CN111690861B - Contains TiO2Cermet cutter material and preparation method thereof - Google Patents

Contains TiO2Cermet cutter material and preparation method thereof Download PDF

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CN111690861B
CN111690861B CN202010574772.1A CN202010574772A CN111690861B CN 111690861 B CN111690861 B CN 111690861B CN 202010574772 A CN202010574772 A CN 202010574772A CN 111690861 B CN111690861 B CN 111690861B
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tio
raw materials
sintering
metal ceramic
tac
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CN111690861A (en
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彭欣
高荣根
杨慧
肖旭凯
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Zhuzhou Huarui Precision Cutting Tools Co ltd
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Zhuzhou Huarui Precision Cutting Tools Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/24—Nitriding

Abstract

The inventionProvides a catalyst containing TiO2The metal ceramic cutting tool material comprises the following raw materials of Ti (C) and a preparation method thereof0.5，N0.5)：35～45％，(Ti39.8，W46.9)C：20～30％，Mo2C：5～15％，TaC：5～10％，Cr2C3：0.5～1.5％，Co+Ni：12～18％，TiO2:1 to 3 percent. Weighing the raw materials according to the proportion, adding a polyethylene glycol forming agent and alcohol, performing ball milling and drying, and pressing into a blank; sintering and rapidly cooling the obtained blank to obtain the product containing TiO2The method can greatly improve the bending strength and the fracture toughness of the metal ceramic, so as to realize good matching of hardness and toughness, improve the cutting stability of the metal ceramic and prolong the service life of the metal ceramic.

Description

Contains TiO2Cermet cutter material and preparation method thereof
Technical Field
The invention relates to the field of metal ceramics, in particular to a titanium dioxide (TiO) -containing ceramic2The metal ceramic cutting tool material and the preparation method thereof.
Background
Cermet, a new hard material, has excellent properties such as high hardness, high wear resistance, and chemical stability, and is widely used as a tool material, a mold material, and a heat-resistant and wear-resistant member. Particularly, as a cutting tool, the metal ceramic has the characteristics of high temperature resistance, small friction coefficient, good metal adhesion resistance and the like, and gradually replaces the traditional hard alloy tool in the aspects of finish machining, semi-finish machining of steel cutting pieces, steel casting, iron casting and the like. However, the cermet cutting tool has the characteristics of poor toughness and chipping resistance, abnormal cutting tool cracking exists, if the content of the binder phase is simply increased, the toughness can be improved, but the wear resistance of the cutting tool is greatly reduced, the plasticity resistance is also reduced, and finally the service life of the cutting tool is poor. In addition, in the cermet, the carbon balance two-phase region is wide, and the low carbon side or the high carbon side is not beneficial to the optimization of the performance of the cermet, so that how to find the optimal value of the carbon balance is also a problem worthy of discussion.
Therefore, it is necessary to provide a TiO-containing material2The preparation method of the metal ceramic cutter material improves the bending strength and the fracture toughness of the metal ceramic cutter and the integral hardness of the material, so that the cutting stability and the service life of the metal ceramic cutter are improved.
Disclosure of Invention
The invention provides a TiO-containing material2The object of which is to improve the TiO content2The bending strength, hardness and fracture toughness of the metal ceramic cutter are improved, and the wear resistance of the metal ceramic cutter is also improved.
In order to achieve the above object, embodiments of the present invention provide a TiO-containing material2The metal ceramic cutting tool material comprises the following raw materials of Ti (C)0.5，N0.5)：35～45％，(Ti39.8，W46.9)C：20～30％，Mo2C：5～15％，TaC：5～10％，Cr2C3：0.5～1.5％，Co+Ni：12～18％， TiO2：1～3％。
Preferably, the Ti (C)0.5，N0.5)、(Ti39.8，W46.9)C、Mo2C、TaC、Cr2C3The particle size of (B) is 0.5 to 2 μm.
Preferably, the nickel powder is carbonyl nickel powder.
Preferably, the TiO is2Is nanometer superfine powder with the particle size of 50-100 nm.
The embodiment of the invention also provides a TiO-containing material2The preparation method of the metal ceramic cutter material comprises the following steps:
step 1, respectively weighing Ti (C) according to the raw material ratio0.5，N0.5)、(Ti39.8，W46.9)C、Mo2C、 TaC、Cr2C3Co, Ni and TiO2Then adding polyethylene glycol accounting for 2-4% of the total mass of the raw materials and 0.70-0.80L/kg of alcohol of the raw materials, mixing, performing ball milling, and drying to obtain a mixture;
step 2, pressing and forming the mixture under the pressing pressure of 80-120 MPa to obtain a blank body;
and 3, sintering the obtained blank in a de-esterification and sintering integrated furnace at the sintering temperature of 1450-1500 ℃ for 60min, introducing nitrogen with the relative atmospheric pressure of 30-40 mbar for surface nitriding treatment during sintering, and performing rapid cooling treatment after sintering to obtain the TiO-containing material2The cermet cutting tool material of (1).
Preferably, in the step 1, the ball milling process is as follows: the rotating speed of the ball mill is 37r/min, the ball-material ratio is 8: 1-10: 1, and the ball milling time is 30-54 h.
Preferably, in step 3, the rapid cooling treatment specifically includes: reducing the temperature from 1450-1500 ℃ to below 800 ℃ within 30 min.
In the invention, the TiO-containing material is prepared by a powder metallurgy method2The nanometer superfine titanium carbonitride base cermet material is added with TiO with the same main component elements as the cermet and high melting point2Ultrafine particles, sintering in a nitrogen atmosphere, can make TiO2The nanometer superfine particles are uniformly distributed in the binding phase of the metal ceramic, and the binding phase is strengthened. At the same time, TiO2The nanometer superfine particles are attached to the surface of titanium carbonitride, can block the growth of crystal grains, so that the Ti (C, N) crystal grains are refined, and the hardness and the fracture toughness of the metal ceramic are improved. And TiO2The nano particles are distributed in dispersion particles or particles at the crystal boundary in the matrix, the dispersion strengthening effect of the oxide with the high melting point can be kept at a higher temperature, when cracks are initiated in the matrix, the dispersion phase exists, the fracture path is induced to deflect, or the bridging mode is adopted, the larger the energy required by crack expansion is, the more difficult the fracture is, the strength and the toughness of the metal ceramic can be obviously improved, and the finer the particles are, the more the particles are uniformly distributed in a dispersion manner, the better the strengthening effect is.
In addition, Ti is a main component of the cermet, TiO2Simultaneously can be used as a carbon balance adjusting means, because of the deviation of the total carbon content in the material preparation process, the carburization phenomenon may occur in the preparation process, and TiO is used as a carbon balance adjusting means2The carbon balance point of the cermet can be adjusted to achieve the optimum carbon balance point, such as TiO2The +3C is TiC +2CO, which can not only solve the redundant problem in the matrixCarbon, and the formed titanium carbide has high hardness, so that the wear resistance of the metal ceramic can be improved to a certain extent.
The nickel powder in the binder phase adopted by the invention is carbonyl nickel powder, and compared with the common electrolytic nickel powder, the carbonyl nickel powder has the characteristics of high purity, uniform and fine granularity and low content of metal impurities, and is beneficial to dispersing the binder metal in the liquid phase sintering process, filling hard phase gaps and improving the bending strength and toughness of the cutter.
The scheme of the invention has the following beneficial effects:
1. the invention introduces TiO into the metal ceramic2Ultra-fine particles by adding a minor amount of TiO2The ultrafine particles can realize the strengthening effect of the binding phase, inhibit the growth of titanium carbonitride grains and induce the deflection of fracture paths, thereby achieving the purpose of improving the hardness and the fracture toughness of the metal ceramic, and the strength, the hardness and the fracture toughness of the metal ceramic are all superior to those of the metal ceramic without adding TiO2The comprehensive performance of the common superfine metal ceramic.
2. TiO-containing compounds prepared by the invention2The metal ceramic cutting tool has less material gaps, the integral hardness is more than HRA92, and the fracture toughness is more than 8.40MPa1/2The bending strength is larger than 2400MPa, the overall performance is improved, the cutting stability of the metal ceramic cutter is improved, and the service life of the metal ceramic cutter is prolonged.
Drawings
FIG. 1 shows TiO-containing compounds prepared in example 1 of the present invention2SEM image of the cermet cutting tool material of (1).
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
Example 1
Respectively weighing Ti (C) according to the raw material ratio0.5,N0.5)、(Ti39.8W46.9)C、Mo2C、TaC、Cr2C. Co, Ni and TiO2The raw material ratio is shown in table 1.
Table 1 contents of raw materials in example 1
Raw materials Ti(C0.5,N0.5) (Ti39.8W46.9)C Mo2C TaC Cr2C3 Co Ni TiO2
Mass percent 40％ 25.5％ 10％ 7％ 1％ 9％ 6％ 1.5％
Pouring the prepared raw materials into a ball mill, adding polyethylene glycol accounting for 3.5 percent of the total mass of the raw materials, wherein the ball-to-material ratio is 10:1, the adding amount of alcohol is 0.75L/kg of the raw materials, the rotating speed of the ball mill is 37r/min, and the ball milling time is 40h, so as to prepare the alloy powder mixture. And pressing the mixture into a blank with a certain size and shape under the pressing pressure of 80-120 MPa. Sintering the obtained blank in a nitrogen atmosphere at the sintering temperature of 1480 ℃ for 60min, and introducing nitrogen with the relative atmospheric pressure of 35mbar for surface nitriding treatment to enable the alloy to have a structure with hard outside and tough inside; after sintering, rapid cooling treatment is carried out, and the temperature is reduced from 1480 ℃ to below 800 ℃ within 30min so as to keep the performance of a high-temperature state and inhibit the growth of crystal grains.
TiO-containing compositions prepared in this example2The hardness of the metal ceramic cutter material is HRA92.8, and the fracture toughness is 8.45MPa.m1/2The bending strength is 2459MPa, the porosity is A02B00C00, the appearance is shown in figure 1, the microstructure has two hard phase structures of black core gray ring and white core gray ring, and the hard phase structures are uniformly dispersed in the bonding metal, and TiO is2The particles are distributed in the hard phase surface and the binding metal.
Example 2
Respectively weighing Ti (C) according to the raw material ratio0.5,N0.5)、(Ti39.8W46.9)C、Mo2C、TaC、Cr2C. Co, Ni and TiO2The raw material ratio is shown in table 2.
Table 2 contents of raw materials in example 2
Raw materials Ti(C0.5,N0.5) (Ti39.8W46.9)C Mo2C TaC Cr2C3 Co Ni TiO2
Mass percent 39.5％ 26.5％ 10％ 6％ 1％ 8％ 7％ 2％
Pouring the prepared mixed raw materials into a ball mill, adding 3.5 percent of polyethylene glycol based on the total weight of the raw materials, wherein the ball-to-material ratio is 8:1, the adding amount of alcohol is 0.75L/kg, the ball milling time is 40h, and the rotating speed of the ball mill is 37r/min, so as to prepare the alloy powder mixture. And pressing the mixture into a green body with a certain size and shape under the pressing pressure of 80-120 MPa. Sintering the obtained pressed compact in nitrogen atmosphere at 1480 deg.C for 60min, and introducing 35mbar surface nitriding treatment to make the alloy have hard outer and tough inner structure; after sintering, carrying out rapid cooling treatment, and reducing the temperature of 1480 ℃ to below 800 ℃ within 30min to keep the performance of a high-temperature state and inhibit the growth of crystal grains.
The hardness of the cermet prepared in this example was HRA93.0 and the fracture toughness 8.65MPa.m1/2The bending strength is 2518MPa, and the porosity is A02B00C 00.
Example 3
Respectively weighing Ti (C) according to the raw material ratio0.5,N0.5)、(Ti39.8W46.9)C、Mo2C、TaC、Cr2C. Co, Ni and TiO2The raw material ratio is shown in table 3.
Table 3 contents of raw materials in example 3
Raw materials Ti(C0.5,N0.5) (Ti39.8W46.9)C Mo2C TaC Cr2C3 Co Ni TiO2
Mass percent 43.5％ 22.5％ 10％ 6％ 1％ 8.5％ 6.5％ 3％
Pouring the prepared raw materials into a ball mill, adding polyethylene glycol accounting for 3.5 percent of the total mass of the raw materials, wherein the ball-to-material ratio is 8:1, the adding amount of alcohol is 0.75L/kg of the raw materials, the rotating speed of the ball mill is 37r/min, and the ball milling time is 40h, so as to prepare the alloy powder mixture. And pressing the mixture into a blank with a certain size and shape under the pressing pressure of 80-120 MPa. Sintering the obtained blank in a nitrogen atmosphere at 1500 ℃, keeping the temperature for 60min, and introducing nitrogen with the relative atmospheric pressure of 35mbar for surface nitriding treatment to enable the alloy to have a structure with hard outside and tough inside; after sintering, rapid cooling treatment is carried out, and the temperature is reduced from 1500 ℃ to below 800 ℃ within 30min so as to keep the performance of a high-temperature state and inhibit the growth of crystal grains.
The hardness of the cermet prepared in this example was HRA93.2 and the fracture toughness was 8.69MPa.m1/2The bending strength is 2445MPa, and the porosity is A04B00C 00.
Comparative example 1
Respectively weighing Ti (C) according to the raw material ratio0.5,N0.5)、(Ti39.8W46.9)C、Mo2C、TaC、Cr2C. The raw material ratios of Co and Ni are shown in Table 4.
Table 4 contents of respective raw materials in comparative example 1
Raw materials Ti(C0.5,N0.5) (Ti39.8W46.9)C Mo2C TaC Cr2C3 Co Ni
Mass percent 40％ 25.5％ 11％ 7％ 1.5％ 9％ 6％
Pouring the prepared raw materials into a ball mill, adding polyethylene glycol accounting for 3.5 percent of the total mass of the raw materials, wherein the ball-to-material ratio is 10:1, the adding amount of alcohol is 0.75L/kg of the raw materials, the rotating speed of the ball mill is 37r/min, and the ball milling time is 40h, so as to prepare the alloy powder mixture. And pressing the mixture into a blank with a certain size and shape under the pressing pressure of 80-120 MPa. Sintering the obtained blank in a nitrogen atmosphere at the sintering temperature of 1480 ℃ for 60min, and introducing nitrogen with the relative atmospheric pressure of 35mbar for surface nitriding treatment to enable the alloy to have a structure with hard outside and tough inside; after sintering, rapid cooling treatment is carried out, and the temperature is reduced from 1480 ℃ to below 800 ℃ within 30min so as to keep the performance of a high-temperature state and inhibit the growth of crystal grains. The hardness of the cermet prepared in the examples was HRA92.0 and the fracture toughness was 8.25MPa.m1/2The flexural strength was 2032MPa, and the porosity was A02B00C 00.
Comparative example 2
Respectively weighing Ti (C) according to the raw material ratio0.5,N0.5)、(Ti39.8W46.9)C、Mo2C、TaC、Cr2C. Co, Ni and TiO2The raw material ratio is shown in table 5.
TABLE 5 content of each raw material in comparative example 2
Raw materials Ti(C0.5,N0.5) (Ti39.8W46.9)C Mo2C TaC Cr2C3 Co Ni TiO2
Mass percent 40％ 25％ 10％ 5％ 1％ 9％ 5％ 5％
Pouring the prepared raw materials into a ball mill, adding polyethylene glycol accounting for 3.5 percent of the total mass of the raw materials, wherein the ball-to-material ratio is 10:1, the adding amount of alcohol is 0.75L/kg of the raw materials, the rotating speed of the ball mill is 37r/min, and the ball milling time is 40h, so as to prepare the alloy powder mixture. And pressing the mixture into a blank with a certain size and shape under the pressing pressure of 80-120 MPa. Sintering the obtained blank in a nitrogen atmosphere at the sintering temperature of 1480 ℃ for 60min, and introducing nitrogen with the relative atmospheric pressure of 35mbar for surface nitriding treatment to enable the alloy to have a structure with hard outside and tough inside; after sintering, rapid cooling treatment is carried out, and the temperature is reduced from 1480 ℃ to below 800 ℃ within 30min so as to keep the performance of a high-temperature state and inhibit the growth of crystal grains. The hardness of the cermet prepared in the examples was HRA93.0 and the fracture toughness was 8.25MPa.m1/2The flexural strength was 1632MPa, and the porosity was A04B02C 00.
TiO2When the content exceeds the protection range, the pores of the material are increased, the wettability is reduced, and the comprehensive mechanical property is reduced.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (1)

1. Contains TiO2The cermet cutting tool material is characterized by comprising the following raw materials of Ti (C)0.5，N0.5)：35~45%，(Ti39.8，W46.9)C：20~30%，Mo2C：5~15%，TaC：5~10%，Cr2C3：0.5~1.5%，Co+Ni：12~18 %，TiO2: 1-3% of the above componentsThe sum of the mass percentages of the raw materials is 100 percent;
the Ti (C)0.5，N0.5)、(Ti39.8，W46.9)C、Mo2C、TaC、Cr2C3The particle size of (A) is 0.5-2 μm;
nickel is carbonyl nickel powder;
the TiO is2Is nano-ultrafine powder with the particle size of 50-100 nm;
the TiO-containing2The preparation method of the metal ceramic cutter material comprises the following steps:
step 1, respectively weighing Ti (C) according to the raw material ratio0.5，N0.5)、(Ti39.8，W46.9)C、Mo2C、TaC、Cr2C3Co, Ni and TiO2Then adding polyethylene glycol accounting for 2-4% of the total mass of the raw materials and 0.70-0.80L/kg of alcohol of the raw materials, mixing, performing ball milling, and drying to obtain a mixture;
step 2, pressing and forming the mixture under the pressing pressure of 80-120 MPa to obtain a blank body;
and 3, sintering the obtained blank in a de-esterification and sintering integrated furnace at the sintering temperature of 1450-1500 ℃ for 60min, introducing nitrogen with the relative atmospheric pressure of 30-40 mbar for surface nitriding treatment during sintering, and performing rapid cooling treatment after sintering to obtain the TiO-containing material2The cermet cutting tool material of (1);
in the step 1, the ball milling process comprises the following steps: the rotating speed of the ball mill is 37r/min, the ball-material ratio is 8: 1-10: 1, and the ball milling time is 30-54 h;
in the step 3, the rapid cooling treatment specifically comprises: reducing the temperature from 1450-1500 ℃ to below 800 ℃ within 30 min.
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