CN114273659B - Graphene/nano Al 2 O 3 Toughened Ti (C, N) -based metal ceramic cutter material and preparation method thereof - Google Patents
Graphene/nano Al 2 O 3 Toughened Ti (C, N) -based metal ceramic cutter material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a graphene/nano Al 2 O 3 A preparation method of toughened Ti (C, N) -based metal ceramic material comprises the steps of preparing Ti (C, N), graphene and nano Al 2 O 3 Preparing slurry, uniformly mixing and drying to obtain composite ceramic material powder, prepressing to obtain a blank, and finally sintering the blank into a Ti (C, N) -based ceramic cutter material by vacuum hot pressing; the vacuum hot-pressing sintering process comprises the following steps: the vacuum degree in the furnace is lower than 0.01MPa, the initial pressure before sintering is set to 15MPa, the pressure is increased to 30MPa in the heat preservation stage, the heating speed is 25 ℃/min, the sintering temperature is 1450 ℃, the heat preservation time is 60min, and the furnace is cooled after the sintering is completed. The invention provides a preparation method of the ceramic cutter. Compared with the traditional ceramic cutter, the ceramic cutter prepared by the method has excellent comprehensive mechanical properties, can meet the increasingly improved performance requirements of the market on the ceramic cutter, and is beneficial to further expanding the application range of the ceramic cutter.
Description
Technical Field
The invention relates to the field of ceramics, in particular to graphene/nano Al 2 O 3 A preparation method of a toughened Ti (C, N) composite ceramic cutter material.
Background
The high-speed cutting technology is a key ring in advanced manufacturing technology, and plays an important role in various contemporary fields of die, automobile, aviation manufacturing and the like. At present, the superhard cutter material has higher manufacturing cost and increasingly tense resource reserve, so the development of the novel ceramic cutter has important influence on the development of high-speed cutting processing, can effectively save resources, reduces cost and is beneficial to realizing sustainable development of the resources.
Ti (C, N) -based cermet is used as a composite ceramic material, which has excellent high-temperature red hardness, wear resistance, oxidation corrosion resistance, adhesion resistance and self-lubricating property; as ceramic cutting tool, the service life and cutting rate can be improved by 2-5 times and 3-10 times respectively compared with those of hard alloy cutting tool, and besides, the ceramic cutting tool has rich raw material resources and lower cost, and is an ideal upgrading substitute product of hard alloy cutting tool. However, the toughness is insufficient, especially the thermal shock resistance is poor, and the application of the material in the fields of high-speed and high-efficiency cutting tools, hot working die materials and the like is limited. Therefore, improving the toughness of Ti (C, N) -based cermet materials is a major problem in developing novel Ti (C, N) -based cermet tool materials.
Nanoparticle toughening is a common toughening method for ceramic materials. The nano additive phase can form a nano composite structure of an intra-crystal type, an inter-crystal type, intra-crystal/inter-crystal and the like in the material, so that the mechanical property of the ceramic cutter material is effectively improved. Meanwhile, the addition of the nano material can refine grains, improve the compactness of the material and further improve the comprehensive performance of the material.
Al 2 O 3 As a ceramic matrix, the ceramic matrix has the advantages of excellent high-temperature strength, oxidation resistance, wear resistance, corrosion resistance and the like. CN1632150a discloses a composite Ti (C, N) ceramic material, which is obtained by adding Al to Ti (C, N) 2 O 3 ，Ti(C,N)/Al 2 O 3 The composite ceramic material has the advantages of both alumina-based ceramic and titanium carbonitride-based ceramic, and has good stability.
CN105112756a discloses a Ti (C, N) composite ceramic material with ultrafine grains, and the hardness of the prepared composite ceramic material is improved from 2050GPa to 2200GPa, so that the wear resistance and the service life of the cutter are improved.
However, in these publications, only the hardness of the material is improved, while the improvement of fracture toughness and flexural strength of the ceramic material is limited, and the overall performance of the ceramic material is still not ideal.
Graphene is a material composed of sp 2 The hybridized carbon atoms are arranged in a hexagonal period to form the two-dimensional carbon nanomaterial. The single layer thickness is 0.335nm, which is the thinnest, strongest and hardest material found at present. In recent years, graphene is widely used in various fields due to its excellent properties. The graphene has excellent mechanical properties and very high tensile modulus and strength, and the graphene is introduced into the ceramic matrix, so that the strength and fracture toughness of the material can be improved through various toughening modes such as crack deflection, bridging and the like.
CN201610528819.4 discloses a graphene-added Si 3 N 4 A base ceramic cutter material and a preparation method thereof. In the invention, the addition of a proper amount of graphene can effectively improve the fracture toughness of the composite ceramic material. However, in the patent, the dispersion method of graphene is too complicated and cumbersome to be suitable for mass production, and has limited practical value.
In view of the above, the present invention proposes to add graphene and nano Al simultaneously to Ti (C, N) cermet 2 O 3 Graphene improves fracture toughness and bending strength of the material, and nano Al 2 O 3 The hardness of the material is improved. Graphene and nano Al 2 O 3 The comprehensive mechanical properties of the composite ceramic material are improved together by synergistic toughening.
Disclosure of Invention
The invention aims to provide a novel Ti (C, N) -based metal ceramic cutter material and a preparation method thereof, so as to improve the toughness problem of a ceramic cutter during high-speed cutting.
In order to solve the technical problems, the invention adopts the following technical scheme:
a novel Ti (C, N) -based metal ceramic cutter is prepared from the following components in parts by mass: carbonitridationTitanium (Ti (C, N)): 47-62%, tungsten carbide (WC): 15% molybdenum carbide (Mo 2 C) 10 percent of nickel (Ni): 8%, cobalt (Co): 4%, nano alumina (Al 2 O 3 ): 0-15%, graphene (GNPs): 0-1.5%.
In the invention, ti (C, N) is adopted as a matrix material, WC and Mo 2 C is carbide reinforcing phase, and Ni, co and other metal phases are selected as binding phase. Graphene and nano Al 2 O 3 Is a strengthening phase.
The invention simultaneously protects a preparation process of a novel Ti (C, N) -based metal ceramic cutter, and the method comprises the following steps:
(1) Mixing the powder according to the mass fraction ratio, and then mixing Ti (C, N), WC and Mo 2 C. The Ni powder, co powder and other powder are poured into a ball milling tank, absolute ethyl alcohol is used as a ball milling medium, ball milling is carried out in a ball mill, and the ball milling tank and ball milling materials are stainless steel.
(2) Dissolving polyvinylpyrrolidone (PVP) in absolute ethyl alcohol to prepare a dispersion solution, wherein the mass fraction of the polyvinylpyrrolidone (PVP) is 75% of the mass of graphene, pouring the graphene into a dispersing agent, and dispersing by using an ultrasonic dispersing machine and mechanically stirring for 30min.
(3) Nano Al 2 O 3 Pouring into absolute ethanol solution, and dispersing for 30min by using an ultrasonic dispersing machine and mechanical stirring.
(4) And (3) pouring the solution obtained in the step (2) and the step (3) into the slurry obtained after ball milling in the step (1), and then performing ball milling.
(5) Pouring the flowing slurry after ball milling into a glassware, and putting into a DZ-1BC II vacuum drying oven for heating and drying.
(6) After drying, cooling to room temperature and sieving with a 150 mesh sieve.
(7) And paving the uniformly mixed powder into the inner sleeve of the metal die.
(8) The press machine adopted for pre-pressing the green body is 769YP-30T powder tablet press, a mode of pouring and taking out a die is adopted for ensuring the integrity of the green body, an upper pressing head, a graphite gasket, a green body, a graphite gasket and a lower pressing head are sequentially arranged from top to bottom, and finally the manufactured green body is put into a graphite die for sintering.
In the step (1) and the step (4), the ball milling time of the two ball milling is 24 hours, the ball material ratio is 8:1, the rotating speed of the ball mill is 275r/min, the forward and reverse rotating direction is automatically changed every 30 minutes, and the middle of the ball mill stops rotating for 5 minutes.
In the step (1), the material comprises the following components in percentage by mass: titanium carbonitride (Ti (C, N)): 47-62%, tungsten carbide (WC): 15% molybdenum carbide (Mo 2 C) 10 percent of nickel (Ni): 8%, cobalt (Co): 4%, nano alumina (Al 2 O 3 ): 0-15%, graphene (GNPs): 0-1.5%.
In the step (5), in order to avoid slurry loss or composite material mutual pollution caused by alcohol boiling during drying, the drying is carried out for 5 hours under the low vacuum degree of 70 ℃ and then the drying is carried out under the high vacuum degree of 110 ℃ until the drying is completed.
In the step (8), the pre-pressing pressure of the green body is 30MPa, and the time is kept for 15min.
Compared with the prior art, the invention has the following remarkable characteristics:
the invention solves the problems of graphene and nano Al in the mixing process by selecting proper dispersing agent and optimal dispersing dosage 2 O 3 The agglomeration problem, by adopting a method of twice ball milling, prepares the relatively uniform Ti (C, N) -based metal composite ceramic material.
Compared with the common Ti (C, N) metal composite ceramic material, the graphene/nano Al 2 O 3 The mechanical properties of the toughened composite ceramic material sample are improved to a certain extent. Bending strength, hardness and fracture toughness of composite ceramic material follow graphene and nano Al 2 The improvement of the O content is improved in different degrees.
Description of the drawings:
FIG. 1 is a graph showing the relationship between the mechanical properties and the graphene content of the composite materials prepared in examples 1 to 4;
FIG. 2 shows the mechanical properties of the composite materials prepared in examples 5, 3, 6 and 7 and nano Al 2 O 3 Relationship of content;
FIG. 3 is a Scanning Electron Microscope (SEM) photograph of the composite material prepared in examples 1-4;
FIG. 4 is a Scanning Electron Microscope (SEM) photograph of the composite material prepared in examples 5, 3, 6, 7;
Detailed Description
In order to enable those skilled in the art to more understand the specific aspects of the invention, the following detailed description of the invention is provided with reference to specific examples.
Example 1
Graphene/nano Al 2 O 3 The preparation method of the toughened Ti (C, N) -based metal ceramic cutter material comprises the following steps:
(1) Weighing: the following powders were weighed in mass fraction, titanium carbonitride (Ti (C, N)): 58%, tungsten carbide (WC): 15% molybdenum carbide (Mo 2 C) 10 percent of nickel (Ni): 8%, cobalt (Co): 4%, nano alumina (Al 2 O 3 )：5％。
(2) Ball milling: proportioning Ti (C, N), WC and Mo 2 C. The powder of Ni, co and the like is poured into a ball milling tank, the ball milling tank is cleaned and dried before use, ball milling beads with different diameters are put into the ball milling tank, the ball material ratio is 8:1, absolute ethyl alcohol is used as a medium for wet milling, the rotating speed of the ball milling tank is 275r/min, the forward and reverse rotating direction is automatically changed every 30 minutes, the middle is stopped for 5 minutes, and the ball milling is carried out for 24 hours.
(3) Dispersing: nano Al 2 O 3 Pouring into absolute ethanol solution, and dispersing for 30min by using an ultrasonic dispersing machine and mechanical stirring to obtain uniformly mixed nano Al 2 O 3 The solution was mixed.
(4) Ball milling: pouring the mixed solution obtained in the step (3) into the uniform slurry obtained in the step (2), continuing ball milling, wherein the ball-material ratio is 8:1, using absolute ethyl alcohol as a medium for wet milling, setting the rotating speed of the ball mill to 275r/min, automatically changing the forward and reverse rotating direction every 30 minutes, stopping rotating for 5 minutes in the middle, and performing ball milling for 24 hours.
(5) And (3) drying: pouring the slurry obtained after ball milling into a clean glass vessel, drying for 5 hours at a low vacuum degree of 70 ℃ and then drying at a high vacuum degree of 110 ℃ until the drying is finished, and cooling to room temperature and sieving with a 150-mesh sieve in order to avoid alcohol boiling phenomenon caused by overhigh temperature.
(6) And (3) forming: pouring the sieved uniform powder into a metal mold, and pressing the green blank by using a 769YP-30T powder tablet press, wherein the pressing pressure of the green blank is 30MPa, and the pressing time is 15min. In order to ensure the integrity of the blank during the mould taking, an inverted mould taking method is adopted.
(7) Sintering: and placing the green body into a graphite mold, then placing the graphite mold into a vacuum hot-pressing sintering furnace, and finally starting vacuum hot-pressing sintering. The sintering temperature is 1450 ℃, the heating rate is 25 ℃/min, and the heat preservation time is 1h. When hot-pressing sintering, the vacuum degree in the furnace is lower than 0.01MPa, and the initial pressure is set to be 15MPa before sintering, so that the pressure is increased to 30MPa in the heat preservation stage. And after sintering, cooling along with a furnace to obtain the Ti (C, N) -based metal composite ceramic cutter material.
Example 2
Graphene/nano Al 2 O 3 The preparation method of the toughened Ti (C, N) -based metal ceramic cutter material comprises the following steps:
(1) Weighing: the following powders were weighed in mass fraction, titanium carbonitride (Ti (C, N)): 57.5%, tungsten carbide (WC): 15% molybdenum carbide (Mo 2 C) 10 percent of nickel (Ni): 8%, cobalt (Co): 4%, nano alumina (Al 2 O 3 ): 5%, graphene (GNPs): 0.5%.
(2) Ball milling: proportioning Ti (C, N), WC and Mo 2 C. The powder of Ni, co and the like is poured into a ball milling tank, the ball milling tank is cleaned and dried before use, ball milling beads with different diameters are put into the ball milling tank, the ball material ratio is 8:1, absolute ethyl alcohol is used as a medium for wet milling, the rotating speed of the ball milling tank is 275r/min, the forward and reverse rotating direction is automatically changed every 30 minutes, the middle is stopped for 5 minutes, and the ball milling is carried out for 24 hours.
(3) Dispersing: dissolving polyvinylpyrrolidone (PVP) in absolute ethyl alcohol to prepare a dispersion solution, wherein the polyvinylpyrrolidone (PVP) accounts for 75% of the mass of graphene, pouring the graphene into a dispersing agent, and performing mechanical stirring for 30min by adopting an ultrasonic dispersing machine to obtain a uniformly mixed graphene solution; nano Al 2 O 3 Pouring into absolute ethanol solution, and dispersing with ultrasonic waveMechanically stirring for 30min to obtain nanometer Al 2 O 3 The solution was mixed.
(4) Ball milling: and (3) pouring the two mixed solutions obtained in the step (3) into the uniform slurry obtained in the step (2), continuing ball milling, setting the ball-material ratio to be 8:1, setting the rotating speed of the ball mill to be 275r/min, automatically changing the forward and reverse rotating direction every 30 minutes, stopping rotating for 5 minutes in the middle, and performing ball milling for 24 hours.
(5) And (3) drying: pouring the slurry obtained after ball milling into a clean glass vessel, drying for 5 hours at a low vacuum degree of 70 ℃ and then drying at a high vacuum degree of 110 ℃ until the drying is finished, and cooling to room temperature and sieving with a 150-mesh sieve in order to avoid alcohol boiling phenomenon caused by overhigh temperature.
(6) And (3) forming: pouring the sieved uniform powder into a metal mold, and pressing the green blank by using a 769YP-30T powder tablet press, wherein the pressing pressure of the green blank is 30MPa, and the pressing time is 15min. In order to ensure the integrity of the blank during the mould taking, an inverted mould taking method is adopted.
(7) Sintering: and placing the green body into a graphite mold, then placing the graphite mold into a vacuum hot-pressing sintering furnace, and finally starting vacuum hot-pressing sintering. The sintering temperature is 1450 ℃, the heating rate is 25 ℃/min, and the heat preservation time is 1h. When hot-pressing sintering, the vacuum degree in the furnace is lower than 0.01MPa, and the initial pressure is set to be 15MPa before sintering, so that the pressure is increased to 30MPa in the heat preservation stage. And after sintering, cooling along with a furnace to obtain the Ti (C, N) -based metal composite ceramic cutter material.
Example 3
This example is identical to example 2, except for the powder formulation. The following powders, titanium carbonitride (Ti (C, N)), were weighed in mass fraction: 57%, tungsten carbide (WC): 15% molybdenum carbide (Mo 2 C) 10 percent of nickel (Ni): 8%, cobalt (Co): 4%, nano alumina (Al 2 O 3 ): 5%, graphene (GNPs): 1%.
Example 4
This example is identical to example 2, except for the powder formulation. Weighing the following powders by mass fraction, and carbonitridingTitanium (Ti (C, N)): 56.5%, tungsten carbide (WC): 15% molybdenum carbide (Mo 2 C) 10 percent of nickel (Ni): 8%, cobalt (Co): 4%, nano alumina (Al 2 O 3 ): 5%, graphene (GNPs): 1.5%.
Example 5
This example is identical to example 2, except for the powder formulation. The following powders, titanium carbonitride (Ti (C, N)), were weighed in mass fraction: 62%, tungsten carbide (WC): 15% molybdenum carbide (Mo 2 C) 10 percent of nickel (Ni): 8%, cobalt (Co): 4%, graphene (GNPs): 1%.
Example 6
This example is identical to example 2, except for the powder formulation. The following powders, titanium carbonitride (Ti (C, N)), were weighed in mass fraction: 52%, tungsten carbide (WC): 15% molybdenum carbide (Mo 2 C) 10 percent of nickel (Ni): 8%, cobalt (Co): 4%, nano alumina (Al 2 O 3 ): 10%, graphene (GNPs): 1%.
Example 7
This example is identical to example 2, except for the powder formulation. The following powders, titanium carbonitride (Ti (C, N)), were weighed in mass fraction: 47%, tungsten carbide (WC): 15% molybdenum carbide (Mo 2 C) 10 percent of nickel (Ni): 8%, cobalt (Co): 4%, nano alumina (Al 2 O 3 ): 15%, graphene (GNPs): 1%.
The mechanical properties of examples 1-4 are shown in FIG. 1. With the increase of the graphene content from 0% to 1.5%, the hardness of the material is slightly increased from 19.8GPa to 21.5GPa (highest in the embodiment 3), and then is reduced to 21.15GPa; the flexural strength of the material was increased from 821.3MPa to 845.9MPa and then decreased to 752.2MPa (highest in example 2); the fracture toughness of the material is 8.53 MPa.m 1/2 Increasing to 10.51 MPa.m 1/2 Then the temperature is reduced to 9.07MPa m 1/2 (highest in example 3). It can be seen that example 3 has the best overall mechanical properties among examples 1-4.
The mechanical properties of examples 5, 3, 6, 7 are shown in FIG. 2. Along with nano Al 2 O 3 From 0% to 15%The hardness of the material is slightly increased from 21.01GPa to 21.5GPa (highest in the embodiment 2) and then reduced to 21.03GPa; the flexural strength of the material was increased from 761.36MPa to 843.85MPa and then decreased to 794.38MPa (highest in example 3); the fracture toughness of the material is from 9.72 MPa.m 1/2 Increasing to 10.51 MPa.m 1/2 Then the mixture is reduced to 9.7MPa m 1/2 (highest in example 2). It can be seen that example 2 has the best overall mechanical properties among examples 5, 3, 6 and 7.
The SEM morphologies of examples 1-4 are shown in FIG. 3. The main component of the white part is Al 2 O 3 The black part is mainly composed of Ti (C, N), and the gray part is a complex solid solution of Ti (C, N). From the graph, as the content of graphene increases, the main fracture mode of the composite ceramic material is changed from crystal-through fracture to crystal-along fracture, because the graphene has excellent mechanical properties, the expansion mode of cracks can be changed, the fracture energy is consumed, and the fracture toughness of the composite ceramic material is further improved. With the increase of the graphene content, the crystal grains of the composite ceramic material become smaller gradually, and the distribution of the crystal grains is more uniform. When the content of graphene is too large, agglomeration of graphene occurs, thereby generating defects such as air holes.
SEM morphology of examples 5, 3, 6, 7 is shown in fig. 4. It can be seen from the figure that with nano Al 2 O 3 The content is increased, the crystal grains of the composite material become uniform gradually, and the crystal grain size is smaller. The nano material can refine grains due to the size effect of the nano material, so that the overall performance of the composite material is improved. Because the nano material is easy to generate agglomeration phenomenon, when nano Al 2 O 3 When the amount of the polymer is excessive, obvious agglomeration phenomenon occurs, and the comprehensive performance of the material is further affected.
The ceramic cutter prepared by the method has good bending strength and fracture toughness, can meet the performance requirement of the ceramic cutter during high-speed cutting processing, and is beneficial to further expanding the application range of the ceramic cutter.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention, and various modifications can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention.
Claims (4)
1. Graphene (GNPs)/nano Al 2 O 3 The preparation method of the toughened Ti (C, N) -based metal ceramic cutter material is characterized by comprising the following steps:
(1) After the required powder is prepared according to the mass fraction proportion, ti (C, N), WC and Mo are firstly mixed 2 C. Pouring Ni and Co powder into a ball milling tank, taking absolute ethyl alcohol as a ball milling medium, and performing ball milling in a ball mill, wherein the ball milling tank and ball milling materials are stainless steel;
(2) Dissolving polyvinylpyrrolidone (PVP) in absolute ethyl alcohol to prepare a dispersion solution, wherein the polyvinylpyrrolidone (PVP) accounts for 75% of the mass of graphene, pouring the graphene into a dispersing agent, and adding mechanical stirring to disperse for 30min by adopting an ultrasonic dispersing machine;
(3) Nano Al 2 O 3 Pouring into absolute ethanol solution, and dispersing for 30min by adopting an ultrasonic dispersing machine and mechanical stirring;
(4) Pouring the solution obtained in the step (2) and the step (3) into the slurry obtained after ball milling in the step (1), and then performing ball milling;
(5) Pouring the flowing slurry after ball milling into a clean glassware, and putting into a DZ-1BC II vacuum drying oven for heating and drying;
(6) Cooling to room temperature after drying, and sieving with a 150-mesh sieve;
(7) Paving and filling the uniformly mixed powder into an inner sleeve of a metal mold;
(8) The method comprises the steps that a press machine adopted for pre-pressing a green body is a 769YP-30T powder tablet press, an inverted die-taking mode is adopted for guaranteeing the integrity of the green body, an upper pressing head, a graphite gasket, a green body, a graphite gasket and a lower pressing head are sequentially arranged from top to bottom, and finally the manufactured green body is placed into a graphite die for sintering;
in the step (1), the material comprises the following components in percentage by mass: titanium carbonitride (Ti (C, N)): 47-62%, tungsten carbide (WC): 15% molybdenum carbide (Mo 2 C) 10 percent of nickel (Ni): 8%, cobalt (Co): 4%, nano alumina (Al 2 O 3 ): 5-15%, graphene (GNPs): 0.5-1.5%.
2. The method according to claim 1, wherein in the steps (1) and (4), the ball milling time in the ball mill is 24 hours, the ball-to-material ratio is 8:1, the ball mill is set at a rotating speed of 275r/min, the forward and reverse rotation directions are automatically changed every 30 minutes, and the intermediate stop is carried out for 5 minutes.
3. The method of claim 1, wherein in step (5), in order to avoid slurry loss or composite material mutual contamination caused by alcohol boiling during drying, the drying is performed at a low vacuum of 70 ℃ for 5 hours, and then at a high vacuum of 110 ℃ until the drying is completed.
4. The method of claim 1, wherein in step (8), the pre-pressing pressure of the green body is 30MPa and the time is 15 minutes.
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| 李帅等.多层石墨烯添加量对Ti(C_(0.7),N_(0.3))基金属陶瓷组织和力学性能的影响.硬质合金.2020,第37卷(第03期),第195-202页. * |
| 纳米Al_2O_3对Ti(C,N)基金属陶瓷性能的影响;徐立强;王随莲;黄传真;侯志刚;刘含莲;;稀有金属材料与工程;第37卷(第04期);732-735 * |
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