CN106892570A - Aluminium nitride fibres cordierite glass-ceramic composite diphase material and preparation method thereof - Google Patents
Aluminium nitride fibres cordierite glass-ceramic composite diphase material and preparation method thereof Download PDFInfo
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- CN106892570A CN106892570A CN201710108885.0A CN201710108885A CN106892570A CN 106892570 A CN106892570 A CN 106892570A CN 201710108885 A CN201710108885 A CN 201710108885A CN 106892570 A CN106892570 A CN 106892570A
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- aluminium nitride
- nitride fibres
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- ceramic composite
- composite diphase
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
- C03C14/002—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of fibres, filaments, yarns, felts or woven material
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0036—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents
- C03C10/0045—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents containing SiO2, Al2O3 and MgO as main constituents
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/02—Fibres; Filaments; Yarns; Felts; Woven material
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/30—Methods of making the composites
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Abstract
The invention discloses a kind of preparation method of aluminium nitride fibres cordierite glass-ceramic composite diphase material, it is comprised the steps of：By MgO powder, SiO2Powder, Al2O3Powder and flux, Nucleating Agent are mixed into homogeneous mixture in proportion；The mixture is melted and is heated；Aluminium nitride fibres are sprayed into fusion pool by nitrogen and is sufficiently stirred for being uniform molten mixture in the latter stage of melting process；Molten mixture is poured into the mould by preheating；The molten mixture annealing in mould will be poured into；To be annealed the parent glass coring containing aluminium nitride fibres that obtains and crystallization obtains aluminium nitride fibres cordierite glass-ceramic composite diphase material.Present invention also offers a kind of aluminium nitride fibres cordierite glass-ceramic composite diphase material prepared by the above method, it includes following components：MgO、SiO2、Al2O3、B2O3、Cr2O3、TiO2And aluminium nitride fibres.
Description
Technical field
The present invention relates to glass ceramic composite field, more particularly to a kind of aluminium nitride fibres cordierite glass-ceramic is answered
Phase material and preparation method thereof.
Background technology
Cordierite glass-ceramic is a kind of devitrified glass of excellent performance, low with dielectric loss, and heat endurance is good and machine
The advantages of tool intensity is high, but due to the bond material that it is crystalline phase and amorphous phase, its general toughness is relatively low.
Devitrified glass is typically prepared using sintering process or fusion method, the cordierite glass-ceramic that wherein prepared by fusion method
Bulk density is of a relatively high, and the porosity is relatively low, but to aluminium nitride fibres are combined with devitrified glass using fusion method, then
First have to solve the problems, such as that aluminium nitride fibres are easily oxidized at high temperature；Its secondary solution aluminium nitride fibres uniformly divides in the melt
The problem of cloth.
Aluminium nitride fibres are combined with cordierite glass-ceramic using fusion method in current there is no in the prior art
Carry out the preparation of aluminium nitride fibres cordierite glass-ceramic composite diphase material.
The content of the invention
For the above-mentioned problems in the prior art, inventor is had found at melt zone end by substantial amounts of creative work
Aluminium nitride fibres are sprayed into bath and are sufficiently stirred for that preferable aluminium nitride fibres dispersion can be obtained simultaneously by the phase with nitrogen stream
Change effect, while the nitrogen for spraying into can manufacture non-oxidizing environment and prevent aluminium nitride fibres from aoxidizing at high temperature, and accelerate molten
The floating discharge of growing up of micro-bubble in pond.Inventor also found the thermal coefficient of expansion and substrate glass base due to aluminium nitride fibres
This is consistent, therefore composite can be avoided to produce structural crack because thermal stress is larger in heat treatment process.
Worked according to the studies above, inventors herein propose aluminium nitride fibres cordierite glass-ceramic complex phase material as described below
Material and preparation method thereof.
A kind of preparation method of aluminium nitride fibres cordierite glass-ceramic composite diphase material, comprises the steps of：
Step 1, by MgO powder, SiO2Powder, Al2O3Powder and flux, Nucleating Agent are mixed into homogeneous mixture；
Step 2, the mixture is melted and is heated；
Step 3, aluminium nitride fibres in the latter stage of melting process sprayed into fusion pool and be sufficiently stirred for as equal by nitrogen
Even molten mixture；
Step 4, molten mixture is poured into the mould by preheating；
Step 5, will be poured into the molten mixture annealing in mould；
Step 6, the parent glass coring containing aluminium nitride fibres that annealing is obtained and crystallization.
Further, aluminium nitride fibres are powdered.
Further, flux is B2O3。
Further, Nucleating Agent is Cr2O3And TiO2。
Further, the weight portion of each component is respectively in step 1：MgO, 50-65 weight portion of 19-28 weight portions
SiO2, 10-26 weight portions Al2O3, 2-7 weight portions B2O3, be respectively 1-3 weight portions Cr2O3And TiO2And 8-16 weight
The aluminium nitride fibres of part.
Further, the melting heating in step 2 is carried out at a temperature of 1550-1600 DEG C.
Further, the melting heat time in step 2 is 2-5 hours.
Further, the preheating of mould is carried out at a temperature of 510-550 DEG C in step 4.
Further, annealing time is 4-8 hours in step 5.
Further, the coring in step 6 is carried out and coring 2-3 hours at a temperature of 550-750 DEG C.
Further, the crystallization in step 6 is carried out and crystallization 4-8 hours at a temperature of 750-980 DEG C.
By the above method, the efficient preparation of aluminium nitride fibres cordierite glass-ceramic composite diphase material is have effectively achieved.
Present invention also offers a kind of aluminium nitride fibres cordierite glass-ceramic composite diphase material prepared by the above method, its
Comprising following components：MgO、SiO2、Al2O3、B2O3、Cr2O3、TiO2And aluminium nitride fibres.
Brief description of the drawings
Of the invention above-mentioned and/or additional aspect and advantage will more in the description carried out to embodiment is combined with accompanying drawing
Plus substantially and be readily appreciated that, wherein：
Fig. 1 shows aluminium nitride fibres cordierite glass-ceramic composite diphase material preparation side according to an embodiment of the invention
The schematic flow sheet of method.
Specific embodiment
It should be appreciated that embodiments of the invention shown in the exemplary embodiment are merely illustrative.Although in this hair
Only a small number of embodiments have been described in detail in bright, but those skilled in the art to be readily appreciated that and depart from the present invention in not essence
In the case of the teaching of theme, various modifications are feasible.Correspondingly, all such modifications should all be included in of the invention
In the range of.Without departing from the spirit of the invention, can be to the design of following exemplary embodiment, operating condition and ginseng
Number etc. makes others and replaces, changes, changes and delete.
Embodiment one
With reference to Fig. 1, in the step s 100, by the MgO powder of 19 weight portions, the SiO of 53 weight portions2Powder, 11 weight portions
Al2O3The flux B of powder, 3 weight portions2O3The Nucleating Agent Cr of powder and respectively 2 weight portions2O3Powder and TiO2Powder
It is mixed into homogeneous mixture.Then in step s 200, said mixture is melted into 4 hours at 1540 DEG C, to ensure to mix
The abundant melting of compound.Then in the melt stage latter stage of step S200, according to shown in step S300, by the powder of 10 weight portions
Shape aluminium nitride fibres are sprayed into by nitrogen stream and bath and are sufficiently stirred for, and make aluminium nitride fibres in the mixture of melting
It is uniformly distributed so as to obtain the molten mixture containing equally distributed aluminium nitride fibres.As shown in step S400, by step
Among the cast of molten mixture that S300 is obtained enters through 550 DEG C of moulds being fully warmed-up, and anneal 3 at a temperature of 550 DEG C
Hour, obtain the parent glass of nitrogen aluminum fiber.Then in step S500, by the parent glass containing aluminium nitride fibres
Coring 2 hours at a temperature of 640 DEG C, then crystallization obtains aluminium nitride fibres cordierite crystallite glass for 4 hours at a temperature of 870 DEG C
Glass composite.
Embodiment two
With reference to Fig. 1, in the step s 100, by the MgO powder of 16 weight portions, the SiO of 52 weight portions2Powder, 11 weight portions
Al2O3The flux B of powder, 2 weight portions2O3The Nucleating Agent Cr of powder and 2 weight portions2O3The TiO of powder and 1 weight portion2
Powder is mixed into homogeneous mixture.Then in step s 200, said mixture is melted into 4 hours at 1550 DEG C, to protect
Demonstrate,prove the abundant melting of mixture.Then in the melt stage latter stage of step S200, according to shown in step S300, by 17 weight portions
Powdered aluminium nitride fibres spray into bath and are sufficiently stirred for by nitrogen stream, make aluminium nitride fibres in the mixing of melting
It is uniformly distributed in thing so as to obtain the molten mixture containing equally distributed aluminium nitride fibres.As shown in step S400, will walk
Among the molten mixture cast that rapid S300 is obtained enters through 550 DEG C of moulds being fully warmed-up, and annealed at a temperature of 550 DEG C
3 hours, the parent glass of nitrogen aluminum fiber is obtained.Then in step S500, by the basic glass containing aluminium nitride fibres
Glass coring 2 hours at a temperature of 650 DEG C, then crystallization obtains aluminium nitride fibres cordierite crystallite for 4 hours at a temperature of 880 DEG C
Glass composite material.
Embodiment three
With reference to Fig. 1, in the step s 100, by the MgO powder of 28 weight portions, the SiO of 65 weight portions2Powder, 25 weight portions
Al2O3The flux B of powder, 7 weight portions2O3The Nucleating Agent Cr of powder and 1 weight portion2O3The TiO of powder and 3 weight portions2
Powder is mixed into homogeneous mixture.Then in step s 200, said mixture is melted into 5 hours at 1550 DEG C, to protect
Demonstrate,prove the abundant melting of mixture.Then in the melt stage latter stage of step S200, according to shown in step S300, by 8 weight portions
Powdered aluminium nitride fibres spray into bath and are sufficiently stirred for by nitrogen stream, make aluminium nitride fibres in the mixing of melting
It is uniformly distributed in thing so as to obtain the molten mixture containing equally distributed aluminium nitride fibres.As shown in step S400, will walk
Among the molten mixture cast that rapid S300 is obtained enters through 490 DEG C of moulds being fully warmed-up, and annealed at a temperature of 520 DEG C
5 hours, the parent glass of nitrogen aluminum fiber is obtained.Then in step S500, by the basic glass containing aluminium nitride fibres
Glass coring 3 hours at a temperature of 550 DEG C, then crystallization obtains aluminium nitride fibres cordierite crystallite for 7 hours at a temperature of 750 DEG C
Glass composite material.
Example IV
With reference to Fig. 1, in the step s 100, by the MgO powder of 16 weight portions, the SiO of 52 weight portions2Powder, 11 weight portions
Al2O3The flux B of powder, 3 weight portions2O3The Nucleating Agent Cr of powder and 2 weight portions2O3The TiO of powder and 1 weight portion2
Powder is mixed into homogeneous mixture.Then in step s 200, said mixture is melted into 2 hours at 1600 DEG C, to protect
Demonstrate,prove the abundant melting of mixture.Then in the melt stage latter stage of step S200, according to shown in step S300, by 11 weight portions
Powdered aluminium nitride fibres spray into bath and are sufficiently stirred for by nitrogen stream, make aluminium nitride fibres in the mixing of melting
It is uniformly distributed in thing so as to obtain the molten mixture containing equally distributed aluminium nitride fibres.As shown in step S400, will walk
Among the molten mixture cast that rapid S300 is obtained enters through 540 DEG C of moulds being fully warmed-up, and annealed at a temperature of 540 DEG C
4 hours, the parent glass of nitrogen aluminum fiber is obtained.Then in step S500, by the basic glass containing aluminium nitride fibres
Glass coring 2 hours at a temperature of 740 DEG C, then crystallization obtains aluminium nitride fibres cordierite crystallite for 4 hours at a temperature of 970 DEG C
Glass composite material.
Presently preferred embodiments of the present invention is the foregoing is only, not for limiting practical range of the invention；If do not taken off
From the spirit and scope of the present invention, the present invention is modified or equivalent, all should covered in the claims in the present invention
In the middle of protection domain.
Claims (8)
1. a kind of preparation method of aluminium nitride fibres cordierite glass-ceramic composite diphase material, it is characterised in that comprise the steps of：
Step 1, by MgO powder, SiO2Powder, Al2O3Powder and flux, Nucleating Agent are mixed into homogeneous mixture；
Step 2, the mixture is melted and is heated；
Step 3, aluminium nitride fibres in the latter stage of melting process sprayed into fusion pool and be sufficiently stirred for as uniform by nitrogen
Molten mixture；
Step 4, the molten mixture is poured into the mould by preheating；
Step 5, will be poured into the molten mixture annealing in mould；
Step 6, the parent glass coring containing aluminium nitride fibres that annealing is obtained and crystallization.
2. the preparation method of aluminium nitride fibres cordierite glass-ceramic composite diphase material according to claim 1, its feature exists
In the aluminium nitride fibres are powdered.
3. the preparation method of aluminium nitride fibres cordierite glass-ceramic composite diphase material according to claim 1, its feature exists
In the flux is B2O3。
4. the preparation method of aluminium nitride fibres cordierite glass-ceramic composite diphase material according to claim 1, its feature exists
In the Nucleating Agent is Cr2O3And TiO2。
5. the preparation method of aluminium nitride fibres cordierite glass-ceramic composite diphase material according to claim 4, its feature exists
In the weight portion of each component is respectively in the step 1：The SiO of MgO, 50-65 weight portion of 19-28 weight portions2, 10-26 weight
Measure the Al of part2O3, 2-7 weight portions B2O3, 1-3 weight portions Cr2O3With the TiO of 1-3 weight portions2And the nitrogen of 8-16 weight portions
Change aluminum fiber.
6. the preparation method of aluminium nitride fibres cordierite glass-ceramic composite diphase material according to claim 1, its feature exists
In the melting heating in the step 2 is carried out at a temperature of 1550-1600 DEG C.
7. the preparation method of aluminium nitride fibres cordierite glass-ceramic composite diphase material according to claim 1, its feature exists
In the preheating of mould is carried out at a temperature of 510-550 DEG C in the step 4.
8. a kind of composite diphase material that prepared by preparation method as described in any of the above-described claim, it is characterised in that the complex phase
Material includes following components：MgO、SiO2、Al2O3、B2O3、Cr2O3、TiO2And aluminium nitride fibres.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1935739A (en) * | 2006-09-28 | 2007-03-28 | 桂林电子科技大学 | Low-sintered glass ceramic composite material and its preparing method |
| CN101648775A (en) * | 2008-10-17 | 2010-02-17 | 韦鸿雁 | High-quality and high-efficiency composite production technology of glass basis fiber composite |
| CN102336523A (en) * | 2011-06-01 | 2012-02-01 | 武汉理工大学 | High thermal conductivity rare earth/AIN/microcrystalline glass composite material and its preparation method |
| CN102531396A (en) * | 2011-12-23 | 2012-07-04 | 云南云天化股份有限公司 | Low-temperature co-fired glass ceramic composites and preparation method thereof |
| CN104496186A (en) * | 2014-12-31 | 2015-04-08 | 海南大学 | Cordierite-based nanometer glass-ceramic and preparation method thereof |
| CN106430981A (en) * | 2016-08-31 | 2017-02-22 | 望江宇花玻璃有限公司 | Cordierite-based glass ceramics containing modified fly ash and preparation process thereof |
-
2017
- 2017-02-27 CN CN201710108885.0A patent/CN106892570A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1935739A (en) * | 2006-09-28 | 2007-03-28 | 桂林电子科技大学 | Low-sintered glass ceramic composite material and its preparing method |
| CN101648775A (en) * | 2008-10-17 | 2010-02-17 | 韦鸿雁 | High-quality and high-efficiency composite production technology of glass basis fiber composite |
| CN102336523A (en) * | 2011-06-01 | 2012-02-01 | 武汉理工大学 | High thermal conductivity rare earth/AIN/microcrystalline glass composite material and its preparation method |
| CN102531396A (en) * | 2011-12-23 | 2012-07-04 | 云南云天化股份有限公司 | Low-temperature co-fired glass ceramic composites and preparation method thereof |
| CN104496186A (en) * | 2014-12-31 | 2015-04-08 | 海南大学 | Cordierite-based nanometer glass-ceramic and preparation method thereof |
| CN106430981A (en) * | 2016-08-31 | 2017-02-22 | 望江宇花玻璃有限公司 | Cordierite-based glass ceramics containing modified fly ash and preparation process thereof |
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