CN113416077B - High-temperature ceramic cutter material with double composite structure and preparation method and application thereof - Google Patents

High-temperature ceramic cutter material with double composite structure and preparation method and application thereof Download PDF

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CN113416077B
CN113416077B CN202110708064.7A CN202110708064A CN113416077B CN 113416077 B CN113416077 B CN 113416077B CN 202110708064 A CN202110708064 A CN 202110708064A CN 113416077 B CN113416077 B CN 113416077B
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temperature
ceramic
zrb
zirconium diboride
ball milling
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CN113416077A (en
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许崇海
张敬宝
肖光春
衣明东
陈照强
张静婕
商锡佐
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Jinan Xinlixin Machinery Manufacturing Co ltd
Qilu University of Technology
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Jinan Xinlixin Machinery Manufacturing Co ltd
Qilu University of Technology
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    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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    • C04B35/58078—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides based on zirconium or hafnium borides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23B—TURNING; BORING
    • B23B27/00—Tools for turning or boring machines; Tools of a similar kind in general; Accessories therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B26—HAND CUTTING TOOLS; CUTTING; SEVERING
    • B26D—CUTTING; DETAILS COMMON TO MACHINES FOR PERFORATING, PUNCHING, CUTTING-OUT, STAMPING-OUT OR SEVERING
    • B26D1/00—Cutting through work characterised by the nature or movement of the cutting member or particular materials not otherwise provided for; Apparatus or machines therefor; Cutting members therefor
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    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23B—TURNING; BORING
    • B23B2226/00—Materials of tools or workpieces not comprising a metal
    • B23B2226/18—Ceramic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B26—HAND CUTTING TOOLS; CUTTING; SEVERING
    • B26D—CUTTING; DETAILS COMMON TO MACHINES FOR PERFORATING, PUNCHING, CUTTING-OUT, STAMPING-OUT OR SEVERING
    • B26D1/00—Cutting through work characterised by the nature or movement of the cutting member or particular materials not otherwise provided for; Apparatus or machines therefor; Cutting members therefor
    • B26D1/0006—Cutting members therefor
    • B26D2001/002—Materials or surface treatments therefor, e.g. composite materials
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
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    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]

Abstract

The invention relates to a high-temperature ceramic cutter material with a double-composite structure, and a preparation method and application thereof. The ceramic cutting tool material consists of ceramic particles and ceramic powder and has a double composite structure. The ceramic powder comprises zirconium diboride, silicon carbide, silicon nitride and yttrium oxide, and the ceramic particles comprise zirconium diboride and silicon carbide. The preparation method of the ceramic cutter material comprises the steps of preparation of ceramic particles, preparation of the ceramic cutter material, spark plasma sintering and the like. The ceramic cutter material obviously improves the high-temperature mechanical property, particularly the fracture toughness, and prolongs the service life of the cutter during high-speed cutting.

Description

High-temperature ceramic cutter material with double composite structure and preparation method and application thereof
Technical Field
The invention relates to a high-temperature ceramic cutter material, in particular to a high-temperature ceramic cutter material with a double-composite structure, and a preparation method and application thereof.
Background
Zirconium diboride (ZrB)2) The zirconium diboride material is an ultrahigh temperature material, but the application of the zirconium diboride material is limited to a certain extent due to the defects of high temperature, easy oxidation, low strength and the like. ZrB2Because of the characteristics of extremely strong covalent bond, extremely high melting point and low self-diffusion coefficient, the powder particles have oxide layers and other impurities on the surfaces and are difficult to sinter. The sintering temperature is usually higher than 2000 ℃ to obtain dense zirconium diboride ceramics, and the main methods for lowering the sintering temperature are to reduce the starting powder particle size and to use sintering additives. In selecting sintering additives, the type and amount must be carefully selected because their addition affects ZrB2Densification, microstructure, phase combination and properties. Metallic (nickel, copper, cobalt, chromium, and iron) and non-metallic (carbide, disilicide, etc.) sintering additives can be used to obtain dense ZrB at relatively low sintering temperatures2A ceramic. Metal additives such as nickel, copper, cobalt, chromium and iron (typically added at less than 2 wt%) are beneficial in achieving near theoretical sintered densities, significantly lowering sintering temperatures due to liquid phase sintering, and improving ZrB2Is very effective in terms of room-temperature mechanical properties. The addition of the carbide sintering additive is mainly carried out by removing ZrB existing in the carbide2Surface oxide impurities on the starting powder to help strengthen ZrB2To densify. The elimination of the surface oxide is very important because it inhibits densification by promoting grain growth through evaporation and condensation of the surface oxide during sintering.
Besides high sintering temperature and poor oxidation and ablation resistance at high temperature, zirconium diboride ceramic material has low fracture toughness, which severely limits its wide application in harsh environments such as high temperature. According to the reports of the prior documents, in the strengthening and toughening research of the zirconium diboride ceramic material, carbon fiber, silicon carbide (SiC) and whisker are frequently usedIs used as a toughening phase and can improve ZrB to a certain degree2Fracture toughness of ceramics. However, the fracture toughness and bending strength of the zirconium diboride ceramic with silicon carbide added are still to be improved, and the fracture toughness and bending strength are also continuously reduced with the increase of temperature. Therefore, for zirconium diboride/silicon carbide high-temperature ceramic cutting tool materials, it is necessary to solve the problem of reduced toughness and strength in high-temperature environments.
At present, ceramic cutter materials, including zirconium diboride ceramics, mostly adopt a hot pressing sintering method. However, the hot-pressing sintering of the zirconium diboride-based ceramic material requires higher sintering temperature, and the ceramic material with higher compactness can be obtained only by sintering at temperature higher than 1900 ℃ or adding sintering aids such as metal and the like; for example, sintering into a ceramic article at a temperature of 2050 ℃ in a hydrogen atmosphere. . The grains of the ceramic material can grow greatly during the sintering process at higher sintering temperature, and the bending strength of the cutter material is reduced by the larger grains according to the Hall-Petch equation. And secondly, the mechanical property of the ceramic material at high temperature is reduced by adding metal and other sintering aids.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a high-temperature ceramic cutter material with a double-composite structure and a preparation method thereof, which solve the problem of reduction of high-temperature fracture toughness of the ceramic cutter material and improve the problem of reduction of bending strength at high temperature.
The invention also provides application of the high-temperature ceramic cutter material with the double-composite structure.
Interpretation of terms:
double composite structure: is ZrB2Composite SiC ceramic particles and ZrB2/SiC/Si3N4The composite ceramic powder is mixed to prepare the composite material.
Summary of the invention: the high-temperature ceramic cutter material consists of ceramic particles and ceramic powder and has a double composite structure. The ceramic powder consists of zirconium diboride, silicon carbide, silicon nitride and yttrium oxide, and the ceramic particles are formed by sintering the zirconium diboride and the silicon carbide. The invention prepares the nearly spherical ZrB by a spray drying technology2Composite SiC ceramic particlesAdding the prepared ceramic particles to ZrB2/SiC/Si3N4In the composite ceramic powder, the high-temperature ceramic cutter material with a double composite structure is prepared by using a spark plasma sintering technology, and unexpectedly, the fracture toughness of the cutter is not reduced but slightly increased under the high temperature condition of 600 plus 1100 ℃; on the other hand, the reduction amplitude of the bending strength is also obviously reduced; thereby improving the mechanical property of the cutter material at high temperature and realizing the application effect of improving the effective cutting distance of the ceramic cutter at high temperature.
The technical scheme of the invention is as follows:
a high-temperature ceramic cutter material with a double composite structure is prepared by sintering the following raw materials in percentage by volume through spark plasma:
5-30% of silicon carbide powder and silicon nitride (Si)3N4)2.5～10％，ZrB25-40% of/SiC composite ceramic particles, 0.5-5% of yttrium oxide and the balance of zirconium diboride, wherein:
said ZrB2the/SiC composite ceramic particles are prepared by uniformly mixing zirconium diboride and silicon carbide powder according to the volume ratio of (3-5) to (0.5-2) in polyethylene glycol-absolute ethyl alcohol, carrying out ball milling, drying, dispersing in a binder-deionized water mixed solution, carrying out ultrasonic stirring and ball milling, carrying out spray drying on ball milling slurry to prepare particles, and carrying out binder removal and sintering.
The high-temperature ceramic cutting tool material with double composite structures takes zirconium diboride as a matrix, yttrium oxide as a sintering aid and ZrB as2Composite SiC ceramic particles and ZrB2/SiC/Si3N4The composite ceramic powder is sintered. Namely, the zirconium diboride-based high-temperature ceramic cutting tool material with a double composite structure.
Preferably according to the invention, said ZrB2The average particle diameter of the/SiC composite ceramic particles is 10-20 mu m.
Preferably, according to the invention, the raw materials used have the following particle sizes:
the average grain size of the zirconium diboride is 1-10 mu m, and the average grain size of the zirconium diboride is preferably 2-7 mu m; the average grain size of the silicon carbide is 0.5-5 μm, and the average grain size of the silicon carbide is more preferably 0.7-2 μm; the average particle size of the silicon nitride is 0.2 to 2 μm, and more preferably 0.4 to 1 μm.
According to the optimization of the invention, the high-temperature ceramic cutter material with a double composite structure comprises the following raw materials in percentage by volume: 5-25% of silicon carbide powder, 4-8% of silicon nitride and ZrB210-35% of/SiC composite ceramic particles, 0.5-2% of yttrium oxide and the balance of zirconium diboride.
Further preferably, the high-temperature ceramic cutting tool material with a double composite structure comprises the following raw materials in percentage by volume: 10-20% of silicon carbide powder, 5-7.5% of silicon nitride and ZrB215-25% of/SiC composite ceramic particles, 1-1.5% of yttrium oxide and the balance of zirconium diboride.
Preferred according to the invention, ZrB2The sum of the SiC content in the/SiC composite ceramic particles and the amount of the silicon carbide powder is 7-40% by volume; among them, the volume ratio is preferably 10 to 30%, most preferably 15 to 25%. The total amount of SiC is controlled in a proper range, which is more beneficial to the bending strength and the bending strength of the ceramic cutter material.
According to the invention, the ZrB is preferred2the/SiC composite ceramic particles are prepared by the following method:
mixing zirconium diboride and silicon carbide powder in a polyethylene glycol-absolute ethyl alcohol according to a proportion, ultrasonically stirring, ball-milling, drying and sieving to obtain composite powder; then, the user can use the device to perform the operation,
dispersing the obtained composite powder in a binder-deionized water mixed solution, wherein the using amount of the binder is 0.25-1.5% of the mass of the zirconium diboride, ultrasonically stirring, carrying out ball milling to obtain ball milling slurry, then,
thirdly, the obtained slurry is sprayed and dried to be made into particles, and the particles are subjected to binder removal and sintering in a vacuum sintering furnace.
The spray drying method has the characteristics of simple operation, short preparation time and good stability, the size of the prepared particles is easy to control, and the shape of the prepared particles can be conveniently controlled. In the present invention, ZrB is preferred2Preparation of/SiC composite ceramic particlesSpherical particles.
According to the invention, said ZrB2In the preparation process of the/SiC composite ceramic particles, the preferable preparation conditions are one or more of the following conditions:
A. the volume ratio of the zirconium diboride to the silicon carbide is (3.5-5) to (0.5-1.5).
B. The content of the polyethylene glycol is 0.5-3% of the mass of the zirconium diboride; more preferably, the content of the polyethylene glycol is 0.5-2% of the mass of the zirconium diboride.
C. In the step I, the ultrasonic stirring time is 30-60 min; the ball milling time is 40-60 h;
D. in the step I, the drying is vacuum drying, the drying temperature is 80-150 ℃, and the drying time is 10-30 h.
D. In the second step, the ultrasonic stirring time is 30-60 min; the ball milling time is 40-60 h;
E. the binder is polyvinyl alcohol, and more preferably, the binder is polyvinyl alcohol 1788 type.
F. The dosage of the binder is 0.25-1% of the mass of the zirconium diboride.
G. The feeding speed of the spray drying is 10-15 mL/min, the inlet temperature is 300-500 ℃, and the outlet temperature is 80-150 ℃.
H. Said ZrB2The temperature of the rubber discharging of the/SiC composite ceramic particles is 300-500 ℃, and the heat preservation time is 20-40 min.
I. Said ZrB2The sintering temperature of the/SiC composite ceramic particles is 1000-1250 ℃, 1050-1200 ℃ is preferred, and 1100 ℃ is most preferred. Preferably, the heat preservation time is 50-90 min.
The spray drying described above uses a spray dryer.
According to the invention, the preparation method of the high-temperature ceramic cutter material with the double-composite structure comprises the following steps:
(1)ZrB2preparation of/SiC composite ceramic particles
Proportionally mixing zirconium diboride and silicon carbide powder in polyethylene glycol-absolute ethyl alcohol, ultrasonically stirring, ball-milling, drying and sieving to obtain composite powder(ii) a Then, dispersing the obtained composite powder in a binder-deionized water mixed solution, wherein the binder consumption is 0.25-1.5% of the mass of zirconium diboride (by ZrB)2The mass of zirconium diboride in the/SiC composite ceramic particles) is measured, ultrasonic stirring is carried out, ball milling is carried out to obtain ball milling slurry, then the obtained slurry is sprayed and dried to prepare particles, and glue discharging and sintering are carried out in a vacuum sintering furnace;
(2)ZrB2/SiC/Si3N4the preparation method of the composite ceramic powder ball-milling liquid comprises the following steps:
a. adding polyethylene glycol into absolute ethyl alcohol until the polyethylene glycol is completely dissolved to obtain a polyethylene glycol-absolute ethyl alcohol solution, weighing zirconium diboride, silicon carbide, silicon nitride and yttrium oxide according to a proportion, pouring the zirconium diboride into the polyethylene glycol-absolute ethyl alcohol solution, and performing ultrasonic dispersion for 20-60 min to obtain a suspension A; respectively adding silicon carbide, silicon nitride and yttrium oxide into a proper amount of absolute ethyl alcohol, and performing ultrasonic dispersion for 20-60 min, and mixing to obtain a suspension B; mixing the suspension A and the suspension B, and ultrasonically stirring for 10-30 min to obtain a suspension C;
b. pouring the suspension C into a ball milling tank, adding ball milling balls, and filling high-purity nitrogen as a protective gas for ball milling for 40-60 hours;
(3) weighing ZrB prepared in the step (1) in proportion2Adding the/SiC composite ceramic particles into the ball milling tank in the step (2), introducing high-purity nitrogen gas, continuing ball milling for 0.5-2 hours, placing the ball-milled slurry into a drying box, performing vacuum drying, and then sieving to obtain cutter material powder;
(4) and (3) putting the cutter material powder into a mould for spark plasma sintering to obtain the high-temperature ceramic cutter material with the double-composite structure.
According to the process of the invention, the preferred preparation conditions are as follows:
in the step (1) and the step (2), the molecular weight of the polyethylene glycol is 2000-10000, and the polyethylene glycol 6000 is particularly preferred; the mass of the polyethylene glycol is 0.5-2% of that of the zirconium diboride.
According to the invention, the ball milling balls for ball milling in the steps (1) and (2) are preferably made of hard alloy; the mass ratio of the ball material is 10-20: 1.
According to the invention, the vacuum drying temperature in the step (3) is preferably 80-150 ℃, and the drying time is 10-30 h.
According to the preferable selection method, in the steps (1) and (3), a 100-300-mesh screen is selected for sieving. Considering that the powder can agglomerate in different degrees in the processing process, the size of the screen is larger than the particle size of the powder.
According to the present invention, in step (4), the discharge plasma sintering conditions are: the sintering temperature is 1700-1800 ℃. Further preferably, the sintering temperature of the spark plasma sintering is 1740-1780 ℃. Applying pressure of 30-50 MPa, and keeping the temperature for 5-15 min; further preferably, the pressure is applied to be 35-40 MPa, and the heat preservation time is 6-8 min.
Preferably, in step (4), the mold is a graphite mold.
The high-temperature ceramic cutter material with the double-composite structure has great advantages when being used under the high temperature conditions of 600-1100 ℃, and has the advantages of high fracture toughness, long cutter service life during high-speed cutting and the like.
According to the invention, the high-temperature ceramic cutting tool material with the double composite structure is applied to high-speed cutting tools under the high-temperature conditions of 600-1100 ℃. When the cutting speed v is 400m/min, the feed amount f is 0.102mm/r and the back cutting amount apUnder 0.1mm, the cutting distance of the high-temperature ceramic cutter with the double composite structure reaches 4000-4700 m.
The invention has the technical characteristics and beneficial effects that:
1. the invention provides a double composite structure of a ceramic cutter material for the first time, which is a double composite material of composite ceramic particles and composite ceramic powder and is formed by ZrB which is completely compact and nearly spherical2the/SiC composite ceramic particles are uniformly dispersed in continuous ZrB2/SiC/Si3N4In the ceramic powder, the mechanical properties of the double-composite structure material can be adjusted through external microstructure characteristics (such as integral components, volume ratio of particles to the ceramic powder, size and distribution of the particles) or internal physical properties (such as thermal expansion coefficient and the like). With conventional ZrB2Ceramic materialCompared with the material, due to the contribution of compact and approximately spherical ceramic particles in the double-composite structure, the double-composite structure system can generate excellent performance. In addition, the elastic or thermal expansion mismatch between the near-spherical ceramic particles and the ceramic powder can be reduced by the double composite structure. Therefore, the high-temperature ceramic cutting tool material with the double composite structure has obvious advantages compared with the traditional zirconium diboride ceramic material.
2. The invention adopts spray drying technology to prepare ZrB2mixing/SiC composite ceramic particles with ZrB2/SiC/Si3N4Preparing the high-temperature ceramic cutter material with a double composite structure from the ceramic powder. It has been unexpectedly found that ZrB2The addition of the/SiC composite ceramic particles solves the problem of reduction of high-temperature fracture toughness of the ceramic cutter material, effectively improves the mechanical property of the ceramic cutter material at high temperature, particularly the high-temperature fracture toughness, and simultaneously improves the cutter service life in high-speed cutting. Experiments prove that the fracture toughness of the high-temperature ceramic cutter material with the double composite structure prepared by the invention at the high temperature of 600-1100 ℃ is not reduced or increased than that at room temperature, and an unexpected excellent effect is achieved.
3. The invention is in the conventional ZrB2Si addition in/SiC ceramic powder3N4Surprisingly, it has been found in the present invention that Si3N4Can slow down the reduction range of the bending strength of the cutter material under the high-temperature condition. Si3N4The addition of the (C) can reduce the rate of reducing the grain boundary strength along with the temperature rise, and effectively increase the grain boundary strength at high temperature, thereby increasing the number of transgranular fractures in the fracture process at high temperature and slowing down ZrB2The bending strength of the/SiC ceramic cutter material is reduced under high temperature conditions. The bending strength of the dual-composite-structure ZrB 2-based high-temperature ceramic cutting tool material is reduced by a smaller extent than that of the conventional ZrB 2-based ceramic material at the high temperature of 600-1100 ℃.
4. The invention adopts Spark Plasma Sintering (SPS) technology to prepare the ceramic particle-added high-temperature ceramic cutting tool material with double composite structure, the existing zirconium diboride ceramic cutting tool is mainly sintered by a hot pressing method, and a small amount of spark plasma sintering is also carried out. Compared with the existing hot-pressing sintering mode, the spark plasma sintering mode has the advantages of high temperature rise speed, low sintering temperature, short heat preservation time and the like. The SPS sintering heating mode is high-frequency coil heating and pulse current heating, so that the sintering time is greatly reduced, and the ceramic material with higher compactness can be obtained at lower sintering temperature.
Drawings
FIG. 1 is ZrB obtained in example 12SEM image of/SiC ceramic particles.
FIG. 2 is an SEM image of a cross section of the dual composite structure high temperature ceramic cutting tool material obtained in example 1.
FIG. 3 is a graph showing the effect of the amount of silicon nitride added on the hardness of a ceramic cutting tool material.
FIG. 4 is a graph showing the effect of the amount of silicon nitride added on the bending strength of a ceramic cutting tool material.
FIG. 5 is a graph showing the effect of the addition of silicon nitride on the fracture toughness of a ceramic cutting tool material.
FIG. 6 is a graph showing a comparison of fracture toughness curves of ceramic cutting tool materials of dual composite structure and non-dual composite structure in the range of room temperature to 1100 deg.C, corresponding to the ceramic cutting tool materials of example 1 and comparative example 1, respectively. The abscissa is temperature and the ordinate is fracture toughness.
Detailed description of the preferred embodiments
The present invention will be further described with reference to specific examples, but the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified.
Example 1
A high-temperature ceramic cutter material with a double composite structure is prepared by sintering the following raw materials in percentage by volume through spark plasma: 16% of silicon carbide, 5% of silicon nitride and ZrB220 percent of/SiC composite ceramic particles (ZrB)2: SiC-4: 1 volume ratio), yttria 1%, and zirconium diboride the remainder. The total amount of SiC in the bulk cutter material was 20 vol%.
1. Adding polyethylene glycol accounting for 1% of the mass of zirconium diboride into a proper amount of absolute ethyl alcohol to be completely dissolved to obtain a polyethylene glycol-absolute ethyl alcohol solution, weighing zirconium diboride with the average particle size of 3 mu m and silicon carbide powder with the average particle size of 1 mu m according to the volume ratio of 4:1, adding the zirconium diboride powder and the silicon carbide powder into the polyethylene glycol-absolute ethyl alcohol solution, and carrying out ultrasonic stirring for 30min to obtain a suspension.
2. And pouring the obtained suspension into a ball ink tank, adding a hard alloy ball grinding ball (ball material ratio is 10:1), filling high-purity nitrogen as protective gas, and carrying out ball milling for 48 hours.
3. Pouring the ball-milled slurry into a tray, putting the tray into a drying oven, drying the tray for 24 hours in vacuum at the temperature of 100 ℃, and then sieving the composite powder with a 200-mesh sieve to obtain the composite powder;
4. polyvinyl alcohol binder (ZrB) accounting for 0.5 percent of the mass of the zirconium diboride2Zirconium diboride in the/SiC composite ceramic particles) is dissolved in deionized water, the composite powder obtained in the step (3) is added, and ultrasonic stirring is carried out for 30min, so as to obtain suspension with the solid content of 40%;
5. carrying out spray drying on the suspension obtained in the step 4 by using a spray dryer, wherein the feeding speed is 12mL/min, the inlet temperature is 400 ℃, and the outlet temperature is 120 ℃; obtaining dry particles;
6. putting the dried particles obtained in the step 5 into a vacuum sintering furnace, carrying out binder removal at 400 ℃ for 30min, then continuously heating to 1100 ℃ for 60min, and sintering to obtain nearly spherical ZrB2the/SiC composite ceramic particles. The average particle diameter is 13 to 17 μm. Resulting ZrB2The SEM image of the/SiC ceramic particles is shown in FIG. 1.
7. Adding polyethylene glycol accounting for 1% of the mass of the rest zirconium diboride into a proper amount of absolute ethanol to be completely dissolved to obtain a polyethylene glycol-absolute ethanol solution, weighing silicon carbide (with the average particle size of 1 mu m), silicon nitride (with the average particle size of 0.5 mu m), yttrium oxide and the rest zirconium diboride (with the average particle size of 3 mu m) according to a proportion, pouring zirconium diboride into the polyethylene glycol-absolute ethanol solution, and performing ultrasonic dispersion for 30min to obtain a suspension A; pouring silicon carbide, silicon nitride and yttrium oxide into a proper amount of absolute ethyl alcohol for ultrasonic dispersion for 30min to obtain a suspension B; and mixing the suspension A and the suspension B, and ultrasonically stirring for 20min to obtain a suspension C.
8. Pouring the suspension C into a ball milling tank, adding a hard alloy ball milling ball (ball-material ratio is 10:1), and filling high-purity nitrogen as protective gas for ball milling for 48 hours;
9. weighing ZrB obtained in step 6 according to proportion2Adding the/SiC composite ceramic particles into the ball milling tank, and filling high-purity nitrogen for continuing ball milling for 1 h;
10. pouring the ball-milled slurry into a tray, putting the tray into a drying oven, drying the tray for 24 hours in vacuum at the temperature of 100 ℃, and then sieving the cutter material powder with a 200-mesh sieve to obtain the cutter material powder;
11. and (3) putting the cutter material powder obtained in the step (10) into a graphite die for spark plasma sintering, wherein the sintering temperature is 1750 ℃, the applied pressure is 40MPa, and the heat preservation time is 8min, so that the high-temperature ceramic cutter material with the double composite structure is obtained. The SEM image of the cross section of the obtained double-composite structure high-temperature ceramic cutter material is shown in FIG. 2.
Cutting, coarse grinding, polishing and chamfering the prepared double-composite-structure high-temperature ceramic cutter material blank to prepare a ceramic sample strip with the thickness of 3mm multiplied by 4mm multiplied by 25mm, and measuring the mechanical property at room temperature: a hardness of 18.0GPa, a bending strength of 589MPa and a fracture toughness of 5.93 MPa-m1/2The mechanical properties at 1100 ℃ are: hardness of 13.39GPa, bending strength of 398MPa and fracture toughness of 6.10 MPa-m1/2。
The sintered high-temperature ceramic cutter material with the double-composite structure is prepared into a high-temperature ceramic cutter with the double-composite structure with the size of 12.7mm multiplied by 5mm, and the cutting performance of the hardened 40Cr steel is tested. When the cutting speed v is 400m/min, the feed amount f is 0.102mm/r and the back cutting amount apUnder 0.1mm, the cutting distance of the high-temperature ceramic cutter with the double composite structure reaches 4000-.
Example 2
A high-temperature ceramic cutter material with a double composite structure is prepared by sintering the following raw materials in percentage by volume through spark plasma: 10% of silicon carbide, 10% of silicon nitride and ZrB220 percent of/SiC composite ceramic particles (ZrB)2: SiC-3: 1 volume ratio), yttria 1%, and zirconium diboride the remainder. The bulk cutter material SiC was 15 vol%.
1. Will occupy ZrB2Polyethylene glycol with the mass of 1 percent of zirconium diboride in the/SiC composite ceramic particles is addedCompletely dissolving in appropriate amount of absolute ethyl alcohol to obtain polyethylene glycol-absolute ethyl alcohol solution, weighing zirconium diboride with the average particle size of 3 mu m and silicon carbide powder with the average particle size of 1 mu m according to the volume ratio of 3:1, adding into the polyethylene glycol-absolute ethyl alcohol solution, and ultrasonically stirring for 25min to obtain suspension.
2. And pouring the obtained suspension into a ball milling tank, adding a hard alloy ball milling ball (ball-material ratio is 11:1), introducing high-purity nitrogen as protective gas, and carrying out ball milling for 40 hours.
3. Pouring the ball-milled slurry into a tray, putting the tray into a drying oven, and drying the tray for 32 hours in vacuum at 100 ℃, and then sieving the composite powder with a 200-mesh sieve to obtain composite powder;
4. dissolving a polyvinyl alcohol binder accounting for 0.5 percent of the mass of zirconium diboride in deionized water, pouring the obtained composite powder into a polyvinyl alcohol-deionized water solution, and ultrasonically stirring for 25min to obtain a suspension liquid with the solid content of 40 percent;
5. carrying out spray drying on the suspension obtained in the step 4 by using a spray dryer at the feed speed of 12mL/min, the inlet temperature of 400 ℃ and the outlet temperature of 120 ℃ to obtain dried particles;
6. placing the ceramic particles into a vacuum sintering furnace for 30min at 400 ℃ to remove the glue, then continuously heating to 1100 ℃ for 60min to sinter to obtain the nearly spherical ZrB2the/SiC composite ceramic particles. The average particle diameter is 13 to 17 μm.
7. Adding 1% of polyethylene glycol accounting for the balance of the mass of zirconium diboride into a proper amount of absolute ethanol for completely dissolving to obtain a polyethylene glycol-absolute ethanol solution, weighing zirconium diboride (with the average particle size of 3 mu m), silicon carbide (with the average particle size of 1 mu m), silicon nitride (with the average particle size of 0.5 mu m) and yttrium oxide according to the proportion, pouring zirconium diboride into the polyethylene glycol-absolute ethanol solution, and performing ultrasonic dispersion for 25min to obtain a suspension A; pouring silicon carbide, silicon nitride and yttrium oxide into a proper amount of absolute ethyl alcohol for ultrasonic dispersion for 25min to obtain a suspension B; and mixing the suspension A and the suspension B, and ultrasonically stirring for 25min to obtain a suspension C.
8. Pouring the suspension C into a ball milling tank, adding a hard alloy ball milling ball (ball-material ratio is 10:1), and filling high-purity nitrogen as protective gas for ball milling for 48 hours;
9. weighing ZrB obtained in step 6 according to proportion2Adding the/SiC composite ceramic particles into the ball milling tank, and filling high-purity nitrogen for continuing ball milling for 1 h;
10. pouring the ball-milled slurry into a tray, putting the tray into a drying oven, and drying the tray for 32 hours in vacuum at 100 ℃, and then sieving the cutter material powder with a 200-mesh sieve to obtain the cutter material powder;
11. and (3) putting the cutter material powder obtained in the step (10) into a graphite die for spark plasma sintering, wherein the sintering temperature is 1780 ℃, the applied pressure is 35MPa, and the heat preservation time is 6min, so that the high-temperature ceramic cutter material with the double-composite structure is obtained.
Cutting, coarse grinding, polishing and chamfering the prepared double-composite-structure high-temperature ceramic cutter material blank to prepare a ceramic sample strip with the thickness of 3mm multiplied by 4mm multiplied by 25mm, and measuring the mechanical property at room temperature: the hardness is 18.2GPa, the bending strength is 636MPa, and the fracture toughness is 6.19 MPa.m1/2The mechanical properties at 1100 ℃ are: hardness of 13.52GPa, bending strength of 412MPa, and fracture toughness of 6.31 MPa-m1/2。
The sintered high-temperature ceramic cutter material with the double-composite structure is prepared into a high-temperature ceramic cutter with the double-composite structure with the size of 12.7mm multiplied by 5mm, and the cutting performance of the hardened 40Cr steel is tested. When the cutting speed v is 400m/min, the feed amount f is 0.102mm/r and the back cutting amount apUnder 0.1mm, the cutting distance of the high-temperature ceramic cutter with the double composite structure reaches 4200-4700 m.
Example 3
A high-temperature ceramic cutter material with a double composite structure is prepared by sintering the following raw materials in percentage by volume through spark plasma: 8% of silicon carbide, 5% of silicon nitride and ZrB235% (ZrB) of/SiC composite ceramic particles2: SiC — 5: 2 volume percent), yttria 1.5 percent, and the balance being zirconium diboride. The bulk cutter material SiC was 18 vol%.
The preparation method is the same as example 1.
The mechanical properties of the obtained material were measured as in example 1, and the data are as follows: at room temperature, the hardness is 18.4GPa, the bending strength is 622MPa, and the fracture toughness is 6.09 MPa.m1/2. At 1100 deg.C, the hardness is 13.61GPa, the bending strength is 387MPa, and the fracture toughness is 6.2 MPa.m1/2。
Example 4
A high-temperature ceramic cutter material with a double composite structure is prepared by sintering the following raw materials in percentage by volume through spark plasma: 20% of silicon carbide, 8% of silicon nitride and ZrB230 percent of/SiC composite ceramic particles (ZrB)2: SiC-5: 1 volume ratio), yttria 2%, and zirconium diboride the remainder. The bulk cutter material SiC was 25 vol%. The preparation method is the same as example 2.
The mechanical properties of the obtained material were measured as in example 1, and the data are as follows: at room temperature, the hardness was 18.6GPa, the bending strength was 647MPa, and the fracture toughness was 6.23MPa · m1/2. At 1100 deg.C, the hardness is 13.31GPa, the bending strength is 429MPa, and the fracture toughness is 6.35 MPa.m1/2。
Comparative example 1: without addition of ZrB2/SiC composite ceramic particles
ZrB2/SiC/Si3N4The ceramic cutter material is prepared by sintering the following raw materials in percentage by volume through spark plasma: 20% of silicon carbide, 5% of silicon nitride, 1% of yttrium oxide and the balance of zirconium diboride.
The preparation method comprises the following steps:
1. adding 1% of polyethylene glycol based on the mass of zirconium diboride into a proper amount of absolute ethyl alcohol to be completely dissolved to obtain a polyethylene glycol-absolute ethyl alcohol solution, weighing zirconium diboride (with the average particle size of 3 mu m), silicon carbide (with the average particle size of 1 mu m), silicon nitride (with the average particle size of 0.5 mu m) and yttrium oxide in proportion, pouring zirconium diboride into the polyethylene glycol-absolute ethyl alcohol solution, and performing ultrasonic dispersion for 30min to obtain a suspension A; pouring silicon carbide, silicon nitride and yttrium oxide into a proper amount of absolute ethyl alcohol for ultrasonic dispersion for 30min to obtain a suspension B; and mixing the suspension A and the suspension B, and ultrasonically stirring for 20min to obtain a suspension C.
2. Pouring the suspension C into a ball ink tank, adding a hard alloy ball grinding ball (ball material ratio is 10:1), and filling high-purity nitrogen as protective gas for ball milling for 48 hours;
3. pouring the ball-milled slurry into a tray, putting the tray into a drying oven, drying the tray for 24 hours in vacuum at the temperature of 100 ℃, and then sieving the cutter material powder with a 200-mesh sieve to obtain the cutter material powder;
4. putting the cutter material powder obtained in the step 3 into a graphite die for spark plasma sintering, wherein the sintering temperature is 1750 ℃, the applied pressure is 40MPa, and the heat preservation time is 8min to obtain ZrB2/SiC/Si3N4High temperature ceramic cutting tool material.
ZrB to be prepared2/SiC/Si3N4Cutting, coarse grinding, polishing and chamfering the ceramic cutter material blank to prepare a ceramic sample strip of 3mm multiplied by 4mm multiplied by 25mm, and measuring the mechanical property at room temperature: the hardness is 17.9GPa, the bending strength is 623MPa, and the fracture toughness is 5.76 MPa.m1/2(ii) a The mechanical properties at 1100 ℃ were: hardness of 13.44GPa, bending strength of 373MPa, and fracture toughness of 3.52 MPa-m1/2。
The sintered ceramic cutter material is prepared into a high-temperature ceramic cutter with the dimensions of 12.7mm multiplied by 5mm, and the cutting performance test is carried out on the hardened 40Cr steel. When the cutting speed v is 400m/min, the feed amount f is 0.102mm/r and the back cutting amount apUnder 0.1mm, the cutting distance of the cutter is 3500-3900 m.
As can be seen from the above comparative examples, the SiC content of comparative example 1 is the same (20 vol%) as that of example 1, and the amount ratio of other components is also the same, but the high temperature fracture toughness of the cutter material of comparative example 1 is significantly inferior to that of example 1 due to the difference in the preparation method.
Comparative example 2: without addition of Si3N4
As described in example 1, except that Si was subtracted therefrom3N4. To obtain ZrB2A SiC ceramic cutter material.
ZrB to be prepared2Cutting, roughly grinding, polishing and chamfering the SiC ceramic cutter material blank to prepare a ceramic sample strip of 3mm multiplied by 4mm multiplied by 25mm, and measuring the mechanical property at room temperature: the hardness is 18.8GPa, the bending strength is 544MPa, and the fracture toughness is 4.62 MPa.m1/2(ii) a The mechanical properties at 1100 ℃ were: the hardness is 11.8GPa, the bending strength is 276MPa, and the fracture toughness is 3.02 MPa.m1/2。
Sintering the ZrB2The SiC ceramic tool material is prepared into a high-temperature ceramic tool with the size of 12.7mm multiplied by 5mm, and the cutting performance of the hardened 40Cr steel is tested. The cutting distance of the cutter is 3200-.
As can be seen from the above comparative examples, comparative example 2 has the same SiC content and the same preparation method as example 1, but since Si is not added3N4The reduction in bending strength of the cutter material of comparative example 2 is significantly higher than that of example 1, while the fracture toughness is significantly lower than that of example 1.
Experimental example 1: si3N4Influence of content on mechanical properties of cutter material
On the basis of comparative example 1, the discharge plasma sintering temperature is set to 1750 ℃, the heat preservation time is set to 8min, and the applied pressure is set to 40 MPa. By changing Si3N4The content, the room temperature mechanical property of the cutting tool material measured at room temperature, the influence curve of the silicon nitride addition amount on the hardness of the ceramic cutting tool material is shown in fig. 3, the influence curve of the silicon nitride addition amount on the bending strength of the ceramic cutting tool material is shown in fig. 4, and the influence curve of the silicon nitride addition amount on the fracture toughness of the ceramic cutting tool material is shown in fig. 5.
Experimental example 2: comparison of fracture toughness at different temperatures for the ceramic tool material products of example 1 and comparative example 1
The ceramic cutting tool material of double composite structure prepared in example 1 and the ceramic cutting tool material of non-double composite structure prepared in comparative example 1 were cut, roughly ground, polished, and chamfered to prepare ceramic sample bars of 3mm × 4mm × 25mm, and fracture toughness was measured at room temperature to 1100 ℃ respectively, and the obtained comparative curve was as shown in fig. 6.

Claims (13)

1. A high-temperature ceramic cutter material with a double composite structure is prepared by sintering the following raw materials in percentage by volume through spark plasma:
5-30% of silicon carbide powder, 2.5-10% of silicon nitride and ZrB25-40% of/SiC composite ceramic particles, 0.5-5% of yttrium oxide and the balance of zirconium diboride, wherein:
said ZrB2the/SiC composite ceramic particles are prepared by uniformly mixing zirconium diboride and silicon carbide powder according to the volume ratio of (3-5) to (0.5-2) in polyethylene glycol-absolute ethyl alcohol, carrying out ball milling, drying, dispersing in a binder-deionized water mixed solution, carrying out ultrasonic stirring and ball milling, carrying out spray drying on ball milling slurry to prepare particles, and carrying out binder removal and sintering; the ZrB2The average particle diameter of the/SiC composite ceramic particles is 10-20 mu m.
2. The dual composite structure high temperature ceramic cutting tool material of claim 1, wherein the volume percentage composition of the raw materials is:
5-25% of silicon carbide powder, 4-8% of silicon nitride and ZrB210-35% of/SiC composite ceramic particles, 0.5-2% of yttrium oxide and the balance of zirconium diboride; alternatively, the first and second electrodes may be,
10-20% of silicon carbide powder, 5-7.5% of silicon nitride and ZrB215-25% of/SiC composite ceramic particles, 1-1.5% of yttrium oxide and the balance of zirconium diboride.
3. A high temperature ceramic cutting tool material of a double composite structure according to claim 1 or 2, characterized in that the raw material grain size is as follows: the average grain size of the zirconium diboride is 1-10 mu m, the average grain size of the silicon carbide is 0.5-5 mu m, and the average grain size of the silicon nitride is 0.2-2 mu m.
4. A high temperature ceramic cutting tool material of a double composite structure as claimed in claim 1 or 2, wherein the grain size of the raw material is as follows: the average particle size of the zirconium diboride is 2-7 mu m; the average grain diameter of the silicon carbide is 0.7-2 mu m; the average grain diameter of the silicon nitride is 0.4-1 μm.
5. A dual composite structure high temperature ceramic cutting tool material as claimed in claim 1, wherein said ZrB2the/SiC composite ceramic particles are prepared by the following method:
mixing zirconium diboride and silicon carbide powder in a polyethylene glycol-absolute ethyl alcohol according to a proportion, ultrasonically stirring, ball-milling, drying and sieving to obtain composite powder; then, the user can use the device to perform the operation,
secondly, dispersing the obtained composite powder in a binder-deionized water mixed solution, wherein the using amount of the binder is 0.25-1.5% of the mass of the zirconium diboride, ultrasonically stirring, performing ball milling to obtain ball milling slurry, then,
thirdly, the obtained slurry is sprayed and dried to be made into particles, and the particles are subjected to binder removal and sintering in a vacuum sintering furnace.
6. The dual composite structure high temperature ceramic cutting tool material of claim 5, wherein the ZrB2During the preparation process of the/SiC composite ceramic particles, the preparation conditions comprise one or more of the following conditions:
A. the volume ratio of the zirconium diboride to the silicon carbide is (3.5-5) to (0.5-1.5);
B. the content of the polyethylene glycol is 0.5-3% of the mass of the zirconium diboride;
C. in the step I, the ultrasonic stirring time is 30-60 min; the ball milling time is 40-60 h;
D. in the step I, the drying is vacuum drying, the drying temperature is 80-150 ℃, and the drying time is 10-30 hours;
E. in the second step, the ultrasonic stirring time is 30-60 min; the ball milling time is 40-60 h;
F. the binder is polyvinyl alcohol;
g, the using amount of the binder is 0.25-1% of the mass of the zirconium diboride;
H. the feeding speed of the spray drying is 10-15 mL/min, the inlet temperature is 300-500 ℃, and the outlet temperature is 80-150 ℃;
I. the ZrB2The temperature of the rubber discharging of the/SiC composite ceramic particles is 300-500 ℃, and the heat preservation time is 20-40 min;
J. said ZrB2The sintering temperature of the/SiC composite ceramic particles is 1000-1250 ℃.
7. A method for preparing a high-temperature ceramic cutting tool material of a double composite structure as claimed in claim 1 or 2, comprising:
（1）ZrB2preparation of/SiC composite ceramic particles
Mixing zirconium diboride and silicon carbide powder in polyethylene glycol-absolute ethyl alcohol according to a certain proportion, ultrasonically stirring, ball-milling, drying and sieving to obtain composite powder; then dispersing the obtained composite powder in a binder-deionized water mixed solution, wherein the use amount of the binder is 0.25-1.5% of the mass of zirconium diboride, ultrasonically stirring, carrying out ball milling to obtain ball milling slurry, then carrying out spray drying on the obtained slurry to prepare particles, and carrying out binder removal and sintering in a vacuum sintering furnace;
（2）ZrB2the preparation method of the/SiC/silicon nitride composite ceramic powder ball-milling liquid comprises the following steps:
a. adding polyethylene glycol into absolute ethyl alcohol until the polyethylene glycol is completely dissolved to obtain a polyethylene glycol-absolute ethyl alcohol solution, weighing zirconium diboride, silicon carbide, silicon nitride and yttrium oxide according to a proportion, pouring the zirconium diboride into the polyethylene glycol-absolute ethyl alcohol solution, and performing ultrasonic dispersion for 20-60 min to obtain a suspension A; respectively adding silicon carbide, silicon nitride and yttrium oxide into a proper amount of absolute ethyl alcohol, and performing ultrasonic dispersion for 20-60 min, and mixing to obtain a suspension B; mixing the suspension A and the suspension B, and ultrasonically stirring for 10-30 min to obtain a suspension C;
b. pouring the suspension C into a ball milling tank, adding ball milling balls, and filling high-purity nitrogen as a protective gas for ball milling for 40-60 hours;
(3) weighing ZrB prepared in the step (1) in proportion2Adding the/SiC composite ceramic particles into the ball milling tank in the step (2), filling high-purity nitrogen gas, continuing ball milling for 0.5-2 h, placing the ball-milled slurry into a drying box, performing vacuum drying, and then sieving to obtain cutter material powder;
(4) and (3) putting the cutter material powder into a mould for spark plasma sintering to obtain the high-temperature ceramic cutter material with the double-composite structure.
8. The method for preparing a high temperature ceramic cutting tool material of a double composite structure as claimed in claim 7, wherein in the step (1) and the step (2), the preparation conditions include one or more of the following:
a. the molecular weight of the polyethylene glycol is 2000-10000;
b. the mass of the polyethylene glycol is 0.5-2% of that of the zirconium diboride;
c. the ball milling balls for ball milling are made of hard alloy;
d. the mass ratio of ball materials for ball milling is 10-20: 1;
e. and sieving by using a 100-300-mesh sieve.
9. The method for preparing a high-temperature ceramic cutting tool material with a double-composite structure according to claim 7, wherein in the step (3), the vacuum drying temperature is 80-150 ℃ and the drying time is 10-30 h.
10. The method for preparing a high-temperature ceramic cutting tool material with a double-composite structure according to claim 7, wherein a 100-300-mesh screen is selected for sieving in the step (3).
11. The method for preparing a high-temperature ceramic cutting tool material of a double composite structure according to claim 7, wherein in the step (4), the preparation conditions include one or more of the following:
i. the temperature of the spark plasma sintering is 1700-1800 ℃;
ii, performing discharge plasma sintering, wherein the applied pressure is 30-50 MPa, and the heat preservation time is 5-15 min;
the mold is a graphite mold.
12. The method for preparing a high-temperature ceramic cutting tool material with a double-composite structure according to claim 7, wherein in the step (4), the sintering temperature of spark plasma sintering is 1740-1780 ℃; applying pressure of 35-40 MPa, and keeping the temperature for 6-8 min.
13. Use of the dual-composite-structure high-temperature ceramic cutting tool material of any one of claims 1-6 as a high-speed cutting tool at the high temperature conditions of 600-1100 ℃.
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