CN101486578B - Silicon nitride based nano complex gradient function ceramic tool material and preparation thereof - Google Patents
Silicon nitride based nano complex gradient function ceramic tool material and preparation thereof Download PDFInfo
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- CN101486578B CN101486578B CN2009100144609A CN200910014460A CN101486578B CN 101486578 B CN101486578 B CN 101486578B CN 2009100144609 A CN2009100144609 A CN 2009100144609A CN 200910014460 A CN200910014460 A CN 200910014460A CN 101486578 B CN101486578 B CN 101486578B
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Abstract
The invention provides a silicon nitride-based nano composite functionally gradient ceramic cutter material and a preparation method thereof. The ceramic cutter material is provided with a five-layer symmetrical gradient level structure; the component contents of the symmetrical layers relative to a central layer are the same and the thickness of each layer is consistent; the components of each layer are all micron Si3N4, nano Si3N4, nano TiC, nano TiN, Al2O3 and Y2O3. The preparation method thereof is as follows: (1) preparing materials according to the content of each component in each layer; (2) dispersing the nano materials in each layer; (3) mixing the other materials in each layer with the dispersed nano materials to obtain the powder material of a composite ceramic material which disperses excellently; and (4) employing a powder layering paving method and a hot pressing sintering technique to carry out loading and sintering. The invention improves the anti-bending intensity andthe fracture toughness property of the materials, and improves the fracture toughness property of the materials; while the gradients of the nano TiC and the nano TiN are arranged in layers, thus leading the mechanical property of the cutter material to be changed in stagewise gradient, and being capable of effectively easing the residual heat stress.
Description
Technical field
The present invention relates to a kind of silicon nitride based nano complex gradient function ceramic tool material and preparation method thereof, belong to the cutter material technical field.
Background technology
Ceramic cutting tool material is owing to have high rigidity, high-wearing feature, high heat resistance and high good performances such as chemical stability, in the high speed cutting field with cut aspect the difficult-to-machine material to compare at interior inserted tool with coated cutting tool and have than remarkable advantages.But ceramice kuife material based on nitrided silicon also has the weakness of itself, and is lower such as intensity and toughness, thermal expansivity is higher, thermal conductivity and heat-shock resistance are relatively poor, thereby limited its range of application.
Also this has been carried out at present both at home and abroad a large amount of research, adopt optimize sintering process, add second-phase, from toughening mechanisms, material is carried out the mechanical property that the toughened and reinforced mechanism of corresponding heat treatment and K cryogenic treatment etc. improves ceramic material.
And the appearance of nano material is so that the raising of ceramic cutting tool material performance has had bigger space, both domestic and external studies show that, in ceramic cutting tool material, add bending strength and fracture toughness that nano particle can the Effective Raise composite ceramic material, obviously improve its mechanical property and high-temperature behavior, such as human TiN particulate reinforcement Si such as J.L.Huang
3N
4Base pottery (.Microstructure such as J.L.Huang, fracture behavior and mechanical properties of TiN/Si
3N
4Composites, Mater.Chem.Phys., 1996,45 (3): 203-210), the human Si such as C.-Y.Chu
3N
4Crystal whisker toughened Si
3N
4Base pottery (the .High-Temperature Failure Mechanisms of Hot-Pressed Si such as C.-Y.Chu
3N
4And Si
3N
4/ Si
3N
4-Whisker-Reinforced Composites.J.Am.Ceram.Soc., 1993,76 (5): 1349-53).The interpolation nano particle can significantly improve the intensity of material, flexible improves then not obvious, even influence the raising of the strength of materials sometimes, therefore how obtaining high intensity and toughness simultaneously is the key point of exploitation silicon nitride based nano complex gradient ceramic material.TiC and TiN are with matrix Si
3N
4Compare have higher hardness, higher cross-breaking strength, the better thermal conductivity of oxidation resistance and Geng Gao, bending strength that can the Effective Raise silicon nitride ceramic material.
Simultaneously, in ceramic cutting tool material, introduce the thermal stresses that gradient-structure can obviously be alleviated ceramic cutting tool material, and the raising heat-shock resistance, as in Shandong Polytechnic Univ's doctorate papers in 1998 " manufacturing and designing and Study on Cutting Performance of novel gradient function ceramics cutter material " to the research of gradient function ceramic tool material.
Summary of the invention
The intensity that the present invention is directed to existing silicon nitride based nano complex gradient ceramic material existence improves significantly and the unconspicuous problem of toughness, a kind of have high strength, high tenacity and high-heat resistance shock resistant are provided, be fit to the silicon nitride based nano complex gradient function ceramic tool material of High-speed machining, a kind of this preparation methods is provided simultaneously.This ceramic cutting tool material combining nano wild phase keeps the original advantage of silicon nitride material simultaneously in the advantage that toughened and reinforced and gradient-structure have on the material high-heat resistance shock resistant,
Silicon nitride based nano complex gradient function ceramic tool material of the present invention has five layers of symmetric gradient hierarchical structure, constituent content is identical in the layer of central core symmetry relatively, each layer thickness is consistent, and the component of ground floor and layer 5 by volume percentage is 61.5% micron Si
3N
4, 20.5% nanometer Si
3N
4, 5% nano TiC, 5% nano TiN, 2% micron Al
2O
3With 6% the micron Y
2O
3, the component of the second layer and the 4th layer by volume percentage is 57.75% micron Si
3N
4, 19.25% nanometer Si
3N
4, 5% nano TiC, 10% nano TiN, 2% micron Al
2O
3With 6% Y
2O
3The micron, the 3rd layer component by volume percentage be 54% the micron Si
3N
4, 18% nanometer Si
3N
4, 10% nano TiC, 10% nano TiN, 2% micron Al
2O
3With 6% the micron Y
2O
3
The preparation method of above-mentioned silicon nitride based nano complex gradient function ceramic tool material may further comprise the steps:
(1) batching: every layer of each component volume ratio batching that according to the form below provides:
| Micron Si 3N 4 | Nanometer Si 3N 4 | Nano TiC | Nano TiN | Micron Al 2O 3 | Micron Y 2O 3 | |
| Ground floor | 61.5 | 20.5 | 5 | 5 | 2 | 6 |
| The second layer | 57.75 | 19.25 | 5 | 10 | 2 | 6 |
| The 3rd layer | 54 | 18 | 10 | 10 | 2 | 6 |
| The 4th layer | 57.75 | 19.25 | 5 | 10 | 2 | 6 |
| Layer 5 | 61.5 | 20.5 | 5 | 5 | 2 | 6 |
(2) dispersion of nano particle in each layer: take polymethylacrylic acid ammonia (PMAA-NH4) as dispersant, take deionized water as decentralized medium, with the nanometer Si in one deck
3N
4, nano TiC and nano TiN add respectively deionized water, being mixed with every kind of nano material, to account for mass fraction be 0.2% suspension, in suspension, add relatively every kind of nano material quality greater than 0 less than 3% dispersant, ultrasonic dispersion was stirred 30 minutes, the pH value of adjusting then suspension is 9.5 ~ 10, is placed at last on the ultrasonic dispersator to disperse 30 minutes again;
(3) batch mixing: with the micron Si in one deck
3N
4, Al
2O
3, Y
2O
3Mix with the suspension of scattered each nano material of this layer, be placed on and disperse on the ultrasonic dispersator to pour in the mixing tank after 30 minutes, ball milling is 72 hours on planetary ball mill, passes through vacuum drying again, sieves, and obtains finely disseminated composite ceramic material powder materials;
(4) charging and sintering: adopt the powder place Min layers to fill out method, five layers of gradient layer consistency of thickness adopt hot-pressing sintering technique, adopt high-purity nitrogen as protective atmosphere, and heat-up rate is 75 ℃/minute ~ 85 ℃/minute during sintering, and pressure slowly adds to 30MPa; The holding stage temperature is 1700 ℃ ~ 1800 ℃, pressure 30MPa, soaking time 30 minutes.
By above step, can make the silicon nitride based nano complex gradient function ceramic tool material that possesses high rigidity, high-flexural strength, high-fracture toughness and high-heat resistance shock resistant.
The present invention adopts the powder place Min layers to fill out method, forms sandwich construction, by to micron Si
3N
4The middle nanometer Si that adds
3N
4, nano TiC and nano TiN, the gradient of controlling every layer of nano TiC and nano TiN distributes, with Al
2O
3And Y
2O
3In order to when sintering, form liquid phase, optimize hot-pressing sintering technique as sintering aid, successfully prepare and have high performance silicon nitride based nano complex gradient function ceramic tool material.Nanometer Si
3N
4The adding of particle, refinement crystal grain, be conducive to form two peak structure, improved bending strength and the fracture toughness of material.Nano TiC that adds and nano TiN can play the effect of nucleus on the one hand, make nucleus quantity increase, can quarter in the crystal boundary of silicon nitride on the other hand, hinder the growth of silicon nitride grain, thereby crystal grain thinning, can also hinder simultaneously the expansion of tiny crack, improve the fracture toughness property of material.And the slice gradient of nano TiC and nano TiN distributes, and the mechanical property that makes cutter material is stepped change in gradient, can effectively alleviate residual thermal stress.The gained silicon nitride based nano complex gradient function ceramic tool material has the good mechanical performance.
Embodiment
Silicon nitride based nano complex gradient function ceramic tool material of the present invention has the symmetric gradient hierarchical structure, and the number of plies is 5 layers, and constituent content is identical in the layer of central core symmetry relatively, and each layer thickness is consistent, and the component in each layer is a micron Si
3N
4, nanometer Si
3N
4, nano TiC, nano TiN, micron Al
2O
3And Y
2O
3Micron.Five layers of symmetric gradient structure increase progressively successively from the top layer to center nano TiC and nano TiN content summation, are respectively 10%, 15%, 20%, each gradient layer Al
2O
3And Y
2O
3Cumulative volume content is 8%.
(vol%) is as shown in the table for the component concentration of five layers of gradient layer
| Micron Si 3N 4 | Nanometer Si 3N 4 | Nano TiC | Nano TiN | Micron Al 2O 3 | Micron Y 2O 3 | |
| Ground floor | 61.5 | 20.5 | 5 | 5 | 2 | 6 |
| The second layer | 57.75 | 19.25 | 5 | 10 | 2 | 6 |
| The 3rd layer | 54 | 18 | 10 | 10 | 2 | 6 |
| The 4th layer | 57.75 | 19.25 | 5 | 10 | 2 | 6 |
| Layer 5 | 61.5 | 20.5 | 5 | 5 | 2 | 6 |
The preparation process of silicon nitride based nano complex gradient function ceramic tool material of the present invention is as follows:
1. every layer of each the component volume ratio that provides by last table prepared burden;
2. the nano material in each layer is disperseed
Take deionized water as decentralized medium, preparation of nano Si
3N
4Mass fraction is 0.2% suspension, adds relative nanometer Si
3N
4Quality is greater than the polymethylacrylic acid ammonia of (optimum content be nano material quality 2%) 0 less than 3%, be placed on the ultrasonic dispersator and disperseed 30 minutes, the pH value of adjusting then suspension is 9.5～10, makes suspension be alkalescence and then ultrasonic dispersion 30 minutes.The dispersion of nano TiC and nano TiN powder and nanometer Si
3N
4Dispersion process the same.
3. with micron Si
3N
4With the nanometer Si that configures
3N
4, nano TiC, nano TiN suspension and Al
2O
3And Y
2O
3Mix, be placed on and disperse on the ultrasonic dispersator to pour in the mixing tank after 30 minutes, mixed 72 hours at planetary ball mill, pass through again vacuum drying, sieve, obtain finely disseminated nano composite powder material.
4. adopt the powder place Min layers method of filling out to carry out hot pressed sintering, each layer thickness equates.Hot-pressing sintering technique is, sintering in the high-purity nitrogen protective atmosphere, heat-up rate are 75 ~ 80 ℃/minute, and pressure slowly adds to 30MPa; The holding stage temperature is 1700 ~ 1800 ℃, pressure 30MPa, soaking time 30 minutes.
The mechanical property of the silicon nitride based nano complex gradient function ceramic tool material by said process preparation is: hardness 17 ~ 17.5GPa, bending strength 860 ~ 980Mpa, fracture toughness property 7 ~ 8.8MPaml/2.
Claims (3)
1. silicon nitride based nano complex gradient function ceramic tool material, have five layers of symmetric gradient hierarchical structure, constituent content is identical in the layer of central core symmetry relatively, and each layer thickness is consistent, it is characterized in that: the component of ground floor and layer 5 by volume percentage is 61.5% micron Si
3N
4, 20.5% nanometer Si
3N
4, 5% nano TiC, 5% nano TiN, 2% micron Al
2O
3With 6% the micron Y
2O
3, the component of the second layer and the 4th layer by volume percentage is 57.75% micron Si
3N
4, 19.25% nanometer Si
3N
4, 5% nano TiC, 10% nano TiN, 2% micron Al
2O
3With 6% the micron Y
2O
3, the 3rd layer component by volume percentage be 54% the micron Si
3N
4, 18% nanometer Si
3N
4, 10% nano TiC, 10% nano TiN, 2% micron Al
2O
3With 6% the micron Y
2O
3
2. the preparation method of the described silicon nitride based nano complex gradient function ceramic tool material of claim 1 may further comprise the steps:
(1) batching: every layer of each component volume ratio batching that according to the form below provides:
(2) dispersion of nano particle in each layer: take polymethylacrylic acid ammonia (PMAA-NH4) as dispersant, take deionized water as decentralized medium, with the nanometer Si in one deck
3N
4, nano TiC and nano TiN add respectively deionized water, being mixed with every kind of nano material, to account for mass fraction be 0.2% suspension, in suspension, add relatively every kind of nano material quality greater than 0 less than 3% dispersant, ultrasonic dispersion was stirred 30 minutes, the pH value of adjusting then suspension is 9.5～10, is placed at last on the ultrasonic dispersator to disperse 30 minutes again;
(3) batch mixing: with the micron Si in one deck
3N
4, Al
2O
3, Y
2O
3Mix with the suspension of scattered each nano material of this layer, be placed on and disperse on the ultrasonic dispersator to pour in the mixing tank after 30 minutes, ball milling is 72 hours on planetary ball mill, passes through vacuum drying again, sieves, and obtains finely disseminated composite ceramic material powder materials;
(4) charging and sintering: adopt the powder place Min layers to fill out method, five layers of gradient layer consistency of thickness adopt hot-pressing sintering technique, adopt high-purity nitrogen as protective atmosphere, and heat-up rate is 75 ℃/minute～85 ℃/minute during sintering, and pressure slowly adds to 30MPa; The holding stage temperature is 1700 ℃～1800 ℃, pressure 30MPa, soaking time 30 minutes.
3. the preparation method of silicon nitride based nano complex gradient function ceramic tool material according to claim 2 is characterized in that: the content of dispersion agent is 2% of nano material quality in the described step (2).
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| CN103992100A (en) * | 2014-06-10 | 2014-08-20 | 山东理工大学 | Process for preparing layered silicon nitride ceramic with high strength and high toughness by utilizing component gradient design |
| CN106431361B (en) * | 2016-10-31 | 2019-03-05 | 东南大学 | A kind of self-lubrication ceramic cutter material adding alumina-coated graphene |
| CN108046808B (en) * | 2018-01-05 | 2020-08-11 | 广东工业大学 | Si3N4Gradient material and preparation method thereof |
| CN109160816A (en) * | 2018-08-27 | 2019-01-08 | 广东工业大学 | A kind of symmetrical and consecutive variations tough silicon nitride graded ceramics of table hard-core and its preparation method and application |
| CN109761622A (en) * | 2019-03-27 | 2019-05-17 | 广东工业大学 | A kind of silicon nitride base gradient composite material and preparation method thereof based on outfield ancillary technique |
| CN112479721B (en) * | 2020-10-30 | 2022-07-15 | 江苏材睿科技有限公司 | High-toughness low-resistance silicon nitride ceramic and preparation method thereof |
| CN114835501B (en) * | 2022-05-19 | 2023-06-23 | 广东工业大学 | Silicon nitride-based textured gradient material and preparation method and application thereof |
| CN115196973B (en) * | 2022-06-29 | 2023-10-17 | 苏州玄陶商务咨询有限公司 | Multilayer silicon nitride ceramic implant and method for making same |
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