CN107056077A - Aluminium nitride fibres baryta fledspar devitrified glass composite diphase material and preparation method thereof - Google Patents

Aluminium nitride fibres baryta fledspar devitrified glass composite diphase material and preparation method thereof Download PDF

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Publication number
CN107056077A
CN107056077A CN201710108295.8A CN201710108295A CN107056077A CN 107056077 A CN107056077 A CN 107056077A CN 201710108295 A CN201710108295 A CN 201710108295A CN 107056077 A CN107056077 A CN 107056077A
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CN
China
Prior art keywords
aluminium nitride
nitride fibres
preparation
devitrified glass
glass composite
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Pending
Application number
CN201710108295.8A
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Chinese (zh)
Inventor
马冬阳
边妙莲
孙辉
陈士朝
吴道洪
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Jiangsu Province Metallurgical Design Institute Co Ltd
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Jiangsu Province Metallurgical Design Institute Co Ltd
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Priority to CN201710108295.8A priority Critical patent/CN107056077A/en
Publication of CN107056077A publication Critical patent/CN107056077A/en
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C14/00Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
    • C03C14/002Glass 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
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • C03B19/02Other methods of shaping glass by casting molten glass, e.g. injection moulding
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B32/00Thermal 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
    • C03B32/02Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C10/00Devitrified 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

Abstract

The invention discloses a kind of preparation method of aluminium nitride fibres baryta fledspar devitrified glass composite diphase material, it is comprised the steps of:By BaO powder, SiO2Powder, Al2O3Powder and fluxing agent, Nucleating Agent are mixed into homogeneous mixture in proportion;The mixture is melted and heated;Aluminium nitride fibres are sprayed into fusion pool and are sufficiently stirred for as uniform molten mixture by nitrogen in the latter stage of melting process;Molten mixture is poured into the mould by preheating;By the molten mixture being poured into mould annealing;To be annealed the obtained parent glass coring containing aluminium nitride fibres and crystallization obtains aluminium nitride fibres baryta fledspar devitrified glass composite diphase material.Present invention also offers a kind of aluminium nitride fibres baryta fledspar devitrified glass composite diphase material prepared by the above method, it includes following components:BaO、SiO2、Al2O3、Li2O、B2O3、ZrO2And aluminium nitride fibres.

Description

Aluminium nitride fibres baryta fledspar devitrified glass composite diphase material and preparation method thereof
Technical field
The present invention relates to glass ceramic composite field, more particularly to a kind of aluminium nitride fibres baryta fledspar devitrified glass is answered Phase material and preparation method thereof.
Background technology
Baryta fledspar devitrified glass has high heat resisting temperature, preferably high mechanical properties, anti-oxidant alkali resistant aggressivity and high The advantages of chemical stability, its extensively using and reflector substrate material, ic substrate material, the neck such as liquid crystal display Domain, but because it is crystal and the noncrystal material being combined with each other, fragility is larger and toughness is relatively low, it is therefore necessary to improve its tough Property.And because thermal conductivity factor is relatively low, its general thermal shock resistance is poor.
Devitrified glass is typically prepared using sintering process or fusion method, the baryta fledspar devitrified glass 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 problem of 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 baryta fledspar devitrified glass using fusion method in current there is no in the prior art Carry out the preparation of aluminium nitride fibres baryta fledspar devitrified glass 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 by the phase with nitrogen stream, and to be sufficiently stirred for obtaining preferable aluminium nitride fibres simultaneously scattered equal Change effect, while the nitrogen sprayed 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 can avoid composite in heat treatment process because thermal stress is larger and produces structural crack.
Worked according to the studies above, inventors herein propose following aluminium nitride fibres baryta fledspar devitrified glass composite diphase material and Its preparation method.
A kind of preparation method of aluminium nitride fibres baryta fledspar devitrified glass composite diphase material, is comprised the steps of:
Step 1, by BaO powder, SiO2Powder, Al2O3Powder and fluxing agent, Nucleating Agent are mixed into homogeneous mixture;
Step 2, mixture is melted and heated;
Step 3, aluminium nitride fibres are sprayed into fusion pool and are sufficiently stirred for be equal by nitrogen in the latter stage of melting process Even molten mixture;
Step 4, molten mixture is poured into the mould by preheating;
Step 5, the molten mixture being poured into mould is annealed;
Step 6, by the obtained parent glass coring containing aluminium nitride fibres and the crystallization of annealing.
Further, aluminium nitride fibres are powdered.
Further, fluxing agent is Li2O and B2O3
Further, Nucleating Agent is ZrO2
Further, the parts by weight of each component are respectively in step 1:BaO, 24-34 parts by weight of 27-39 parts by weight SiO2, 22-31 parts by weight Al2O3, be respectively 2-4 parts by weight Li2O and B2O3, 1-3 parts by weight ZrO2And 11-20 weights Measure the aluminium nitride fibres of part.
Further, the melting heating in step 2 is carried out at a temperature of 1630-1700 DEG C.
Further, the melting heat time in step 2 is 2-4 hours.
Further, the preheating of mould is carried out at a temperature of 550-750 DEG C in step 4.
Further, annealing time is 2-4 hours in step 5.
Further, the coring in step 6 carries out simultaneously coring 2-3 hours at a temperature of 600-800 DEG C.
Further, the crystallization in step 6 carries out simultaneously crystallization 2-4 hours at a temperature of 800-1050 DEG C.
By the above method, the efficient preparation of aluminium nitride fibres baryta fledspar devitrified glass composite diphase material have effectively achieved.
Present invention also offers a kind of aluminium nitride fibres baryta fledspar devitrified glass composite diphase material prepared by the above method, its Include following components:BaO、SiO2、Al2O3、Li2O、B2O3、ZrO2And aluminium nitride fibres.
Brief description of the drawings
The above-mentioned and/or additional aspect and advantage of the present invention 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 baryta fledspar devitrified glass composite diphase material preparation side according to an embodiment of the invention The schematic flow sheet of method.
Embodiment
It should be appreciated that shown embodiments of the invention are merely illustrative in the exemplary embodiment.Although in this hair Only a small number of embodiments are described in detail in bright, but those skilled in the art are readily appreciated that and depart from the present invention in not essence In the case of the teaching of theme, a variety of modifications are feasible.Correspondingly, all such modifications should all be included in the present invention's In the range of.Without departing from the spirit of the invention, design, operating condition and ginseng that can be to following exemplary embodiment Number etc. makes others and replaces, changes, changes and delete.
Embodiment one
With reference to Fig. 1, in the step s 100, by the BaO powder of 29 parts by weight, the SiO of 30 parts by weight2Powder, 22 parts by weight Al2O3The fluxing agent of powder, respectively 2 parts by weight is Li2O powder and B2O3The Nucleating Agent ZrO of powder and 2 parts by weight2Powder End is mixed into homogeneous mixture.Then in step s 200, said mixture is melted into 3 hours at 1650 DEG C, to ensure The abundant melting of mixture.Then in step S200 melt stage latter stage, according to shown in step S300, by the powder of 13 parts by weight Last shape aluminium nitride fibres spray into bath by nitrogen stream and are sufficiently stirred for, and make aluminium nitride fibres in the mixture of melting In be uniformly distributed so as to obtaining 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 580 DEG C of moulds being fully warmed-up, and anneal at a temperature of 580 DEG C 3 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 650 DEG C, then crystallization obtains aluminium nitride fibres baryta fledspar 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 BaO powder of 31 parts by weight, the SiO of 32 parts by weight2Powder, 22 parts by weight Al2O3The fluxing agent of powder, respectively 2 parts by weight is Li2O powder and B2O3The Nucleating Agent ZrO of powder and 2 parts by weight2Powder End is mixed into homogeneous mixture.Then in step s 200, said mixture is melted into 3 hours at 1650 DEG C, to ensure The abundant melting of mixture.Then in step S200 melt stage latter stage, according to shown in step S300, by the powder of 11 parts by weight Last shape aluminium nitride fibres spray into bath by nitrogen stream and are sufficiently stirred for, and make aluminium nitride fibres in the mixture of melting In be uniformly distributed so as to obtaining 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 580 DEG C of moulds being fully warmed-up, and anneal at a temperature of 580 DEG C 3 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 630 DEG C, then crystallization obtains aluminium nitride fibres baryta fledspar crystallite glass for 4 hours at a temperature of 850 DEG C Glass composite.
Embodiment three
With reference to Fig. 1, in the step s 100, by the BaO powder of 39 parts by weight, the SiO of 24 parts by weight2Powder, 31 parts by weight Al2O3The fluxing agent of powder, respectively 4 parts by weight is Li2O powder and B2O3The Nucleating Agent ZrO of powder and 1 parts by weight2Powder End is mixed into homogeneous mixture.Then in step s 200, said mixture is melted into 4 hours at 1660 DEG C, to ensure The abundant melting of mixture.Then in step S200 melt stage latter stage, according to shown in step S300, by the powder of 19 parts by weight Last shape aluminium nitride fibres spray into bath by nitrogen stream and are sufficiently stirred for, and make aluminium nitride fibres in the mixture of melting In be uniformly distributed so as to obtaining 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 740 DEG C of moulds being fully warmed-up, and anneal at a temperature of 740 DEG C 2 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 780 DEG C, then crystallization obtains aluminium nitride fibres baryta fledspar crystallite for 2 hours at a temperature of 1040 DEG C Glass composite material.
Example IV
With reference to Fig. 1, in the step s 100, by the BaO powder of 31 parts by weight, the SiO of 32 parts by weight2Powder, 22 parts by weight Al2O3The fluxing agent of powder, respectively 2 parts by weight is Li2O powder and B2O3The Nucleating Agent ZrO of powder and 3 parts by weight2Powder End is mixed into homogeneous mixture.Then in step s 200, said mixture is melted into 2 hours at 1680 DEG C, to ensure The abundant melting of mixture.Then in step S200 melt stage latter stage, according to shown in step S300, by the powder of 11 parts by weight Last shape aluminium nitride fibres spray into bath by nitrogen stream and are sufficiently stirred for, and make aluminium nitride fibres in the mixture of melting In be uniformly distributed so as to obtaining 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 580 DEG C of moulds being fully warmed-up, and anneal at a temperature of 580 DEG C 4 Hour, obtain the parent glass of nitrogen aluminum fiber.Then in step S500, by the parent glass containing aluminium nitride fibres Coring 3 hours at a temperature of 630 DEG C, then crystallization obtains aluminium nitride fibres baryta fledspar crystallite glass for 4 hours at a temperature of 850 DEG C Glass composite.
The foregoing is only presently preferred embodiments of the present invention, not for limit the present invention practical range;If do not taken off From the spirit and scope of the present invention, the present invention is modified or equivalent substitution, all should covered in the claims in the present invention Among protection domain.

Claims (8)

1. a kind of preparation method of aluminium nitride fibres baryta fledspar devitrified glass composite diphase material, it is characterised in that comprise the steps of:
Step 1, by BaO powder, SiO2Powder, Al2O3Powder and fluxing agent, Nucleating Agent are mixed into homogeneous mixture;
Step 2, the mixture is melted and heated;
Step 3, aluminium nitride fibres are sprayed into fusion pool and are sufficiently stirred for be uniform by nitrogen in the latter stage of melting process Molten mixture;
Step 4, the molten mixture is poured into the mould by preheating;
Step 5, the molten mixture being poured into mould is annealed;
Step 6, by the obtained parent glass coring containing aluminium nitride fibres and the crystallization of annealing.
2. the preparation method of aluminium nitride fibres baryta fledspar devitrified glass 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 baryta fledspar devitrified glass composite diphase material according to claim 1, its feature exists In the fluxing agent is Li2O and B2O3
4. the preparation method of aluminium nitride fibres baryta fledspar devitrified glass composite diphase material according to claim 1, its feature exists In the Nucleating Agent is ZrO2
5. the preparation method of aluminium nitride fibres baryta fledspar devitrified glass composite diphase material according to claim 4, its feature exists In the parts by weight of each component are respectively in the step 1:The SiO of BaO, 24-34 parts by weight of 27-39 parts by weight2, 22-31 weight Measure the Al of part2O3, be respectively 2-4 parts by weight Li2O and B2O3, 1-3 parts by weight ZrO2And the aluminium nitride of 11-20 parts by weight Fiber.
6. the preparation method of aluminium nitride fibres baryta fledspar devitrified glass 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 1630-1700 DEG C.
7. the preparation method of aluminium nitride fibres baryta fledspar devitrified glass composite diphase material according to claim 1, its feature exists In the melting heat time in the step 2 is 2-4 hours.
8. a kind of composite diphase material 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:BaO、SiO2、Al2O3、Li2O、B2O3、ZrO2And aluminium nitride fibres.
CN201710108295.8A 2017-02-27 2017-02-27 Aluminium nitride fibres baryta fledspar devitrified glass composite diphase material and preparation method thereof Pending CN107056077A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1101027A (en) * 1993-09-29 1995-04-05 中国建筑材料科学研究院 Technology for production of fiber reinforced glass and glass-ceramic base composite material
CN101648775A (en) * 2008-10-17 2010-02-17 韦鸿雁 High-quality and high-efficiency composite production technology of glass basis fiber composite
CN105174725A (en) * 2015-08-17 2015-12-23 昆明理工大学 Microcrystalline glass and preparation method thereof
CN105948515A (en) * 2016-05-11 2016-09-21 张书诚 High-strength glass ceramics and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1101027A (en) * 1993-09-29 1995-04-05 中国建筑材料科学研究院 Technology for production of fiber reinforced glass and glass-ceramic base composite material
CN101648775A (en) * 2008-10-17 2010-02-17 韦鸿雁 High-quality and high-efficiency composite production technology of glass basis fiber composite
CN105174725A (en) * 2015-08-17 2015-12-23 昆明理工大学 Microcrystalline glass and preparation method thereof
CN105948515A (en) * 2016-05-11 2016-09-21 张书诚 High-strength glass ceramics and preparation method thereof

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