CN101955359A - Method for preparing porous silicon nitride wave transmitting ceramic with low dielectric constant and high strength - Google Patents
Method for preparing porous silicon nitride wave transmitting ceramic with low dielectric constant and high strength Download PDFInfo
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- CN101955359A CN101955359A CN2009101500988A CN200910150098A CN101955359A CN 101955359 A CN101955359 A CN 101955359A CN 2009101500988 A CN2009101500988 A CN 2009101500988A CN 200910150098 A CN200910150098 A CN 200910150098A CN 101955359 A CN101955359 A CN 101955359A
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Abstract
The invention discloses a method for preparing a porous silicon nitride wave transmitting ceramic with low dielectric constant and high strength. The method comprises the following steps of: (1) proportioning: uniformly mixing 80-90 weight percent of silicon nitride powder and 10-20 weight percent of metallic oxide to obtain a powder mixture; (2) mixing: adding absolute ethanol in an amount which is 30 to 60 percent based on the total mass of the material-powder mixture, and mixing the material-powder mixture and agate balls in the mass ratio of 1:2 for 12 to 24 hours to obtain the wet mixed material, wherein the agate balls are taken as mill balls; (3) forming: drying the wet mixed material, then sieving the mixed material with a screen, and performing compression forming to obtain a blank; and (4) sintering: sintering the blank in a protective atmosphere to obtain the porous silicon nitride wave transmitting ceramic. The method does not need a special pore former; a pore is formed by overlapping the columnar silicon nitride; and the method has the advantages of uniform and diffused pore, simplicity and low cost.
Description
Technical field
The invention belongs to the features ceramics processing, be specifically related to the preparation method of a kind of low-k, high intensity, porous silicon nitride nano wave-pervious pottery.
Background technology
Porous ceramics is to be a class stupalith of principal phase with the gas phase.Generally, hole in the material, comprise that storage pore and open pores are occupied by air, and the specific inductivity of air is generally speaking near 1, and loss tangent is especially near 0, so void content is big more, the specific inductivity of material, loss tangent are low more, promptly in saturating wave process, reflection and thermal losses all reduce, and saturating ripple rate raises.
Silicon nitride ceramics is one of over-all properties best material in the structural ceramics, it had both given prominence to hard, heat-resisting, wear-resisting, the corrosion resistant advantage of general stupalith, characteristic such as possessed good thermal shock, high temperature resistant creep again, self-lubricating is good, chemical stability is good, (specific inductivity and dielectric loss are respectively 7 and 4～4.5 * 10 also to have superior dielectric properties such as relatively low density and low specific inductivity, dielectric loss
-3), its anti-ablation property is better than fused quartz, can stand 6～7 Mach of anti-thermal shocks under the flying condition.U.S. Geogia technical institute is called most promising radome material with this material.Before and after 1980 so far, Si
3N
4Cause people's very big interest as electromagnetic wave transparent material always.
At present, the research of silicon nitride nano wave-pervious material mainly concentrates on Si
3N
4/ BN, Si
3N
4/ BN/SiO
2, Si
3N
4In/the phosphate system, adopt sintering methods such as hot pressing, air pressure, hot isostatic pressing mostly,, improve its intensity, but usually cause specific inductivity to remain high (specific inductivity＞4), have a strong impact on its use properties in the hope of by improving density.In this case, the saturating ripple pottery of porous silicon nitride causes people's attention.
At present, preparation for the saturating ripple pottery of porous, adopting the pore-forming material method mostly, is raw material such as the silicon nitride of space equality people (Chinese patent, application number 200610024146.5) employing once, silicon-dioxide, make pore-forming material with graphite, 1100-1500 ℃ of following sintering under air atmosphere prepared the porous SiN ceramic of silica bound, and its void content is 32.4% o'clock, bending strength is 35.1 ± 4.2MPa, and specific inductivity is 3.8 (1GHz).People such as Zhang Weiru (Chinese patent, application number 200510104409.9) be raw material with quartz, aluminum phosphate, silicon nitride, add the inorganic liquid whipping agent, through the 100MPa cold isostatic compaction, 930-980 ℃ of sintering, preparing void content is 60%, and bending strength is 15MPa, and specific inductivity is 1.98 wave-transparent porous ceramic.People such as Zhang Weiru (Chinese patent, application number 200610070747.X) adopting silicon nitride and rare-earth oxide is raw material, add starch, carbon dust is a pore former, cold isostatic compaction under 80-150MPa, through 300-600 ℃ of eliminating pore former, at 0.1-2MPa, 1500-1760 ℃ of following gas pressure sintering, preparing void content is 52%, specific inductivity is 2.7, and bending strength is the saturating ripple pottery of the porous of 166MPa.Aforesaid method all is to adopt the pore-forming material method to form pore, and pore-forming material must be got rid of in sintering process, causes pore size bigger, and even air hole distribution is difficult to control.Simultaneously, the method complexity, cost is higher.
Summary of the invention
The objective of the invention is to seek the preparation method of a kind of method high strength simple, with low cost, the saturating ripple pottery of low-k porous silicon nitride.
Technical scheme of the present invention: the preparation method of a kind of low-k, high intensity, porous silicon nitride nano wave-pervious pottery may further comprise the steps:
(1) batching: is that the ratio uniform mixing of 80-90%: 10-20% obtains expecting powder mixture with beta-silicon nitride powder, metal oxide according to weight percent;
(2) batch mixing: the 30-60% by material powder mixture total mass adds dehydrated alcohol, as mill ball, is 1: 2 ratio batch mixing 12-24 hour according to the quality proportioning of material powder mixture and agate ball with agate ball, obtains wet mixed feed;
(3) moulding: will sieve after the wet mixed feed oven dry, compression molding obtains blank;
(4) sintering:, obtain the saturating ripple pottery of porous silicon nitride with blank sintering under protective atmosphere.
Beta-silicon nitride powder described in the step (1) is the α type, and particle diameter is the 0.3-3 micron.
Metal oxide described in the step (1) is one or more combinations in aluminum oxide, yttrium oxide and the silicon oxide, and the purity of every kind of metal oxide＞98%.
Forming pressure described in the step (3) is controlled in the 10-100MPa scope.
Sintering process described in the step (4) is carried out stage by stage: 1 ℃/minute of temperature rise rate below 800 ℃, atmosphere is vacuum; Rise to sintering temperature with 10 ℃/minute more than 800 ℃, sintering temperature 1500-1800 ℃, atmosphere is nitrogen, is incubated 0.5-3 hour.
The invention has the advantages that: in (1) porous ceramics preparation process, need not add pore-forming material specially, only utilize moulding and sintering come control material in the material preparation process void content and microtexture, avoid the eliminating link of pore-forming material in the material preparation process, thereby method is simple, and cost is low.(2) porous ceramics that utilizes this method to prepare, pore is that the overlap joint by the column silicon nitride forms, the existence of column crystal can suppress the densification of base substrate in the sintering process again in the while sintering process, thereby porous ceramics void content height, tiny, the disperse of pore of preparation, and the strength of materials is higher.(3) utilize the saturating ripple pottery of the porous for preparing in this method, because additive level is low, thereby glassy phase content is less in the sintering process, causes low (0.78-3.5 * 10 of dielectric material loss
-3).
Description of drawings
Fig. 1 is a method flow of the present invention;
Fig. 2 is prepared porous ceramics void content and the bending strength change curve with sintering temperature;
Fig. 3 is the XRD analysis figure of the porous SiN ceramic that obtains by method of the present invention;
Fig. 4 is the SEM photo of the porous SiN ceramic fracture that obtains by method of the present invention.
Embodiment
Below in conjunction with accompanying drawing the present invention is done and to describe in further detail:
Shown in Fig. 3 and 4, the principal crystalline phase of porous ceramics is Si
3N
4, whole silicon nitride sinter is made up of the silicon nitride column crystal, and pore is to be formed by column crystal overlap joint, and pore is tiny, be evenly distributed.
Embodiment 1
Take by weighing 90 gram silicon nitride powders, the silicon nitride particle diameter is the 0.3-3 micron, and the α phase content is greater than 93%, and purity is greater than 99.9%.Add the aluminum oxide and the 5 gram yttrium oxide of 5 grams, wherein the aluminum oxide median size is 0.3 micron, and purity is greater than 99.8%, and the yttrium oxide particle diameter is the 1-10 micron, and purity is greater than 99%.The three is mixed, and is medium with analytical pure alcohol, adds by 30% of material powder total mass, uses agate ball as mill ball, the material powder: agate ball=1: 2 (mass ratio), and batch mixing was made slip in 12 hours, and dry powder is made in oven dry, and sieves.Then mixed powder is encased in the mould that diameter is 60mm, through the 50MPa extrusion forming, with the base substrate after the moulding under the vacuum protective atmosphere, 1600 ℃ of sintering.Concrete sintering process is carried out stage by stage: 1 ℃/minute of temperature rise rate below 800 ℃, atmosphere are vacuum; Rise to sintering temperature with 10 ℃/minute more than 800 ℃, atmosphere is nitrogen, is incubated 1 hour.
Through test, its performance index see the following form.
Embodiment 2
Take by weighing 85 gram silicon nitride powders, the silicon nitride particle diameter is the 0.3-3 micron, and the α phase content is greater than 93%, and purity is greater than 99.9%.Add the yttrium oxide and the 5 gram silicon oxide of 10 grams, wherein the yttrium oxide particle diameter is the 1-10 micron, and purity is greater than 99%, silicon oxide purity＞99%, median size＜100 nanometers.The three is mixed, and is medium with analytical pure alcohol, adds by 60% of material powder total mass, uses agate ball as mill ball, the material powder: agate ball=1: 2 (mass ratio), and batch mixing was made slip in 24 hours, and dry powder is made in oven dry, and sieves.Then mixed powder is encased in the mould that diameter is 60mm, through the 70MPa extrusion forming, with the base substrate after the moulding under the vacuum protective atmosphere, 1700 ℃ of sintering.Concrete sintering process is carried out stage by stage: 1 ℃/minute of temperature rise rate below 800 ℃, atmosphere are vacuum; Rise to sintering temperature with 10 ℃/minute more than 800 ℃, atmosphere is nitrogen, is incubated 2 hours.
Through test, its performance index see the following form.
Take by weighing 85 gram silicon nitride powders, the silicon nitride particle diameter is the 0.3-3 micron, and the α phase content is greater than 93%, and purity is greater than 99.9%.Add the yttrium oxide and the 5 gram aluminum oxide of 10 grams, wherein the yttrium oxide particle diameter is the 1-10 micron, and purity is greater than 99%, silicon oxide purity＞99%, median size＜100 nanometers.The three is mixed, and is medium with analytical pure alcohol, adds by 40% of material powder total mass, uses agate ball as mill ball, the material powder: agate ball=1: 2 (mass ratio), and batch mixing was made slip in 20 hours, and dry powder is made in oven dry, and sieves.Then mixed powder is encased in the mould that diameter is 60mm, through the 100MPa extrusion forming, with the base substrate after the moulding under the vacuum protective atmosphere, 1800 ℃ of sintering.Concrete sintering process is carried out stage by stage: 1 ℃/minute of temperature rise rate below 800 ℃, atmosphere are vacuum; Rise to sintering temperature with 10 ℃/minute more than 800 ℃, atmosphere is nitrogen, is incubated 3 hours.
Through test, its performance index see the following form.
Embodiment 4
Take by weighing 80 gram silicon nitride powders, the silicon nitride particle diameter is the 0.3-3 micron, and the α phase content is greater than 93%, and purity is greater than 99.9%.Add the yttrium oxide and the 5 gram silicon oxide of 5 grams, wherein the yttrium oxide particle diameter is the 1-10 micron, and purity is greater than 99%, silicon oxide purity＞99%, median size＜100 nanometers.The three is mixed, and is medium with analytical pure alcohol, adds by 40% of material powder total mass, uses agate ball as mill ball, the material powder: agate ball=1: 2 (mass ratio), and batch mixing was made slip in 16 hours, and dry powder is made in oven dry, and sieves.Then mixed powder is encased in the mould that diameter is 60mm, through the 10MPa extrusion forming, with the base substrate after the moulding under the vacuum protective atmosphere, 1500 ℃ of sintering.Concrete sintering process is carried out stage by stage: 1 ℃/minute of temperature rise rate below 800 ℃, atmosphere are vacuum; Rise to sintering temperature with 10 ℃/minute more than 800 ℃, atmosphere is nitrogen, is incubated 0.5 hour, makes low-k of the present invention, high intensity, porous silicon nitride nano wave-pervious pottery.
Through test, its performance index see the following form.
Above content is to further describing that the present invention did in conjunction with concrete preferred implementation; can not assert that the specific embodiment of the present invention only limits to this; for the general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; can also make some simple deduction or replace, all should be considered as belonging to the present invention and determine scope of patent protection by claims of being submitted to.
Confirm the low-k, high intensity, porous silicon nitride nano wave-pervious ceramic void content＞40%, bending strength＞70MPa, normal temperature specific inductivity＜3.5, dielectric loss＜6.5 * 10 that prepare with present method through test
-3Void content height, tiny, the disperse of pore, the strength of materials is higher.In the porous ceramics preparation process, need not add pore-forming material specially, only utilize moulding and sintering come control material in the material preparation process void content and microtexture, avoided the eliminating link of pore-forming material in the material preparation process, method is simple, and cost is low.
Claims (5)
1. the preparation method of a low-k, high intensity, porous silicon nitride nano wave-pervious pottery is characterized in that this method may further comprise the steps:
(1) batching: is that the ratio uniform mixing of 80-90%: 10-20% obtains expecting powder mixture with beta-silicon nitride powder, metal oxide according to weight percent;
(2) batch mixing: the 30-60% by material powder mixture total mass adds dehydrated alcohol, as mill ball, is 1: 2 ratio batch mixing 12-24 hour according to the quality proportioning of material powder mixture and agate ball with agate ball, obtains wet mixed feed;
(3) moulding: will sieve after the wet mixed feed oven dry, compression molding obtains blank;
(4) sintering:, obtain the saturating ripple pottery of porous silicon nitride with blank sintering under protective atmosphere.
2. according to the preparation method of the described a kind of low-k of claim 1, high intensity, porous silicon nitride nano wave-pervious pottery, it is characterized in that: the beta-silicon nitride powder described in the step (1) is the α type, and particle diameter is the 0.3-3 micron.
3. according to the preparation method of the described a kind of low-k of claim 1, high intensity, porous silicon nitride nano wave-pervious pottery, it is characterized in that: the metal oxide described in the step (1) is one or more combinations in aluminum oxide, yttrium oxide and the silicon oxide, and the purity of every kind of metal oxide＞98%.
4. according to the preparation method of the described a kind of low-k of claim 1, high intensity, porous silicon nitride nano wave-pervious pottery, it is characterized in that: the forming pressure described in the step (3) is controlled in the 10-100MPa scope.
5. according to the preparation method of the described a kind of low-k of claim 1, high intensity, porous silicon nitride nano wave-pervious pottery, it is characterized in that: the sintering process described in the step (4) is carried out stage by stage: 1 ℃/minute of temperature rise rate below 800 ℃, atmosphere is vacuum; Rise to sintering temperature with 10 ℃/minute more than 800 ℃, sintering temperature 1500-1800 ℃, atmosphere is nitrogen, is incubated 0.5-3 hour.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102757225A (en) * | 2012-01-01 | 2012-10-31 | 洛阳北苑特种陶瓷有限公司 | Method for preparing oxide and silicon nitride product |
| CN102951906A (en) * | 2012-11-08 | 2013-03-06 | 航天特种材料及工艺技术研究所 | Method for preparing self-toughening silicon nitride ceramics |
| CN109734455A (en) * | 2018-06-08 | 2019-05-10 | 河北高富氮化硅材料有限公司 | A method of preparing porous silicon nitride ceramic |
| CN113735598A (en) * | 2021-08-05 | 2021-12-03 | 西安交通大学 | High-strength high-temperature-ablation-resistant high-wave-transmission silicon nitride-based composite ceramic and preparation method thereof |
| CN115504795A (en) * | 2022-09-22 | 2022-12-23 | 衡阳凯新特种材料科技有限公司 | High-strength silicon nitride wave-transparent ceramic and preparation method thereof |
| CN116283237A (en) * | 2023-01-06 | 2023-06-23 | 衡阳凯新特种材料科技有限公司 | Low-thermal-conductivity silicon nitride wave-transparent ceramic material and preparation method thereof |
| CN116666293A (en) * | 2023-05-15 | 2023-08-29 | 杭州大和江东新材料科技有限公司 | Ceramic vacuum chuck with high flatness |
-
2009
- 2009-07-13 CN CN2009101500988A patent/CN101955359A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102757225A (en) * | 2012-01-01 | 2012-10-31 | 洛阳北苑特种陶瓷有限公司 | Method for preparing oxide and silicon nitride product |
| CN102757225B (en) * | 2012-01-01 | 2015-08-12 | 洛阳北苑特种陶瓷有限公司 | A kind of oxide compound is in conjunction with the preparation method of silicon nitride goods |
| CN102951906A (en) * | 2012-11-08 | 2013-03-06 | 航天特种材料及工艺技术研究所 | Method for preparing self-toughening silicon nitride ceramics |
| CN109734455A (en) * | 2018-06-08 | 2019-05-10 | 河北高富氮化硅材料有限公司 | A method of preparing porous silicon nitride ceramic |
| CN113735598A (en) * | 2021-08-05 | 2021-12-03 | 西安交通大学 | High-strength high-temperature-ablation-resistant high-wave-transmission silicon nitride-based composite ceramic and preparation method thereof |
| CN113735598B (en) * | 2021-08-05 | 2022-10-28 | 西安交通大学 | High-strength high-temperature-ablation-resistant high-wave-transmission silicon nitride-based composite ceramic and preparation method thereof |
| CN115504795A (en) * | 2022-09-22 | 2022-12-23 | 衡阳凯新特种材料科技有限公司 | High-strength silicon nitride wave-transparent ceramic and preparation method thereof |
| CN116283237A (en) * | 2023-01-06 | 2023-06-23 | 衡阳凯新特种材料科技有限公司 | Low-thermal-conductivity silicon nitride wave-transparent ceramic material and preparation method thereof |
| CN116666293A (en) * | 2023-05-15 | 2023-08-29 | 杭州大和江东新材料科技有限公司 | Ceramic vacuum chuck with high flatness |
| CN116666293B (en) * | 2023-05-15 | 2024-01-16 | 杭州大和江东新材料科技有限公司 | Ceramic vacuum chuck with high flatness |
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Application publication date: 20110126 |