CN105198475A - Method for producing complex-shaped porous silicon nitride ceramic product - Google Patents
Method for producing complex-shaped porous silicon nitride ceramic product Download PDFInfo
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- CN105198475A CN105198475A CN201510623703.4A CN201510623703A CN105198475A CN 105198475 A CN105198475 A CN 105198475A CN 201510623703 A CN201510623703 A CN 201510623703A CN 105198475 A CN105198475 A CN 105198475A
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Abstract
The invention relates to a method for producing a complex-shaped porous silicon nitride ceramic product. The method includes: using Si3N4 powder, Si powder, sintering auxiliaries, pore forming agent and silica sol to prepare mixed slurry; producing a male die with an outer surface identical with the appearance and size of the inner cavity of the product, and coating paraffin on the surface of the die; soaking the die into the slurry to allow the slurry to be adhered to the surface of the die, and then spraying Si3N4 coarse powder to the surface of the die to allow a layer of Si3N4 coarse powder to be evenly adhered to the slurry adhered to the surface of the die; drying the die in a ventilated environment for 1-3 hours to consolidate and harden the slurry on the surface of the die; repeating the soaking, spraying and drying process for multiple times until the thickness of the outer powder layer of the die meets the requirement; placing the die into an oven to melt the paraffin so as to separate a ceramic green body from the die; performing nitridation sintering on the green body to obtain the porous silicon nitride ceramic product. The bending strength of the porous silicon nitride ceramic product produced by the method is not lower than 50MPa, and the porous silicon nitride ceramic product is good in wave transmission performance.
Description
Technical field
The invention belongs to stupalith field, relate to a kind of method preparing complicated shape porous silicon nitride ceramic goods.
Background technology
Electromagnetic wave transparent material is a kind of structure-function integration material, is mainly used in radome and the radome of aircraft.Electromagnetic wave transparent material needs to completely cut off external environment, ensures the normal work of radar, antenna, also will have higher Electromagnetic wave penetrating percentage simultaneously, realizes the functions such as detection, guidance to make aircraft.In order to meet the needs of aeronautical and space technology and military technique development, electromagnetic wave transparent material needs to possess good mechanical property, thermal stability, the capable energy of environment and wave penetrate capability simultaneously.Porous silicon nitride ceramic, due to the over-all properties of its excellence, causes the attention of people.
In order to ensure the aeroperformance of aircraft, radome and radome are designed to complicated shape more.Stupalith is difficult to processing, and therefore, traditional compression moulding cannot satisfy the demands, and needs the near-net-shape technology developing stupalith, to reduce the manufacturing cycle and to reduce costs.Sizing material forming is suitable for producing complex-shaped, large-sized ceramic, obtains a wide range of applications.But existing multiple sizing material forming method still exists many deficiencies, such as, injection forming easily causes density gradient in product thickness direction, and green strength is lower; Gel injection molding and forming technology control is improper easily causes product surface be full of cracks etc.
Patent publication No. is that the Chinese patent of CN103214264A discloses a beta-silicon nitride nanowire and strengthens the preparation method of porous SiN ceramic, and forming method is isostatic cool pressing sintering, cannot the goods of forming shape complexity; Patent publication No. is a kind of method that the Chinese patent of CN103508749A discloses extrusion molding and prepares silicon nitride honeycomb pottery, silicon nitride powder, sintering aid and binding agent are dry mixed, then water is in succession added and glycerine rolling obtains uniform pug, then extrusion molding, sinters after dry binder removal.Containing a large amount of organism in pug, binder removal difficulty and easily cause product defect.
Summary of the invention
The technical problem solved
In order to avoid the deficiencies in the prior art part, the present invention proposes a kind of method preparing complicated shape porous silicon nitride ceramic goods, overcomes the problem that existing preparation method is difficult to prepare complicated shape porous silicon nitride ceramic goods.
Technical scheme
Prepare a method for complicated shape porous silicon nitride ceramic goods, it is characterized in that step is as follows:
Step 1, preparation Si
3n
4powder and Si powder mixed slurry: be that 1:1 ~ 1:1.5 powder and silicon sol carry out ball milling 12 ~ 24h by mass ratio, obtain finely dispersed slurry; In described powder: Si
3n
4the massfraction of powder is the massfraction of 50% ~ 80%, Si powder is 10% ~ 40%, and the massfraction of sintering aid is 3% ~ 10%;
Step 2: be dipped in the paraffin of thawing with goods inner chamber outward appearance and measure-alike formpiston by outside surface, makes die surface and superscribes one deck paraffin;
Step 3, dip-coating slurry: the slurry in step 1 is vacuumized de-bubble 30min, mould step 2 processed is dipped in slurry, makes die surface stick the thick slurry of 0.1 ~ 0.5mm, then takes out mould;
Step 4, stucco: spray Si at die surface
3n
4meal, makes the slurry of dip-coating stick last layer Si uniformly
3n
4meal, is placed in ventilated environment drying 1 ~ 3 hour by mould, make the slurry consolidation on surface, sclerosis;
Step 5: circulation step 3 dip-coating slurry and step 4 stucco, makes the powder layer thickness of die surface reach design requirements, obtains the green compact of goods after bisque drying;
Step 6, the demoulding: the paraffin layer of heating and melting die surface, make the green compact of goods be separated with mould;
Step 7, nitridation sintered: the goods green compact be separated with mould to be placed in nitriding furnace and to carry out nitridation sintered, obtain complicated shape porous silicon nitride ceramic goods.
The nitridation sintered technique of described step 7 is: first at 1200 DEG C, carries out pre-nitriding in nitrogen atmosphere, then in 1400 DEG C ~ 1650 DEG C nitrogen atmospheres, carries out nitrogenize, finally sinters in 1800 DEG C ~ 1900 DEG C nitrogen atmospheres.
The pore-forming material that massfraction is 5% ~ 15% is added in the powder of step 1.
In described step 2, the thickness of paraffin is 0.1 ~ 0.3mm.
Described sintering aid is Lu
2o
3or Y
2o
3one or more.
Described pore-forming material is resol, polyvinyl alcohol or Natvosol.
Described Si
3n
4powder is the α-Si of particle diameter 0.3 ~ 1.5 μm
3n
4powder.
Described Si
3n
4meal particle diameter is 10 ~ 60 μm.
Beneficial effect
A kind of method preparing complicated shape porous silicon nitride ceramic goods that the present invention proposes, adopts at die surface repeatedly dip-coating Si
3n
4powder and Si powder mixed slurry be dry method of hardening also, until green compact thickness reaches requirement, then the demoulding is nitridation sintered, obtains ceramic.Goods have good mechanical property and wave penetrate capability.
The invention has the beneficial effects as follows: adopt the method at die surface repeatedly dip-coating slurry, can the ceramic of shaping complicated shape.Silicon nitride ceramics adopts nitridation sintered technique, and in sintering process, product size is shunk little, and is easy to after pre-nitriding carry out mechanical workout.The present invention is a kind of simple to operate, the ceramic moulding process that equipment requirements is low.
Accompanying drawing explanation
Fig. 1 is preparation method's schema of height thermal conductive silicon nitride pottery of the present invention
Embodiment
Now in conjunction with the embodiments, the invention will be further described for accompanying drawing:
Example 1: select particle diameter to be the α-Si of 0.4 μm
3n
4the Lu that the Si powder that powder, particle diameter are 0.5 μm, particle diameter are 0.3 μm
2o
3powder and silicon sol (in powder, α-Si
3n
4powder, Si powder, Lu
2o
3the massfraction of powder is respectively 70%, 25%, 5%, and the mass ratio of powder and silicon sol is 1:1), preparation Si
3n
4powder and Si powder mixed slurry.Slurry is put into sealed can, vacuumizes de-bubble 30min.Metal die (mould maximum diameter is 60mm, high 100mm) submergence surface being scribbled the radome shape of one deck paraffin in the slurry, the slurry making die surface apply a layer thickness to be equably about 0.5mm.Taking out mould, is the α-Si of 20 μm at the slurry uppermost spray particle diameter of die surface
3n
4powder, makes that slurry is evenly low sticks last layer Si
3n
4meal.Mould is placed in ventilated environment dry.After the slurry consolidation and sclerosis of top layer, proceed the technical process of dip-coating slurry and stucco.Circulate after 15 times, the ceramic green thickness on mould top layer reaches 5mm.Mould is put into 120 baking oven 30min, paraffin melting, the green compact demoulding is also polished a little, its shape and size are met the demands.Green compact are placed in nitriding furnace, and desalination sintering in the nitrogen atmosphere of 1200 DEG C ~ 1650 DEG C, after the complete nitrogenize of silica flour, carry out reheating knot further, reheating temperature is 1800 DEG C, and protective atmosphere is 0.3MPaN
2, soaking time 2h.Through inspection, the porosity of gained porous silicon nitride ceramic is 35%, and intensity is 50MPa, and specific inductivity is 6.64, and dielectric loss is 2.67 × 10
-2.
Example 2: select particle diameter to be the α-Si of 0.4 μm
3n
4the Lu that the Si powder that powder, particle diameter are 0.5 μm, particle diameter are 0.3 μm
2o
3powder and silicon sol (in powder, α-Si
3n
4powder, Si powder, Lu
2o
3the massfraction of powder is respectively 55%, 40%, 5%, and the mass ratio of powder and silicon sol is 1:1), preparation Si
3n
4powder and Si powder mixed slurry.Slurry is put into sealed can, vacuumizes de-bubble 30min.Metal die (mould maximum diameter is 60mm, high 100mm) submergence surface being scribbled the radome shape of one deck paraffin in the slurry, the slurry making die surface apply a layer thickness to be equably about 0.5mm.Taking out mould, is the α-Si of 20 μm at the slurry uppermost spray particle diameter of die surface
3n
4powder, makes that slurry is evenly low sticks last layer Si
3n
4meal.Mould is placed in ventilated environment dry.After the slurry consolidation and sclerosis of top layer, proceed the technical process of dip-coating slurry and stucco.Circulate after 15 times, the ceramic green thickness on mould top layer reaches 5mm.Mould is put into 120 baking oven 30min, paraffin melting, the green compact demoulding is also polished a little, its shape and size are met the demands.Green compact are placed in nitriding furnace, and desalination sintering in the nitrogen atmosphere of 1200 DEG C ~ 1650 DEG C, after the complete nitrogenize of silica flour, carry out reheating knot further, reheating temperature is 1800 DEG C, and protective atmosphere is 0.3MPaN
2, soaking time 2h.Through inspection, the porosity of gained porous silicon nitride ceramic is 30%, and intensity is 70MPa, and specific inductivity is 5.10, and dielectric loss is 3.50 × 10
-2.
Example 3: select particle diameter to be the α-Si of 1.2 μm
3n
4the Lu that the Si powder that powder, particle diameter are 0.5 μm, particle diameter are 0.3 μm
2o
3powder and silicon sol (in powder, α-Si
3n
4powder, Si powder, Lu
2o
3the massfraction of powder is respectively 70%, 25%, 5%, and the mass ratio of powder and silicon sol is 1:1), preparation Si
3n
4powder and Si powder mixed slurry.Slurry is put into sealed can, vacuumizes de-bubble 30min.Metal die (mould maximum diameter is 60mm, high 100mm) submergence surface being scribbled the radome shape of one deck paraffin in the slurry, the slurry making die surface apply a layer thickness to be equably about 0.5mm.Taking out mould, is the α-Si of 20 μm at the slurry uppermost spray particle diameter of die surface
3n
4powder, makes that slurry is evenly low sticks last layer Si
3n
4meal.Mould is placed in ventilated environment dry.After the slurry consolidation and sclerosis of top layer, proceed the technical process of dip-coating slurry and stucco.Circulate after 15 times, the ceramic green thickness on mould top layer reaches 5mm.Mould is put into 120 baking oven 30min, paraffin melting, the green compact demoulding is also polished a little, its shape and size are met the demands.Green compact are placed in nitriding furnace, and desalination sintering in the nitrogen atmosphere of 1200 DEG C ~ 1650 DEG C, after the complete nitrogenize of silica flour, carry out reheating knot further, reheating temperature is 1800 DEG C, and protective atmosphere is 0.3MPaN
2, soaking time 2h.Through inspection, the porosity of gained porous silicon nitride ceramic is 45%, and intensity is 60MPa, and specific inductivity is 4.5, and dielectric loss is 2.30 × 10
-2.
Example 4: select particle diameter to be the α-Si of 1.2 μm
3n
4the Lu that the Si powder that powder, particle diameter are 0.5 μm, particle diameter are 0.3 μm
2o
3powder, Xylo-Mucine and silicon sol (in powder, α-Si
3n
4powder, Si powder, Lu
2o
3the massfraction of powder, Xylo-Mucine is respectively 60%, 25%, 5%, 10%, and the mass ratio of powder and silicon sol is 1:1), preparation Si
3n
4powder and Si powder mixed slurry.Slurry is put into sealed can, vacuumizes de-bubble 30min.Metal die (mould maximum diameter is 60mm, high 100mm) submergence surface being scribbled the radome shape of one deck paraffin in the slurry, the slurry making die surface apply a layer thickness to be equably about 0.5mm.Taking out mould, is the α-Si of 20 μm at the slurry uppermost spray particle diameter of die surface
3n
4powder, makes that slurry is evenly low sticks last layer Si
3n
4meal.Mould is placed in ventilated environment dry.After the slurry consolidation and sclerosis of top layer, proceed the technical process of dip-coating slurry and stucco.Circulate after 15 times, the ceramic green thickness on mould top layer reaches 5mm.Mould is put into 120 baking oven 30min, paraffin melting, the green compact demoulding is also polished a little, its shape and size are met the demands.Green compact are placed in box-type furnace, are incubated 2h, carry out binder removal process under 500 DEG C of air atmospheres, temperature rise rate is 3 DEG C/min.After binder removal, green compact are placed in nitriding furnace, desalination sintering in the nitrogen atmosphere of 1200 DEG C ~ 1650 DEG C, after the complete nitrogenize of silica flour, carry out reheating knot further, reheating temperature is 1800 DEG C, and protective atmosphere is 0.3MPaN
2, soaking time 2h.Through inspection, the porosity of gained porous silicon nitride ceramic is 55%, and intensity is 55MPa, and specific inductivity is 3.5, and dielectric loss is 1.25 × 10
-2.
Claims (8)
1. prepare a method for complicated shape porous silicon nitride ceramic goods, it is characterized in that step is as follows:
Step 1, preparation Si
3n
4powder and Si powder mixed slurry: be that 1:1 ~ 1:1.5 powder and silicon sol carry out ball milling 12 ~ 24h by mass ratio, obtain finely dispersed slurry; In described powder: Si
3n
4the massfraction of powder is the massfraction of 50% ~ 80%, Si powder is 10% ~ 40%, and the massfraction of sintering aid is 3% ~ 10%;
Step 2: be dipped in the paraffin of thawing with goods inner chamber outward appearance and measure-alike formpiston by outside surface, makes die surface and superscribes one deck paraffin;
Step 3, dip-coating slurry: the slurry in step 1 is vacuumized de-bubble 30min, mould step 2 processed is dipped in slurry, makes die surface stick the thick slurry of 0.1 ~ 0.5mm, then takes out mould;
Step 4, stucco: spray Si at die surface
3n
4meal, makes the slurry of dip-coating stick last layer Si uniformly
3n
4meal, is placed in ventilated environment drying 1 ~ 3 hour by mould, make the slurry consolidation on surface, sclerosis;
Step 5: circulation step 3 dip-coating slurry and step 4 stucco, makes the powder layer thickness of die surface reach design requirements, obtains the green compact of goods after bisque drying;
Step 6, the demoulding: the paraffin layer of heating and melting die surface, make the green compact of goods be separated with mould;
Step 7, nitridation sintered: the goods green compact be separated with mould to be placed in nitriding furnace and to carry out nitridation sintered, obtain complicated shape porous silicon nitride ceramic goods.
2. prepare the method for complicated shape porous silicon nitride ceramic goods according to claim 1, it is characterized in that: the nitridation sintered technique of described step 7 is: first at 1200 DEG C, pre-nitriding is carried out in nitrogen atmosphere, then in 1400 DEG C ~ 1650 DEG C nitrogen atmospheres, carry out nitrogenize, finally sinter in 1800 DEG C ~ 1900 DEG C nitrogen atmospheres.
3. prepare the method for complicated shape porous silicon nitride ceramic goods according to claim 1, it is characterized in that: in the powder of step 1, add the pore-forming material that massfraction is 5% ~ 15%.
4. prepare the method for complicated shape porous silicon nitride ceramic goods according to claim 1, it is characterized in that: in described step 2, the thickness of paraffin is 0.1 ~ 0.3mm.
5. prepare the method for complicated shape porous silicon nitride ceramic goods according to claim 1, it is characterized in that: described sintering aid is Lu
2o
3or Y
2o
3one or more.
6. prepare the method for complicated shape porous silicon nitride ceramic goods according to claim 3, it is characterized in that: described pore-forming material is resol, polyvinyl alcohol or Natvosol.
7. prepare the method for complicated shape porous silicon nitride ceramic goods according to claim 1, it is characterized in that: described Si
3n
4powder is the α-Si of particle diameter 0.3 ~ 1.5 μm
3n
4powder.
8. prepare the method for complicated shape porous silicon nitride ceramic goods according to claim 1, it is characterized in that: described Si
3n
4meal particle diameter is 10 ~ 60 μm.
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Cited By (10)
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|---|---|---|---|---|
| CN108436037A (en) * | 2018-02-11 | 2018-08-24 | 清华大学 | A method of inhibiting casting thermal fragmentation |
| CN108751998A (en) * | 2018-06-12 | 2018-11-06 | 汉江弘源襄阳碳化硅特种陶瓷有限责任公司 | A kind of silicon nitride combined silicon carbide ceramic filter and preparation method thereof |
| CN109560381A (en) * | 2018-11-28 | 2019-04-02 | 北京遥感设备研究所 | A kind of ceramic radome improves the pre- Enhancement Method of intensity |
| CN110078521A (en) * | 2019-05-13 | 2019-08-02 | 西北工业大学 | A kind of submicron order silicon nitride hollow microsphere and preparation method |
| CN110357659A (en) * | 2019-07-06 | 2019-10-22 | 陈波 | A kind of preparation method nitrogenizing silicon substrate composite foamed ceramic |
| CN111423247A (en) * | 2020-03-31 | 2020-07-17 | 深圳麦克韦尔科技有限公司 | Porous ceramic, preparation method and heating element thereof |
| CN111589873A (en) * | 2020-05-13 | 2020-08-28 | 华誉智造(上海)新材料有限公司 | Combined roller and preparation method thereof |
| CN113800917A (en) * | 2021-08-17 | 2021-12-17 | 航天特种材料及工艺技术研究所 | Preparation method of homogenized large-size silicon nitride ceramic flat plate |
| CN115849919A (en) * | 2022-12-12 | 2023-03-28 | 广东技术师范大学 | High-performance silicon nitride conductive ceramic and preparation method and application thereof |
| US11703361B2 (en) | 2018-07-02 | 2023-07-18 | Beijing U-Precision Tech Co., Ltd. | Five-degree-of-freedom heterodyne grating interferometry system |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108436037A (en) * | 2018-02-11 | 2018-08-24 | 清华大学 | A method of inhibiting casting thermal fragmentation |
| CN108751998A (en) * | 2018-06-12 | 2018-11-06 | 汉江弘源襄阳碳化硅特种陶瓷有限责任公司 | A kind of silicon nitride combined silicon carbide ceramic filter and preparation method thereof |
| CN108751998B (en) * | 2018-06-12 | 2021-05-11 | 汉江弘源襄阳碳化硅特种陶瓷有限责任公司 | Silicon nitride and silicon carbide combined ceramic filter and preparation method thereof |
| US11703361B2 (en) | 2018-07-02 | 2023-07-18 | Beijing U-Precision Tech Co., Ltd. | Five-degree-of-freedom heterodyne grating interferometry system |
| CN109560381A (en) * | 2018-11-28 | 2019-04-02 | 北京遥感设备研究所 | A kind of ceramic radome improves the pre- Enhancement Method of intensity |
| CN110078521A (en) * | 2019-05-13 | 2019-08-02 | 西北工业大学 | A kind of submicron order silicon nitride hollow microsphere and preparation method |
| CN110078521B (en) * | 2019-05-13 | 2021-06-11 | 西北工业大学 | Submicron silicon nitride hollow microsphere and preparation method thereof |
| CN110357659A (en) * | 2019-07-06 | 2019-10-22 | 陈波 | A kind of preparation method nitrogenizing silicon substrate composite foamed ceramic |
| CN111423247A (en) * | 2020-03-31 | 2020-07-17 | 深圳麦克韦尔科技有限公司 | Porous ceramic, preparation method and heating element thereof |
| CN111589873A (en) * | 2020-05-13 | 2020-08-28 | 华誉智造(上海)新材料有限公司 | Combined roller and preparation method thereof |
| CN113800917A (en) * | 2021-08-17 | 2021-12-17 | 航天特种材料及工艺技术研究所 | Preparation method of homogenized large-size silicon nitride ceramic flat plate |
| CN115849919A (en) * | 2022-12-12 | 2023-03-28 | 广东技术师范大学 | High-performance silicon nitride conductive ceramic and preparation method and application thereof |
| CN115849919B (en) * | 2022-12-12 | 2024-04-05 | 广东技术师范大学 | High-performance silicon nitride conductive ceramic and preparation method and application thereof |
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Application publication date: 20151230 |