CN106673450A - Silicon carbide fiber toughened phlogopite glass-ceramic multi-phase material and preparation method thereof - Google Patents
Silicon carbide fiber toughened phlogopite glass-ceramic multi-phase material and preparation method thereof Download PDFInfo
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- CN106673450A CN106673450A CN201611191040.4A CN201611191040A CN106673450A CN 106673450 A CN106673450 A CN 106673450A CN 201611191040 A CN201611191040 A CN 201611191040A CN 106673450 A CN106673450 A CN 106673450A
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- Prior art keywords
- silicon carbide
- powder
- carbide fibre
- phlogopite
- preparation
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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
- 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
- C03C10/0009—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 silica as main constituent
-
- 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
- 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
Abstract
The invention discloses a preparation method of a silicon carbide fiber toughened phlogopite glass-ceramic multi-phase material. The preparation method comprises the following steps: mixing K2CO3 powder, MgO powder, SiO2 powder, Al2O3 powder, a fluxing agent and a nucleating agent in proportion to form a uniform mixture; melting and heating the mixture; spraying silicon carbide fibers into a melting tank through nitrogen gas at the final period of a melting process, and sufficiently mixing to form a uniform melted mixture; pouring the melted mixture into a pre-heated mold; annealing the melted mixture poured into the mold; and nucleating basic glass which is obtained by annealing and contains the silicon carbide fibers, and crystallizing to obtain the silicon carbide fiber toughened phlogopite glass-ceramic multi-phase material. The invention further provides the multi-phase material prepared by the method, and the multi-phase material comprises K2CO3, MgO, SiO2, Al2O3, B2O3, Cr2O3, TiO2 and the silicon carbide fibers.
Description
Technical field
The present invention relates to glass ceramic composite field, more particularly to a kind of silicon carbide fibre toughness reinforcing phlogopite crystallite glass
Glass composite diphase 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 limit
Its range of application.Silicon carbide fibre strength and toughness is high, heat conductivity is high, thermal coefficient of expansion and microcrystal glass material are close, resistance to
Mill performance is good, and it is widely used in various ceramic matrixs as toughened fiber.If Phlogopite Based Glass-Ceramics and carborundum are fine
Dimension is combined, then silicon carbide fibre greatly improves can the toughness of Phlogopite Based Glass-Ceramics.There is scholar by adopting sintering process
Carbon fiber is combined with machinable Phlogopite Based Glass-Ceramics, carbon fiber-Phlogopite Based Glass-Ceramics composite diphase material is prepared for,
Achieve preferable toughening effect.But sintering process has many deficiencies, the devitrified glass volume for being primarily present sintering process preparation is close
Degree is relatively low, and the porosity is higher, the problems such as glass-ceramic matrix is combined poor with fiber.
Devitrified glass is typically prepared using sintering process or fusion method, the Phlogopite Based Glass-Ceramics that wherein prepared by fusion method
Bulk density is of a relatively high, and the porosity is relatively low, but to silicon carbide fibre is combined with devitrified glass using fusion method, then
First have to solve the problems, such as that silicon carbide fibre is easily oxidized at high temperature;Its secondary solution silicon carbide fibre uniformly divides in the melt
The problem of cloth.
There is no in current prior art silicon carbide fibre is combined with Phlogopite Based Glass-Ceramics using fusion method
Carry out the preparation of silicon carbide fibre toughness reinforcing 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 through substantial amounts of creative work
Silicon carbide fibre is sprayed into bath and is sufficiently stirred for that preferable silicon carbide fibre 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 silicon carbide fibre from aoxidizing at high temperature, and add fast thawing
The floating of growing up of micro-bubble is discharged in pond.Inventor also has found the thermal coefficient of expansion and substrate glass base due to silicon carbide fibre
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 silicon carbide fibre toughness reinforcing Phlogopite Based Glass-Ceramics as described below and answer
Phase material and preparation method thereof.
A kind of preparation method of silicon carbide fibre toughness reinforcing Phlogopite Based Glass-Ceramics composite diphase material, comprises the steps of:
Step 1, by K2CO3Powder, MgO powder, SiO2Powder, Al2O3Powder and flux, Nucleating Agent are mixed into uniformly
Mixture;
Step 2, mixture melting is heated;
Step 3, silicon carbide fibre in the latter stage of melting process sprayed in fusion pool and be sufficiently stirred for as equal by nitrogen
Even molten mixture;
Step 4, molten mixture is poured in the mould through preheating;
Step 5, by the molten mixture being poured in mould annealing;
Step 6, the parent glass coring containing silicon carbide fibre that annealing is obtained and crystallization.
Further, the weight portion of each component is respectively in step 1:The K of 4-9 weight portions2CO3, 10-22 weight portions
The SiO of MgO, 44-60 weight portion2, 10-17 weight portions Al2O3, the B of 3-8 weight portions2O3, be respectively 1-3 weight portions Cr2O3
And TiO2And the silicon carbide fibre of 10-20 weight portions.
Further, silicon carbide fibre is powder.
Further, the particle diameter of aforementioned each component powder is below 200 mesh.
Further, flux is B2O3。
Further, Nucleating Agent is Cr2O3And TiO2。
Further, the melting heating in step 2 is carried out at a temperature of 1420-1580 DEG C.
Further, the melting heat time heating time in step 2 is 2-4 hours.
Further, the preheating of mould is carried out at a temperature of 430-630 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 hour at a temperature of 730-930 DEG C.
By said method, the efficient system of silicon carbide fibre toughness reinforcing Phlogopite Based Glass-Ceramics composite diphase material is have effectively achieved
It is standby.
Present invention also offers a kind of silicon carbide fibre toughness reinforcing Phlogopite Based Glass-Ceramics complex phase prepared by said method
Material, it includes following components:K2CO3、MgO、SiO2、Al2O3、B2O3、Cr2O3、TiO2And silicon carbide fibre.
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 it is obvious and easy to understand, wherein:
Fig. 1 shows silicon carbide fibre toughness reinforcing Phlogopite Based Glass-Ceramics composite diphase material system according to an embodiment of the invention
The schematic flow sheet of Preparation Method.
Specific embodiment
It should be appreciated that embodiments of the invention shown in the exemplary embodiment are merely illustrative.Although at this
Only minority embodiment has 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 the present invention's
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, the MgO powder of 16 weight portions, 47 weight portions
SiO2The Al of powder, 11 weight portions2O3The flux B of powder and 4 weight portions2O3Powder, the Nucleating Agent for being respectively 2 weight portions
Cr2O3Powder and TiO2Powder is mixed into homogeneous mixture.Subsequently in step s 200, said mixture is melted at 1550 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 institute
Show, by the powder silicon carbide fibre of 13 weight portions is by nitrogen stream penetrating bath and is sufficiently stirred for, make carborundum
Fiber is uniformly distributed so as to obtain the molten mixture containing equally distributed silicon carbide fibre in the mixture of melting.As walked
Shown in rapid S400, the molten mixture that step S300 is obtained is poured into a mould among 590 DEG C of moulds being fully warmed-up of Jing, and
Anneal 3 hours at a temperature of 590 DEG C, obtained the parent glass of silicon carbide-containing fiber.Subsequently in step S500, carbon will be contained
The parent glass of SiClx fiber coring 2 hours at a temperature of 640 DEG C, then crystallization is carbonized for 4 hours at a temperature of 870 DEG C
Silica fibre toughness reinforcing Phlogopite Based Glass-Ceramics composite.
Embodiment two
With reference to Fig. 1, in the step s 100, by the K of 6 weight portions2CO3Powder, the MgO powder of 16 weight portions, 45 weight portions
SiO2The Al of powder, 10 weight portions2O3The flux B of powder and 5 weight portions2O3Powder, the Nucleating Agent for being respectively 2 weight portions
Cr2O3Powder and TiO2Powder is mixed into homogeneous mixture.Subsequently in step s 200, said mixture is melted at 1480 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 institute
Show, by the powder silicon carbide fibre of 11 weight portions is by nitrogen stream penetrating bath and is sufficiently stirred for, make carborundum
Fiber is uniformly distributed so as to obtain the molten mixture containing equally distributed silicon carbide fibre in the mixture of melting.As walked
Shown in rapid S400, the molten mixture that step S300 is obtained is poured into a mould among 580 DEG C of moulds being fully warmed-up of Jing, and
Anneal 3 hours at a temperature of 580 DEG C, obtained the parent glass of silicon carbide-containing fiber.Subsequently in step S500, carbon will be contained
The parent glass of SiClx fiber coring 2 hours at a temperature of 630 DEG C, then crystallization is carbonized for 4 hours at a temperature of 850 DEG C
Silica fibre toughness reinforcing Phlogopite Based Glass-Ceramics composite.
Embodiment three
With reference to Fig. 1, in the step s 100, by the K of 4 weight portions2CO3Powder, the MgO powder of 10 weight portions, 44 weight portions
SiO2The Al of powder, 17 weight portions2O3The flux B of powder and 3 weight portions2O3Powder, the Nucleating Agent for being respectively 1 weight portion
Cr2O3Powder and TiO2Powder is mixed into homogeneous mixture.Subsequently in step s 200, said mixture is melted at 1480 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 institute
Show, by the powder silicon carbide fibre of 19 weight portions is by nitrogen stream penetrating bath and is sufficiently stirred for, make carborundum
Fiber is uniformly distributed so as to obtain the molten mixture containing equally distributed silicon carbide fibre in the mixture of melting.As walked
Shown in rapid S400, the molten mixture that step S300 is obtained is poured into a mould among 450 DEG C of moulds being fully warmed-up of Jing, and
Anneal 4 hours at a temperature of 450 DEG C, obtained the parent glass of silicon carbide-containing fiber.Subsequently in step S500, carbon will be contained
The parent glass of SiClx fiber coring 3 hours at a temperature of 550 DEG C, then crystallization is carbonized for 2 hours at a temperature of 910 DEG C
Silica fibre toughness reinforcing Phlogopite Based Glass-Ceramics composite.
Example IV
With reference to Fig. 1, in the step s 100, by the K of 9 weight portions2CO3Powder, the MgO powder of 10 weight portions, 44 weight portions
SiO2The Al of powder, 12 weight portions2O3The flux B of powder and 8 weight portions2O3Powder, the Nucleating Agent for being respectively 3 weight portions
Cr2O3Powder and TiO2Powder is mixed into homogeneous mixture.Subsequently in step s 200, said mixture is melted at 1480 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 institute
Show, by the powder silicon carbide fibre of 10 weight portions is by nitrogen stream penetrating bath and is sufficiently stirred for, make carborundum
Fiber is uniformly distributed so as to obtain the molten mixture containing equally distributed silicon carbide fibre in the mixture of melting.As walked
Shown in rapid S400, the molten mixture that step S300 is obtained is poured into a mould among 610 DEG C of moulds being fully warmed-up of Jing, and
Anneal 2 hours at a temperature of 610 DEG C, obtained the parent glass of silicon carbide-containing fiber.Subsequently in step S500, carbon will be contained
The parent glass of SiClx fiber coring 2 hours at a temperature of 710 DEG C, then crystallization is carbonized for 4 hours at a temperature of 750 DEG C
Silica fibre toughness reinforcing Phlogopite Based Glass-Ceramics composite.
Embodiment five
With reference to Fig. 1, in the step s 100, by the K of 5 weight portions2CO3Powder, the MgO powder of 22 weight portions, 46 weight portions
SiO2The Al of powder, 10 weight portions2O3The flux B of powder and 4 weight portions2O3Powder, the Nucleating Agent for being respectively 1 weight portion
Cr2O3Powder and TiO2Powder is mixed into homogeneous mixture.Subsequently in step s 200, said mixture is melted at 1480 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 institute
Show, by the powder silicon carbide fibre of 10 weight portions is by nitrogen stream penetrating bath and is sufficiently stirred for, make carborundum
Fiber is uniformly distributed so as to obtain the molten mixture containing equally distributed silicon carbide fibre in the mixture of melting.As walked
Shown in rapid S400, the molten mixture that step S300 is obtained is poured into a mould among 610 DEG C of moulds being fully warmed-up of Jing, and
Anneal 2 hours at a temperature of 610 DEG C, obtained the parent glass of silicon carbide-containing fiber.Subsequently in step S500, carbon will be contained
The parent glass of SiClx fiber coring 2 hours at a temperature of 710 DEG C, then crystallization is carbonized for 4 hours at a temperature of 750 DEG C
Silica fibre toughness reinforcing Phlogopite Based Glass-Ceramics composite.
Embodiment six
With reference to Fig. 1, in the step s 100, by the K of 4 weight portions2CO3Powder, the MgO powder of 10 weight portions, 60 weight portions
SiO2The Al of powder, 10 weight portions2O3The flux B of powder and 3 weight portions2O3Powder, the Nucleating Agent for being respectively 1 weight portion
Cr2O3Powder and TiO2Powder is mixed into homogeneous mixture.Subsequently in step s 200, said mixture is melted at 1480 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 institute
Show, by the powder silicon carbide fibre of 10 weight portions is by nitrogen stream penetrating bath and is sufficiently stirred for, make carborundum
Fiber is uniformly distributed so as to obtain the molten mixture containing equally distributed silicon carbide fibre in the mixture of melting.As walked
Shown in rapid S400, the molten mixture that step S300 is obtained is poured into a mould among 610 DEG C of moulds being fully warmed-up of Jing, and
Anneal 2 hours at a temperature of 610 DEG C, obtained the parent glass of silicon carbide-containing fiber.Subsequently in step S500, carbon will be contained
The parent glass of SiClx fiber coring 2 hours at a temperature of 710 DEG C, then crystallization is carbonized for 4 hours at a temperature of 750 DEG C
Silica fibre toughness reinforcing Phlogopite Based Glass-Ceramics 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, all should be covered in the claims in the present invention
In the middle of protection domain.
Claims (10)
1. a kind of preparation method of silicon carbide fibre toughness reinforcing Phlogopite Based Glass-Ceramics composite diphase material, it is characterised in that comprising following
Step:
Step 1, by K2CO3Powder, MgO powder, SiO2Powder, Al2O3Powder and flux, Nucleating Agent are mixed into uniform mixing
Thing;
Step 2, mixture melting is heated;
Step 3, silicon carbide fibre in the latter stage of melting process sprayed in fusion pool and be sufficiently stirred for as uniform by nitrogen
Molten mixture;
Step 4, the molten mixture is poured in the mould through preheating;
Step 5, by the molten mixture being poured in mould annealing;
Step 6, the parent glass coring containing silicon carbide fibre that annealing is obtained and crystallization.
2. the preparation method of silicon carbide fibre toughness reinforcing Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, it is special
Levy and be, the weight portion of each component is respectively in the step 1:The K of 4-9 weight portions2CO3, 10-22 weight portions MgO, 44-60
The SiO of weight portion2, 10-17 weight portions Al2O3, the B of 3-8 weight portions2O3, be respectively 1-3 weight portions Cr2O3And TiO2And
The silicon carbide fibre of 10-20 weight portions.
3. the preparation method of silicon carbide fibre toughness reinforcing Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, it is special
Levy and be, the silicon carbide fibre is powder.
4. the preparation method of silicon carbide fibre toughness reinforcing Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, it is special
Levy and be, the flux is B2O3。
5. the preparation method of silicon carbide fibre toughness reinforcing Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, it is special
Levy and be, the Nucleating Agent is Cr2O3And TiO2。
6. the preparation method of silicon carbide fibre toughness reinforcing Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, it is special
Levy and be, the melting heating in the step 2 is carried out at a temperature of 1420-1580 DEG C.
7. the preparation method of silicon carbide fibre toughness reinforcing Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, it is special
Levy and be, the melting heat time heating time in the step 2 is 2-4 hours.
8. the preparation method of silicon carbide fibre toughness reinforcing Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, it is special
Levy and be, the preheating of mould in the step 4 is carried out at a temperature of 430-630 DEG C.
9. the preparation method of silicon carbide fibre toughness reinforcing Phlogopite Based Glass-Ceramics composite diphase material according to claim 1, it is special
Levy and be, annealing time is 2-4 hours in the step 5.
10. a kind of composite diphase material that prepared by preparation method by 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 silicon carbide fibre.
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CN114890675A (en) * | 2022-06-10 | 2022-08-12 | 杨晓战 | High-crystallization microcrystalline glass, preparation method thereof and processable ceramic product |
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