CN101555141A - Preparation method of silicon nitride ceramic - Google Patents
Preparation method of silicon nitride ceramic Download PDFInfo
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- CN101555141A CN101555141A CNA2009100152361A CN200910015236A CN101555141A CN 101555141 A CN101555141 A CN 101555141A CN A2009100152361 A CNA2009100152361 A CN A2009100152361A CN 200910015236 A CN200910015236 A CN 200910015236A CN 101555141 A CN101555141 A CN 101555141A
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Abstract
The invention relates to a preparation method of a silicon nitride ceramic, which belongs to the technical field of the special ceramic. The method comprises the following steps of blending, molding and burning and is characterized in that the silicon nitride ceramic comprises the following components of 82-88 percent of alpha-Si3N4 powder, 5-10 percent of AL2O3, 3-6 percent of ZrO2 and 1-3 percent of Y2O3 by weight; the components are evenly mixed by ball milling by taking water as the medium, then the polyvinyl alcohol with 0.8-1.2 percent of the total component weight is added in for mixing for 1-5-3 hours to obtain pulp, the pulp is dried for granulation, and the isostatic compaction is performed at the pressure of 110-180 MPa to obtain blank; the blank is loaded in a nitriding furnace and is protected in the nitrogen atmosphere, and the burnt temperature is controlled between 1550-1720 DEG C. The invention is low in cost, is easy for realization of the industrialization production and extends the application range.
Description
Technical field
The present invention relates to a kind of preparation method of silicon nitride ceramics, belong to special cermacis radix field.
Background technology
Silicon nitride ceramics has excellent performance as a kind of high-temperature structural ceramics, and at high temperature, at a high speed, have special use value in the strong corrosive medium, Chinese scholars is competitively launched the research and development to silicon nitride ceramic material, and its range of application is constantly enlarged.
Because silicon nitride is the strong covalent bond compound, self-diffusion coefficient is very low, only has when sintering temperature during near the silicon nitride decomposition temperature, enough ion migration velocities are just arranged, so solid-phase sintering is difficult to obtain the silicon nitride ceramics of densification.Therefore the normal oxidesintering auxiliary agent that adds, at high temperature the silicon-dioxide on itself and top layer and silicon nitride reaction generate oxynitride liquid phase acceleration of sintering, but these liquid phases often are present between the silicon nitride grain with amorphous glassy phase or crystal boundary precipitated phase in process of cooling, influenced the performance of silicon nitride ceramics to a great extent, in order to obtain the high-performance silicon nitride ceramic material, usually adopt hot-pressing sintering technique, the big cost height of this process energy consumption, and can only make the fairly simple goods of shape, be difficult to realize industrialization, the Application Areas of silicon nitride ceramics is restricted.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of silicon nitride ceramics, cost is low, is easy to realize industrialization production, widens its Application Areas.
The preparation method of silicon nitride ceramics of the present invention comprises batching, moulding and burns till, and its ingredients by weight percentage composition is:
α-Si
3N
4Powder 82-88%, AL
2O
35-10%, ZrO
23-6% and Y
2O
31-3%.
Wherein:
α-Si
3N
4In the α phase content require＞88%.
The batching particle diameter is controlled to be respectively: α-Si
3N
42-30 μ m, AL
2O
31-3 μ m, ZrO
20.5-1 μ m and Y
2O
31-2 μ m.
To prepare burden with water to after the medium ball milling mixes, the polyvinyl alcohol mixing that adds 0.8-1.2% again obtained slurry in 1.5-3 hour, the oven dry granulation, and granulation is controlled between the 60-120 mesh sieve, and isostatic pressing gets base substrate under 110-180Mpa pressure.
Base substrate is packed in the nitriding furnace, and with nitrogen atmosphere protection, the control firing temperature is 1550-1720 ℃, and soaking time is 3-10 hour.
The present invention is take zirconia, aluminium oxide, yittrium oxide as sinter additives, different from the sintering agent that prior art adopts, can ensure to form the Y-Si-Al-O-Zr-N liquid phase, make silicon nitride ceramic material obtain at a lower temperature best minute-pressure sintering, because this liquid phase viscosity height makes β-Si
3N
4Particle along the C axle grow to form high length through than, and the intergranular liquid phase is present in Si more
3N
4Grain boundaries is easy to separate out the little crystal grain of secondary in heating and cooling process, give the serviceability of silicon nitride ceramics excellence, is easy to industrialization production, and cost is low, and the good product performance of acquisition has been widened the application of product.The product performance index that obtains is as follows:
Density:＞3.0g/cm
3
Normal temperature bending strength:＞850MPa
1000 ℃ of bending strength:＞800MPa
Hardness: Hv＞1950kg/mm
3
Fracture toughness property:＞5.5MPa.m
1/2
The hardness height, fracture toughness property is good, the high temperature use properties is good.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
The preparation method of silicon nitride ceramics of the present invention comprises batching, moulding and burns till, and its ingredients by weight percentage composition is:
α-Si
3N
4Powder 85%, AL
2O
310%, ZrO
24% and Y
2O
31%.
Wherein:
α-Si
3N
4In the α phase content be 90%.
The batching particle diameter is controlled to be respectively: α-Si
3N
42-30 μ m, AL
2O
31-3 μ m, ZrO
20.5-1 μ m and Y
2O
31-2 μ m.
To prepare burden with water to after the medium ball milling mixes; adding 1.0% polyvinyl alcohol again mixes and obtained slurry in 2 hours; the oven dry granulation; granulation is controlled between the 60-120 mesh sieve; isostatic pressing gets base substrate under 150Mpa pressure; burn till under 1650 ℃ of temperature, nitrogen atmosphere protection the oven dry back, is incubated 3 hours.
The silicon nitride ceramics technical target of the product that obtains is: density 3.05g/cm
3, normal temperature bending strength 880MPa, 1000 ℃ of bending strength 850Mpa, hardness Hv1995kg/mm
2, fracture toughness property 5.9MPa.m
1/2
Embodiment 2
The preparation method of silicon nitride ceramics of the present invention comprises batching, moulding and burns till, and its ingredients by weight percentage composition is:
α-Si
3N
4Powder 86%, AL
2O
38%, ZrO
24% and Y
2O
32%.
Wherein:
α-Si
3N
4In the α phase content be 89%.
The batching particle diameter is controlled to be respectively: α-Si
3N
42-30 μ m, AL
2O
31-3 μ m, ZrO
20.5-1 μ m and Y
2O
31-2 μ m.
To prepare burden with water to after the medium ball milling mixes; adding 1.1% polyvinyl alcohol again mixes and obtained slurry in 2.5 hours; the oven dry granulation; granulation is controlled between the 60-120 mesh sieve; isostatic pressing gets base substrate under 150Mpa pressure; burn till under 1700 ℃ of temperature, nitrogen atmosphere protection the oven dry back, is incubated 3 hours.
The silicon nitride ceramics technical target of the product that obtains is: density 3.09g/cm
3, normal temperature bending strength 910MPa, 1000 ℃ of bending strength 890Mpa, hardness Hv2110kg/mm
2, fracture toughness property 5.9MPa.m
1/2
Embodiment 3
The preparation method of silicon nitride ceramics of the present invention comprises batching, moulding and burns till, and its ingredients by weight percentage composition is:
α-Si
3N
4Powder 88%, AL
2O
36%, ZrO
25% and Y
2O
31%.
Wherein:
α-Si
3N
4In the α phase content be 92%.
The batching particle diameter is controlled to be respectively: α-Si
3N
42-30 μ m, AL
2O
31-3 μ m, ZrO
20.5-1 μ m and Y
2O
31-2 μ m.
To prepare burden with water to after the medium ball milling mixes; adding 1.2% polyvinyl alcohol again mixes and obtained slurry in 2 hours; the oven dry granulation; granulation is controlled between the 60-120 mesh sieve; isostatic pressing gets base substrate under 160Mpa pressure; burn till under 1720 ℃ of temperature, nitrogen atmosphere protection the oven dry back, is incubated 4 hours.
The silicon nitride ceramics technical target of the product that obtains is: density 3.09g/cm
3, normal temperature bending strength 950MPa, 1000 ℃ of bending strength 910Mpa, hardness Hv2180kg/mm
2, fracture toughness property 6.2MPa.m
1/2
Embodiment 4
The preparation method of silicon nitride ceramics of the present invention comprises batching, moulding and burns till, and its ingredients by weight percentage composition is:
α-Si
3N
4Powder 88%, AL
2O
36%, ZrO
25% and Y
2O
31%.
Wherein:
α-Si
3N
4In the α phase content be 90%.
The batching particle diameter is controlled to be respectively: α-Si
3N
42-30 μ m, AL
2O
31-3 μ m, ZrO
20.5-1 μ m and Y
2O
31-2 μ m.
To prepare burden with water to after the medium ball milling mixes; adding 0.9% polyvinyl alcohol again mixes and obtained slurry in 3 hours; the oven dry granulation; granulation is controlled between the 60-120 mesh sieve; isostatic pressing gets base substrate under 180Mpa pressure; burn till under 1600 ℃ of temperature, nitrogen atmosphere protection the oven dry back, is incubated 5 hours.
The silicon nitride ceramics technical target of the product that obtains is: density 3.10g/cm
3, normal temperature bending strength 950MPa, 1000 ℃ of bending strength 910Mpa, hardness Hv2120kg/mm
2, fracture toughness property 6.5MPa.m
1/2
Embodiment 5
The preparation method of silicon nitride ceramics of the present invention comprises batching, moulding and burns till, and its ingredients by weight percentage composition is:
α-Si
3N
4Powder 85%, AL
2O
37%, ZrO
26% and Y
2O
32%.
Wherein:
α-Si
3N
4In the α phase content be 89%.
The batching particle diameter is controlled to be respectively: α-Si
3N
42-30 μ m, AL
2O
31-3 μ m, ZrO
20.5-1 μ m and Y
2O
31-2 μ m.
To prepare burden with water to after the medium ball milling mixes; adding 0.9% polyvinyl alcohol again mixes and obtained slurry in 2.5 hours; the oven dry granulation; granulation is controlled between the 60-120 mesh sieve; isostatic pressing gets base substrate under 170Mpa pressure; burn till under 1660 ℃ of temperature, nitrogen atmosphere protection the oven dry back, is incubated 4 hours.
The silicon nitride ceramics technical target of the product that obtains is: density 3.08g/cm
3, normal temperature bending strength 920MPa, 1000 ℃ of bending strength 900Mpa, hardness Hv2110kg/mm
2, fracture toughness property 6.3MPa.m
1/2
Claims (6)
1, a kind of preparation method of silicon nitride ceramics comprises batching, moulding and burns till, and it is characterized in that its ingredients by weight percentage composition is:
α-Si
3N
4Powder 82-88%, AL
2O
35-10%, ZrO
23-6% and Y
2O
31-3%.
2, the preparation method of silicon nitride ceramics according to claim 1 is characterized in that α-Si
3N
4In α phase content＞88%.
3, the preparation method of silicon nitride ceramics according to claim 1 and 2, the particle diameter that it is characterized in that preparing burden is respectively:
α-Si
3N
42-30 μ m, AL
2O
31-3 μ m, ZrO
20.5-1 μ m and Y
2O
31-2 μ m.
4, the preparation method of silicon nitride ceramics according to claim 3, it is characterized in that batching with water for after the medium ball milling mixes, the polyvinyl alcohol mixing that adds the 0.8-1.2% of total ingredients by weight again obtained slurry in 1.5-3 hour, the oven dry granulation, isostatic pressing gets base substrate under 110-180Mpa pressure.
5, the preparation method of silicon nitride ceramics according to claim 4 is characterized in that granulation is controlled between the 60-120 mesh sieve.
6, the preparation method of silicon nitride ceramics according to claim 5 is characterized in that base substrate is packed in the nitriding furnace, and with nitrogen atmosphere protection, the control firing temperature is 1550-1720 ℃, pressure 0.01-0.08MPa, and soaking time is 3-10 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100152361A CN101555141A (en) | 2009-05-15 | 2009-05-15 | Preparation method of silicon nitride ceramic |
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|---|---|---|---|
| CNA2009100152361A CN101555141A (en) | 2009-05-15 | 2009-05-15 | Preparation method of silicon nitride ceramic |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913879A (en) * | 2010-09-03 | 2010-12-15 | 北京中材人工晶体研究院有限公司 | Silicon nitride material and preparation method thereof, as well as silicon nitride heating device and production method thereof |
| CN101962297A (en) * | 2010-10-20 | 2011-02-02 | 北京中材人工晶体研究院有限公司 | Preparation method of silicon nitride ceramics ring for polysilicon reduction furnace |
| CN106810264A (en) * | 2015-11-27 | 2017-06-09 | 衡阳凯新特种材料科技有限公司 | A kind of preparation method of silicon nitride ceramics |
| CN108675798A (en) * | 2018-08-03 | 2018-10-19 | 广东工业大学 | A kind of silicon nitride ceramics and preparation method thereof |
| CN109206141A (en) * | 2018-08-27 | 2019-01-15 | 广东工业大学 | A kind of high hard high-ductility silicon nitride ceramics and its preparation method and application |
-
2009
- 2009-05-15 CN CNA2009100152361A patent/CN101555141A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913879A (en) * | 2010-09-03 | 2010-12-15 | 北京中材人工晶体研究院有限公司 | Silicon nitride material and preparation method thereof, as well as silicon nitride heating device and production method thereof |
| CN101913879B (en) * | 2010-09-03 | 2013-05-22 | 北京中材人工晶体研究院有限公司 | Silicon nitride material and preparation method thereof, as well as silicon nitride heating device and production method thereof |
| CN101962297A (en) * | 2010-10-20 | 2011-02-02 | 北京中材人工晶体研究院有限公司 | Preparation method of silicon nitride ceramics ring for polysilicon reduction furnace |
| CN101962297B (en) * | 2010-10-20 | 2013-05-22 | 北京中材人工晶体研究院有限公司 | Preparation method of silicon nitride ceramics ring for polysilicon reduction furnace |
| CN106810264A (en) * | 2015-11-27 | 2017-06-09 | 衡阳凯新特种材料科技有限公司 | A kind of preparation method of silicon nitride ceramics |
| CN108675798A (en) * | 2018-08-03 | 2018-10-19 | 广东工业大学 | A kind of silicon nitride ceramics and preparation method thereof |
| CN109206141A (en) * | 2018-08-27 | 2019-01-15 | 广东工业大学 | A kind of high hard high-ductility silicon nitride ceramics and its preparation method and application |
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Open date: 20091014 |