CN106892569A - Aluminium nitride fibres Phlogopite Based Glass-Ceramics composite diphase material and preparation method thereof - Google Patents
Aluminium nitride fibres Phlogopite Based Glass-Ceramics composite diphase material and preparation method thereof Download PDFInfo
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- CN106892569A CN106892569A CN201710107898.6A CN201710107898A CN106892569A CN 106892569 A CN106892569 A CN 106892569A CN 201710107898 A CN201710107898 A CN 201710107898A CN 106892569 A CN106892569 A CN 106892569A
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- aluminium nitride
- nitride fibres
- phlogopite
- based glass
- powder
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Classifications
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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
- 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
-
- 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 Phlogopite Based Glass-Ceramics composite diphase material, it is comprised the steps of:By K2CO3Powder, 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 Phlogopite Based Glass-Ceramics composite diphase material.Present invention also offers a kind of aluminium nitride fibres Phlogopite Based Glass-Ceramics composite diphase material prepared by the above method, it includes following components:K2CO3、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 Phlogopite Based Glass-Ceramics are answered
Phase material and preparation method thereof.
Background technology
Phlogopite Based Glass-Ceramics have the advantages that machinability is good, but because its fragility is larger, toughness is relatively low, therefore limitation
Its range of application.
Devitrified glass is typically prepared using sintering process or fusion method, the Phlogopite Based Glass-Ceramics that wherein prepared by fusion method
With preferable toughening effect, but there are many deficiencies in sintering process, mainly there is devitrified glass volume density phase prepared by sintering process
To relatively low, the porosity is higher, the problems such as glass-ceramic matrix is combined poor with fiber.
Aluminium nitride fibres are combined with Phlogopite Based Glass-Ceramics using fusion method in current there is no in the prior art
Carry out the preparation of aluminium nitride fibres Phlogopite Based Glass-Ceramics 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 Phlogopite Based Glass-Ceramics complex phase material as described below
Material and preparation method thereof.
A kind of preparation method of aluminium nitride fibres Phlogopite Based Glass-Ceramics composite diphase material, comprises the steps of:
Step 1, by K2CO3Powder, MgO powder, SiO2Powder, Al2O3Powder and flux B2O3, Nucleating Agent is 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, Nucleating Agent is Cr2O3And TiO2。
Further, the weight portion of each component is respectively in step 1:The K of 4-9 weight portions2CO3, 15-22 weight portions
The SiO of MgO, 44-60 weight portion2, 10-17 weight portions Al2O3, 3-8 weight portions B2O3, be respectively 1-3 weight portions Cr2O3
And TiO2And the aluminium nitride fibres of 10-20 weight portions.
Further, the melting heating in step 2 is carried out at a temperature of 1380-1420 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 530-590 DEG C in step 4.
Further, annealing time is 2-4 hours in step 5.
Further, the coring in step 6 is carried out and coring 2-3 hours at a temperature of 550-730 DEG C.
Further, the crystallization in step 6 is carried out and crystallization 2-4 hours at a temperature of 730-930 DEG C.
By the above method, the efficient preparation of aluminium nitride fibres Phlogopite Based Glass-Ceramics composite diphase material is have effectively achieved.
Present invention also offers a kind of aluminium nitride fibres Phlogopite Based Glass-Ceramics composite diphase material prepared by the above method, its
Comprising following components:K2CO3、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 Phlogopite Based Glass-Ceramics 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 K of 5 weight portions2CO3Powder, by the MgO powder of 16 weight portions, 47 weight portions
SiO2The Al of powder, 11 weight portions2O3The flux B of powder, 4 weight portions2O3Powder and the respectively Nucleating Agent of 2 weight portions
Cr2O3Powder and TiO2Powder is mixed into homogeneous mixture.Then in step s 200, said mixture is melted at 1410 DEG C
Melt 4 hours, to ensure the abundant melting of mixture.Then in the melt stage latter stage of step S200, according to step S300 institutes
Show, by the powdered aluminium nitride fibres of 13 weight portions are by nitrogen stream penetrating bath and are sufficiently stirred for, make aluminium nitride
Fiber is uniformly distributed so as to obtain the molten mixture containing equally distributed aluminium nitride fibres in the mixture of melting.As walked
Shown in rapid S400, among the molten mixture cast that step S300 is obtained enters through 580 DEG C of moulds being fully warmed-up, and
Annealed 3 hours at a temperature of 580 DEG C, obtained the parent glass of nitrogen aluminum fiber.Then in step S500, nitrogen will be contained
The parent glass of change aluminum fiber coring 2 hours at a temperature of 640 DEG C, then crystallization is nitrogenized for 4 hours at a temperature of 870 DEG C
Aluminum fiber Phlogopite Based Glass-Ceramics composite.
Embodiment two
With reference to Fig. 1, in the step s 100, by the K of 6 weight portions2CO3Powder, by the MgO powder of 16 weight portions, 45 weight portions
SiO2The Al of powder, 10 weight portions2O3The flux B of powder, 5 weight portions2O3Powder and the respectively Nucleating Agent of 2 weight portions
Cr2O3Powder and TiO2Powder is mixed into homogeneous mixture.Then in step s 200, said mixture is melted at 1380 DEG C
Melt 3 hours, to ensure the abundant melting of mixture.Then in the melt stage latter stage of step S200, according to step S300 institutes
Show, by the powdered aluminium nitride fibres of 11 weight portions are by nitrogen stream penetrating bath and are sufficiently stirred for, make aluminium nitride
Fiber is uniformly distributed so as to obtain the molten mixture containing equally distributed aluminium nitride fibres in the mixture of melting.As walked
Shown in rapid S400, among the molten mixture cast that step S300 is obtained enters through 570 DEG C of moulds being fully warmed-up, and
Annealed 3 hours at a temperature of 570 DEG C, obtained the parent glass of nitrogen aluminum fiber.Then in step S500, nitrogen will be contained
The parent glass of change aluminum fiber coring 2 hours at a temperature of 630 DEG C, then crystallization is nitrogenized for 4 hours at a temperature of 850 DEG C
Aluminum fiber Phlogopite Based Glass-Ceramics composite.
Embodiment three
With reference to Fig. 1, in the step s 100, by the K of 4 weight portions2CO3Powder, by the MgO powder of 15 weight portions, 44 weight portions
SiO2The Al of powder, 17 weight portions2O3The flux B of powder, 3 weight portions2O3Powder and the respectively Nucleating Agent of 1 weight portion
Cr2O3Powder and TiO2Powder is mixed into homogeneous mixture.Then in step s 200, said mixture is melted at 1420 DEG C
Melt 2 hours, to ensure the abundant melting of mixture.Then in the melt stage latter stage of step S200, according to step S300 institutes
Show, by the powdered aluminium nitride fibres of 10 weight portions are by nitrogen stream penetrating bath and are sufficiently stirred for, make aluminium nitride
Fiber is uniformly distributed so as to obtain the molten mixture containing equally distributed aluminium nitride fibres in the mixture of melting.As walked
Shown in rapid S400, among the molten mixture cast that step S300 is obtained enters through 550 DEG C of moulds being fully warmed-up, and
Annealed 4 hours at a temperature of 550 DEG C, obtained the parent glass of nitrogen aluminum fiber.Then in step S500, nitrogen will be contained
The parent glass of change aluminum fiber coring 3 hours at a temperature of 560 DEG C, then crystallization is nitrogenized for 2 hours at a temperature of 920 DEG C
Aluminum fiber Phlogopite Based Glass-Ceramics composite.
Example IV
With reference to Fig. 1, in the step s 100, by the K of 9 weight portions2CO3Powder, by the MgO powder of 22 weight portions, 60 weight portions
SiO2The Al of powder, 11 weight portions2O3The flux B of powder, 8 weight portions2O3Powder and the respectively Nucleating Agent of 3 weight portions
Cr2O3Powder and TiO2Powder is mixed into homogeneous mixture.Then in step s 200, said mixture is melted at 1400 DEG C
Melt 3 hours, to ensure the abundant melting of mixture.Then in the melt stage latter stage of step S200, according to step S300 institutes
Show, by the powdered aluminium nitride fibres of 20 weight portions are by nitrogen stream penetrating bath and are sufficiently stirred for, make aluminium nitride
Fiber is uniformly distributed so as to obtain the molten mixture containing equally distributed aluminium nitride fibres in the mixture of melting.As walked
Shown in rapid S400, among the molten mixture cast that step S300 is obtained enters through 570 DEG C of moulds being fully warmed-up, and
Annealed 2 hours at a temperature of 570 DEG C, obtained the parent glass of nitrogen aluminum fiber.Then in step S500, nitrogen will be contained
The parent glass of change aluminum fiber coring 2 hours at a temperature of 720 DEG C, then crystallization is nitrogenized for 3 hours at a temperature of 880 DEG C
Aluminum fiber Phlogopite Based Glass-Ceramics composite.
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 Phlogopite Based Glass-Ceramics composite diphase material, it is characterised in that comprise the steps of:
Step 1, by K2CO3Powder, MgO powder, SiO2Powder, Al2O3Powder and flux B2O3, Nucleating Agent is mixed into uniformly
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 Phlogopite Based Glass-Ceramics 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 Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, its feature exists
In the Nucleating Agent is Cr2O3And TiO2。
4. the preparation method of aluminium nitride fibres Phlogopite Based Glass-Ceramics composite diphase material according to claim 3, its feature exists
In the weight portion of each component is respectively in the step 1:The K of 4-9 weight portions2CO3, 15-22 weight portions MgO, 44-60 weight
The SiO of part2, 10-17 weight portions Al2O3, 3-8 weight portions B2O3, 1-3 weight portions Cr2O3With the TiO of 1-3 weight portions2With
And the aluminium nitride fibres of 10-20 weight portions.
5. the preparation method of aluminium nitride fibres Phlogopite Based Glass-Ceramics 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 1380-1420 DEG C.
6. the preparation method of aluminium nitride fibres Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, its feature exists
In the melting heat time in the step 2 is 2-4 hours.
7. the preparation method of aluminium nitride fibres Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, its feature exists
In the coring in the step 6 is carried out at a temperature of 550-730 DEG C.
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:K2CO3、MgO、SiO2、Al2O3、B2O3、Cr2O3、TiO2And aluminium nitride fibres.
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH069224A (en) * | 1992-03-06 | 1994-01-18 | Carl Zeiss:Fa | Method for refining molten oxide |
CN101648775A (en) * | 2008-10-17 | 2010-02-17 | 韦鸿雁 | High-quality and high-efficiency composite production technology of glass basis fiber composite |
-
2017
- 2017-02-27 CN CN201710107898.6A patent/CN106892569A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH069224A (en) * | 1992-03-06 | 1994-01-18 | Carl Zeiss:Fa | Method for refining molten oxide |
CN101648775A (en) * | 2008-10-17 | 2010-02-17 | 韦鸿雁 | High-quality and high-efficiency composite production technology of glass basis fiber composite |
Non-Patent Citations (1)
Title |
---|
林广新等: ""碳纤维增强可切削金云母微晶玻璃复合材料的制备及其特性"", 《材料科学进展》 * |
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