CN111574209A - Self-lubricating ceramic cutter with self-repairing capability and preparation method, repairing method and application thereof - Google Patents

Self-lubricating ceramic cutter with self-repairing capability and preparation method, repairing method and application thereof Download PDF

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CN111574209A
CN111574209A CN202010429650.3A CN202010429650A CN111574209A CN 111574209 A CN111574209 A CN 111574209A CN 202010429650 A CN202010429650 A CN 202010429650A CN 111574209 A CN111574209 A CN 111574209A
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self
repairing
lubricating ceramic
tib
powder
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陈照强
季良刚
许崇海
肖光春
衣明东
张静婕
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Qilu University of Technology
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Qilu University of Technology
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Abstract

The invention relates to the technical field of self-repairing cutters, in particular to a self-lubricating ceramic cutter with self-repairing capability, and a preparation method, a repairing method and application thereof, wherein the ceramic cutter comprises the following components of α -Al in percentage by volume2O355‑64％，TiC 22‑28％，TiB25‑10％，h‑BN@Al2O35-10% of MgO, 0.5% of MgO; the h-BN @ Al2O3Is Al2O3The core-shell structure is formed by coating the flaky nano h-BN. In the ceramic cutting tool, TiB2For repairing agents, h-BN @ Al2O3Is a solid lubricant and a repairing agent, Al2O3As matrix, TiC as reinforcing phase, MgO as sintering aid, in TiB2And h-BN @ Al2O3The crack repairing effect and the self-lubricating capability of the cutter material are improved under the synergistic effect of the components, and the comprehensive mechanical property of the cutter material is enhanced.

Description

Self-lubricating ceramic cutter with self-repairing capability and preparation method, repairing method and application thereof
Technical Field
The invention relates to the technical field of self-repairing cutters, in particular to a self-lubricating ceramic cutter with self-repairing capability, and a preparation method, a repairing method and application thereof.
Background
The information disclosed in this background of the invention is only for enhancement of understanding of the general background of the invention and is not necessarily to be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Ceramic tool materials have received increasing attention and use over the last decades due to their excellent properties, such as high temperature resistance, corrosion resistance, wear resistance and high strength. However, the ceramic cutting tool material also has obvious disadvantages, such as easy generation of microcracks due to mechanical impact and thermal shock acting force in the high-speed dry cutting process, high friction coefficient, sensitivity to defects and the like. This will result in the cutter reaching the failure criteria in advance and the entire blade facing scrapping, resulting in significant resource and economic waste. Therefore, if the balance between the excellent cutting performance and the service life of the ceramic cutting tool can be achieved, the ceramic cutting tool has excellent cutting performance and the service life is prolonged, and the problem to be solved in the research and development of the ceramic cutting tool is urgent.
In view of the above problems, in recent years, researchers have developed self-repairing ceramics and self-lubricating ceramics. The cutter material has the functions of crack repair and self lubrication by adding components with specific functions into the ceramic matrix. Thereby meeting the requirements of dry cutting processing.
The self-repairing ceramic material is prepared by adding a specific repairing agent into a ceramic matrix, and when a crack is generated in the material, the crack is healed through proper treatment, so that the strength of the material is recovered, and the service life of the material is prolonged. For example: there is research disclosing a crack self-healingA method for preparing a ceramic material. The self-repairing ceramic prepared in the research is thermally treated in a high-temperature aerobic environment, and the oxidation product SiO of SiC is utilized2And repairing and healing the crack. However, when SiC is oxidized, a gaseous oxide of C is generated, which is not favorable for enhancing the strength of the material.
The self-lubricating ceramic is prepared by adding a solid lubricant to a ceramic matrix, so that the material has self-lubricating capability. But because the mechanical property of the solid lubricant is poor, the mechanical property of the material is seriously influenced by directly adding the solid lubricant into a ceramic matrix. In recent years, part of researchers have designed and developed novel self-lubricating ceramic cutting tool materials with addition of coated solid lubricants. The specific method is that a layer of material with higher strength is coated on the surface of the solid lubricant in a modified way, and then the material is added into a ceramic matrix to prepare the self-lubricating ceramic material. Research discloses a self-lubricating ceramic cutting tool material added with nickel-phosphorus alloy coated calcium fluoride composite powder and a preparation method thereof. However, the inventor researches and discovers that: the nickel-phosphorus alloy coating layer and the substrate material have physical or chemical difference, so that residual stress is easily generated in the subsequent sintering process, and the strength of the material is reduced.
Disclosure of Invention
Aiming at the problems, the invention provides a self-lubricating ceramic cutter with self-repairing capability and a preparation method, a repairing method and application thereof, wherein a repairing agent titanium boride (TiB) is added2) And a coated solid lubricant (h-BN @ Al)2O3) The prepared self-lubricating ceramic cutter material with the self-repairing capability has good crack repairing capability and lubricating effect. In order to achieve the above object, the technical solution of the present invention is as follows.
In a first aspect of the invention, a self-lubricating ceramic cutter with self-repairing capability is disclosed, and comprises the following components in percentage by volume α -Al2O355-64％，TiC 22-28％，TiB25-10％，h-BN@Al2O35-10% of MgO, 0.5% of MgO; wherein, the h-BN @ Al2O3Is Al2O3The core-shell structure is formed by coating the flaky nano h-BN.
Further, the ceramic cutter comprises the following components in percentage by volume of α -Al2O356.65-62.65，TiC 23.85-26.85％，TiB25-10％，h-BN@Al2O35-10% of MgO and 0.5% of MgO. In the invention, when the cutter material in the range is selected, the comprehensive mechanical property is better.
Further, the α -Al2O3Has an average particle diameter of 0.2 to 1 μm; the average grain diameter of TiC is 0.5-1 μm; TiB2Has an average particle diameter of 0.5 to 1 μm; the average grain diameter of MgO is 0.5-2 μm; h-BN @ Al2O3Has an average particle diameter of 0.1 to 0.5. mu.m.
In the ceramic cutting tool according to the first aspect of the present invention, TiB is used2For repairing agents, h-BN @ Al2O3Is a solid lubricant and a repairing agent, Al2O3As a matrix, TiC as a reinforcing phase and MgO as a sintering aid, wherein h-BN @ Al of a core-shell structure2O3Coating a layer of Al on the surface of h-BN by a non-uniform nucleation method2O3The shell is used for improving the mechanical property of the lubricant. The cutter material has good sintering compactness, and the comprehensive mechanical property of the cutter material is enhanced. At the same time, in TiB2And h-BN @ Al2O3The crack repairing effect and the self-lubricating capability of the cutter material are improved under the synergistic effect of the components, and the comprehensive mechanical property of the cutter material is enhanced.
In a second aspect of the present invention, a method for preparing the self-lubricating ceramic tool with self-repairing capability is disclosed, which comprises the following steps:
(1) α -Al2O3、TiC、TiB2Respectively mixed with volatile dispersion medium, then ultrasonically dispersed and stirred to obtain α -Al2O3Suspensions, TiC suspensions and TiB2And (4) mixing the three suspensions to obtain a complex phase suspension for later use.
(2) Dissolving a dispersing agent in a volatile solvent, then adding the complex phase suspension liquid in the step (1), adding MgO, performing ultrasonic dispersion and stirring to obtain a precursor suspension liquid for later use.
(3) Ball-milling the precursor suspension in the step (2) in a protective atmosphere, and then adding h-BN @ Al2O3Continuously ball-milling the suspension to obtain ball-milling liquid; and then drying the ball milling liquid to obtain mixed powder.
(4) And (4) carrying out hot-pressing sintering on the mixed powder obtained in the step (3) under a vacuum condition after cold-pressing forming.
Further, the stirring time in the steps (1) and (2) is 10-20min and 20-40min respectively.
Further, in the step (2), the dispersant is any one of polyethylene glycol 6000 and polyvinylpyrrolidone (PVP), and the adding proportion is α -Al2O31-5% of the mass. The dispersing agent mainly has the function of preventing the powder raw materials from agglomerating and uniformly dispersing the raw materials in a liquid phase medium. The reason why the dispersant is added to the MgO is that the dispersant can effectively disperse Al2O3、TiC、TiB2The powder has little MgO addition amount, does not need good dispersion action, and mainly plays a role of a sintering aid in the sintering process. When the content of the dispersing agent is too high, the powder generates a bridging effect, so that the acting force among the powder is strengthened, and agglomeration is generated. When the content is too small, the dispersing effect is poor.
Further, in the step (3), ball milling balls are added according to the ball-material weight ratio of 9-15:1 for ball milling for 35-45h, and the ball milling time is continued for 3-7 h; the protective atmosphere includes any one of nitrogen, argon, and the like. Optionally, the material of the ball grinding ball is cemented carbide YG6 or YG 8.
Further, in the step (3), the h-BN @ Al2O3The preparation method of the suspension comprises the following steps: h-BN @ Al2O3Dissolving the powder in a volatile dispersion medium, and then performing ultrasonic dispersion and stirring to obtain the nano-composite material. Optionally, the stirring time is 5-15 min.
Further, the volatile dispersion medium and the volatile solvent are both absolute ethyl alcohol.
Further, in the step (3), the drying temperature is 80-120 ℃ and the time is 12-24 hours.
Further, in the step (4), the hot pressing sintering parameters are as follows: the heating rate is 10-20min/min, the sintering temperature is 1550-.
In a third aspect of the invention, the h-BN @ Al is disclosed2O3The preparation method of (1) refers to the Chinese patent application with the application number of 2020103917018.
In a fourth aspect of the present invention, a method for repairing the self-lubricating ceramic tool with self-repairing capability is disclosed, wherein the self-lubricating ceramic tool with self-repairing capability with cracks is heated to a set temperature in an aerobic environment and then is subjected to heat preservation. Optionally, the set temperature is 700-.
In a fifth aspect of the invention, the application of the self-lubricating ceramic cutter with self-repairing capability in mechanical cutting machining and the like is disclosed.
Compared with the prior art, the invention has the following beneficial effects:
(1) the self-lubricating ceramic cutting tool of the invention is TiB2For repairing phase, high-temperature oxidation is carried out to generate liquid phase B2O3And TiO2The surface cracks of the healing material are repaired, and other gas oxides cannot be generated to reduce the strength of the material. And TiB2Compared with SiC, the oxidation reaction can be carried out at a lower temperature, and the strength of the cutter material is effectively recovered.
(2) The self-lubricating ceramic cutter is prepared from h-BN @ Al2O3The coated solid lubricant is a lubricating phase, and compared with the method of directly adding h-BN, the mechanical property of the cutter material is obviously improved. And with Al2O3Is a coating layer, can well react with Al in the sintering process2O3The substrate is fused into a whole, so that the sintering compactness of the material is improved, and the strength of the cutter material is improved.
(3) TiB in the self-lubricating ceramic cutter2And h-BN can be oxidized to generate oxide B when exposed to high-temperature aerobic environment2O3The oxidizing substances can effectively repair the crack defects of the cutter material and can also provide excellent lubricating effect for the cutter material, namely TiB2And h-BNHas the function of synergistically healing cracks.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 shows TiB in an embodiment of the present invention2And h-BN to form a liquid phase B2O3And TiO2Schematic representation of (a).
Fig. 2 is a schematic view of surface crack healing of the self-lubricating ceramic cutter in the embodiment of the invention.
Fig. 3 is a crack morphology image (SEM) of the ceramic cutting tool prepared according to the first embodiment of the present invention after heat treatment, wherein the right image is an enlarged view of the white frame area of the left image.
Fig. 4 is a surface XRD pattern before and after heat treatment of the ceramic cutting tool prepared in the first embodiment of the present invention.
Fig. 5 is a crack morphology (SEM) after heat treatment of a ceramic cutting tool made according to a second embodiment of the present invention.
FIG. 6 is a crack morphology (SEM) after heat treatment of a ceramic cutting tool made according to a comparative example of the present invention.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular is intended to include the plural unless the context clearly dictates otherwise. Furthermore, it will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
As described above, in some conventional self-lubricating ceramic cutting tools in which a nickel-phosphorus alloy is added to coat a calcium fluoride composite powder, because the nickel-phosphorus alloy coating layer and a base material have a physical or chemical difference, residual stress is easily generated in a subsequent sintering process, and the material strength is reduced. Therefore, the invention provides a self-lubricating ceramic cutter with self-repairing capability and a preparation method and a repairing method thereof; the invention will now be further described with reference to the drawings and specific examples.
In the following examples, said α -Al2O3The average particle diameter of the powder is 0.2-1 μm. The average grain diameter of the TiC powder is 0.5-1 μm. TiB2The average particle diameter of the powder is 0.5-1 μm. The average grain diameter of the MgO powder is 0.5-2 μm. h-BN @ Al2O3The average particle diameter of the powder is 0.1-0.5 μm.
In the following examples, the h-BN @ Al2O3The preparation method of the powder comprises the following steps:
(1) 0.2g of h-BN powder with the particle size of 100nm is weighed and put into HF solution for acid washing for 20min, and is cleaned by absolute ethyl alcohol after being centrifuged for 5min at 4000 r/min. And dispersing the powder after the acid washing in 100mL of absolute ethyl alcohol, adding a proper amount of dispersant PVP, performing ultrasonic dispersion for 30min, adding 50mL of distilled water, and continuing performing ultrasonic stirring for 10 min.
(2) To the above solution was added 30g/L of aluminum nitrate nonahydrate solution (Al (NO)3)3·9H2O), and ultrasonically stirring for 10 min. The obtained mixed solution is placed in a magnetic stirrer to be heated and stirred in a water bath, and the temperature is kept between 75 ℃. Simultaneously adding sodium acetate buffer solution to control the pH value to be 4.5.
(3) And slowly dropwise adding dilute ammonia water into the mixed solution to adjust the pH value to 7.5, wherein the dropwise adding speed is 0.15 mL/min. After the dropwise addition, the temperature is kept for 30min, and then the mixture is kept stand at room temperature for 12 h.
(4) Centrifuging the obtained suspension at 5000r/min for 6min, and washing with anhydrous ethanol for 4 times. After the cleaning, the mixture is placed at 85 ℃ for vacuum drying for 24 hours to obtain Al (OH) with nano h-BN as a core3h-BN @ Al (OH) as shell3And (3) composite powder. Calcining the powder for 1h at 1200 ℃ in a nitrogen atmosphere to obtain h-BN @ Al2O3And (3) composite powder.
First embodiment
The self-lubricating ceramic cutter with self-repairing capability is prepared from α -Al in volume percentage2O359.15% of powder, 25.35% of TiC powder and TiB210% of powder, h-BN @ Al2O35% of powder and 0.5% of MgO powder; the method comprises the following steps:
(1) weighing α -Al in proportion2O3TiC and TiB2Adding 100ml of anhydrous ethanol as dispersion medium into the powder respectively, ultrasonically dispersing and mechanically stirring for 15min to obtain α -Al2O3Suspensions, TiC suspensions and TiB2A suspension; mixing the three suspensions to obtain a complex phase suspension.
(2) Weighing Al2O3Polyethylene glycol 6000 which is 3 wt% of the powder is used as a dispersing agent, the dispersing agent is dissolved by absolute ethyl alcohol and then added into the complex phase suspension liquid in the step (1), and then MgO powder is added in proportion, ultrasonically dispersed and mechanically stirred for 30 min; the obtained suspension is poured into a ball milling tank, ball milling balls (cemented carbide YG6) are added according to the weight ratio of 10:1 of the ball materials, and ball milling is carried out for 40h under the nitrogen atmosphere, so as to obtain precursor suspension.
(3) Weighing h-BN @ Al in proportion2O3Preparing powder into suspension by using absolute ethyl alcohol as a dispersion medium, and simultaneously carrying out ultrasonic dispersion and stirring for 10 min; adding the obtained suspension into the precursor suspension in the step (2), and continuing ball milling for 5 hours in a nitrogen atmosphere to obtain ball milling liquid; and drying the ball milling liquid for 18 hours at the temperature of 100 ℃ in a vacuum drying oven, and then sieving the ball milling liquid through a 100-mesh sieve to obtain target powder.
(4) Putting the target powder in the step (3) into a graphite mold, and putting the graphite mold into a vacuum hot-pressing sintering furnace for hot-pressing sintering after cold press molding; hot pressing sintering parameters: the heating rate is 15min/min, the sintering temperature is 1650 ℃, the heat preservation time is 15min, and the hot pressing pressure is 32 MPa.
The self-lubricating ceramic cutter prepared in the embodiment is cut into standard strip-shaped test pieces of 3mm × 4mm × 35mm, and then the test pieces are subjected to coarse grinding, chamfering and polishing treatment, and the mechanical property test shows that the bending strength of the material is 610.36MPa, the hardness is 17.89GPa, and the fracture of the material is 17.89GPaThe toughness is 5.88 MPa.M1/2。
The self-lubricating ceramic cutting tool prepared in the embodiment is preformed with cracks with the length of about 400-500 μm and the depth of about 36 μm by using a Vickers hardness tester. Repairing the crack sample in a high-temperature air furnace (the temperature is 700 ℃, and the temperature is kept for 60 min); the crack sample after repairing is subjected to room temperature bending strength test, the strength of the sample is increased from 165.73MPa when cracks occur to 599.36MPa, and the strength of the sample is recovered to 98.20% of that of a smooth sample. The crack was found to substantially heal by observing the morphology of the crack site of the material (shown in FIG. 3). It was found by XRD analysis (shown in FIG. 4) that this is due to TiB2And B formed by oxidation of h-BN2O3And TiO2The cracks are repaired, the generation of oxidation substances is beneficial to the lubricating effect of the cutter, the repairing principle refers to figures 1 and 2, TiB2And Al damaged by cracks2O3The h-BN of the outer shell can be oxidized to generate oxide B when exposed to high-temperature aerobic environment2O3The oxidizing substances can effectively repair the crack defects of the cutter material.
Second embodiment
The self-lubricating ceramic cutter with self-repairing capability is prepared from α -Al in volume percentage2O356.65% of powder, 23.85% of TiC powder and TiB210% of powder, h-BN @ Al2O310% of powder and 0.5% of MgO powder; the method comprises the following steps:
(1) weighing α -Al in proportion2O3TiC and TiB2Adding 100ml of anhydrous ethanol as dispersion medium into the powder respectively, ultrasonically dispersing and mechanically stirring for 20min to obtain α -Al2O3Suspensions, TiC suspensions and TiB2A suspension; mixing the three suspensions to obtain a complex phase suspension.
(2) Weighing Al2O3Polyethylene glycol 6000 which is 5 wt% of the powder in weight is used as a dispersing agent, the dispersing agent is dissolved by absolute ethyl alcohol and then added into the complex phase suspension liquid in the step (1), and then MgO powder is added in proportion, ultrasonically dispersed and mechanically stirred for 20 min; pouring the obtained suspension into a ball milling tank, and adding ball milling balls (hard) according to the ball material weight ratio of 15:1And YG8) under nitrogen atmosphere to obtain precursor suspension.
(3) Weighing h-BN @ Al in proportion2O3Preparing powder into suspension by using absolute ethyl alcohol as a dispersion medium, and simultaneously carrying out ultrasonic dispersion and stirring for 15 min; and (3) adding the obtained suspension into the precursor suspension in the step (2), and continuing ball milling for 5 hours in a nitrogen atmosphere to obtain ball milling liquid. And drying the ball milling liquid in a vacuum drying oven at 120 ℃ for 24 hours, and then sieving the ball milling liquid through a 100-mesh sieve to obtain target powder.
(4) Putting the target powder obtained in the step (3) into a graphite mold, and putting the graphite mold into a vacuum hot-pressing sintering furnace for hot-pressing sintering after cold press molding; hot pressing sintering parameters: the heating rate is 20min/min, the sintering temperature is 1700 ℃, the heat preservation time is 10min, and the hot pressing pressure is 30 MPa.
The self-lubricating ceramic cutter prepared in the embodiment is cut into standard strip-shaped test samples of 3mm × 4mm × 35mm, and then the test samples are subjected to coarse grinding, chamfering and polishing, and the mechanical property test shows that the bending strength of the material is 564.94MPa, the hardness is 16.89GPa, and the fracture toughness is 5.58 MPa.M1/2。
The self-lubricating ceramic cutting tool prepared in the embodiment is preformed with cracks with the length of about 500-600 μm and the depth of about 61 μm by using a Vickers hardness tester. Repairing the crack sample in a high-temperature air furnace (the temperature is 800 ℃, and the temperature is kept for 30 min); the heat-treated crack sample is subjected to room temperature bending strength test, the strength of the sample is increased from 134.46MPa when cracks occur to 513.84MPa, and the strength of the sample is recovered to 90.95 percent of that of a smooth sample. By observing the crack morphology of the material (shown in figure 5), most cracks are healed, the cracks can not be completely repaired only at the initial end of the cracks, the cracks are wide and deep, and the generated oxides can not completely fill the cracks.
Third embodiment
The self-lubricating ceramic cutter with self-repairing capability is prepared from α -Al in volume percentage2O362.65% of powder, 26.85% of TiC powder and TiB25% of powder, h-BN @ Al2O35% of powder and 0.5% of MgO powder; the method comprises the following steps:
(1) weighing α -Al in proportion2O3TiC and TiB2Adding 100ml of anhydrous ethanol as dispersion medium into the powder respectively, ultrasonically dispersing and mechanically stirring for 20min to obtain α -Al2O3Suspensions, TiC suspensions and TiB2A suspension; mixing the three suspensions to obtain a complex phase suspension.
(2) Weighing Al2O3Polyethylene glycol 6000 which is 3 wt% of the powder is used as a dispersing agent, the dispersing agent is dissolved by absolute ethyl alcohol and then added into the complex phase suspension liquid in the step (1), and then MgO powder is added in proportion, ultrasonically dispersed and mechanically stirred for 20 min; and pouring the obtained suspension into a ball milling tank, adding ball milling balls (hard alloy YG8) according to the weight ratio of the ball materials of 15:1, and carrying out ball milling for 40h in a nitrogen atmosphere to obtain precursor suspension.
(3) Weighing h-BN @ Al in proportion2O3Preparing powder into suspension by using absolute ethyl alcohol as a dispersion medium, and simultaneously carrying out ultrasonic dispersion and stirring for 15 min; and (3) adding the obtained suspension into the precursor suspension in the step (2), and continuing ball milling for 5 hours in a nitrogen atmosphere to obtain ball milling liquid. And drying the ball milling liquid in a vacuum drying oven at 120 ℃ for 24 hours, and then sieving the ball milling liquid through a 100-mesh sieve to obtain target powder.
(4) Putting the target powder obtained in the step (3) into a graphite mold, and putting the graphite mold into a vacuum hot-pressing sintering furnace for hot-pressing sintering after cold press molding; hot pressing sintering parameters: the heating rate is 20min/min, the sintering temperature is 1700 ℃, the heat preservation time is 10min, and the hot pressing pressure is 30 MPa.
The self-lubricating ceramic cutter prepared in the embodiment is cut into standard strip-shaped test samples of 3mm × 4mm × 35mm, and then the test samples are subjected to coarse grinding, chamfering and polishing, and the mechanical property test shows that the bending strength of the material is 572.63MPa, the hardness is 17.26GPa, and the fracture toughness is 5.52 MPa.M1/2。
The self-lubricating ceramic cutting tool prepared in the embodiment is prefabricated with cracks with the length of 400-500 mu m and the depth of 36 mu m on the surface by using a Vickers hardness tester. Repairing the crack sample in a high-temperature air furnace (the temperature is 700 ℃, and the temperature is kept for 60 min); the heat-treated crack sample is subjected to room temperature bending strength test, the strength of the sample is increased from 151.82MPa when cracks occur to 483.94MPa, and the strength of the sample is recovered to 84.51% of that of a smooth sample.
Fourth embodiment
The self-lubricating ceramic cutter with self-repairing capability is prepared from α -Al in volume percentage2O355% of powder, 28% of TiC powder and TiB210% of powder, h-BN @ Al2O36.5 percent of powder and 0.5 percent of MgO powder; the method comprises the following steps:
(1) weighing α -Al in proportion2O3TiC and TiB2Adding 100ml of anhydrous ethanol as dispersion medium into the powder respectively, ultrasonically dispersing and mechanically stirring for 20min to obtain α -Al2O3Suspensions, TiC suspensions and TiB2A suspension; mixing the three suspensions to obtain a complex phase suspension.
(2) Weighing Al2O3Polyethylene glycol 6000 which is 3 wt% of the powder is used as a dispersing agent, the dispersing agent is dissolved by absolute ethyl alcohol and then added into the complex phase suspension liquid in the step (1), and then MgO powder is added in proportion, ultrasonically dispersed and mechanically stirred for 20 min; and pouring the obtained suspension into a ball milling tank, adding ball milling balls (hard alloy YG8) according to the weight ratio of the ball materials of 15:1, and carrying out ball milling for 45 hours in a nitrogen atmosphere to obtain precursor suspension.
(3) Weighing h-BN @ Al in proportion2O3Preparing powder into suspension by using absolute ethyl alcohol as a dispersion medium, and simultaneously carrying out ultrasonic dispersion and stirring for 15 min; and (3) adding the obtained suspension into the precursor suspension in the step (2), and continuing ball milling for 5 hours in a nitrogen atmosphere to obtain ball milling liquid. And drying the ball milling liquid in a vacuum drying oven at 120 ℃ for 24 hours, and then sieving the ball milling liquid through a 100-mesh sieve to obtain target powder.
(4) Putting the target powder obtained in the step (3) into a graphite mold, and putting the graphite mold into a vacuum hot-pressing sintering furnace for hot-pressing sintering after cold press molding; hot pressing sintering parameters: the heating rate is 20min/min, the sintering temperature is 1650 ℃, the heat preservation time is 15min, and the hot pressing pressure is 32 MPa.
The self-lubricating ceramic cutter prepared in this example was cut into standard strip specimens of 3mm × 4mm × 35mm, and thenAnd (5) carrying out coarse grinding, chamfering and polishing treatment on the sample strip. The mechanical property test shows that the bending strength of the material is 590.31MPa, the hardness is 17.46GPa, and the fracture toughness is 5.61 MPa.M1/2。
The self-lubricating ceramic cutting tool prepared in the embodiment is prefabricated with cracks with the length of 400-500 mu m and the depth of 36 mu m on the surface by using a Vickers hardness tester. Repairing the crack sample in a high-temperature air furnace (the temperature is 700 ℃, and the temperature is kept for 30 min); the heat treated crack specimens were tested for room temperature flexural strength and the crack specimens recovered to 78.55% of the smooth specimens.
Fifth embodiment
The self-lubricating ceramic cutter with self-repairing capability is prepared from α -Al in volume percentage2O364% of powder, 22% of TiC powder and TiB25.5% of powder, h-BN @ Al2O38% of powder and 0.5% of MgO powder; the method comprises the following steps:
(1) weighing α -Al in proportion2O3TiC and TiB2Adding 100ml of anhydrous ethanol as dispersion medium into the powder respectively, ultrasonically dispersing and mechanically stirring for 20min to obtain α -Al2O3Suspensions, TiC suspensions and TiB2A suspension; mixing the three suspensions to obtain a complex phase suspension.
(2) Weighing Al2O3Polyethylene glycol 6000 which is 3 wt% of the powder is used as a dispersing agent, the dispersing agent is dissolved by absolute ethyl alcohol and then added into the complex phase suspension liquid in the step (1), and then MgO powder is added in proportion, ultrasonically dispersed and mechanically stirred for 20 min; and pouring the obtained suspension into a ball milling tank, adding ball milling balls (hard alloy YG8) according to the weight ratio of the ball materials of 15:1, and carrying out ball milling for 45 hours in a nitrogen atmosphere to obtain precursor suspension.
(3) Weighing h-BN @ Al in proportion2O3Preparing powder into suspension by using absolute ethyl alcohol as a dispersion medium, and simultaneously carrying out ultrasonic dispersion and stirring for 15 min; and (3) adding the obtained suspension into the precursor suspension in the step (2), and continuing ball milling for 5 hours in a nitrogen atmosphere to obtain ball milling liquid. Drying the ball milling liquid in a vacuum drying oven at 120 ℃ for 24 hours, and sieving the ball milling liquid through a 100-mesh sieveAnd obtaining the target powder.
(4) Putting the target powder obtained in the step (3) into a graphite mold, and putting the graphite mold into a vacuum hot-pressing sintering furnace for hot-pressing sintering after cold press molding; hot pressing sintering parameters: the heating rate is 20min/min, the sintering temperature is 1650 ℃, the heat preservation time is 10min, and the hot pressing pressure is 30 MPa.
The self-lubricating ceramic cutter prepared in the embodiment is cut into standard strip-shaped test samples of 3mm × 4mm × 35mm, and then the test samples are subjected to rough grinding, chamfering and polishing treatment, and the mechanical property test shows that the bending strength of the material is 572.31MPa, the hardness is 17.26GPa, and the fracture toughness is 5.62 MPa.M1/2。
The self-lubricating ceramic cutting tool prepared in the embodiment is prefabricated with cracks with the length of 400-500 mu m and the depth of 36 mu m on the surface by using a Vickers hardness tester. Repairing the crack sample in a high-temperature air furnace (the temperature is 800 ℃, and the temperature is kept for 60 min); and (4) testing the room-temperature bending strength of the crack sample after heat treatment, wherein the strength of the crack sample is recovered to 72.39% of that of the smooth sample.
First comparative example
The self-lubricating ceramic cutter with self-repairing capability is prepared from α -Al in volume percentage2O369.65% of powder, 29.85% of TiC powder and TiB 20% of powder, h-BN @ Al2O30% of powder and 0.5% of MgO powder; the method comprises the following steps:
(1) weighing α -Al in proportion2O3Adding 100ml of absolute ethyl alcohol into TiC powder respectively as a dispersion medium, performing ultrasonic dispersion and mechanically stirring for 10min to obtain α -Al2O3Suspensions and TiC suspensions; mixing the two suspensions to obtain a complex phase suspension.
(2) Weighing Al2O33 wt% of polyethylene glycol 6000 in weight is used as a dispersing agent, the dispersing agent is dissolved by absolute ethyl alcohol, added into the multiphase suspension liquid in the step (1), added with MgO powder in proportion, ultrasonically dispersed and mechanically stirred for 20 min; pouring the obtained suspension into a ball milling tank, adding ball milling balls (hard alloy YG6) according to the ball material weight ratio of 10:1, and carrying out ball milling for 40h in a nitrogen atmosphere; to obtainAnd (3) precursor suspension.
(3) And (3) drying the precursor suspension obtained in the step (2) for 24 hours at the temperature of 100 ℃ in a vacuum drying oven, and then sieving the dried precursor suspension through a 100-mesh sieve to obtain the target powder.
(4) Putting the mixed powder obtained in the step (3) into a graphite mold, and putting the graphite mold into a vacuum hot-pressing sintering furnace for hot-pressing sintering after cold press molding; hot pressing sintering parameters: the heating rate is 15min/min, the sintering temperature is 1650 ℃, the heat preservation time is 15min, and the hot pressing pressure is 32 MPa.
The self-lubricating ceramic cutter prepared in the embodiment is cut into standard strip-shaped test pieces with the thickness of 3mm × 4mm × 35mm, and then the test pieces are subjected to rough grinding, chamfering and polishing treatment, and the mechanical property test shows that the bending strength of the material is 624MPa, the hardness is 17.9GPa, and the fracture toughness is 5.2 MPa.M1/2。
The length of the crack prefabricated on the surface of the self-lubricating ceramic cutting tool prepared in the embodiment is 400-500 mu m by using a Vickers hardness tester, and the depth of the crack is 36 mu m. Repairing the crack sample in a high-temperature air furnace (the temperature is 700 ℃, and the temperature is kept for 60 min); the heat-treated crack sample is subjected to room temperature bending strength test, the strength of the sample is increased from 207.67MPa when cracks occur to 304.51MPa, and the strength of the sample is recovered to 48.7% of that of a smooth sample. After observing the appearance of the cracks of the material, the cracks are not substantially healed (shown in figure 6), and still can be clearly seen, because the cracks are not repaired by oxide generated by oxidation reaction. While the material strength is partly restored due to the release of residual stresses inside the tool at high temperatures restoring part of its strength.
Finally, it should be understood that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. Although the embodiments of the present invention have been described with reference to the accompanying drawings, it is not intended to limit the scope of the present invention, and it should be understood by those skilled in the art that various modifications and variations can be made without inventive efforts by those skilled in the art based on the technical solution of the present invention.

Claims (10)

1. The self-lubricating ceramic cutter with self-repairing capability is characterized by comprising the following components in percentage by volume of α -Al2O355-64％，TiC 22-28％，TiB25-10％，h-BN@Al2O35-10% of MgO, 0.5% of MgO; the h-BN @ Al2O3Is Al2O3The core-shell structure is formed by coating the flaky nano h-BN.
2. The self-lubricating ceramic cutter with self-repairing capability is characterized by comprising the following components in percentage by volume of α -Al2O356.65-62.65，TiC 23.85-26.85％，TiB25-10％，h-BN@Al2O35-10％，MgO 0.5％。
3. The self-lubricating ceramic tool with self-repairing capability of claim 1 or 2, wherein the α -Al is2O3Has an average particle diameter of 0.2 to 1 μm; the average grain diameter of TiC is 0.5-1 μm; TiB2Has an average particle diameter of 0.5 to 1 μm; the average grain diameter of MgO is 0.5-2 μm; h-BN @ Al2O3Has an average particle diameter of 0.1 to 0.5. mu.m.
4. The method for preparing the self-lubricating ceramic tool with self-repairing capability of any one of claims 1 to 3, characterized by comprising the following steps:
(1) α -Al2O3、TiC、TiB2Respectively mixed with volatile dispersion medium, then ultrasonically dispersed and stirred to obtain α -Al2O3Suspensions, TiC suspensions and TiB2Suspension, mixing the three suspensions to obtain complex phase suspension for later use;
(2) dissolving a dispersing agent in a volatile solvent, then adding the complex phase suspension liquid in the step (1), adding MgO, performing ultrasonic dispersion and stirring to obtain a precursor suspension liquid for later use;
(3) suspending the precursor in the step (2)Ball-milling the suspension in a protective atmosphere, and then adding h-BN @ Al2O3Continuously ball-milling the suspension to obtain ball-milling liquid; then drying the ball milling liquid to obtain mixed powder;
(4) and (4) carrying out hot-pressing sintering on the mixed powder obtained in the step (3) under a vacuum condition after cold-pressing forming.
5. The method for preparing the self-lubricating ceramic cutter with the self-repairing capability according to claim 4, wherein the stirring time in the steps (1) and (2) is 10-20min and 20-40min respectively;
or, in the step (2), the dispersant is any one of polyethylene glycol 6000 and polyvinylpyrrolidone, and the adding proportion of the dispersant is α -Al2O31-5% of the mass.
6. The preparation method of the self-lubricating ceramic cutter with the self-repairing capability according to claim 4, wherein in the step (3), ball milling balls are added according to a ball material weight ratio of 9-15:1 for ball milling for 35-45h, and the ball milling time is continued for 3-7 h; the protective atmosphere comprises any one of nitrogen, argon and the like; preferably, the material of the ball grinding ball is cemented carbide YG6 or YG 8;
alternatively, in step (3), the h-BN @ Al2O3The preparation method of the suspension comprises the following steps: h-BN @ Al2O3Dissolving the powder in a volatile dispersion medium, and then ultrasonically dispersing and stirring to obtain the nano-composite material; preferably, the stirring time is 5-15 min;
or the volatile dispersion medium and the volatile solvent are both absolute ethyl alcohol.
7. The method for preparing the self-lubricating ceramic cutter with the self-repairing capability according to the claim 4, wherein in the step (3), the drying temperature is 80-120 ℃, and the drying time is 12-24 hours.
8. The method for preparing the self-lubricating ceramic tool with self-repairing capability according to any one of claims 4-7, wherein in the step (4), the hot-pressing sintering parameters are as follows: the heating rate is 10-20min/min, the sintering temperature is 1550-.
9. The method for repairing the self-lubricating ceramic tool with self-repairing capability, which is prepared by the preparation method of any one of claims 4 to 7, is characterized in that the self-lubricating ceramic tool with self-repairing capability, which is cracked, is heated to a set temperature in an aerobic environment and then is subjected to heat preservation; preferably, the set temperature is 700-.
10. Use of the self-lubricating ceramic tool with self-repairing capability of any one of claims 1-3 or the self-lubricating ceramic tool with self-repairing capability prepared by the method of any one of claims 4-7 in mechanical cutting machining.
CN202010429650.3A 2020-05-20 2020-05-20 Self-lubricating ceramic cutter with self-repairing capability and preparation method, repairing method and application thereof Pending CN111574209A (en)

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