CN106830694A - A kind of preparation method of aluminium nitride fibres-diopside devitrified glass composite diphase material - Google Patents
A kind of preparation method of aluminium nitride fibres-diopside devitrified glass composite diphase material Download PDFInfo
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- CN106830694A CN106830694A CN201710108648.4A CN201710108648A CN106830694A CN 106830694 A CN106830694 A CN 106830694A CN 201710108648 A CN201710108648 A CN 201710108648A CN 106830694 A CN106830694 A CN 106830694A
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- aluminium nitride
- glass
- nitride fibres
- diopside
- weight portions
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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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
-
- 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
-
- 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
Abstract
The invention discloses a kind of preparation method of aluminium nitride fibres-diopside devitrified glass composite diphase material, the method includes：By CaO powder, MgO powder, SiO2Powder, Al2O3Powder, is well mixed by a certain percentage with flux, Nucleating Agent etc., is melted 26 hours under 1,450 1500 DEG C of air atmospheres；By melt stage latter stage, certain proportion aluminium nitride fibres are sprayed into bath and be stirred by nitrogen stream and is allowed to be uniformly distributed, during the fused raw material casting containing aluminium nitride fibres passed into the mould of preheating afterwards, annealed at a certain temperature again, the parent glass of nitrogen aluminum fiber is obtained.Parent glass is carried out into coring and Crystallizing treatment, makes parent glass crystallization completely, that is, obtain aluminium nitride fibres-diopside devitrified glass composite diphase material.There is aluminium nitride fibres enhancing diopside microcrystal glass material thermal shock resistance to significantly improve obtained in the method, and the porosity is far below Sintering of Glass-Ceramics, and aluminium nitride fibres are tightly combined with substrate glass, the features such as toughness of material is greatly improved.
Description
Technical field
The present invention relates to glass ceramic composite field, more particularly to a kind of aluminium nitride fibres-diopside devitrified glass
The preparation method of composite diphase material.
Background technology
Diopside devitrified glass is a kind of devitrified glass of excellent performance, with wearability and intensity very high very high,
But its general fragility is higher and toughness is relatively low, and because thermal conductivity factor is relatively low, its general thermal shock resistance is poor.
Aluminium nitride fibres belong to DLC nitride, and highest can be stabilized to 2200 DEG C, good mechanical property, and rupture strength is higher than
Al2O3Ceramics, and intensity is slower with the rising decline of temperature.Thermal conductivity is good, and thermal conductivity is (about 200W/mK) high, is Al2O35
It is good heat shock resistance material more than times, thermal coefficient of expansion is small, about 4.5 × 10-6 DEG C, close with microcrystal glass material.
If diopside devitrified glass and aluminium nitride are combined, on the one hand aluminium nitride fibres can increase substantially brightness
The mechanical strength of stone devitrified glass, on the one hand due to its good thermal conductivity, contributes to the heat conduction of diopside glass-ceramic matrix
The raising of ability, can greatly improve the thermal shock resistance of diopside devitrified glass.
Devitrified glass is typically prepared using sintering process or fusion method, and the devitrified glass volume that wherein prepared by fusion method is close
Degree 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 has to
Solve the problems, such as that aluminium nitride fibres are easily oxidized at high temperature；Secondary solution aluminium nitride fibres are equally distributed in the melt asks for its
Topic.
There is no at present aluminium nitride fibres are combined with diopside devitrified glass using fusion method, prepare aluminium nitride fine
The report of dimension-diopside devitrified glass composite diphase material.
The content of the invention
It is contemplated that at least solving one of technical problem present in prior art.Therefore, one object of the present invention
It is to propose a kind of preparation method of aluminium nitride fibres-diopside devitrified glass composite diphase material, wherein, aluminium nitride fibres-thoroughly
Pyroxene crystallites glass complex phase material has that good thermal shock, wearability are high, intensity is high, toughness is high, can make as functional material
With the method is with CaO powder, MgO, SiO2Powder, Al2O3Powder etc. adds a certain proportion of flux as primary raw material
CaF2, Nucleating Agent P2O5With TiO2Deng, raw materials melt is turned into by liquid by fusion method, aluminium nitride fibres are led in melting latter stage
Cross nitrogen stream and spray into and bath and stir, then cast, annealing obtains the parent glass of nitrogen aluminum fiber, parent glass
It is again that can obtain aluminium nitride fibres-diopside devitrified glass composite diphase material by heat treatment processes such as coring, crystallization.
Inventor through numerous studies, creatively using Melting Synthesis, answer by aluminium nitride fibres-diopside devitrified glass
Phase material.Inventor has found that aluminium nitride fibres are sprayed into bath with nitrogen stream in melt zone latter stage stirs and can obtain simultaneously
Preferable aluminium nitride fibres dispersion homo-effect.The nitrogen for spraying into simultaneously can manufacture non-oxidizing environment prevents aluminium nitride fibres
Aoxidize at high temperature, and accelerate the floating discharge of growing up of micro-bubble in molten bath.Inventor is had found due to the heat of aluminium nitride fibres
The coefficient of expansion is basically identical with substrate glass, therefore composite can be avoided to be produced because thermal stress is larger in heat treatment process
Raw structural crack.The method effectively realizes the efficient preparation of aluminium nitride fibres-diopside devitrified glass composite diphase material.
Thus, according to an aspect of the present invention, the invention provides a kind of aluminium nitride fibres-diopside devitrified glass
The preparation method of composite diphase material, the method includes：
By CaO powder, MgO, SiO2Powder, Al2O3Powder, flux, Nucleating Agent are mixed in proportion, to obtain
Mixed material；
By the mixed material in 1450-1500 DEG C or so melting, to obtain molten state raw material；
Aluminium nitride fibres are sprayed into bath by nitrogen injection in melt zone latter stage and is stirred, nitrogen is nitrogenized in protection
While aluminum fiber is not oxidized, it is uniformly distributed aluminium nitride fibres and promotes the micro-bubble in molten bath to grow up and discharge；
The fused raw material of aluminium nitride fibres that is mixed with is cast among preheated mould again by annealing, with
Obtain the parent glass of nitrogen aluminum fiber；
The parent glass of nitrogen aluminum fiber has just obtained aluminium nitride fibres-diopside crystallite by nucleus crystallization process
Glass complex phase material.
In addition, can also have following additional technical feature according to the present invention：
Embodiments in accordance with the present invention, chemical composition CaO, MgO, SiO2、Al2O3Content range be respectively CaO 13-22
Weight portion, MgO 8-17 weight portions, SiO247-62 weight portions, Al2O36-13 weight portions.
Embodiments in accordance with the present invention, the flux of addition is CaF2, Nucleating Agent is P2O5With TiO2, its content is CaF21-
4 weight portions, P2O5And TiO2Respectively 2-6 weight portions.
Embodiments in accordance with the present invention, above-mentioned raw materials are mixed in proportion, and 2-6 is melted at 1450-1500 DEG C
Hour, it is ensured that raw material can be melted fully.
Embodiments in accordance with the present invention, lead to the aluminium nitride fibres of 13-20 weight portions in melt zone latter stage by a certain percentage
Cross nitrogen stream to spray into bath and stir, nitrogen can protect aluminium nitride fibres not to be oxidized at high temperature, and realize aluminium nitride
Fiber being uniformly distributed in the melt, and promote the minute bubbles for being difficult discharge in melt to float to grow up and discharge, finally give and contain
There is the fused raw material of aluminium nitride fibres.
Embodiments in accordance with the present invention, are carried out among fused raw material casting is passed into the 450-510 DEG C of mould of preheating
Casting, obtains the parent glass of nitrogen aluminum fiber.
Embodiments in accordance with the present invention, the parent glass of nitrogen aluminum fiber needs to be annealed 2-5 hours at 450-510 DEG C.
Embodiments in accordance with the present invention, the parent glass of nitrogen aluminum fiber 500-700 DEG C coring 2-4 hours, then
700-950 DEG C, obtain within coring 2-5 hours aluminium nitride fibres-diopside glass ceramic composite.
Additional aspect of the invention and advantage will be set forth in part in the description, and will partly become from the following description
Obtain substantially, or recognized by practice of the invention.
Brief description of the drawings
Of the invention above-mentioned and/or additional aspect and advantage will become from the following description of the accompanying drawings of embodiments
It is apparent and be readily appreciated that, wherein：
Fig. 1 shows and according to an embodiment of the invention prepares aluminium nitride fibres-diopside devitrified glass composite diphase material
Method schematic flow sheet.
Specific embodiment
Embodiments of the invention are described below in detail, the example of the embodiment is shown in the drawings, wherein from start to finish
Same or similar label represents same or similar element or the element with same or like function.Below with reference to attached
It is exemplary to scheme the embodiment of description, is only used for explaining the present invention, and is not considered as limiting the invention.
According to an aspect of the present invention, the invention provides a kind of aluminium nitride fibres-diopside devitrified glass complex phase material
The preparation method of material.With reference to Fig. 1, embodiments in accordance with the present invention, the preparation to the aluminium nitride fibres-diopside devitrified glass
Method is explained, and the method includes：
S100 mixes in proportion
Embodiments in accordance with the present invention, by CaO powder, MgO powder, SiO2Powder, Al2O3Powder, flux CaF2, it is brilliant
Core agent P2O5With TiO2Mix in proportion, the content range of each composition is CaO 13-22 weight portions, MgO 8-17 weight portions,
SiO247-62 weight portions, Al2O36-13 weight portions, CaF21-4 weight portions, P2O52-6 weight portions, TiO22-6 weight portions,
Above material is sufficiently mixed uniformly in proportion, has obtained preparing the primary raw material of diopside devitrified glass；
S200 is fully melted
Embodiments in accordance with the present invention, the primary raw material of the diopside devitrified glass is added in 1450-1500 DEG C of melting
It is hot 2-6 hours, material is fully melted homogenizing, each chemical constituents analysis uniform.
S300 aluminium nitride fibres are sprayed into and stirred
Embodiments in accordance with the present invention, in melt zone latter stage, by the aluminium nitride fibres powder end of 13-20 weight portions with nitrogen
Stream sprays into bath and stirs, and obtains the fused raw material containing aluminium nitride fibres.
The effect of nitrogen stream has three, and first is manufacture non-oxidizing atmosphere, protects aluminium nitride fibres powder end inexcessive
Oxidation；Second is to promote aluminium nitride fibres powder end in the dispersed of bath；3rd be promote fused raw material in it is original
Micro-bubble floating of growing up.
S400 casts and anneals
Embodiments in accordance with the present invention, 450-510 DEG C is passed into advance by the fused raw material casting containing aluminium nitride fibres
In the mould of heat, annealing 2-5 lowered the temperature with stove again after as a child, obtained the parent glass of nitrogen aluminum fiber；
S500 coring and crystallization
Embodiments in accordance with the present invention, by the parent glass of nitrogen aluminum fiber coring 4-8 hours at 500-700 DEG C,
700-900 DEG C is warming up to again crystallization 4-8 hours, obtain aluminium nitride fibres-diopside devitrified glass composite diphase material.
The preparation method of aluminium nitride fibres according to embodiments of the present invention-diopside devitrified glass composite diphase material, using nitrogen
Gas blowout is blown and realizes aluminium nitride fibres being uniformly distributed in molten bath, and the parent glass for obtaining is combined very tight with aluminium nitride fibres
It is close.
Below with reference to specific embodiment, the present invention will be described, it is necessary to explanation, these embodiments are only explanation
Property, and be not considered as limiting the invention.
Embodiment 1
In the present embodiment, with the weight portions of CaO 13, the weight portions of MgO 11, SiO249 weight portions, Al2O36 weight portions, CaF2
2 weight portions, P2O52 weight portions, TiO22 weight portions are the master for preparing aluminium nitride fibres-diopside devitrified glass composite diphase material
Material is wanted, specific method is as follows：
Above-mentioned material is mixed in proportion in step S100,3 hours is melted at 1500 DEG C, it is ensured that raw material energy
Fully melting.
The aluminium nitride fibres of 14 weight portions are sprayed into bath simultaneously by nitrogen stream in melt zone latter stage in step S200
Stirring, to realize being uniformly distributed for aluminium nitride fibres, finally gives the fused raw material containing aluminium nitride fibres.
Among fused raw material casting is passed into 510 DEG C of moulds being fully warmed-up by step S300, and in 510 DEG C of annealing
3 hours, the parent glass of nitrogen aluminum fiber is obtained.
Step S400 nitrogen aluminum fibers parent glass in 650 DEG C of coring 2 hours, then in 850 DEG C of crystallization 4 hours
To aluminium nitride fibres-diopside glass ceramic composite.
Embodiment 2
In the present embodiment, with the weight portions of CaO 15, the weight portions of MgO 10, SiO248 weight portions, Al2O36 weight portions,
CaF24 weight portions, P2O52 weight portions, TiO22 weight portions are to prepare aluminium nitride fibres-diopside devitrified glass composite diphase material
Main material, specific method is as follows：
Above-mentioned material is mixed in proportion in step S100,4 hours is melted at 1490 DEG C, it is ensured that raw material energy
Fully melting.
The aluminium nitride fibres of 13 weight portions are sprayed into bath simultaneously by nitrogen stream in melt zone latter stage in step S200
Stirring, to realize being uniformly distributed for aluminium nitride fibres, the nitrogen being blown into can also make to be difficult the minute bubbles floating length of discharge in melt
It is big and discharge, finally give the fused raw material containing aluminium nitride fibres.
Cast among fused raw material casting is passed into 470 DEG C of moulds of preheating by step S300, and at 470 DEG C
Annealing 2 hours, obtains the parent glass of nitrogen aluminum fiber.
Step S400 nitrogen aluminum fibers parent glass in 630 DEG C of coring 2 hours, then in 830 DEG C of crystallization 4 hours
To aluminium nitride fibres-diopside glass ceramic composite.
Embodiment 3
In the present embodiment, with the weight portions of CaO 13, the weight portions of MgO 17, SiO247 weight portions, Al2O313 weight portions,
CaF21 weight portion, P2O52 weight portions, TiO22 weight portions are to prepare aluminium nitride fibres-diopside devitrified glass composite diphase material
Main material, specific method is as follows：
Above-mentioned material is mixed in proportion in step S100,2 hours is melted at 1460 DEG C, it is ensured that raw material energy
Fully melting.
The aluminium nitride fibres of 13 weight portions are sprayed into bath simultaneously by nitrogen stream in melt zone latter stage in step S200
Stirring, to realize being uniformly distributed for aluminium nitride fibres, the nitrogen being blown into can also make to be difficult the minute bubbles floating length of discharge in melt
It is big and discharge, finally give the fused raw material containing aluminium nitride fibres.
Cast among fused raw material casting is passed into 450 DEG C of moulds of preheating by step S300, and at 450 DEG C
Annealing 5 hours, obtains the parent glass of nitrogen aluminum fiber.
Step S400 nitrogen aluminum fibers parent glass in 500 DEG C of coring 4 hours, then in 700 DEG C of crystallization 5 hours
To aluminium nitride fibres-diopside glass ceramic composite.
Embodiment 4
In the present embodiment, with the weight portions of CaO 13, the weight portions of MgO 8, SiO262 weight portions, Al2O36 weight portions, CaF2
4 weight portions, P2O56 weight portions, TiO26 weight portions are the master for preparing aluminium nitride fibres-diopside devitrified glass composite diphase material
Material is wanted, specific method is as follows：
Above-mentioned material is mixed in proportion in step S100,6 hours is melted at 1500 DEG C, it is ensured that raw material energy
Fully melting.
The aluminium nitride fibres of 20 weight portions are sprayed into bath simultaneously by nitrogen stream in melt zone latter stage in step S200
Stirring, to realize being uniformly distributed for aluminium nitride fibres, the nitrogen being blown into can also make to be difficult the minute bubbles floating length of discharge in melt
It is big and discharge, finally give the fused raw material containing aluminium nitride fibres.
Cast among fused raw material casting is passed into 480 DEG C of moulds of preheating by step S300, and at 480 DEG C
Annealing 2 hours, obtains the parent glass of nitrogen aluminum fiber.
Step S400 nitrogen aluminum fibers parent glass in 700 DEG C of coring 2 hours, then in 950 DEG C of crystallization 2 hours
To aluminium nitride fibres-diopside glass ceramic composite.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means to combine specific features, structure, material or spy that the embodiment or example are described
Point is contained at least one embodiment of the invention or example.In this manual, to the schematic representation of above-mentioned term not
Necessarily refer to identical embodiment or example.And, the specific features of description, structure, material or feature can be any
One or more embodiments or example in combine in an appropriate manner.
Although an embodiment of the present invention has been shown and described, it will be understood by those skilled in the art that：Not
Can these embodiments be carried out with various changes, modification, replacement and modification in the case of departing from principle of the invention and objective, this
The scope of invention is limited by claim and its equivalent.
Claims (10)
1. the preparation method of a kind of aluminium nitride fibres-diopside devitrified glass composite diphase material, it is comprised the following steps：
(1) by CaO powder, MgO powder, SiO2Powder, Al2O3Powder, flux, Nucleating Agent mix by a certain percentage, are mixed
Compound material；
(2) mixed material is melted and is heated, sprayed into aluminium nitride fibres powder by nitrogen injection in melt zone latter stage molten
Pond inside is simultaneously sufficiently stirred for, and obtains the fused raw material containing aluminium nitride fibres；
(3) in fused raw material casting being passed into the mould of preheating, annealing obtains the parent glass of nitrogen aluminum fiber；
(4) by parent glass coring, the crystallization of the nitrogen aluminum fiber, make the parent glass crystallization completely, nitrogenized
Aluminum fiber-diopside devitrified glass composite diphase material.
2. method according to claim 1, it is characterised in that CaO, MgO, SiO in the step (1)2、Al2O3Ratio
Respectively CaO 13-22 weight portions, MgO 8-17 weight portions, SiO247-62 weight portions, Al2O36-13 weight portions.
3. method according to claim 1, it is characterised in that flux described in the step (2) is CaF2, the crystalline substance
Core agent is P2O5With TiO2。
4. method according to claim 3, it is characterised in that the flux CaF2Additional proportion be 1-4 weight portions,
The Nucleating Agent P2O5With TiO2Additional proportion be respectively 2-6 weight portions.
5. method according to claim 1, it is characterised in that the melting heating of mixed material described in the step (2) is
2-6 hour is melted at 1450-1500 DEG C.
6. method according to claim 1, it is characterised in that the aluminium nitride fibres powder added in the step (2)
The weight portion at end is 13-20.
7. method according to claim 1, it is characterised in that mould described in the step (3) is pre- at 450-510 DEG C
Heat.
8. method according to claim 1, it is characterised in that annealing process is described in the step (3)：In 450-
510 DEG C are annealed 2-5 hours.
9. method according to claim 1, it is characterised in that the basis of nitrogen aluminum fiber described in the step (4)
The coring of glass, crystallization process are：Coring 4-8 hours at 500-700 DEG C, then to be warming up to 700-900 DEG C of crystallization 4-8 small
When.
10. aluminium nitride fibres-diopside crystallite glass that any described method is prepared in a kind of 1-9 according to claim
Glass.
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Citations (3)
| 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 |
| CN101805128A (en) * | 2010-04-20 | 2010-08-18 | 香港福山实业有限公司 | Jade-type glass-ceramic and preparation method thereof |
-
2017
- 2017-02-27 CN CN201710108648.4A patent/CN106830694A/en active Pending
Patent Citations (3)
| 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 |
| CN101805128A (en) * | 2010-04-20 | 2010-08-18 | 香港福山实业有限公司 | Jade-type glass-ceramic and preparation method thereof |
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