CN103739292A - Method for preparing silicon nitride-tungsten carbide titanium nano-composite ceramic cutting tool material - Google Patents

Method for preparing silicon nitride-tungsten carbide titanium nano-composite ceramic cutting tool material Download PDF

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CN103739292A
CN103739292A CN201410001211.7A CN201410001211A CN103739292A CN 103739292 A CN103739292 A CN 103739292A CN 201410001211 A CN201410001211 A CN 201410001211A CN 103739292 A CN103739292 A CN 103739292A
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nanometer
micron
composite ceramic
silicon nitride
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赵军
田宪华
刘帅
宫兆超
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Shandong University
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Abstract

The invention belongs to the technical field of material science, and particularly relates to a method for preparing a silicon nitride-tungsten carbide titanium nano-composite ceramic cutting tool material. The method is characterized in that proper amount of nanoscale alpha-Si3N4 and micron-sized (W, Ti) C powder are added into micron-sized alpha-Si3N4 matrix, Al2O3 and Y2O3 are taken as sintering aid, the compound powder is sintered in vacuum environment by hot pressed sintering technologies of temperature rise section by section and uniform heating. The nano-composite ceramic cutting tool material has high hardness, bending strength and fracture toughness, good wear resistance and high temperature stability. The gradient nano-composite ceramic material is applicable to manufacturing cutting tools and nozzles having high requirement on high temperature resistance and wear resistance.

Description

A kind of preparation method of silicon nitride-silicon carbide tungsten titanium nano composite ceramic cutter material
Technical field
The invention belongs to technical field of ceramic material, relate to a kind of preparation method of silicon nitride-silicon carbide tungsten titanium nano composite ceramic cutter material.
Background technology
Machining is prevailing working method in machinery manufacturing industry, the development of cutter material plays a decisive role to the progress of machining, sintex has the advantages such as high wear resistance, thermotolerance, oxidation-resistance because of it, since the eighties, make a breakthrough, ceramic cutting tool material will become one of topmost cutter material of Construction Technologies in Twenty-one Century.Silicon nitride ceramics, owing to having a series of premium propertiess such as high strength, high-heat resistance shock resistant, high-wearing feature, chemical stability, be widely used in cutting tool, but its hardness and fracture toughness is lower.
In stupalith, add nano particle can effectively improve the bending strength of composite ceramic material and fracture toughness (Sternitzke M..Review:Structural Ceramic Nanocomposites[J] .J.Eur.Ceram.Soc, 1997,17:1061-1082), and obviously improve its high-temperature behavior (Li Guanghai, Jiang'an is complete, Zhang Lide. add nanometer to the impact of ceramic toughening and enhancing [J]. Acta Metallurgica Sinica, 1996,32 (12): 1285-1288).At micron Si 3n 4in matrix, add nanometer Si 3n 4particle, is conducive to crystal grain thinning, promotes β-Si 3n 4formation, promote body material long column shape class whisker crystal grain diameter size to be bimodal distribution feature, improve bending strength and the fracture toughness of material.In silicon nitride matrix material, add SiC particle can obviously improve its bending strength, but hardness and toughness still very limited (Hirano T, Niihara K.Microstructure and mechanical properties of Si 3n 4/ SiC composites[J] .Mater Lett, 1995,22 (5): 249-254.).When adding TiN particle, can obviously improve intensity and the toughness of silicon nitride ceramics, but hardness lower (Zou B still, Huang C, Chen M, et al.Study of the mechanical properties, toughening and strengthening mechanisms of Si 3n 4/ Si 3n 4w/TiN nanocomposite ceramic tool materials[J] .Acta Mater, 2007,55 (12): 4193-4202.).
Therefore, how to obtain high intensity, toughness and hardness, be the key point of exploitation silicon nitride based nano composite ceramic material simultaneously.
Summary of the invention
The object of the invention is to overcome above-mentioned the deficiencies in the prior art, by in micron order silicon nitride matrix, add appropriate nanophase silicon nitride and wild phase tungsten carbide, a kind of preparation method of silicon nitride-silicon carbide tungsten titanium nano composite ceramic cutter material is provided, and preparation has the silicon nitride-silicon carbide tungsten titanium nano composite ceramic cutter material of high strength, high rigidity, high tenacity and good high-temperature stability.
The present invention is achieved in the following ways.
A preparation method for silicon nitride-silicon carbide tungsten titanium nano composite ceramic cutter material, is characterized in that comprising the following steps:
(1) preparation of raw material: use dehydrated alcohol as medium, respectively to micron α-Si 3n 4, nanometer α-Si 3n 4, micron Al 2o 3and micron (W, Ti) C raw material powder, carry out ball milling, to break up larger agglomerating particles, obtain more uniform powder, to pass through afterwards vacuum-drying, sieve, encapsulation is with standby;
(2) dispersion of nano particle: the good nanometer α-Si of ball milling in applying step (1) 3n 4powder, dispersion process be take dehydrated alcohol as dispersion medium, adds relative nanometer α-Si 3n 4quality is the polyoxyethylene glycol that 0.5% molecular weight is 4000, is mixed with suspension; Adopt ammonia water titration method that the pH value of suspension is adjusted into 9.5～10, make suspension be alkalescence; Then be placed on ultrasonic dispersator and disperse 25～30 minutes, obtain finely disseminated α-Si 3n 4suspension;
(3) batch mixing: by volume per-cent is prepared burden, wherein sintering aid Y 2o 3with Al 2o 3be fixed as respectively 4.8% and 3.2%, (W, Ti) C is 10～30%; Nanometer and micron α-Si 3n 4powder total amount is 62～82%, and nanometer α-Si wherein 3n 4in alpha-silicon nitride powders, proportion is 20～50%; By the good nano grade alpha-Si of ball milling in step (1) 3n 4, (W, Ti) C powder and Y 2o 3, Al 2o 3the suspension of the nano material that powder is scattered with step (2) mixes, be placed on ultrasonic dispersator and disperse to pour in mixing tank after 15～20 minutes, ball milling on ball mill, so that each phase material mixing is more even, pass through again vacuum-drying, sieve, obtain finely disseminated composite ceramic material powder materials;
(4) charging and sintering: pack the composite ceramic material powder mixing into graphite jig, in vacuum environment, the hot-pressing sintering technique that adopt segmentation temperature rise, evenly pressurizes; During in room temperature～1200 ℃, heat-up rate is 90～100 ℃/min, and pressure adds to 8Mpa; During from 1200 ℃ to 1700 ℃, heat-up rate is 45～50 ℃/min, and pressure evenly adds to 30MPa; Heat-insulation pressure keeping phase temperature is 1700 ℃, and pressure is 30MPa, and the heat-insulation pressure keeping time is 45min, cools to afterwards room temperature with the furnace.
By above step, can make even particle size distribution, bending strength is high, fracture toughness property good, hardness is high and the silicon nitride-silicon carbide tungsten titanium nano composite ceramic cutter material of excellent high performance.
This preparation method passes through at micron-sized α-Si 3n 4in matrix, add nanometer alpha-Si 3n 4(W, Ti) C solid-solution powder, and control nanometer α-Si 3n 4particle and micron α-Si 3n 4the content of the proportion of particle and (W, Ti) C, with Y 2o 3, Al 2o 3for sintering agent, the vacuum hot pressing sintering technique that adopt segmentation temperature rise, evenly pressurizes.Nanometer α-Si 3n 4the introducing of particle, refinement crystal grain, be conducive to promote β-Si 3n 4formation, promote body material long column shape class whisker crystal grain diameter size to be bimodal distribution feature, improve bending strength and the fracture toughness property of material; (W, Ti) C particle in raw material, when effectively improving material hardness, suppresses β-Si 3n 4too grow up, promote the generation of material transgranular fracture, improved the fracture toughness property of material.Prepared nano composite ceramic cutter material has good mechanical property.This nanocomposite ceramic material is suitable for making metal cutting tool that high temperature and wear resistance have relatively high expectations, nozzle etc.
Embodiment
Provide three most preferred embodiments of the present invention below.
Embodiment mono-
Submicron alpha-Si 3n 4(0.5 μ m)+nanometer α-Si 3n 4(25nm)+micron (W, Ti) C (1 μ m), in nano composite material, the content of each component (volume percent) is: 54% micron of α-Si 3n 4, 18% nanometer α-Si 3n 4, 4.8% high-purity Y 2o 3, 3.2% micron of Al 2o 3, 20% micron of (W, Ti) C.
The preparation process of gradient nano composite ceramic tool material of the present invention is as follows:
1. the preparation of raw material: use dehydrated alcohol as medium, respectively to micron α-Si 3n 4, nanometer α-Si 3n 4, micron Al 2o 3and micron (W, Ti) C raw material powder, carrying out ball milling, mechanical milling process carries out on planetary ball mill.α-Si wherein 3n 4, Al 2o 3powder ball milling 24h, to break up larger agglomerating particles, obtains more uniform powder, and (W, Ti) C powder ball milling 240h, to reduce powder diameter to 1 μ m left and right, passes through afterwards vacuum-drying, sieves, and encapsulation is with standby;
2. pair nanometer powder disperses: the good nanometer α-Si of ball milling in applying step (1) 3n 4powder, dispersion process be take dehydrated alcohol as dispersion medium, adds relative nanometer α-Si 3n 4quality is the polyoxyethylene glycol that 0.5% molecular weight is 4000, is mixed with nanometer α-Si 3n 4the massfraction suspension that is 0.2%; Adopt ammonia water titration method that the pH value of suspension is adjusted into 9.5～10, make suspension be alkalescence; Then be placed on ultrasonic dispersator and disperse 30 minutes;
3. batch mixing: by volume per-cent is prepared burden, wherein sintering aid Y 2o 3with Al 2o 3be fixed as respectively 4.8% and 3.2%, (W, Ti) C is 20%, micron α-Si 3n 4be 54%, nanometer α-Si 3n 4be 18%; By the good nano grade alpha-Si of ball milling in step (1) 3n 4, (W, Ti) C powder and Y 2o 3, Al 2o 3the suspension of the nano material that powder is scattered with step (2) mixes, be placed on ultrasonic dispersator and disperse to pour in mixing tank after 15～20 minutes, ball milling on ball mill, so that each phase material mixing is more even, pass through again vacuum-drying, sieve, obtain finely disseminated composite ceramic material powder materials;
4. feed and sintering: pack the composite ceramic material powder mixing into graphite jig, in vacuum environment, the hot-pressing sintering technique that adopt segmentation temperature rise, evenly pressurizes; During in room temperature～1200 ℃, heat-up rate is 90～100 ℃/min, and pressure adds to 8Mpa; During from 1200 ℃ to 1700 ℃, heat-up rate is 45～50 ℃/min, and pressure evenly adds to 30MPa; Heat-insulation pressure keeping phase temperature is 1700 ℃, and pressure is 30MPa, and the heat-insulation pressure keeping time is 45min, cools to afterwards room temperature with the furnace.
The mechanical property of the gradient nano composite ceramic tool material of preparing by said process is: bending strength 907～1050MPa, fracture toughness property 7.3～9.2MPam 1/2, Vickers' hardness 17.3～18.2GPa.
Embodiment bis-
Submicron alpha-Si 3n 4(0.5 μ m)+nanometer α-Si 3n 4(25nm)+micron (W, Ti) C (1 μ m), in nano composite material, the content of each component (volume percent) is: 57.75% micron of α-Si 3n 4, 19.25% nanometer α-Si 3n 4, 4.8% high-purity Y 2o 3, 3.2% micron of Al 2o 3, 15% micron of (W, Ti) C.
The preparation process of gradient nano composite ceramic tool material of the present invention is as follows:
1. the preparation of raw material: use dehydrated alcohol as medium, respectively to micron α-Si 3n 4, nanometer α-Si 3n 4, micron Al 2o 3and micron (W, Ti) C raw material powder, carrying out ball milling, mechanical milling process carries out on planetary ball mill.α-Si wherein 3n 4, Al 2o 3powder ball milling 24h, to break up larger agglomerating particles, obtains more uniform powder, and (W, Ti) C powder ball milling 240h, to reduce powder diameter to 1 μ m left and right, passes through afterwards vacuum-drying, sieves, and encapsulation is with standby;
2. pair nanometer powder disperses: the good nanometer α-Si of ball milling in applying step (1) 3n 4powder, dispersion process be take dehydrated alcohol as dispersion medium, adds relative nanometer α-Si 3n 4quality is the polyoxyethylene glycol that 0.5% molecular weight is 4000, is mixed with nanometer α-Si 3n 4the massfraction suspension that is 0.2%; Adopt ammonia water titration method that the pH value of suspension is adjusted into 9.5～10, make suspension be alkalescence; Then be placed on ultrasonic dispersator and disperse 30 minutes;
3. batch mixing: by volume per-cent is prepared burden, wherein sintering aid Y 2o 3with Al 2o 3be fixed as respectively 4.8% and 3.2%, (W, Ti) C is 15%, micron α-Si 3n 4be 57.75%, nanometer α-Si 3n 4be 19.25%; By the good nano grade alpha-Si of ball milling in step (1) 3n 4, (W, Ti) C powder and Y 2o 3, Al 2o 3the suspension of the nano material that powder is scattered with step (2) mixes, be placed on ultrasonic dispersator and disperse to pour in mixing tank after 15～20 minutes, ball milling on ball mill, so that each phase material mixing is more even, pass through again vacuum-drying, sieve, obtain finely disseminated composite ceramic material powder materials;
4. feed and sintering: pack the composite ceramic material powder mixing into graphite jig, in vacuum environment, the hot-pressing sintering technique that adopt segmentation temperature rise, evenly pressurizes; During in room temperature～1200 ℃, heat-up rate is 90～100 ℃/min, and pressure adds to 8Mpa; During from 1200 ℃ to 1700 ℃, heat-up rate is 45～50 ℃/min, and pressure evenly adds to 30MPa; Heat-insulation pressure keeping phase temperature is 1700 ℃, and pressure is 30MPa, and the heat-insulation pressure keeping time is 45min, cools to afterwards room temperature with the furnace.
The mechanical property of the gradient nano composite ceramic tool material of preparing by said process is: bending strength 830～950MPa, fracture toughness property 7.8～9.1MPam 1/2, Vickers' hardness 17.0～17.4GPa.
Embodiment tri-
Submicron alpha-Si 3n 4(0.5 μ m)+nanometer α-Si 3n 4(25nm)+micron (W, Ti) C (1 μ m), in nano composite material, the content of each component (volume percent) is: 50.25% micron of α-Si 3n 4, 16.75% nanometer α-Si 3n 4, 4.8% high-purity Y 2o 3, 3.2% micron of Al 2o 3, 20% micron of (W, Ti) C.
The preparation process of gradient nano composite ceramic tool material of the present invention is as follows:
1. the preparation of raw material: use dehydrated alcohol as medium, respectively to micron α-Si 3n 4, nanometer α-Si 3n 4, micron Al 2o 3and micron (W, Ti) C raw material powder, carrying out ball milling, mechanical milling process carries out on planetary ball mill.α-Si wherein 3n 4, Al2O3 powder ball milling 24h to be to break up larger agglomerating particles, obtains more uniform powder, (W, Ti) C powder ball milling 240h, to reduce powder diameter to 1 μ m left and right, afterwards through vacuum-drying, sieve, encapsulation is with standby;
2. pair nanometer powder disperses: the good nanometer α-Si of ball milling in applying step (1) 3n 4powder, dispersion process be take dehydrated alcohol as dispersion medium, adds relative nanometer α-Si 3n 4quality is the polyoxyethylene glycol that 0.5% molecular weight is 4000, is mixed with nanometer α-Si 3n 4the massfraction suspension that is 0.2%; Adopt ammonia water titration method that the pH value of suspension is adjusted into 9.5～10, make suspension be alkalescence; Then be placed on ultrasonic dispersator and disperse 30 minutes;
3. batch mixing: by volume per-cent is prepared burden, wherein sintering aid Y 2o 3with Al 2o 3be fixed as respectively 4.8% and 3.2%, (W, Ti) C is 25%, and micron α-Si3N4 is 50.25%, nanometer α-Si 3n 4be 16.75%; By the good nano grade alpha-Si of ball milling in step (1) 3n 4, (W, Ti) C powder and Y 2o 3, Al 2o 3the suspension of the nano material that powder is scattered with step (2) mixes, be placed on ultrasonic dispersator and disperse to pour in mixing tank after 15～20 minutes, ball milling on ball mill, so that each phase material mixing is more even, pass through again vacuum-drying, sieve, obtain finely disseminated composite ceramic material powder materials;
4. feed and sintering: pack the composite ceramic material powder mixing into graphite jig, in vacuum environment, the hot-pressing sintering technique that adopt segmentation temperature rise, evenly pressurizes; During in room temperature～1200 ℃, heat-up rate is 90～100 ℃/min, and pressure adds to 8Mpa; During from 1200 ℃ to 1700 ℃, heat-up rate is 45～50 ℃/min, and pressure evenly adds to 30MPa; Heat-insulation pressure keeping phase temperature is 1700 ℃, and pressure is 30MPa, and the heat-insulation pressure keeping time is 45min, cools to afterwards room temperature with the furnace.
The mechanical property of the gradient nano composite ceramic tool material of preparing by said process is: bending strength 785～880MPa, fracture toughness property 7.8～9.3MPam 1/2, Vickers' hardness 17.4～18.5GPa.

Claims (3)

1. a preparation method for silicon nitride-silicon carbide tungsten titanium nano composite ceramic cutter material, its feature comprises the following steps:
(1) preparation of raw material: use dehydrated alcohol as medium, respectively to micron α-Si 3n 4, nanometer α-Si 3n 4, micron Al 2o 3and micron (W, Ti) C raw material powder, carry out ball milling, to pass through afterwards vacuum-drying, sieve, encapsulation is with standby;
(2) dispersion of nano particle: the good nanometer α-Si of ball milling in applying step (1) 3n 4powder, dispersion process be take dehydrated alcohol as dispersion medium, adds relative nanometer α-Si 3n 4quality is the polyoxyethylene glycol that 0.5% molecular weight is 4000, is mixed with nanometer α-Si 3n 4the massfraction suspension that is 0.2%; Adopt ammonia water titration method that the pH value of suspension is adjusted into 9.5～10, make suspension be alkalescence; Then be placed on ultrasonic dispersator and disperse, obtain finely disseminated α-Si 3n 4suspension;
(3) batch mixing: by volume per-cent is prepared burden, wherein sintering aid Y 2o 3with Al 2o 3be fixed as respectively 4.8% and 3.2%, (W, Ti) C is 10～30%, nanometer and micron α-Si 3n 4powder total amount is 62～82%, and nanometer α-Si wherein 3n 4in alpha-silicon nitride powders, proportion is 20～50%; By the good nano grade alpha-Si of ball milling in step (1) 3n 4, (W, Ti) C powder and Y 2o 3, Al 2o 3the suspension of the nano material that powder is scattered with step (2) mixes, be placed on after being uniformly dispersed on ultrasonic dispersator and pour in mixing tank, ball milling on ball mill, then through vacuum-drying, sieve, obtain finely disseminated composite ceramic material powder materials;
(4) charging and sintering: the raw material powder mixing is packed in graphite jig into the hot-pressing sintering technique that adopt segmentation temperature rise in vacuum environment, evenly pressurizes; During in room temperature～1200 ℃, heat-up rate is 90～100 ℃/min, and pressure adds to 8Mpa; During from 1200 ℃ to 1700 ℃, heat-up rate is 45～50 ℃/min, and pressure steadily evenly adds to 30MPa; Heat-insulation pressure keeping phase temperature is 1700 ℃, and pressure is 30MPa, and the heat-insulation pressure keeping time is 45min, cools to afterwards room temperature with the furnace.
2. the preparation method of a kind of silicon nitride-silicon carbide tungsten titanium nano composite ceramic cutter material according to claim 1, is characterized in that: in step (1), and micron α-Si 3n 4, nanometer α-Si 3n 4with micron Al 2o 3powder ball milling 24h, to break up larger agglomerating particles, obtains more uniform powder; (W, Ti) C powder ball milling 240h, to reduce powder diameter to 1 μ m left and right; In step (3), Ball-milling Time is 48 hours.
3. the preparation method of a kind of silicon nitride-silicon carbide tungsten titanium nano composite ceramic cutter material according to claim 1, is characterized in that in step (3), wild phase (W, Ti) C optimum content is volume fraction 15% and 20%; Nanometer α-Si in step (3) 3n 4powder shared optimum proportion in alpha-silicon nitride powders is 25%.
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CN104446481A (en) * 2014-10-29 2015-03-25 安徽省皖捷液压科技有限公司 Non-phosphorus ceramic nozzle and manufacturing method thereof
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CN105801120A (en) * 2016-03-03 2016-07-27 刘佩佩 Tungsten carbide-tungsten silicide-tungsten nitride compound ceramic material and preparation method thereof
CN106316398A (en) * 2016-08-17 2017-01-11 齐鲁工业大学 Tungsten titanium carbide-based ceramic tool material added with cubic boron nitride and preparation method of material
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CN115386759A (en) * 2022-08-26 2022-11-25 西安工业大学 Ti (C7, N3)/TiB 2/WC micro-nano composite metal ceramic cutter material and preparation method thereof

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CN114538930B (en) * 2022-03-23 2023-01-17 山东大学 Crack self-healing gradient functional ceramic cutter material and preparation method thereof
CN115386759A (en) * 2022-08-26 2022-11-25 西安工业大学 Ti (C7, N3)/TiB 2/WC micro-nano composite metal ceramic cutter material and preparation method thereof
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Application publication date: 20140423