CN106747449B - Novel tungsten carbide composite material and preparation method thereof - Google Patents

Novel tungsten carbide composite material and preparation method thereof Download PDF

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CN106747449B
CN106747449B CN201611217164.5A CN201611217164A CN106747449B CN 106747449 B CN106747449 B CN 106747449B CN 201611217164 A CN201611217164 A CN 201611217164A CN 106747449 B CN106747449 B CN 106747449B
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composite material
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tungsten carbide
tungsten
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CN106747449A (en
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钟凤芝
翟东升
王长文
高波
吴德忠
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Harbin Vocational and Technical College
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Abstract

The invention belongs to the field of new materials, and particularly relates to a novel tungsten carbide composite material and a preparation method thereof. Aiming at the problem that the existing tungsten carbide composite material is difficult to simultaneously meet the requirements of high strength, high wear resistance and low viscosity, the invention provides a novel tungsten carbide composite material, which comprises the following raw materials: 80-82 parts of WC and Al2O34-6 parts of ZrO25-8 parts of cobalt, 2-4 parts of cobalt, 3-6 parts of germanium dioxide and 3-5 parts of tungsten powder. The invention also provides a preparation method of the composite material, which comprises the steps of compounding the tungsten carbide and the tungsten powder, and then adding other raw materials for compounding. The WC composite material is made of Al2O3And ZrO2The ceramic toughened WC composite material has high hardness, wear resistance, oxidation resistance and good toughness, and is suitable for being used as a cutter, a drill bit or a die material; the method has the advantages of simple operation, easily obtained raw materials, low cost and suitability for popularization and application.

Description

Novel tungsten carbide composite material and preparation method thereof
Technical Field
The invention belongs to the field of new materials, and particularly relates to a novel tungsten carbide composite material and a preparation method thereof.
Background
WC-Co hard alloy is a common and important hard alloy type (YG series), is widely applied to the fields of modern cutter materials, wear-resistant materials, corrosion-resistant materials and high-temperature-resistant materials, and is called as teeth in modern industry. Pure WC materials are difficult to sinter and compact, even if the pure WC materials are sintered and compact, the sintering temperature is often above 2000 ℃, the high sintering temperature is also a damage to equipment, and the fracture toughness after sintering is only 4 MPa.m 1/2. Co is used as a binding phase in the process of WC sintering, WC has very good wettability, the sintering temperature of WC can be reduced to 1400 ℃, Co becomes a liquid phase in the process of sintering, the diffusion rate of WC particles is greatly increased, the sintering is compact, and the fracture toughness of the sintered tungsten carbide composite material is usually 12 MPa.m 1/2. However, the Co resource in China is extremely scarce and depends heavily on import. With the limited export of strategic resources in various countries, the power of international Co price increase is very strong, and the supply of Co raw materials has a plurality of unstable factors. Meanwhile, Co is used as a binder, so that the hardness, corrosion resistance and high temperature resistance of the WC material are reduced, and the application of the WC material in some extreme service environments is limited. Therefore, it is very important to find a common material which has wide sources and does not form a binder phase in WC to replace Co, get rid of dependence on foreign countries, and improve the hardness and the high-temperature performance of WC cemented carbide. At present, in the research of a non-bonding phase WC material, the addition of a ceramic phase is a thought, and the ceramic material is emphasized due to excellent performances such as high temperature resistance, corrosion resistance, wear resistance and the like, but the application of the ceramic material is quite limited due to the brittleness problem (low toughness and plasticity, low strength, poor performance stability and controllability).
The invention aims to provide a novel tungsten carbide composite material and a preparation method thereof, and the tungsten carbide composite material with high strength, high wear resistance and low bonding viscosity is prepared by selecting a novel material to replace Co.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the existing tungsten carbide composite material is difficult to simultaneously meet the requirements of high strength, high wear resistance and low viscosity.
The technical scheme for solving the technical problem of the invention is as follows: provides a novel tungsten carbide composite material and a preparation method thereof.
The novel tungsten carbide composite material comprises the following components: 80-82 parts of WC and Al2O34-6 parts of ZrO25-8 parts of cobalt, 2-4 parts of cobalt, 3-6 parts of germanium dioxide and 3-5 parts of tungsten powder.
Wherein, the novel tungsten carbide composite material also comprises molybdenum powder accounting for 1-3% of the total weight of the rest raw materials.
Wherein, in the novel tungsten carbide composite material, the grain diameter of the WC is 100-150 um.
Wherein, in the novel tungsten carbide composite material, the particle size of the cobalt is 50-100 um.
Wherein, in the novel tungsten carbide composite material, the purity of the tungsten powder is 99.9%.
The invention also provides a preparation method of the novel tungsten carbide composite material, which comprises the following steps:
a. mixing WC powder and tungsten powder in proportion, heating to 500-600 ℃, preserving heat for 15-20 min to decarbonize the surface of tungsten carbide to form a mixture of tungsten and tungsten oxide, introducing argon gas for reduction, heating to 650-750 ℃, and preserving heat for 10-20min to prepare composite powder of tungsten and tungsten carbide;
b. mixing Al2O3，ZrO2After cobalt and germanium dioxide are weighed according to a proportion, adding the weighed cobalt and germanium dioxide into the composite powder in the step a, adding 100-150 parts of ethanol or water, mixing and ball-milling for 15-30min to form mixed slurry;
c. drying the mixed slurry until the water content or ethanol content is less than or equal to 1%, sintering in a sintering furnace at the sintering temperature of 1400 ℃ and 1500 ℃, at the pressure of 40-50MPa, and keeping the temperature for 10-15 min.
Wherein, in the preparation method of the novel tungsten carbide composite material, the sintering temperature in the step c is increased from room temperature to 1400-1500 ℃ within 3-5 min.
The invention has the beneficial effects that: the WC composite material prepared by the invention is Al2O3And ZrO2The ceramic toughened WC composite material has high hardness, wear resistance, oxidation resistance and good toughness, and is suitable for being used as a cutter, a drill bit or a die material; due to Al2O3And ZrO2WC and ZrO2Solid solution can be formed between the two components to promote the densification of the composite material, so that the ternary composite material is almost fully densified when being sintered at 1400 ℃, the dense binding-phase-free WC composite material is prepared at a lower temperature, and the energy is saved and the efficiency is high; the invention also plates the tungsten powder coating on the WC surface, which can prevent the generation of binding phase and effectively improve the wear resistance and toughness of the WC composite material. The method has the advantages of simple operation, easily obtained raw materials, low cost and suitability for popularization and application.
Detailed Description
The invention provides a novel tungsten carbide composite material, which comprises the following components: 80-82 parts of WC and Al2O34-6 parts of ZrO25-8 parts of cobalt, 2-4 parts of cobalt, 3-6 parts of germanium dioxide, and tungsten3-5 parts of powder.
Wherein, the novel tungsten carbide composite material also comprises molybdenum powder accounting for 1-3% of the total weight of the rest raw materials.
Wherein, in the novel tungsten carbide composite material, the grain diameter of the WC is 100-150 um.
Wherein, in the novel tungsten carbide composite material, the particle size of the cobalt is 50-100 um.
Wherein, in the novel tungsten carbide composite material, the purity of the tungsten powder is 99.9%.
The invention also provides a preparation method of the novel tungsten carbide composite material, which comprises the following steps:
a. mixing WC powder and tungsten powder in proportion, heating to 500-600 ℃, preserving heat for 15-20 min to decarbonize the surface of tungsten carbide to form a mixture of tungsten and tungsten oxide, introducing argon gas for reduction, heating to 650-750 ℃, and preserving heat for 10-20min to prepare composite powder of tungsten and tungsten carbide;
b. mixing Al2O3，ZrO2After cobalt and germanium dioxide are weighed according to a proportion, adding the weighed cobalt and germanium dioxide into the composite powder in the step a, adding 100-150 parts of ethanol or water, mixing and ball-milling for 15-30min to form mixed slurry;
c. drying the mixed slurry until the water content or ethanol content is less than or equal to 1%, sintering in a sintering furnace at the sintering temperature of 1400 ℃ and 1500 ℃, at the pressure of 40-50MPa, and keeping the temperature for 10-15 min.
Wherein, in the preparation method of the novel tungsten carbide composite material, the sintering temperature in the step c is increased from room temperature to 1400-1500 ℃ within 3-5 min.
In the novel tungsten carbide composite material, tungsten carbide is taken as a main raw material and is matched with a ceramic material Al2O3，ZrO2The three components form a stable three-phase structure, the structure is compact, the wear resistance of the composite material is enhanced, and the hardness of the tungsten carbide material is not influenced; meanwhile, metal materials such as cobalt, germanium dioxide, tungsten powder and the like are added, and a certain amount of molybdenum powder can be added to enhance the high-temperature resistance and the oxidation resistance of the composite material, so that the composite material is preparedThe prepared composite material has good high temperature resistance and strong wear resistance, avoids the formation of a bonding phase and has more stable structure.
In the preparation process, the tungsten powder is firstly plated on the surfaces of the tungsten carbide particles, so that the generation of a bonding phase is prevented, and the hardness and the wear resistance of the tungsten carbide are effectively stabilized.
The following examples further illustrate specific embodiments of the present invention, but are not intended to limit the scope of the present invention to the examples.
Example 1 preparation of a tungsten carbide composite Material by the method of the invention
The raw materials comprise: 80 parts of WC, Al2O34 part of ZrO25 parts of cobalt, 2 parts of germanium dioxide and 3 parts of tungsten powder.
The preparation steps are as follows:
a. mixing WC powder and tungsten powder in proportion, heating to 500 ℃, preserving heat for 15min to ensure that the surface of tungsten carbide is decarburized to form a mixture of tungsten and tungsten oxide, introducing argon gas for reduction, heating to 650 ℃, and preserving heat for 10min to prepare composite powder of tungsten and tungsten carbide;
b. mixing Al2O3，ZrO2B, weighing cobalt and germanium dioxide in proportion, adding the cobalt and germanium dioxide into the composite powder in the step a, adding 100 parts of water, mixing and ball-milling for 15min to form mixed slurry;
c. drying the mixed slurry until the water content or ethanol content is less than or equal to 1%, sintering in a sintering furnace at 1400 ℃ under 40MPa for 10 min.
Example 2 preparation of a tungsten carbide composite Material by the method of the invention
The raw materials comprise: 82 parts of WC, Al2O36 parts of ZrO28 parts of cobalt, 4 parts of germanium dioxide and 3 parts of tungsten powder.
The preparation steps are as follows:
a. mixing WC powder and tungsten powder in proportion, heating to 600 ℃, preserving heat for 20min to ensure that the surface of tungsten carbide is decarburized to form a mixture of tungsten and tungsten oxide, introducing argon gas for reduction, heating to 750 ℃, and preserving heat for 20min to prepare composite powder of tungsten and tungsten carbide;
b. mixing Al2O3，ZrO2B, weighing cobalt and germanium dioxide in proportion, adding the cobalt and germanium dioxide into the composite powder in the step a, adding 150 parts of ethanol, mixing and ball-milling for 30min to form mixed slurry;
c. drying the mixed slurry until the water content or ethanol content is less than or equal to 1%, sintering in a sintering furnace at 1500 deg.C under 50MPa for 15 min.
Example 3 preparation of a tungsten carbide composite Material by the method of the invention
The raw materials comprise: 80 parts of WC, Al2O36 parts of ZrO28 parts of cobalt, 4 parts of germanium dioxide, 3 parts of tungsten powder and 2 parts of molybdenum powder.
The preparation steps are as follows:
a. mixing WC powder and tungsten powder in proportion, heating to 550 ℃, preserving heat for 18min to decarbonize the surface of tungsten carbide to form a mixture of tungsten and tungsten oxide, introducing argon gas for reduction, heating to 700 ℃, and preserving heat for 15min to prepare composite powder of tungsten and tungsten carbide;
b. mixing Al2O3，ZrO2B, weighing cobalt, molybdenum powder and germanium dioxide in proportion, adding the weighed cobalt, molybdenum powder and germanium dioxide into the composite powder in the step a, adding 120 parts of water, mixing and ball-milling for 20min to form mixed slurry;
c. drying the mixed slurry until the water content or ethanol content is less than or equal to 1%, sintering in a sintering furnace at 1450 ℃ under 45MPa for 13 min.
Example 4 preparation of a tungsten carbide composite Material by the method of the invention
The raw materials comprise: 80 parts of WC, Al2O36 parts of ZrO25 parts of cobalt, 4 parts of germanium dioxide and 5 parts of tungsten powder.
The preparation steps are as follows:
a. mixing WC powder, tungsten powder and Al2O3，ZrO2After cobalt and germanium dioxide are weighed according to a proportion, 150 parts of ethanol is added, and mixed and ball-milled for 20min to form mixed slurry;
b. drying the mixed slurry until the water content or ethanol content is less than or equal to 1%, sintering in a sintering furnace at 1400 ℃ under 50MPa for 15 min.
The composite materials prepared in examples were subjected to property measurement to obtain the results shown in table 1 below.
TABLE 1 Performance Table for different tungsten carbide composites
Figure BDA0001191987140000061
The embodiment shows that the tungsten carbide composite material with compact structure, high hardness and good wear resistance can be prepared by combining the raw material proportion and the production process of the invention, and has important economic benefit.

Claims (6)

1. Novel tungsten carbide composite material, its characterized in that, the constitution includes: according to the weight portion, WC80-82 portions, Al2O34-6 parts of ZrO25-8 parts of cobalt, 2-4 parts of cobalt, 3-6 parts of germanium dioxide and 3-5 parts of tungsten powder;
the preparation method of the novel carbide composite material comprises the following steps:
a. mixing WC powder and tungsten powder in proportion, heating to 500-600 ℃, preserving heat for 15-20 min to decarbonize the surface of tungsten carbide to form a mixture of tungsten and tungsten oxide, introducing argon gas for reduction, heating to 650-750 ℃, and preserving heat for 10-20min to prepare composite powder of tungsten and tungsten carbide;
b. mixing Al2O3，ZrO2After cobalt and germanium dioxide are weighed according to a proportion, adding the weighed cobalt and germanium dioxide into the composite powder in the step a, adding 100-150 parts of ethanol or water, mixing and ball-milling for 15-30min to form mixed slurry;
c. drying the mixed slurry until the water content or ethanol content is less than or equal to 1%, sintering in a sintering furnace at the sintering temperature of 1400 ℃ and 1500 ℃, at the pressure of 40-50MPa, and keeping the temperature for 10-15 min.
2. The novel tungsten carbide composite material according to claim 1, characterized in that: the composition also comprises molybdenum powder accounting for 1-3% of the total weight of the rest raw materials.
3. The novel tungsten carbide composite material according to claim 1, characterized in that: the grain size of the WC is 100-150 um.
4. The novel tungsten carbide composite material according to claim 1, characterized in that: the particle size of the cobalt is 50-100 um.
5. The novel tungsten carbide composite material according to claim 1, characterized in that: the purity of the tungsten powder is 99.9%.
6. The novel tungsten carbide composite material according to claim 1, characterized in that: the sintering temperature in step c is increased from the room temperature to 1400-1500 ℃ within 3-5 min.
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