CN103964861A - Production method for high-wear-resistance silicon nitride ceramic - Google Patents
Production method for high-wear-resistance silicon nitride ceramic Download PDFInfo
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- CN103964861A CN103964861A CN201310311553.4A CN201310311553A CN103964861A CN 103964861 A CN103964861 A CN 103964861A CN 201310311553 A CN201310311553 A CN 201310311553A CN 103964861 A CN103964861 A CN 103964861A
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Abstract
The invention discloses a production method for high-wear-resistance silicon nitride ceramic, and concretely relates to a production method for alpha-beta multiphase silicon nitride ceramic. The silicon nitride ceramic is characterized by comprising the following raw materials in percent by mass: 92% of silicon nitride, 5% of yttrium oxide and 3% of aluminium oxide. The production method is characterizing by comprising mixing the above compositions for blanking making, and employing a three-step air-pressure sintering technology for production; specifically, first step, sintering ceramic blanks at a low sintering temperature of 1600-1650 DEG C under a low pressure of 1 MPa in nitrogen atmosphere until pores are completely closed; second step, heightening the sintering temperature to 1750-1780 DEG C, increasing the nitrogen pressure to 6 MPa, and staying momently at the high temperature; and third step, rapidly cooling to a sintering temperature 1400-1450 DEG C with the cooling speed of 40 DEG C/min, and keeping warmth for a long time until sintering is compact. The produced silicon nitride ceramic has relatively good wear resistance.
Description
Technical field
The present invention relates to a kind of technical field of ceramic material, be specifically related to a kind of method that three step alternating temperature gas pressure sinterings are produced high abrasion silicon nitride ceramics.
Background technology
Silicon nitride (Si
3n
4) pottery has high strength, high-wearing feature, high temperature resistant, corrosion-resistant, acid-and base-resisting, can in seawater, use for a long time, and there is the superperformance of the exhausted magnetic of insulation.In the time of 800 DEG C, intensity, hardness are almost constant, and its density is 3.20g/cm
3, be almost 1/3 weight of bearing steel, when rotation, centrifugal force is little, can realize and running up.Also have self lubricity, it can use in the environment of unlubricated medium high pollution.Become ceramic bearing, the first-selected ball of hybrid ceramic ball bearing.For this reason, become as the wear resistance of the silicon nitride ceramics of bearing the important indicator that ceramist pays close attention to.
α phase silicon nitride, for waiting axle shape crystal formation, has higher hardness and heat-shock resistance, and beta phase silicon nitride is long column shape crystal formation, has higher intensity and toughness, and the former is low temperature modification, and the latter is high temperature modification.α phase and complementarity in the mutually microstructural difference of β and performance, make to prepare alpha-beta complex-phase silicon nitride ceramic and be expected to have more excellent performance.By improving the content of α phase in complex-phase silicon nitride ceramic, can in a big way, improve the wear resisting property of silicon nitride ceramics.Silicon nitride ceramics raw material is α phase, and α starts to change into β phase at 1450～1550 DEG C, and silicon nitride ceramics is lower in normal sintering temperature (1750～1800 DEG C) is β phase, is difficult to retain α phase.The application adopts three step alternating temperature gas pressure sintering methods to make α fail to be mutually transformed into β phase completely, thereby prepares alpha-beta complex-phase silicon nitride ceramic, and then improves its wear resistance.
Through the literature search to prior art, do not find to adopt three step alternating temperature gas pressure sintering methods to produce the report of alpha-beta complex-phase silicon nitride ceramic.
Summary of the invention
Technical problem to be solved by this invention is, improves the wear resistance of existing silicon nitride ceramics, and a kind of production method of alpha-beta complex-phase silicon nitride ceramic is provided.
The technical problem that will solve required for the present invention, can be achieved through the following technical solutions:
A production method for alpha-beta complex-phase silicon nitride ceramic, is characterized in that, the each component of described silicon nitride ceramics starting material and mass percentage content are: silicon nitride 92%, yttrium oxide 5%, aluminium sesquioxide 3%.In above-mentioned silicon nitride, α phase silicon nitride mass percentage content is greater than 94%, and yttrium oxide and aluminium sesquioxide purity (mass percent) are all greater than 99%.The particle diameter of above-mentioned each component is respectively: silicon nitride 0.4～0.6 μ m, yttrium oxide 1～3 μ m, aluminium sesquioxide 0.3～0.5 μ m.Above-mentioned each component is mixed to base, adopt three step gas pressure sintering explained hereafter, the first step, burns ceramic body to pore closure completely, 1600～1650 DEG C of sintering temperatures, nitrogen pressure 1MPa, soaking time 30～60min at low-temp low-pressure nitrogen atmosphere; Second step, heightens temperature, strengthens nitrogen pressure, at high temperature short stay, 1750～1780 DEG C of sintering temperatures, nitrogen pressure 6MPa, soaking time 10-15min; The 3rd step, cooling rapidly, insulation for a long time, 1400～1450 DEG C of sintering temperatures, nitrogen pressure 6MPa, soaking time 180～360min, is 40 DEG C/min by high temperature to the rate of temperature fall of low temperature, until densified sintering product.
Because the present invention has adopted three step alternating temperature gas pressure sintering methods, part α phase silicon nitride is not transformed into β phase, improves the wear resistance of silicon nitride ceramics.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach object and effect is easy to understand; elaborate below in conjunction with embodiments of the invention: the present embodiment is implemented under taking technical solution of the present invention as prerequisite; provided detailed embodiment and process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1:
Each component and mass percentage content are: silicon nitride 92%, yttrium oxide 5%, aluminium sesquioxide 3%.Above-mentioned each component is mixed to base, adopt three step gas pressure sintering explained hereafter, the first step, 1600 DEG C of sintering temperatures, nitrogen pressure 1MPa, under soaking time 60min condition, burns to pore completely closed by ceramic body; Second step, heightens temperature, strengthens nitrogen pressure, 1780 DEG C of sintering temperatures, and nitrogen pressure 6MPa, under soaking time 15min condition, short stay; The 3rd step, cooling rapidly, insulation for a long time, 1400 DEG C of sintering temperatures, nitrogen pressure 6MPa, under soaking time 180min condition, completes low-temperature sintering, is 40 DEG C/min, until densified sintering product by high temperature to the rate of temperature fall of low temperature.
The volume density of the alpha-beta complex-phase silicon nitride ceramic that the present embodiment obtains is 3.28g/cm
3, folding strength is 780MPa, microhardness is 16.8GPa.Wherein α phase silicon nitride mass percentage content is 25%.
Embodiment 2:
Each component and mass percentage content are: silicon nitride 92%, yttrium oxide 5%, aluminium sesquioxide 3%.Above-mentioned each component is mixed to base, adopt three step gas pressure sintering explained hereafter, the first step, 1650 DEG C of sintering temperatures, nitrogen pressure 1MPa, under soaking time 30min condition, burns to pore completely closed by ceramic body; Second step, heightens temperature, strengthens nitrogen pressure, 1750 DEG C of sintering temperatures, and nitrogen pressure 6MPa, under soaking time 15min condition, short stay; The 3rd step, cooling rapidly, insulation for a long time, 1450 DEG C of sintering temperatures, nitrogen pressure 6MPa, under soaking time 360min condition, completes low-temperature sintering, is 40 DEG C/min, until densified sintering product by high temperature to the rate of temperature fall of low temperature.
The volume density of the alpha-beta complex-phase silicon nitride ceramic that the present embodiment obtains is 3.29g/cm
3, folding strength is 790MPa, microhardness is 16.2GPa.Wherein α phase silicon nitride mass percentage content is 15%.
Embodiment 3:
Each component and mass percentage content are: silicon nitride 92%, yttrium oxide 5%, aluminium sesquioxide 3%.Above-mentioned each component is mixed to base, adopt three step gas pressure sintering explained hereafter, the first step, 1600 DEG C of sintering temperatures, nitrogen pressure 1MPa, under soaking time 60min condition, burns to pore completely closed by ceramic body; Second step, heightens temperature, strengthens nitrogen pressure, 1780 DEG C of sintering temperatures, and nitrogen pressure 6MPa, under soaking time 10min condition, short stay; The 3rd step, cooling rapidly, insulation for a long time, 1450 DEG C of sintering temperatures, nitrogen pressure 6MPa, under soaking time 240min condition, completes low-temperature sintering, is 40 DEG C/min, until densified sintering product by high temperature to the rate of temperature fall of low temperature.
The volume density of the alpha-beta complex-phase silicon nitride ceramic that the present embodiment obtains is 3.28g/cm
3, folding strength is 790MPa, microhardness is 16.6GPa.Wherein α phase silicon nitride mass percentage content is 22%.
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (2)
1. a production method for alpha-beta complex-phase silicon nitride ceramic, is characterized in that, the each component of described silicon nitride ceramics starting material and mass percentage content are: silicon nitride 92%, yttrium oxide 5%, aluminium sesquioxide 3%.In above-mentioned silicon nitride, α phase silicon nitride mass percentage content is greater than 94%, and yttrium oxide and aluminium sesquioxide purity (mass percent) are all greater than 99%.The particle diameter of above-mentioned each component is respectively: silicon nitride 0.4～0.6 μ m, yttrium oxide 1～3 μ m, aluminium sesquioxide 0.3～0.5 μ m.Above-mentioned each component is mixed to base, adopt three step gas pressure sintering explained hereafter.
2. the production method of a kind of alpha-beta complex-phase silicon nitride ceramic according to claim 1, is characterized in that, the first step, at low-temp low-pressure nitrogen atmosphere, ceramic body is burnt to pore completely closed, 1600～1650 DEG C of sintering temperatures, nitrogen pressure 1MPa, soaking time 30～60min; Second step, heightens temperature, strengthens nitrogen pressure, at high temperature short stay, 1750～1780 DEG C of sintering temperatures, nitrogen pressure 6MPa, soaking time 10-15min; The 3rd step, cooling rapidly, insulation for a long time, 1400～1450 DEG C of sintering temperatures, nitrogen pressure 6MPa, soaking time 180～360min, is 40 DEG C/min by high temperature to the rate of temperature fall of low temperature, until densified sintering product.
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| CN201310311553.4A CN103964861A (en) | 2013-07-23 | 2013-07-23 | Production method for high-wear-resistance silicon nitride ceramic |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104909764A (en) * | 2015-05-18 | 2015-09-16 | 上海海大技术转移有限公司 | Modified heterogeneous Sialon (Si-Al-O-N) ceramic and preparation method and use thereof |
| CN113880592A (en) * | 2021-11-08 | 2022-01-04 | 北京理工大学 | Preparation process of high-hardness high-toughness silicon nitride ceramic complex structural member |
-
2013
- 2013-07-23 CN CN201310311553.4A patent/CN103964861A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104909764A (en) * | 2015-05-18 | 2015-09-16 | 上海海大技术转移有限公司 | Modified heterogeneous Sialon (Si-Al-O-N) ceramic and preparation method and use thereof |
| CN113880592A (en) * | 2021-11-08 | 2022-01-04 | 北京理工大学 | Preparation process of high-hardness high-toughness silicon nitride ceramic complex structural member |
| CN113880592B (en) * | 2021-11-08 | 2022-07-05 | 北京理工大学 | Preparation process of high-hardness high-toughness silicon nitride ceramic complex structural member |
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Application publication date: 20140806 |