, and has a series of excellent properties such as high hardness, wear resistance, good strength and toughness, heat resistance, corrosion resistance and the like, so that the hard alloy material is widely applied to various industries. Among them, cemented carbide is also used as a material for preparing some molds.
For injection molds or other molds, in the process of finished products, the hard alloy is required to bear high temperature, high pressure, abrasion and other states, and becomes an ideal material for preparing hot forging molds, hot extrusion molds and internal thread pipe molds.
The traditional hard alloy takes Co, Ni and Fe simple substance elements as binding phase and WC as hard phase. With the rise of the use temperature, particularly above 400 ℃, Co, Ni and Fe elementary substance elements as a binding phase and a WC hard phase begin to be oxidized, so that the bending strength, the hardness and other properties of the traditional hard alloy are obviously reduced, and the high-temperature service life is also obviously reduced.
Disclosure of Invention
In order to solve the technical problems, the invention provides a high-temperature-resistant high-toughness hard alloy material for a die and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
a high-temperature-resistant high-toughness hard alloy material for a die comprises the following materials in parts by weight:
85-89 parts of tungsten carbide, 10-14 parts of cobalt, 0.5-0.8 part of vanadium carbide, 5-10 parts of rhenium-molybdenum-nickel alloy powder, 5-10 parts of hafnium carbide, 1-3 parts of chromium carbide, 2-8 parts of graphite oxide, 2-5 parts of titanium carbide, 6-10 parts of tantalum carbide and 10-15 parts of iron.
The dosage ratio of rhenium, molybdenum and nickel in the rhenium-molybdenum-nickel alloy powder is 1:1: 2-3.
The rhenium-molybdenum-nickel alloy powder is prepared by the following steps: according to a set dosage proportion, adding rhenium powder, molybdenum powder and nickel powder into a ball mill, adding alloy balls according to the ball-to-material weight ratio of 2-4:1, ball milling for 36-65h to obtain uniformly mixed powder, carrying out co-reduction at 1400-1700 ℃ in a hydrogen atmosphere to prepare rhenium-molybdenum-nickel alloy, and crushing and screening to obtain rhenium-molybdenum-nickel alloy powder with the particle size of 1-3 microns.
The particle size of the cobalt is 0.5-1.0 mu m, the particle size of the iron is 3.0-8.0 mu m, the particle size of the tungsten carbide is 6.0-7.0 mu m, the particle size of the titanium carbide is 5.0-15 mu m, the particle size of the vanadium carbide is 4.0-6.0 mu m, and the particle size of the tantalum carbide is 5.0-15 mu m.
A preparation method of a high-temperature-resistant high-toughness hard alloy material for a die comprises the following steps:
mixing the raw materials according to a set weight part ratio, and then putting the mixed raw materials into a mixer for fully mixing, wherein the rotating speed of the mixer is 15-40 r/min;
ball-milling the mixed raw materials and the organic solvent together by using a ball mill, wherein the volume ratio of the raw materials to the organic solvent to the balls is 1.5 (0.4-0.8) to (3-4), so as to obtain slurry;
after the obtained slurry is subjected to spray drying, sieving to obtain material particles, and then pressing and forming the material particles to obtain a green compact;
and placing the pressed compact into a sintering furnace for sintering, and then naturally cooling to room temperature to obtain the hard alloy material.
The organic solvent is one or a mixture of ethanol, citric acid and fatty alcohol-polyoxyethylene ether.
In the sintering process, heating is firstly carried out in a vacuum environment, the temperature is preserved for 1-3h when the temperature is between 800 and 1000 ℃ for presintering treatment, then the temperature is continuously raised to 1500 to 1800 ℃ after hydrogen is introduced, and the sintering treatment is carried out for 2-6 h.
The hard alloy obtained by the invention has the advantages of uniform particle distribution, high toughness, high temperature resistance, certain corrosion resistance, and obviously improved bending strength, hardness and service life.
Detailed Description
The invention will be further illustrated with reference to the following specific examples.
Example one
The high-temperature-resistant high-toughness hard alloy material for the die comprises the following materials in parts by weight: 85 parts of tungsten carbide, 10 parts of cobalt, 0.5 part of vanadium carbide, 5 parts of rhenium-molybdenum-nickel alloy powder, 5 parts of hafnium carbide, 1 part of chromium carbide, 2 parts of graphite oxide, 2 parts of titanium carbide, 6 parts of tantalum carbide and 10 parts of iron. The dosage ratio of rhenium, molybdenum and nickel in the rhenium-molybdenum-nickel alloy powder is 1:1: 2.
The rhenium-molybdenum-nickel alloy powder is prepared by the following steps: according to a set dosage proportion, rhenium powder, molybdenum powder and nickel powder are taken and added into a ball mill, alloy balls are added according to the ball material weight ratio of 2:1, the powder which is uniformly mixed is obtained after ball milling for 36h, rhenium-molybdenum-nickel alloy is prepared by co-reduction at 1400 ℃ in hydrogen atmosphere, and rhenium-molybdenum-nickel alloy powder with the particle size of 1 mu m is obtained by crushing and screening.
The grain size of the cobalt is 0.5 mu m, the grain size of the iron is 3.0 mu m, the grain size of the tungsten carbide is 6.0 mu m, the grain size of the titanium carbide is 5.0 mu m, the grain size of the vanadium carbide is 4.0 mu m, and the grain size of the tantalum carbide is 5.0 mu m.
And (3) putting the prepared raw materials into a mixer for fully mixing, wherein the rotating speed of the mixer is 15 r/min.
And ball-milling the mixed raw materials and the organic solvent together by using a ball mill, wherein the volume ratio of the raw materials to the organic solvent to the balls is 1.5:0.4:3, and the organic solvent is the mixture of ethanol, citric acid and fatty alcohol-polyoxyethylene ether to form slurry.
After the obtained slurry is subjected to spray drying, sieving to obtain material particles, and then pressing and forming the material particles to obtain a green compact;
and (3) placing the pressed compact into a sintering furnace for sintering, firstly heating the pressed compact in a vacuum environment, preserving heat for 1h to 800 ℃ for presintering treatment, then introducing hydrogen, continuing to heat to 1500 ℃ and carrying out sintering treatment for 2 h. And naturally cooling to room temperature to obtain the hard alloy material.
In this embodiment, for the overall formulation composition, 85 parts of tungsten carbide, 10 parts of cobalt, 0.5 part of vanadium carbide, 5 parts of rhenium-molybdenum-nickel alloy powder, 5 parts of hafnium carbide, 1 part of chromium carbide, 2 parts of graphite oxide, 2 parts of titanium carbide, 6 parts of tantalum carbide, and 10 parts of iron, wherein the improvement of high temperature resistance can be achieved by the hafnium carbide. With the above limitation of the amount, when the amount is too high, the cost is wasted, and the performance of other materials is also affected. The overall strength and hardness of the product can be effectively enhanced by using the graphite oxide. And the rhenium-molybdenum-nickel alloy powder is utilized, so that the mechanical deformation process of pure molybdenum from single sliding to twin crystal action and sliding combination in hot working and cold working is changed, the embrittlement action of carbon and oxygen is inhibited, and the physical and chemical properties, the thermoelectric property and the like of the molybdenum alloy are improved. Therefore, the above component materials are indispensable, and can improve the overall performance.
Example two
The high-temperature-resistant high-toughness hard alloy material for the die comprises the following materials in parts by weight: 87 parts of tungsten carbide, 12 parts of cobalt, 0.7 part of vanadium carbide, 8 parts of rhenium-molybdenum-nickel alloy powder, 8 parts of hafnium carbide, 2 parts of chromium carbide, 5 parts of graphite oxide, 3 parts of titanium carbide, 8 parts of tantalum carbide and 13 parts of iron. The dosage ratio of rhenium, molybdenum and nickel in the rhenium-molybdenum-nickel alloy powder is 1:1: 2.
The rhenium-molybdenum-nickel alloy powder is prepared by the following steps: according to a set dosage proportion, rhenium powder, molybdenum powder and nickel powder are taken and added into a ball mill, alloy balls are added according to the ball material weight ratio of 3:1, the powder which is uniformly mixed is obtained after ball milling for 50h, rhenium-molybdenum-nickel alloy is prepared by co-reduction at 1600 ℃ in hydrogen atmosphere, and rhenium-molybdenum-nickel alloy powder with the particle size of 2 mu m is obtained by crushing and screening.
The grain size of the cobalt is 0.8 mu m, the grain size of the iron is 5.0 mu m, the grain size of the tungsten carbide is 6.5 mu m, the grain size of the titanium carbide is 12 mu m, the grain size of the vanadium carbide is 5.0 mu m, and the grain size of the tantalum carbide is 8 mu m.
The raw materials are mixed according to the set weight part ratio, and then the mixed raw materials are put into a mixer for fully mixing, wherein the rotating speed of the mixer is 25 r/m.
And ball-milling the mixed raw materials and the organic solvent together by using a ball mill, wherein the volume ratio of the raw materials to the organic solvent to the balls is 1.5:0.6:4, and the organic solvent is the mixture of ethanol and citric acid to form slurry to obtain slurry.
And (3) after the obtained slurry is subjected to spray drying, sieving to obtain material particles, and then pressing and forming the material particles to obtain a green compact.
And (3) placing the pressed compact into a sintering furnace for sintering, preserving heat for 2h when the temperature is 900 ℃, performing presintering treatment, introducing hydrogen, continuing to heat to 1600 ℃, performing sintering treatment for 4h, and naturally cooling to room temperature to obtain the hard alloy material.
EXAMPLE III
The high-temperature-resistant high-toughness hard alloy material for the die comprises the following materials in parts by weight: 89 parts of tungsten carbide, 4 parts of cobalt, 0.8 part of vanadium carbide, 10 parts of rhenium-molybdenum-nickel alloy powder, 10 parts of hafnium carbide, 3 parts of chromium carbide, 8 parts of graphite oxide, 5 parts of titanium carbide, 10 parts of tantalum carbide and 15 parts of iron. The dosage ratio of rhenium, molybdenum and nickel in the rhenium-molybdenum-nickel alloy powder is 1:1: 3.
The rhenium-molybdenum-nickel alloy powder is prepared by the following steps: according to a set dosage proportion, rhenium powder, molybdenum powder and nickel powder are taken and added into a ball mill, alloy balls are added according to the ball material weight ratio of 4:1, the powder which is uniformly mixed is obtained after ball milling for 60 hours, rhenium-molybdenum-nickel alloy is prepared by co-reduction at 1700 ℃ in hydrogen atmosphere, and rhenium-molybdenum-nickel alloy powder with the particle size of 3 mu m is obtained by crushing and screening.
The grain size of the cobalt is 1.0 mu m, the grain size of the iron is 8.0 mu m, the grain size of the tungsten carbide is 7.0 mu m, the grain size of the titanium carbide is 15 mu m, the grain size of the vanadium carbide is 6.0 mu m, and the grain size of the tantalum carbide is 15 mu m
The raw materials are mixed according to the set weight part ratio, and then the mixed raw materials are put into a mixer for fully mixing, wherein the rotating speed of the mixer is 35 r/m.
And ball-milling the mixed raw materials and the organic solvent together by using a ball mill, wherein the volume ratio of the raw materials to the organic solvent to the balls is 1.5:0.6:4, and the organic solvent is the mixture of ethanol, citric acid and fatty alcohol-polyoxyethylene ether to form slurry, so as to obtain the slurry.
And (3) after the obtained slurry is subjected to spray drying, sieving to obtain material particles, and then pressing and forming the material particles to obtain a green compact.
And (3) placing the pressed compact into a sintering furnace for sintering, preserving heat for 2h when the temperature is 900 ℃, performing presintering treatment, introducing hydrogen, continuing to heat to 1600 ℃, performing sintering treatment for 4h, and naturally cooling to room temperature to obtain the hard alloy material.
Comparative example 1
The difference compared to example 1 is that no rhenium-molybdenum-nickel alloy powder was added.
Comparative example 2
Compared with example 2, the difference is that the rhenium-molybdenum-nickel alloy powder is added in 20 parts by weight.
Comparative example 3
Compared with example 3, the difference is that the rhenium-molybdenum-nickel alloy powder is added in 1 part by weight.
According to the above method, the prepared cemented carbide materials of example 1, example 2, example 3, comparative example 1, comparative example 2 and comparative example 3 were respectively subjected to fracture toughness tests as follows:
fracture toughness detection result/Mpa.m 1/2
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| 13.25 | 13.18 | 12.95 | 9.05 | 11.12 | 10.01 |
Therefore, by adding the rhenium-molybdenum-nickel alloy powder, the mechanical deformation process of pure molybdenum from single sliding to twin crystal action and sliding combination in hot working and cold working is changed, the embrittlement action of carbon and oxygen is inhibited, and the overall performance can be improved.
Although the present invention has been described in detail with reference to the embodiments, it will be apparent to those skilled in the art that modifications, equivalents, improvements, and the like can be made in the technical solutions of the foregoing embodiments or in some of the technical features of the foregoing embodiments, but those modifications, equivalents, improvements, and the like are all within the spirit and principle of the present invention.
Claims (7)
1. The high-temperature-resistant high-toughness hard alloy material for the die is characterized by comprising the following materials in parts by weight:
85-89 parts of tungsten carbide, 10-14 parts of cobalt, 0.5-0.8 part of vanadium carbide, 5-10 parts of rhenium-molybdenum-nickel alloy powder, 5-10 parts of hafnium carbide, 1-3 parts of chromium carbide, 2-8 parts of graphite oxide, 2-5 parts of titanium carbide, 6-10 parts of tantalum carbide and 10-15 parts of iron.
2. The high-temperature-resistant and high-toughness cemented carbide material for molds according to claim 1, wherein the rhenium, molybdenum, and nickel are used in the rhenium-molybdenum-nickel alloy powder in a ratio of 1:1: 2-3.
3. The high-temperature-resistant high-toughness cemented carbide material for molds according to claim 2, wherein the rhenium-molybdenum-nickel alloy powder is prepared by: according to a set dosage proportion, adding rhenium powder, molybdenum powder and nickel powder into a ball mill, adding alloy balls according to the ball-to-material weight ratio of 2-4:1, ball milling for 36-65h to obtain uniformly mixed powder, carrying out co-reduction at 1400-1700 ℃ in a hydrogen atmosphere to prepare rhenium-molybdenum-nickel alloy, and crushing and screening to obtain rhenium-molybdenum-nickel alloy powder with the particle size of 1-3 microns.
4. The high-temperature-resistant high-toughness cemented carbide material for molds according to claim 3, wherein the cobalt has a particle size of 0.5 to 1.0 μm, the iron has a particle size of 3.0 to 8.0 μm, the tungsten carbide has a particle size of 6.0 to 7.0 μm, the titanium carbide has a particle size of 5.0 to 15 μm, the vanadium carbide has a particle size of 4.0 to 6.0 μm, and the tantalum carbide has a particle size of 5.0 to 15 μm.
5. A preparation method of a high-temperature-resistant high-toughness hard alloy material for a die is characterized by comprising the following steps of:
mixing the raw materials according to a set weight part ratio, and then putting the mixed raw materials into a mixer for fully mixing, wherein the rotating speed of the mixer is 15-40 r/min;
ball-milling the mixed raw materials and the organic solvent together by using a ball mill, wherein the volume ratio of the raw materials to the organic solvent to the balls is 1.5 (0.4-0.8) to (3-4), so as to obtain slurry;
after the obtained slurry is subjected to spray drying, sieving to obtain material particles, and then pressing and forming the material particles to obtain a green compact;
and placing the pressed compact into a sintering furnace for sintering, and then naturally cooling to room temperature to obtain the hard alloy material.
6. The method for preparing the high-temperature-resistant high-toughness hard alloy material for the mold according to claim 5, wherein the organic solvent is one or a mixture of ethanol, citric acid and fatty alcohol-polyoxyethylene ether.
7. The method for preparing the high-temperature-resistant high-toughness hard alloy material for the mold according to claim 6, wherein in the sintering process, the hard alloy material is firstly heated in a vacuum environment, is subjected to heat preservation for 1-3 hours when the temperature is between 800 and 1000 ℃ for pre-sintering treatment, is continuously heated to 1500 to 1800 ℃ after hydrogen is introduced, and is subjected to sintering treatment for 2-6 hours.
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