CN103803986B - A kind of Si-Al-O-N-B diphase ceramic material and preparation method thereof - Google Patents
A kind of Si-Al-O-N-B diphase ceramic material and preparation method thereof Download PDFInfo
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- CN103803986B CN103803986B CN201410091336.3A CN201410091336A CN103803986B CN 103803986 B CN103803986 B CN 103803986B CN 201410091336 A CN201410091336 A CN 201410091336A CN 103803986 B CN103803986 B CN 103803986B
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Abstract
A kind of Si-Al-O-N-B diphase ceramic material and preparation method thereof.This Si-Al-O-N-B diphase ceramic material is by silicon nitride 25 ~ 55 weight part, aluminium nitride 10 ~ 40 weight part, the mixed powder of aluminum oxide 5 ~ 40 weight part is pressed into biscuit, then by the liquid precursor boron azine of described biscuit dipping BN, then through crosslinking curing, Pintsch process, sintering form; Its specific inductivity is less than 6.Diphase ceramic material of the present invention is not easy to crack; Preparation technology is simple, also can according to the character adjusting process parameter of target product, and the rheological characteristics that simultaneously precursor can be utilized good solves the problem of the shaping difficulty of complex component.
Description
Technical field
The present invention relates to technical field of functional ceramics, specifically, relate to a kind ofly be applicable to the Si-Al-O-N-B diphase ceramic material in space flight wave transparent field and preparation method thereof.
Background technology
Along with the high speed development of science and technology, numerous high-tech area such as Aeronautics and Astronautics, the energy all proposes more and more urgent demand to high performance material.There is due to pottery the characteristics such as excellent high temperature resistant, anti-yaw damper, wear-resistant, high rigidity, and there is higher Young's modulus and lower density, some ceramic matric composite also has many good function such as solar heat protection, heat insulation, wave transparent concurrently, therefore, each developed country of the world all regards stupalith as has the hi tech and new material of material impact to human future and gives primary study.Sialon is a kind of substitutional solid solution based on silicon nitride crystal structure, and it has the characteristic of several potteries such as silicon nitride, aluminum oxide concurrently, and designs by the overall performance of content to material changing wherein certain component.Due to the performance such as mechanics, dielectric that Sialon is good, be considered to one of candidate material of space flight electromagnetic wave transparent material.
Research about Sialon has lot of documents report.
Chinese patent application 200610106997.4 discloses a kind of preparation method of sialon porous material, take flyash as raw material, with silica flour, aluminium powder for reductive agent, adopts reduction-nitridation technique to prepare sialon porous material.
Chinese patent application 200710052469.X discloses a kind of Sialon matrix material and preparation method thereof, and with aluminium ash, bauxitic clay, silicon-dioxide, aluminium powder, silica flour etc. for raw material, after mixing, in nitrogen, reacting by heating obtains Sialon.Above the method is simple to operate, but easily remains the material of some high dielectrics, as silicon, aluminium etc., is not suitable for electromagnetic wave transparent material.
201110132271.9 disclose a kind of low cost S ialon pottery and preparation method thereof, and by raw material mixing, compression moldings such as silica flour, aluminum oxide, Samarium trioxides, at high temperature sintering forms.
201310216965.X discloses a kind of preparation method of beta-Sialon, is ground altogether by the raw materials such as burnt cash, 60 alumina, clay, hard coal, makes wet feed, smears shaping, then sinter in nitriding furnace stove and form.
The purity that above method obtains material is limited, and the problem of all unresolved shaping difficulty brought when preparing complex component.
Two US Patent No. 5891815 of Lockheed Martin Corporation and US5925584 individually disclose a kind of Sialon-BN pottery and preparation method thereof, are all the mixed powders adopting raw material, when adding sintering aid, high temperature sintering forms.The density of US 5891815 resulting materials is 2.80-2.85 g/cm
3, specific inductivity is 7.14-9.52; The density of US5925584 material is 2.70-2.74 g/cm
3, specific inductivity is 6.616-7.67.The specific inductivity of these materials is all higher (6 ~ 10), the problem of the unresolved equally shaping difficulty brought when preparing complex component.
Summary of the invention
Technical problem to be solved by this invention is, overcome that current material purity is limited, specific inductivity is higher, the complex component not defect such as easy-formation, the Si-Al-O-N-B diphase ceramic material that a kind of over-all properties is good, be applicable to space flight wave transparent field is provided, and a kind of preparation method of easily shaping Si-Al-O-N-B diphase ceramic material is provided.
The Si-Al-O-N-B diphase ceramic material of the present invention is be pressed into biscuit by the mixed powder of following raw material and weight part: silicon nitride 25 ~ 55 weight part, aluminium nitride 8 ~ 40 weight part, aluminum oxide 5 ~ 45 weight part; Again the liquid precursor boron azine of BN is dipped in biscuit, then forms through crosslinking curing, Pintsch process, sintering; Its specific inductivity is less than 6.
Further, described raw material also comprises silicon oxide 5 ~ 30 weight part.
Further, described following raw material and weight part are: silicon nitride 30 ~ 50 weight part, aluminium nitride 10 ~ 35 weight part, aluminum oxide 10 ~ 40 weight part.
Further, described following raw material and weight part are: silicon nitride: 35 ~ 50 weight parts; Aluminium nitride 10 ~ 25 weight part; Aluminum oxide 15 ~ 40 weight part.
Further, described silicon oxide is 15 ~ 28 weight parts.
Further, described silicon oxide is 20 ~ 25 weight parts.
The preparation method of the Si-Al-O-N-B diphase ceramic material of the present invention, comprises the following steps:
(1) biscuit is shaping: be the raw material silicon nitride of 1nm ~ 20 μm by particle diameter, aluminium nitride, aluminum oxide, silicon oxide mix by predetermined proportion, ball milling 1 ~ 35h, then mixed powder is pressed into biscuit;
(2) the liquid precursor boron azine of BN is impregnated in step (1) gained biscuit; Make the liquid level of liquid precursor exceed biscuit upper surface 2 ~ 30mm, leave standstill 0.5 ~ 5h, the biscuit of boron azine must be impregnated with;
(3) biscuit being impregnated with boron azine is placed in encloses container, under the protection of inert atmosphere, is warming up to 60 ~ 200 DEG C, boron azine is occurred crosslinked, insulation >=20h, until solidification, must closely bond the biscuit of crosslinking curing boron azine;
(4) biscuit step (3) gained being closely bonded crosslinking curing boron azine is placed in High Temperature Furnaces Heating Apparatus; under vacuum or under inert atmosphere protection condition; be warming up to 1200 ~ 1850 DEG C; make the cracking of boron azine; make complex phase ceramic sinter simultaneously; cracking sintering time is 0.5 ~ 3h, namely obtains Si-Al-O-N-B diphase ceramic material.
Further, in step (1), Ball-milling Time is 10 ~ 30h preferably,
Further, in step (3), the crosslinking curing temperature of boron azine preferably 80 ~ 150 DEG C.
Further, in step (4), the temperature of described boron azine cracking is 1300 ~ 1800 DEG C.
Further, the method for described dipping is the combination of one or more in vacuum impregnation technology, Soaking, impregnating by pressure method.
The liquid precursor boron azine of BN, primarily of Sialon and BN composition, is immersed in biscuit, has both served bonding effect, effectively can reduce specific inductivity again by Si-Al-O-N-B diphase ceramic material of the present invention; Its specific inductivity is less than 6; Product is not easy to crack; Preparation technology is simply controlled, also can according to the character adjusting process parameter of target product, and the rheological characteristics that simultaneously precursor can be utilized good solves the shaping difficult problem of complex component.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of embodiment 1 Si-Al-O-N-B diphase ceramic material;
Fig. 2 is the microscopic appearance photo of embodiment 2 Si-Al-O-N-B diphase ceramic material.
Embodiment
Embodiment 1:
The present embodiment Si-Al-O-N-B diphase ceramic material is pressed into biscuit by the mixed powder of following raw material and weight part: silicon nitride 100g, aluminium nitride 50g, aluminum oxide 55g; Be impregnated in biscuit by the liquid precursor boron azine of BN again, then through crosslinking curing, Pintsch process, sintering form; Its specific inductivity is 4.73.
Preparation:
(1) biscuit is shaping: the ratio of 100g silicon nitride (particle diameter 0.5 μm), 50g aluminium nitride (particle diameter 0.8 μm), 55g aluminum oxide (particle diameter 1.0 μm) mixed, ball milling 24h, then adopt mechanical compression-moulding methods by mixed powder compression moulding, molding pressure is 150MPa.
(2) adopt vacuum (initial gas pressure the is 100Pa) mode of flooding, be immersed in biscuit by the liquid precursor boron azine of BN, the add-on of boron azine is for till covering biscuit upper surface 5mm; Leave standstill 1h, precursor is fully infiltrated in biscuit.
(3) by flooding the biscuit of boron azine as in encloses container, under the protection of nitrogen, being warming up to 100 DEG C, boron azine being occurred crosslinked, insulation 50h, until solidification.
(4) biscuit is placed in High Temperature Furnaces Heating Apparatus with the bonding mixture of boron azine after solidification, under nitrogen protection, is warming up to 1650 DEG C; soaking time 2.5h; make boron azine generation cracking, make complex phase ceramic sinter simultaneously, namely obtain Si-Al-O-N-B complex phase ceramic electromagnetic wave transparent material.The XRD figure spectrum of this material as shown in Figure 1.In this material, the content of BN is 15wt%, and measuring specific inductivity is 4.73.Product is not easy to crack.
Embodiment 2
The present embodiment Si-Al-O-N-B diphase ceramic material is pressed into biscuit by the mixed powder of following raw material and weight part: silicon nitride 60g, aluminium nitride 80g, aluminum oxide 20g, silicon oxide 40 g; Be impregnated in biscuit by the liquid precursor boron azine of BN again, then through crosslinking curing, Pintsch process, sintering form; Its specific inductivity is 3.55.
Preparation:
(1) biscuit is shaping: 60g silicon nitride (particle diameter 100nm), 80g aluminium nitride (particle diameter 200nm), 20g aluminum oxide (particle diameter 80nm), 40g silicon oxide (particle diameter 200nm) are mixed, ball milling 12h, then adopts the method for gel injection to be prepared by mixed powder shaping.
(2) adopt the mode of impregnating by pressure, be immersed in biscuit by the liquid precursor boron azine of BN, the add-on of boron azine is for till covering biscuit upper surface 5mm; Leave standstill 5h, boron azine precursor is fully infiltrated in biscuit; Apply pressure 5MPa, medium is nitrogen.
(3) by flooding the biscuit of boron azine as in encloses container, under the protection of argon gas, being warming up to 80 DEG C, boron azine being occurred crosslinked, insulation 80h, until solidification.
(4) biscuit is placed in High Temperature Furnaces Heating Apparatus with the bonding mixture of boron azine after solidification, under vacuum, is warming up to 1760 DEG C, insulation 1.5h, make boron azine generation cracking, make complex phase ceramic sinter simultaneously, namely obtain Si-Al-O-N-B complex phase ceramic electromagnetic wave transparent material.In this material, the content of BN is 28wt%, and measuring specific inductivity is 3.55.Product is not easy to crack.
Embodiment 3
The present embodiment Si-Al-O-N-B diphase ceramic material is pressed into biscuit by the mixed powder of following raw material and weight part: silicon nitride 50g, aluminium nitride 40g, aluminum oxide 50g, silicon oxide 60 g; Be impregnated in biscuit by the liquid precursor boron azine of BN again, then through crosslinking curing, Pintsch process, sintering form; Its specific inductivity is for being 4.41.
Preparation:
(1) biscuit is shaping: 50g silicon nitride (particle diameter 10 μm), 40g aluminium nitride (particle diameter 5 μm), 50g aluminum oxide (particle diameter 3 μm), 60g silicon oxide (particle diameter 2 μm) are mixed, ball milling 30h, then adopt the method for isostatic cool pressing to be prepared by mixed powder shaping, pressure is about 240MPa.
(2) adopt the mode of impregnating by pressure, be immersed in biscuit by the liquid precursor boron azine of BN, the add-on of boron azine is for till covering biscuit upper surface 5mm; Then, in container, be filled with nitrogen to 2MPa, leave standstill 5h, boron azine precursor is fully infiltrated in biscuit.
(3) biscuit flooding boron azine is placed in encloses container, under the protection of argon gas, is warming up to 150 DEG C, boron azine is occurred crosslinked, insulation 30h, until solidification.
(4) biscuit is placed in High Temperature Furnaces Heating Apparatus with the bonding mixture of boron azine after solidification, under vacuum, is warming up to 1300 DEG C, soaking time 3h, make boron azine generation cracking, make complex phase ceramic sinter simultaneously, namely obtain Si-Al-O-N-B complex phase ceramic electromagnetic wave transparent material.In this material, the content of BN is 21wt%, and measuring specific inductivity is 4.41.Product is not easy to crack.
Claims (8)
1. a Si-Al-O-N-B diphase ceramic material, it is characterized in that, be pressed into biscuit by the mixed powder of following raw material and weight part: silicon nitride 25 ~ 55 weight part, aluminium nitride 8 ~ 40 weight part, aluminum oxide 5 ~ 45 weight part, and silicon oxide 5 ~ 30 weight part; Be impregnated in biscuit by the liquid precursor boron azine of BN again, then through crosslinking curing, Pintsch process, sintering form; Its specific inductivity is less than 6;
Preparation method's concrete operation step of described Si-Al-O-N-B diphase ceramic material is:
(1) biscuit is shaping: be the raw material silicon nitride of 1nm ~ 20 μm by particle diameter, aluminium nitride, aluminum oxide, silicon oxide mix by predetermined proportion, ball milling 1 ~ 30h, then mixed powder is pressed into biscuit;
(2) the liquid precursor boron azine of BN is impregnated in step (1) gained biscuit; Make the liquid level of liquid precursor exceed biscuit upper surface 2 ~ 30mm, leave standstill 0.5 ~ 5 h;
(3) biscuit being impregnated with boron azine is placed in encloses container, under the protection of inert atmosphere, is warming up to 60 ~ 200 DEG C, boron azine is occurred crosslinked, insulation >=20h, until solidification, must closely bond the biscuit of crosslinking curing boron azine;
(4) biscuit step (3) gained being closely bonded crosslinking curing boron azine is placed in High Temperature Furnaces Heating Apparatus; under vacuum or under inert atmosphere protection condition; be warming up to 1200 ~ 1850 DEG C; make the cracking of boron azine; make complex phase ceramic sinter simultaneously; cracking sintering time is 0.5 ~ 3h, namely obtains Si-Al-O-N-B diphase ceramic material.
2. Si-Al-O-N-B diphase ceramic material according to claim 1, is characterized in that, the weight part of described raw material silicon nitride, aluminium nitride, aluminum oxide is: silicon nitride 30 ~ 50 weight part, aluminium nitride 10 ~ 35 weight part, aluminum oxide 10 ~ 40 weight part.
3. Si-Al-O-N-B diphase ceramic material according to claim 1, is characterized in that, the weight part of described silicon nitride, aluminium nitride, aluminum oxide is: silicon nitride: 35 ~ 50 weight parts; Aluminium nitride 10 ~ 25 weight part; Aluminum oxide 15 ~ 40 weight part.
4. the Si-Al-O-N-B diphase ceramic material according to claim 1 or 2 or 3, is characterized in that, described silicon oxide is 15 ~ 28 weight parts.
5. the Si-Al-O-N-B diphase ceramic material according to claim 1 or 2 or 3, is characterized in that, described silicon oxide is 20 ~ 25 weight parts.
6. according to the Si-Al-O-N-B diphase ceramic material one of claims 1 to 3 Suo Shu, it is characterized in that, in the operation steps (3) of described preparation method, described temperature is 80 ~ 150 DEG C.
7. according to the Si-Al-O-N-B diphase ceramic material one of claims 1 to 3 Suo Shu, it is characterized in that, in the operation steps (4) of described preparation method, the temperature of described boron azine cracking is 1300 ~ 1800 DEG C.
8. according to the Si-Al-O-N-B diphase ceramic material one of claims 1 to 3 Suo Shu, it is characterized in that, in the operation steps (2) of described preparation method, the method for described dipping is the combination of one or more in vacuum impregnation technology, Soaking, impregnating by pressure method.
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| CN112028647A (en) * | 2020-08-25 | 2020-12-04 | 贵阳明通炉料有限公司 | High-performance sialon corundum plastic material and preparation method thereof |
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| CN102093058A (en) * | 2010-12-23 | 2011-06-15 | 大连海事大学 | Alpha-SiAlON/BN composite ceramic material and preparation method thereof |
| CN102642845A (en) * | 2012-04-23 | 2012-08-22 | 中国人民解放军国防科学技术大学 | Method and device for preparing borazine |
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| CN102093058A (en) * | 2010-12-23 | 2011-06-15 | 大连海事大学 | Alpha-SiAlON/BN composite ceramic material and preparation method thereof |
| CN102642845A (en) * | 2012-04-23 | 2012-08-22 | 中国人民解放军国防科学技术大学 | Method and device for preparing borazine |
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