CN115448730A - High-strength high-heat-conductivity silicon nitride ceramic cutter and preparation method and application thereof - Google Patents
High-strength high-heat-conductivity silicon nitride ceramic cutter and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a high-strength high-heat-conductivity silicon nitride ceramic cutter as well as a preparation method and application thereof, belonging to the technical field of ceramic materials. The high-strength high-heat-conductivity silicon nitride ceramic cutting tool provided by the invention is prepared from 70-90% of alpha-Si in percentage by mass 3 N 4 Powder, 0.5-1% beta-Si 3 N 4 Seed crystal, 2-5% of rare earth oxide, 5-10% of diamond with metal coating and the balance of sintering aid. The results of the examples show that the bending strength of the high-strength high-heat-conductivity silicon nitride ceramic cutter provided by the invention exceeds 1100MPa, and the fracture toughness exceeds 11.5MPa/m 2 Hardness of VickersThe degree exceeds 18GPa.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a high-strength high-heat-conductivity silicon nitride ceramic cutter and a preparation method and application thereof.
Background
The high-temperature alloy is classified according to matrix elements and mainly comprises iron-based, nickel-based, cobalt-based and other high-temperature alloys. The nickel-based high-temperature alloy has higher hardness, excellent high-temperature strength, thermal stability and thermal fatigue resistance, plays a special important role in the whole high-temperature alloy field, is mainly used for manufacturing the hottest end parts of an aviation jet engine and various industrial gas turbines, and is widely applied to the industries of aerospace, ships, nuclear industry, power stations and the like. At present, the high-temperature alloy is processed mainly by cutting, but because the high-temperature alloy has high strength, high hardness and good high-temperature stability, the high-temperature alloy needs great cutting force in the cutting process, the temperature in the cutting process is very high and can reach about 1000 ℃, the cutting tool for cutting is seriously hardened in a machining mode, the plastic deformation is large, the cutting tool is easy to wear, the cutting tool needs to be frequently replaced, the production cost is increased, and the cutting effect is easily influenced.
In recent years, silicon nitride ceramic cutting tools have been widely used in modern machining fields due to their high hardness, strength, fracture toughness, small expansion coefficient, high temperature resistance, and inexhaustible elements such as silicon and nitrogen in the natural world. The properties of the silicon nitride ceramic material depend on the microstructure thereof, scientists change the microstructure thereof by adding auxiliary agents and changing the sintering mode, and the ceramic material consisting of a beta silicon nitride phase and a grain boundary phase is obtained by adjusting the sintering auxiliary agents and adding beta silicon nitride seed crystals by adopting a hot pressing method in the United states patent US7968484, wherein the bending strength at room temperature is 1000MPa, and the fracture toughness is 9MPa/m 2 However, the ceramic material produced by the method has low hardness and poor heat conductivity, cannot meet general requirements in the application of cutters, and is quickly worn in the high-speed cutting process, so that the service life of the cutters is shortened, and the cutters are frequently replaced.
Therefore, it is an urgent technical problem to be solved in the art to provide a ceramic cutting tool with high strength, good heat conductivity and long service life.
Disclosure of Invention
The invention aims to provide a high-strength high-heat-conductivity silicon nitride ceramic cutter as well as a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a high-strength high-heat-conductivity silicon nitride ceramic cutting tool, which is prepared from 70-90% of alpha-Si in percentage by mass 3 N 4 Powder, 0.5-1% beta-Si 3 N 4 Seed crystal, 2-5% of rare earth oxide, 5-10% of diamond with metal coating and the balance of sintering aid.
Preferably, the beta-Si is 3 N 4 The length-diameter ratio of the seed crystal is (2-5): 1.
preferably, the rare earth oxide comprises Y 2 O 3 、La 2 O 3 、Yb 2 O 3 、Sc 2 O 3 、Ce 2 O 3 、Pr 2 O 3 、Nd 2 O 3 、Lu 2 O 3 、Tb 2 O 3 And Tm 2 O 3 At least one of (1).
Preferably, the diamond having the metal plating layer has a particle size of 10 to 100 μm.
Preferably, the material of the metal coating in the diamond with the metal coating is Ni or Ti, and the thickness of the metal coating is 50-300 nm.
Preferably, the sintering aid comprises MgO and Al 2 O 3 And AlN.
The invention provides a preparation method of the high-strength high-heat-conductivity silicon nitride ceramic cutter in the technical scheme, which comprises the following steps:
(1) Mixing the raw materials of the high-strength high-heat-conductivity silicon nitride ceramic cutter, and then carrying out ball milling to obtain a mixture;
(2) And (2) sequentially carrying out hot-pressing sintering and annealing treatment on the mixture obtained in the step (1) to obtain the high-strength high-heat-conductivity silicon nitride ceramic cutter.
Preferably, the pressure of the hot-pressing sintering in the step (2) is 10-50 MPa, the temperature of the hot-pressing sintering is 1400-1900 ℃, and the time of the hot-pressing sintering is 20-180 min.
Preferably, the temperature of the annealing treatment in the step (2) is 950-1200 ℃, and the time of the annealing treatment is 30-120 min.
The invention provides the application of the high-strength high-heat-conductivity silicon nitride ceramic cutting tool in the technical scheme or the application of the high-strength high-heat-conductivity silicon nitride ceramic cutting tool prepared by the preparation method in cutting hard alloy.
The invention provides a high-strength high-heat-conductivity silicon nitride ceramic cutting tool, which is prepared from 70-90% of alpha-Si in percentage by mass 3 N 4 Powder, 0.5-1% beta-Si 3 N 4 Seed crystal, 2-5% of rare earth oxide, 5-10% of diamond with metal coating and the balance of sintering aid. The invention uses alpha-Si 3 N 4 The powder is used as the base material of ceramic by adding small amount of beta-Si 3 N 4 Seed crystals capable of promoting alpha-Si 3 N 4 Powder is sintered to beta-Si 3 N 4 The density, hardness, fracture toughness and wear resistance of the silicon nitride ceramic cutter are effectively improved, and the service life of the silicon nitride ceramic cutter during high-speed dry cutting is prolonged; the rare earth oxide and the sintering aid can reduce the grain boundary phase and further promote the alpha-Si 3 N 4 To beta-Si 3 N 4 The heat conductivity and the toughness of the ceramic material are improved, and the sintering aid function is achieved, so that the sintering temperature can be reduced, and the compactness of the ceramic material can be improved; the cutting performance of the silicon nitride ceramic cutter can be improved by adding a certain amount of diamond, so that the service life of the cutter is prolonged; the metal layer is plated on the surface of the diamond, so that the diamond can be prevented from graphitizing at high temperature, the cutting performance of the cutter can be ensured, and meanwhile, the interface bonding strength of the diamond and silicon nitride can be improved, and the service life of the cutter can be prolonged. The results of the examples showIt shows that the bending strength of the high-strength high-heat-conductivity silicon nitride ceramic cutter provided by the invention exceeds 1100MPa, and the fracture toughness exceeds 11.5MPa/m 2 The Vickers hardness exceeds 18GPa.
Detailed Description
The invention provides a high-strength high-heat-conductivity silicon nitride ceramic cutting tool, which is prepared from 70-90% of alpha-Si in percentage by mass 3 N 4 Powder of 0.5 to 1% of beta-Si 3 N 4 Seed crystal, 2-5% of rare earth oxide, 5-10% of diamond with metal coating and the balance of sintering aid.
The specific sources of the raw materials for preparing the high-strength high-heat-conductivity silicon nitride ceramic cutting tool are not particularly limited, and the high-strength high-heat-conductivity silicon nitride ceramic cutting tool can be prepared by using commercially available products or self-preparation products which are well known to those skilled in the art.
The raw material for preparing the high-strength high-heat-conductivity silicon nitride ceramic cutting tool comprises 70-90% of alpha-Si by mass percent 3 N 4 The powder is preferably 75 to 85%, more preferably 80%. In the present invention, the α -Si is 3 N 4 The particle size of the powder is preferably 0.1 to 5 μm, more preferably 0.5 to 4 μm, and still more preferably 1 to 3 μm. The invention adopts alpha-Si 3 N 4 The powder is used as matrix raw material, and can be converted into long columnar beta-Si during high-temperature sintering 3 N 4 Thereby improving the compactness of the ceramic cutter, further improving the strength and the hardness of the ceramic cutter, and prolonging the service life of the silicon nitride ceramic cutter during high-speed dry cutting; by controlling alpha-Si 3 N 4 The strength and hardness of the ceramic cutting tool can be further improved by the using amount and the grain diameter of the powder.
The raw material for preparing the high-strength high-heat-conductivity silicon nitride ceramic cutting tool comprises 0.5-1% of beta-Si in percentage by mass 3 N 4 The seed crystal is preferably 0.6 to 0.8%. In the present invention, the beta-Si is 3 N 4 The aspect ratio of the seed crystal is preferably (2 to 5): 1, more preferably (3 to 4): 1; the beta-Si 3 N 4 The crystal axis length of the seed crystal is preferably 1 to 3 μm. The invention adds beta-Si 3 N 4 The seed crystal can promote alpha-Si 3 N 4 Powder is sintered to beta-Si 3 N 4 Thereby effectively improving the density, hardness, fracture toughness and wear resistance of the silicon nitride ceramic cutter; by controlling beta-Si 3 N 4 The parameters of the crystal seeds can further improve the fracture toughness and the wear resistance of the ceramic cutter.
The raw materials for preparing the high-strength high-heat-conductivity silicon nitride ceramic cutting tool comprise 2-5% of rare earth oxide by mass percentage, and preferably 3-4% of rare earth oxide by mass percentage. In the present invention, the rare earth oxide includes Y 2 O 3 、La 2 O 3 、Yb 2 O 3 、Sc 2 O 3 、Ce 2 O 3 、Pr 2 O 3 、Nd 2 O 3 、Lu 2 O 3 、Tb 2 O 3 And Tm 2 O 3 More preferably Y 2 O 3 、La 2 O 3 、Yb 2 O 3 、Sc 2 O 3 、Ce 2 O 3 、Pr 2 O 3 、Nd 2 O 3 、Lu 2 O 3 、Tb 2 O 3 And Tm 2 O 3 At least two kinds of (2), more preferably Y 2 O 3 、La 2 O 3 And Yb 2 O 3 Most preferably Y 2 O 3 、La 2 O 3 And Yb 2 O 3 . The invention can reduce the grain boundary phase by adding the rare earth oxide and further promote the alpha-Si 3 N 4 To beta-Si 3 N 4 The heat conductivity and the toughness of the ceramic material are improved, and the sintering aid effect is achieved to improve the compactness of the ceramic material; the heat-conducting property of the ceramic cutter can be further improved by the synergistic effect of the compounding of various rare earth oxides.
The raw materials for preparing the high-strength high-thermal conductivity silicon nitride ceramic cutting tool comprise, by mass, 5-10% of diamond with a metal coating, preferably 6-9%, and more preferably 7-8%. In the present invention, the diamond in the diamond having the metal plating layer preferably has a particle size of 10 to 100 μm. In the invention, the material of the metal coating in the diamond with the metal coating is preferably Ni or Ti, and more preferably Ti; the thickness of the metal plating layer is preferably 50 to 300nm, more preferably 100 to 200nm, and still more preferably 150 to 200nm. The cutting performance of the silicon nitride ceramic cutter can be improved by adding a certain amount of diamond, so that the service life of the cutter is prolonged; the metal layer is plated on the surface of the diamond, so that the diamond can be prevented from graphitizing at high temperature, the cutting performance of the cutter can be ensured, and the interface bonding strength of the diamond and silicon nitride can be improved, so that the service life of the cutter is prolonged.
In the present invention, when the material of the metal plating layer in the diamond with a metal plating layer is Ni, the method for preparing the diamond with a metal plating layer preferably includes the steps of:
1) Sequentially carrying out alkaline degreasing, sensitization, activation and reduction on the diamond particles to obtain pretreated diamond particles;
2) Carrying out chemical nickel plating on the pretreated diamond particles obtained in the step 1) to obtain the diamond with a metal coating.
In the invention, the diamond particles are preferably subjected to alkaline degreasing, coarsening, sensitization, activation and reduction in sequence to obtain the pretreated diamond particles.
In the present invention, the diamond particles preferably have a particle size of 10 to 20 μm. The invention is beneficial to better nickel plating by controlling the grain diameter of the diamond grains.
In the present invention, the alkali solution used for the alkaline degreasing preferably comprises: 10g/L of sodium hydroxide, 20g/L of sodium carbonate, 30g/L of sodium phosphate, 10g/L of sodium silicate, 2g/L of OP emulsifier and the balance of water. In the invention, the temperature of the alkaline oil removal is preferably 35-40 ℃, and more preferably 36 ℃; the time for alkaline degreasing is preferably 5 to 20min, and more preferably 10min. According to the invention, the diamond is subjected to alkaline degreasing, so that impurities on the surface can be removed, and a foundation is laid for subsequent treatment.
After the alkaline degreasing is finished, the product of the alkaline degreasing is preferably washed by water. The specific operation of the washing in the present invention is not particularly limited, and may be determined according to the general technical knowledge of those skilled in the art.
In the present invention, the coarsening agent used for the coarsening preferably includes: 1mol/L sulfuric acid, 1mol/L hydrofluoric acid and the balance of water. In the invention, the temperature for coarsening is preferably 35-40 ℃, and more preferably 36 ℃; the roughening time is preferably 5 to 20min, and more preferably 10min. The invention is beneficial to improving the bonding strength of the diamond and the nickel and preventing the diamond from falling off by coarsening the diamond.
After the end of the coarsening, the present invention preferably performs a water wash on the coarsened product. The specific operation of the washing in the present invention is not particularly limited, and may be determined according to the general technical knowledge of those skilled in the art.
In the present invention, the sensitizer used for sensitization preferably includes: 20g/L SnCl 2 0.1-1 mol/L HCl and the balance of water. In the present invention, the temperature of the sensitization is preferably 35 to 40 ℃, more preferably 36 ℃; the time for sensitization is preferably 5 to 20min, more preferably 10min. The invention is beneficial to further improving the bonding strength of the diamond and the nickel by sensitizing the diamond.
After the sensitization is finished, the invention preferably carries out water washing on the sensitized product. The specific operation of the washing in the present invention is not particularly limited, and may be determined according to the general technical knowledge of those skilled in the art.
In the present invention, the activating agent used for the activation preferably includes: 0.2g/L of palladium chloride, 0.05-0.5 mol/L of HCl and the balance of water. In the present invention, the temperature of the activation is preferably 35 to 40 ℃, more preferably 36 ℃; the activation time is preferably 5 to 20min, more preferably 10min. The invention can activate the structure of the diamond surface by activating the diamond, thereby being beneficial to nickel plating.
After the activation is finished, the activated product is preferably washed by water in the invention. The specific operation of the washing in the present invention is not particularly limited, and may be determined according to the general technical knowledge of those skilled in the art.
In the present invention, the reducing agent used for the reduction preferably includes: 20g/L of NaH 2 PO 2 And the balance water. According to the invention, the diamond is reduced, so that the bonding strength between the diamond surface and the metal nickel is improved, and a foundation is laid for subsequent nickel plating.
After the reduction is completed, the present invention preferably washes the reduced product with water. The specific operation of the washing in the present invention is not particularly limited, and may be determined according to the general technical knowledge of those skilled in the art.
After obtaining the pretreated diamond particles, the present invention preferably performs electroless nickel plating on the pretreated diamond particles to obtain diamond having a metal plating layer.
In the present invention, the plating solution used for electroless nickel plating preferably includes: 30g/L of nickel chloride hexahydrate and 20g/L of NaH 2 PO 2 10-15 g/L of citric acid, 0.05g/L of thiourea and the balance of water. In the invention, the temperature of the chemical nickel plating is preferably 50-80 ℃, more preferably 60-70 ℃, and further preferably 65 ℃; the pH of the electroless nickel plating is preferably 4.8 to 5.2, more preferably 5.0. In the present invention, the ratio of the mass of the pretreated diamond particles to the volume of the plating solution is preferably (0.5 to 2.5) g:1L, more preferably (1.0 to 2.0) g:1L, more preferably 1.5g:1L of the compound. In the present invention, the electroless nickel plating is preferably under stirring conditions. The time and stirring rate of the electroless nickel plating are not particularly limited in the present invention, and can be determined according to the technical common knowledge of the skilled person in the art. The invention can make the nickel layer thicker and evenly distributed by controlling the components of the reagent used in the chemical nickel plating.
In the present invention, when the material of the metal plating layer in the diamond with a metal plating layer is Ti, the method for preparing the diamond with a metal plating layer preferably includes the steps of:
I. carrying out alkaline degreasing on the diamond particles to obtain pretreated diamond particles;
II. And (3) carrying out vacuum micro-evaporation plating on the pretreated diamond particles obtained in the step (I) to obtain the diamond with a metal coating.
The present invention preferably subjects the diamond particles to alkaline degreasing to obtain pretreated diamond particles.
In the present invention, the diamond particles preferably have a particle size of 30 to 100 μm, more preferably 50 to 80 μm.
In the present invention, the process of alkaline degreasing is preferably the same as the process of alkaline degreasing, and is not described herein again.
After the alkaline degreasing is finished, the product of the alkaline degreasing is preferably washed by water. The specific operation of the washing in the present invention is not particularly limited, and may be determined according to the general technical knowledge of those skilled in the art.
After obtaining the pretreated diamond particles, the invention preferably carries out vacuum micro-evaporation plating on the pretreated diamond particles to obtain the diamond with a metal coating.
In the invention, the granularity of the titanium powder used for the vacuum micro-evaporation plating is preferably 300-400 meshes; the temperature of the vacuum micro-evaporation plating is preferably 700-800 ℃, and more preferably 750-760 ℃; the vacuum degree of the vacuum micro-evaporation plating is preferably 5-7 Pa; the time of the vacuum micro-evaporation plating is preferably 0.5 to 1 hour, and more preferably 0.5 hour. The invention is beneficial to improving the quality of the plating layer by controlling the parameters of the vacuum micro-evaporation plating.
The raw materials for preparing the high-strength high-thermal conductivity silicon nitride ceramic cutting tool comprise, by mass, 1-20% of sintering aid in balance, preferably 2-16%, and more preferably 5-14%. In the present invention, the sintering aid preferably includes MgO, al 2 O 3 And AlN, more preferably MgO or Al 2 O 3 And AlN. In the present invention, the particle size of the sintering aid is preferably 100 to 1000nm, and more preferably 150 to 500nm. The sintering aid added in the invention can play a synergistic effect with the rare earth oxide to reduce the grain boundary phase and promote the alpha-Si 3 N 4 To beta-Si 3 N 4 Thereby improving the thermal conductivity and toughness of the ceramic material, and the sintering aid can play a role in sinteringThe sintering temperature can be reduced, and the compactness of the ceramic material can be improved.
According to the high-strength high-heat-conductivity silicon nitride ceramic cutter, the cutting performance of the cutter is improved by adding diamond particles, the diamond is used as a material with the highest hardness, a good cutting effect can be achieved on hard alloy, and meanwhile, a certain amount of rare earth elements are added into the ceramic cutter to improve the heat conduction performance of the ceramic cutter, so that heat generated in the cutting process can be quickly dissipated into the air through the cutter, the cutting hardening caused by overhigh temperature of the ceramic cutter is avoided, and the ceramic cutter has a longer service life.
The invention provides a preparation method of the high-strength high-heat-conductivity silicon nitride ceramic cutter in the technical scheme, which comprises the following steps:
(1) Mixing the raw materials of the high-strength high-heat-conductivity silicon nitride ceramic cutter, and then carrying out ball milling to obtain a mixture;
(2) And (2) sequentially carrying out hot-pressing sintering and annealing treatment on the mixture obtained in the step (1) to obtain the high-strength high-heat-conductivity silicon nitride ceramic cutter.
The invention mixes the raw materials of the high-strength high-heat-conductivity silicon nitride ceramic cutter and then ball-mills the mixture to obtain the mixture.
The mixing mode of the raw materials is not particularly limited, and the conventional mixing mode can be adopted.
In the invention, the grinding balls used for ball milling are preferably silicon nitride grinding balls, and the diameter of the grinding balls is preferably 5-10 mm; the ball-material ratio of the ball mill is preferably (3-4): 1; the ball milling medium is preferably ethanol; the time for ball milling is preferably 20 to 24 hours. The amount of ethanol used in the present invention is not particularly limited, and it may be added according to the common technical knowledge of those skilled in the art. The raw materials are subjected to ball milling, so that the raw materials can be fully and uniformly mixed, and the compactness, strength, hardness, toughness and heat conductivity of the ceramic cutter are further improved.
After the ball milling is finished, the ball-milled products are preferably dried and crushed in sequence. The invention has no special limit on the drying temperature and time, and can completely volatilize the ethanol. The specific operation of the crushing treatment is not particularly limited, and the dried material is crushed.
After the mixture is obtained, the mixture is sequentially subjected to hot-pressing sintering and annealing treatment to obtain the high-strength high-heat-conductivity silicon nitride ceramic cutter.
In the present invention, the pressure for the hot press sintering is preferably 10 to 50MPa, more preferably 15 to 40MPa, and still more preferably 20 to 30MPa. The invention can further improve the compactness of the ceramic cutter by controlling the pressure of hot-pressing sintering, thereby improving the strength and the hardness of the ceramic cutter and leading the ceramic cutter to have better cutting performance.
In the invention, the temperature of hot-pressing sintering is preferably 1400-1900 ℃; the time of the hot-pressing sintering is preferably 20-180 min. The invention can further improve the compactness of the ceramic cutter by controlling the temperature and time of hot-pressing sintering, thereby leading the ceramic cutter to have good mechanical property.
In the present invention, the hot-pressing sintering is preferably performed by first sintering the mixture at 1400 to 1500 ℃ and then performing second sintering at 1600 to 1900 ℃, and more preferably by first sintering the mixture at 1420 to 1450 ℃ and then performing second sintering at 1700 to 1800 ℃. In the present invention, the time for the primary sintering is preferably 3 to 10min, and more preferably 4 to 5min; the time for the secondary sintering is preferably 17 to 170min, more preferably 20 to 150min, and still more preferably 30 to 120min. According to the invention, by adopting a sectional sintering mode, materials are preliminarily combined by pre-sintering at a lower temperature, and then sintering is carried out at a high temperature, so that the sintering effect is further improved, and the cutter material has better mechanical properties.
In the present invention, the hot press sintering is preferably performed in a protective atmosphere, which is preferably nitrogen or argon. The invention reduces the influence of air on the raw materials by carrying out hot-pressing sintering in the protective atmosphere, thereby further improving the effect of hot-pressing sintering.
After the hot-press sintering is finished, the invention preferably cools the hot-press sintered product to room temperature. The cooling method is not particularly limited, and air cooling or furnace cooling can be adopted.
In the invention, the temperature of the annealing treatment is preferably 950 to 1200 ℃, more preferably 1000 to 1150 ℃, and further preferably 1050 to 1100 ℃; the time for the annealing treatment is preferably 30 to 120min, more preferably 45 to 90min, and still more preferably 60 to 75min. In the present invention, the rate of temperature increase to the annealing temperature is not particularly limited, and may be determined according to the technical common knowledge of those skilled in the art. The cooling method of the annealing treatment in the present invention is not particularly limited, and any cooling method such as air cooling or furnace cooling may be employed. According to the invention, the ceramic cutter is annealed, so that the toughness of the ceramic cutter is improved, the cutter material is prevented from being broken due to overlarge stress, and the service life of the ceramic cutter is further prolonged.
In the present invention, the annealing treatment is preferably performed in a protective atmosphere, which is preferably nitrogen or argon. According to the invention, the effect of oxygen on the cutter is reduced by carrying out annealing treatment in a protective atmosphere.
The invention provides the application of the high-strength high-heat-conductivity silicon nitride ceramic cutting tool in the technical scheme or the application of the high-strength high-heat-conductivity silicon nitride ceramic cutting tool prepared by the preparation method in cutting hard alloy.
The specific mode of the application is not particularly limited, and the method can be applied by adopting the mode of cutting the hard alloy in the prior art.
When the high-strength high-heat-conductivity silicon nitride ceramic cutter provided by the invention is used for cutting hard alloy, the high-strength high-heat-conductivity silicon nitride ceramic cutter has the characteristics of good cutting effect, long service life and the like.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The high-strength high-heat-conductivity silicon nitride ceramic cutting tool comprises the following raw materials in percentage by mass: 70% of alpha-Si 3 N 4 Powder, 1% beta-Si 3 N 4 Seed crystal, 4% of rare earth oxide, 10% of diamond with a metal coating and 15% of sintering aid;
the alpha-Si 3 N 4 The particle size of the powder is 0.1-5 μm;
the beta-Si 3 N 4 The length-diameter ratio of the seed crystal is (2-5): 1; the beta-Si 3 N 4 The length of the crystal axis of the crystal seed is 1-3 mu m;
the rare earth oxide is formed by Y 2 O 3 And La 2 O 3 Composition of, said Y 2 O 3 And La 2 O 3 The mass ratio of (1): 1;
the particle size of diamond in the diamond with the metal coating is 10-20 mu m; the material of the metal coating in the diamond with the metal coating is Ni; the thickness of the metal coating is 200nm;
the sintering aid is MgO, and the particle size of the sintering aid is 150-500 nm;
the preparation method of the high-strength high-heat-conductivity silicon nitride ceramic cutter comprises the following steps:
(1) Mixing the raw materials of the high-strength high-heat-conductivity silicon nitride ceramic cutter, performing ball milling, and then drying and crushing to obtain a mixture; the grinding balls used for ball milling are silicon nitride grinding balls, and the diameter of each grinding ball is 5-10 mm; the ball-milling ball-material ratio is 3:1; the ball milling medium is ethanol; the ball milling time is 24 hours;
(2) Sequentially carrying out hot-pressing sintering and annealing treatment on the mixture obtained in the step (1) to obtain a high-strength high-heat-conductivity silicon nitride ceramic cutter; the hot-pressing sintering mode is that the mixture is sintered for the first time at 1450 ℃, and then sintered for the second time at 1800 ℃; the time of the primary sintering is preferably 5min, and the time of the secondary sintering is 30min; the pressure of the hot-pressing sintering is 30MPa; the temperature of the annealing treatment is 1050 ℃; the time of the annealing treatment is 50min; the hot-pressing sintering and the annealing treatment are carried out in nitrogen.
Example 2
The high-strength high-heat-conductivity silicon nitride ceramic cutting tool comprises the following raw materials in percentage by mass: 70% of alpha-Si 3 N 4 Powder, 0.5% beta-Si 3 N 4 Seed crystal, 5% of rare earth oxide, 8% of diamond with a metal coating and 16.5% of sintering aid;
other conditions were the same as in example 1.
Example 3
The high-strength high-heat-conductivity silicon nitride ceramic cutting tool comprises the following raw materials in percentage by mass: 75% of alpha-Si 3 N 4 Powder, 1% beta-Si 3 N 4 Seed crystal, 3% of rare earth oxide, 7% of diamond with a metal coating and 14% of sintering aid;
other conditions were the same as in example 1.
Example 4
A high-strength high-heat-conductivity silicon nitride ceramic cutting tool comprises the following raw materials in percentage by mass: 75% of alpha-Si 3 N 4 Powder, 0.5% beta-Si 3 N 4 Seed crystal, 2% of rare earth oxide, 6% of diamond with a metal coating and 16.5% of sintering aid;
other conditions were the same as in example 1.
Example 5
The high-strength high-heat-conductivity silicon nitride ceramic cutting tool comprises the following raw materials in percentage by mass: 80% of alpha-Si 3 N 4 Powder, 1% beta-Si 3 N 4 Seed crystal, 3% of rare earth oxide, 5% of rare earth oxide withDiamond of the metal coating and 11% of sintering aid;
other conditions were the same as in example 1.
Example 6
The high-strength high-heat-conductivity silicon nitride ceramic cutting tool comprises the following raw materials in percentage by mass: 80% of alpha-Si 3 N 4 Powder, 1% beta-Si 3 N 4 Seed crystal, 3% of rare earth oxide, 10% of diamond with a metal coating and 6% of sintering aid;
other conditions were the same as in example 1.
Example 7
The high-strength high-heat-conductivity silicon nitride ceramic cutting tool comprises the following raw materials in percentage by mass: 85% of alpha-Si 3 N 4 Powder, 0.5% beta-Si 3 N 4 Seed crystal, 4% of rare earth oxide, 6% of diamond with a metal coating and 4.5% of sintering aid;
other conditions were the same as in example 1.
Example 8
The high-strength high-heat-conductivity silicon nitride ceramic cutting tool comprises the following raw materials in percentage by mass: 85% of alpha-Si 3 N 4 Powder, 1% beta-Si 3 N 4 Seed crystal, 3% of rare earth oxide, 5% of diamond with a metal coating and 6% of sintering aid;
other conditions were the same as in example 1.
Example 9
The high-strength high-heat-conductivity silicon nitride ceramic cutting tool comprises the following raw materials in percentage by mass: 90% of alpha-Si 3 N 4 Powder, 0.8% beta-Si 3 N 4 Seed crystal, 2% of rare earth oxide, 5% of diamond with a metal coating and 2.5% of sintering aid;
other conditions were the same as in example 1.
Example 10
The high-strength high-heat-conductivity silicon nitride ceramic cutting tool comprises the following raw materials in percentage by mass: 90% of alpha-Si 3 N 4 Powder, 1% beta-Si 3 N 4 Seed crystal, 3% of rare earth oxide, 5% of diamond with a metal coating and 1% of sintering aid;
other conditions were the same as in example 1.
Comparative example 1
A silicon nitride ceramic cutting tool comprises the following raw materials in percentage by mass: 70% of alpha-Si 3 N 4 Powder, 4% of rare earth oxide, 5% of diamond with a metal coating and 21% of sintering aid;
other conditions were the same as in example 1.
Comparative example 2
A silicon nitride ceramic cutting tool comprises the following raw materials in percentage by mass: 70% of alpha-Si 3 N 4 Powder, 1% beta-Si 3 N 4 Seed crystal, 10% of diamond with metal coating and 19% of sintering aid;
other conditions were the same as in example 1.
Comparative example 3
A silicon nitride ceramic cutting tool comprises the following raw materials in percentage by mass: 70% of alpha-Si 3 N 4 Powder, 1% beta-Si 3 N 4 Seed crystal, 4% of rare earth oxide and 25% of sintering aid;
other conditions were the same as in example 1.
The performance of the high-strength and high-thermal conductivity silicon nitride ceramic cutting tools prepared in examples 1 to 10 and the performance of the silicon nitride ceramic cutting tools prepared in comparative examples 1 to 3 were tested, and the results are shown in table 1:
TABLE 1 Properties of high-strength, high-thermal conductivity silicon nitride ceramic cutting tools prepared in examples 1 to 10 and silicon nitride ceramic cutting tools prepared in comparative examples 1 to 3
As can be seen from the comparison of examples 1 to 10 with comparative examples 1 to 3, when the content of the raw material in the high-strength and high-thermal-conductivity silicon nitride ceramic cutting tool was adjusted, the properties thereof were also varied in a small degree, and when beta-Si was omitted 3 N 4 When seeded, results in alpha-Si during hot press sintering 3 N 4 Cannot be completely converted into beta-Si 3 N 4 Resulting in a decrease in the performance of the ceramic cutting tool; when the rare earth oxide is omitted, the strength, the hardness and the toughness of the ceramic cutting tool are reduced in different ranges, which shows that the mechanical property of the ceramic cutting tool can be greatly improved by adding the rare earth oxide; when the diamond having the metal coating layer is omitted, the cutting performance of the ceramic cutting tool is lowered, and the service life thereof is reduced, although the strength, hardness and toughness of the ceramic cutting tool are not greatly affected.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The high-strength high-heat-conductivity silicon nitride ceramic cutting tool is prepared from 70-90% of alpha-Si in percentage by mass 3 N 4 Powder, 0.5-1% beta-Si 3 N 4 Seed crystal, 2-5% of rare earth oxide, 5-10% of diamond with metal coating and the balance of sintering aid.
2. A high strength high thermal conductivity silicon nitride ceramic cutting tool according to claim 1, wherein the β -Si is 3 N 4 The length-diameter ratio of the seed crystal is (2-5): 1.
3. a high strength, high thermal conductivity silicon nitride ceramic cutting tool according to claim 1, wherein the rare earth oxide comprises Y 2 O 3 、La 2 O 3 、Yb 2 O 3 、Sc 2 O 3 、Ce 2 O 3 、Pr 2 O 3 、Nd 2 O 3 、Lu 2 O 3 、Tb 2 O 3 And Tm 2 O 3 At least one of (1).
4. A high-strength high-thermal conductivity silicon nitride ceramic cutting tool according to claim 1, wherein the diamond in the diamond with metal coating has a particle size of 10 to 100 μm.
5. The high-strength high-thermal-conductivity silicon nitride ceramic tool according to claim 1, wherein the material of the metal coating in the diamond with the metal coating is Ni or Ti, and the thickness of the metal coating is 50 to 300nm.
6. A high-strength high-thermal-conductivity silicon nitride ceramic cutting tool according to claim 1, wherein the sintering aid comprises MgO, al 2 O 3 And AlN.
7. The method for preparing the high-strength high-thermal conductivity silicon nitride ceramic cutting tool of any one of claims 1 to 6, comprising the following steps:
(1) Mixing the raw materials of the high-strength high-heat-conductivity silicon nitride ceramic cutter, and then carrying out ball milling to obtain a mixture;
(2) And (2) sequentially carrying out hot-pressing sintering and annealing treatment on the mixture obtained in the step (1) to obtain the high-strength high-heat-conductivity silicon nitride ceramic cutter.
8. The preparation method according to claim 7, wherein the pressure of the hot-pressing sintering in the step (2) is 10 to 50MPa, the temperature of the hot-pressing sintering is 1400 to 1900 ℃, and the time of the hot-pressing sintering is 20 to 180min.
9. The method according to claim 7, wherein the temperature of the annealing treatment in the step (2) is 950 to 1200 ℃ and the time of the annealing treatment is 30 to 120min.
10. Use of the high-strength high-thermal conductivity silicon nitride ceramic cutting tool according to any one of claims 1 to 6 or the high-strength high-thermal conductivity silicon nitride ceramic cutting tool prepared by the preparation method according to any one of claims 7 to 9 in cutting hard alloys.
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